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WO2018120511A1 - Film à points quantiques et procédé de fabrication associé - Google Patents

Film à points quantiques et procédé de fabrication associé Download PDF

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Publication number
WO2018120511A1
WO2018120511A1 PCT/CN2017/080607 CN2017080607W WO2018120511A1 WO 2018120511 A1 WO2018120511 A1 WO 2018120511A1 CN 2017080607 W CN2017080607 W CN 2017080607W WO 2018120511 A1 WO2018120511 A1 WO 2018120511A1
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quantum dot
quantum
precursor
radial direction
structural unit
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Chinese (zh)
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刘政
杨一行
曹蔚然
钱磊
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TCL Corp
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TCL Corp
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00—Organic light-emitting devices
    • H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
    • H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers
    • H10K50/115—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers comprising active inorganic nanostructures, e.g. luminescent quantum dots
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00—Organic light-emitting devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K2102/00—Constructional details relating to the organic devices covered by this subclass
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10—Deposition of organic active material
    • H10K71/16—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering
    • H10K71/164—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering using vacuum deposition

Definitions

  • the invention relates to the technical field of quantum dots, in particular to a quantum dot film and a preparation method thereof.
  • Quantum dots are special materials that are limited to the order of nanometers in three dimensions. This remarkable quantum confinement effect makes quantum dots have many unique nano properties: the emission wavelength is continuously adjustable, and the emission wavelength is narrow. Wide absorption spectrum, high luminous intensity, long fluorescence lifetime and good biocompatibility. These characteristics make quantum dots have broad application prospects in the fields of flat panel display, solid state lighting, photovoltaic solar energy, and biomarkers. Especially in flat panel display applications, Quantum dot light-emitting diodes (QLEDs) based on quantum dot materials have been displaying image quality, device performance, and performance by virtue of the characteristics and optimization of quantum dot nanomaterials. Manufacturing costs and other aspects have shown great potential.
  • QLEDs Quantum dot light-emitting diodes
  • quantum dots have been researched and developed as a classic nanomaterial for more than 30 years, the research time of using the excellent luminescent properties of quantum dots and applying them as luminescent materials in QLED devices and corresponding display technologies is still short; Therefore, the development and research of most of the current QLED devices are based on the existing quantum dot materials of classical structural systems, and the corresponding quantum dot materials are screened. And the standard of optimization is basically based on the luminescent properties of the quantum dots themselves, such as the luminescence peak width of quantum dots, the solution quantum yield, and the like. The above quantum dots are directly applied to the QLED device structure to obtain corresponding device performance results.
  • QLED devices and corresponding display technologies are a complex optoelectronic device system, and there are many factors that affect the performance of the device.
  • the quantum dot material that is the core luminescent layer material
  • the quantum dot performance metrics that need to be weighed are much more complicated.
  • quantum dots exist in the form of solid-state films of quantum dot luminescent layers in QLED devices. Therefore, the luminescent properties of quantum dot materials originally obtained in solution may show significant differences after forming solid films: for example In the solid film, the luminescence peak wavelength will have different degrees of red shift (moving to long wavelength), the luminescence peak width will become larger, and the quantum yield will be reduced to different extents, that is, the quantum luminescent material has excellent luminescence in solution. Performance is not fully inherited into the quantum dot solid state film of QLED devices. Therefore, in designing and optimizing the structure and synthetic formulation of quantum dot materials, it is necessary to simultaneously consider the optimization of the luminescent properties of the quantum dot material itself and the luminescence inheritance of the quantum dot material in the state of the solid film.
  • the luminescence of quantum dot materials in QLED devices is achieved by electro-excitation, that is, energization of holes and electrons from the anode and cathode of the QLED device, respectively, and the transport of holes and electrons through the corresponding functional layers in the QLED device.
  • electro-excitation that is, energization of holes and electrons from the anode and cathode of the QLED device, respectively, and the transport of holes and electrons through the corresponding functional layers in the QLED device.
  • photons are emitted by means of radiation transitions to achieve luminescence. It can be seen from the above process that the luminescent properties of the quantum dots themselves, such as luminescence efficiency, only affect the efficiency of the radiation transition in the above process, and the overall luminescence efficiency of the QLED device is also affected by the charge of holes and electrons in the quantum dot material in the above process.
  • quantum dot materials Injection and transport efficiency, relative charge balance of holes and electrons in quantum dot materials, recombination of holes and electrons in quantum dot materials, and the like. Therefore, in designing and optimizing the structure of quantum dot materials, especially the fine core-shell nanostructures of quantum dots, it is also necessary to consider the electrical properties of quantum dots after forming solid films: for example, charge injection and conduction properties of quantum dots, fineness of quantum dots. Energy band structure, exciton lifetime of quantum dots, etc.
  • the solution method is prepared by, for example, inkjet printing. Therefore, the material design and development of the quantum dots need to consider the processing properties of the quantum dot solution, such as the dispersible solubility of the quantum dot solution or the printing ink, the colloidal stability, the print film forming property, and the like. . At the same time, the development of quantum dot materials is also coordinated with the other functional layer materials of QLED devices and the overall fabrication process and requirements of the devices.
  • the traditional quantum dot structure design which only considers the improvement of the quantum dot self-luminescence performance, can not meet the comprehensive requirements of QLED devices and corresponding display technologies for the optical properties, electrical properties and processing properties of quantum dot materials.
  • the fine core-shell structure, composition, energy level, etc. of the quantum dot luminescent material need to be tailored to the requirements of the QLED device and the corresponding display technology.
  • a semiconductor shell layer containing another semiconductor material can be grown on the outer surface of the original quantum dot to form a core-shell structure of the quantum dot, which can significantly improve the luminescent properties of the quantum dot and increase the quantum. Point stability.
  • the quantum dot materials that can be applied to the development of high-performance QLED devices are mainly quantum dots with a core-shell structure, the core and shell components are respectively fixed and the core shell has a clear boundary, such as a quantum dot with a CdSe/ZnS core-shell structure (J .Phys. Chem., 1996, 100(2), 468–471), Quantum Dots with CdSe/CdS Core-Shell Structure (J. Am. Chem. Soc.
  • Quantum dots with CdS/ZnS core-shell structure Quantum dots with CdS/ZnS core-shell structure, quantum dots with CdS/CdSe/CdS core+multilayer shell structure (Patent US 7,919,012B2), quantum dots with CdSe/CdS/ZnS core+multilayer shell structure (J. Phys. Chem. B, 2004, 108 (49), 18826 - 18831) and the like.
  • the composition of the core and the shell is generally fixed and different, and is generally a binary compound system composed of a cation and an anion.
  • the boundary between the core and the shell is clear, that is, the core and the shell can be distinguished.
  • the development of such core-shell quantum dots has improved the original Luminescence quantum efficiency, monodispersity, and quantum dot stability of single-component quantum dots.
  • quantum dots of the core-shell structure described above partially improve the performance of the quantum dots, the luminescent properties of the quantum dots themselves need to be improved, both in terms of design ideas and optimization schemes, and the luminescence properties have yet to be improved. Consider the special requirements of semiconductor devices for other aspects of quantum dot materials.
  • the liquid crystal display has been developed quite mature as a current mainstream display.
  • a white light emitting diode LED
  • a backlight of the liquid crystal is realized by a reasonable combination of the light guide plate and the optical film.
  • white LEDs used in the backlight module: one is to emit yellow light through the blue light emitted by the LED itself, and the two colors are mixed to form white light; the other is that the LED unit is mixed by the three primary color LED light sources to form white light;
  • the third type is LED blue light. By exciting two red and green quantum dot phosphors, the three colors of light mix to form white light.
  • the third method is one of the more researched methods that can improve the color gamut of displays from 70% NTSC to 100% NTSC.
  • Quantum dots are nano-sized particles with unique optical and electrical properties and are currently in the midst of a wide range of research applications, including illumination, display, solar energy conversion, and molecular and cellular imaging.
  • quantum dots have been used in the field of display devices, which can greatly improve the display effect, improve the color vividness, color gamut and color rendering index, and increase the color gamut of the display from 70% NTSC to 110% NTSC.
  • the red and green quantum dots can be placed in three positions: first on the LED chip; second on the edge of the light guide; and third in the backlight module. The first position quantum dots are used in a small amount, but the LED chips have a high temperature and the quantum dots have a short lifetime.
  • the third type generally disperses the quantum dots on the diaphragm, which is farthest from the LED and has a low temperature, but the quantum dots are used in a large amount and at a high cost.
  • the second type of quantum dot is used between the first type and the second type, and it is generally suitable to use a large-sized display.
  • the third research is to spread the quantum dots on the diaphragm.
  • the main consideration is the small-size LCD screen with high added value. Since the quantum yield of quantum dots is constant, how to increase the light conversion rate is the key to reducing the cost.
  • the object of the present invention is to provide a quantum dot film and a preparation method thereof, which aim to solve the problem that the optical conversion rate of the existing quantum dots is still low after being dispersed into the film.
  • Quantum dot 0.01-40.0%; the quantum dot includes at least one quantum dot structural unit sequentially arranged in a radial direction, the quantum dot structural unit being a graded alloy composition structure in which a change in energy level width in a radial direction Or a uniform composition of uniform energy levels in the radial direction;
  • the quantum dot film wherein the quantum dot structural unit is a graded alloy composition structure in which the width of the outer level is wider in the radial direction, and the energy of the quantum dot structural unit adjacent in the radial direction The level is continuous.
  • the quantum dot film wherein the quantum dot comprises at least three quantum dot structural units arranged in a radial direction, wherein the quantum at the center and the surface of the at least three quantum dot structural units
  • the point structure unit is a graded alloy composition structure in which the width of the outer level is wider in the radial direction, and the energy level of the quantum dot structure unit of the graded alloy composition adjacent in the radial direction is continuous;
  • a quantum dot structural unit between the central and surface quantum dot structural units is a homogeneous composition structure.
  • the quantum dot film wherein the quantum dots comprise two types of quantum dot structural units, wherein one type of quantum dot structural unit is a graded alloy composition having a wider outer layer width in a radial direction
  • Another type of quantum dot structural unit is a graded alloy composition structure in which the width of the outer level is narrower in the radial direction, and the two types of quantum dot structural units are alternately arranged in the radial direction and in the radial direction.
  • the energy levels of the quantum dot structural units adjacent in the direction are continuous.
  • the quantum dot film wherein the quantum dot structural unit is a graded alloy composition structure in which the width of the outer level is wider in the radial direction, and the energy levels of adjacent quantum dot structural units are discontinuous. .
  • the quantum dot structural unit is a graded alloy composition structure in which the width of the outer level is narrower in the radial direction, and the energy levels of adjacent quantum dot structural units are discontinuous. .
  • the quantum dot film wherein the quantum dot comprises two quantum dot structural units, wherein one quantum dot structural unit is a graded alloy composition structure in which a width of the outer energy level is wider in the radial direction, and the other
  • the quantum dot structural unit is a homogeneous component structure, and the interior of the quantum dot includes one or more quantum dot structural units of a graded alloy composition structure, and quantum dots of a graded alloy composition structure adjacent in a radial direction
  • the energy levels of the structural units are continuous; the exterior of the quantum dots includes one or more quantum dot structural units of a uniform composition structure.
  • the quantum dot film wherein the quantum dot comprises two quantum dot structural units, wherein one quantum dot structural unit has a uniform composition structure, and the other quantum dot structural unit has an outer energy level in a radial direction. a wider width of the graded alloy composition structure, the interior of the quantum dot comprising one or more quantum dot structural units of a uniform composition structure, the outer portion of the quantum dot comprising one or more graded alloy composition structures.
  • the quantum dot structural unit, and the energy level of the quantum dot structural unit of the graded alloy composition structure adjacent in the radial direction is continuous.
  • the quantum dot film wherein the quantum dot structural unit is a graded alloy component structure or a uniform alloy component structure comprising a group II and group VI element.
  • each of the quantum dot structural units comprises 2-20 layers of a single atomic layer, or each of the quantum dot structural units comprises a 1-10 layer of a unit cell layer.
  • the quantum dot film wherein the quantum dots have an emission peak wavelength ranging from 400 nm to 700 nm.
  • the half peak width of the luminescence peak of the quantum dot is from 12 nm to 80 nm.
  • the quantum dot film wherein the medium comprises at least one polymer material.
  • the quantum dot film wherein the medium comprises at least one polymeric prepolymer material.
  • the quantum dot film wherein the medium comprises at least one oligomer material.
  • the quantum dot film wherein the medium comprises at least one small molecule material.
  • the quantum dot film wherein the medium comprises at least one inorganic material.
  • the quantum dot film wherein the medium comprises at least one host dielectric material.
  • the quantum dot film wherein the host dielectric material comprises at least one organic material.
  • the quantum dot film wherein the host dielectric material comprises at least one inorganic material.
  • the quantum dot film wherein the medium comprises at least one non-polar liquid.
  • the quantum dot film wherein the medium comprises at least one polar liquid.
  • a method for preparing a quantum dot film according to any one of the preceding claims comprising the steps of: first dispersing a quantum dot in a medium according to the above formula, and then stirring for 20 to 40 minutes to obtain a quantum dot film; wherein the quantum dot And including at least one quantum dot structural unit sequentially arranged in a radial direction, wherein the quantum dot structural unit is a gradual alloy composition structure in which a change in energy level width in a radial direction or a uniform energy level width in a radial direction Substructure.
  • the method for preparing a quantum dot film comprises the steps of:
  • a cation exchange reaction occurs between the first compound and the second compound to form quantum dots, and the luminescence peak wavelength of the quantum dots exhibits one or more of blue shift, red shift, and constant.
  • the quantum dot film After the above quantum dots are formed into a film, the quantum dot film has high light conversion rate; the semiconductor device made of the above quantum dot film has excellent optical and electrical device properties.
  • 1 is a graph showing the energy level structure of a quantum dot specific structure 1 of the present invention.
  • FIG. 2 is a graph showing the energy level structure of a quantum dot specific structure 2 of the present invention.
  • 3 is a graph showing the energy level structure of a quantum dot specific structure 3 of the present invention.
  • FIG. 4 is a graph showing the energy level structure of a quantum dot specific structure 4 of the present invention.
  • FIG. 5 is a graph showing the energy level structure of a quantum dot specific structure 5 of the present invention.
  • FIG. 6 is a graph showing the energy level structure of a quantum dot specific structure 6 of the present invention.
  • FIG. 7 is a graph showing the energy level structure of a quantum dot specific structure 7 of the present invention.
  • FIG. 8 is a schematic structural view of a quantum dot light emitting diode according to Embodiment 37 of the present invention.
  • FIG. 9 is a schematic structural view of a quantum dot light emitting diode according to Embodiment 38 of the present invention.
  • FIG. 10 is a schematic structural view of a quantum dot light emitting diode according to Embodiment 39 of the present invention.
  • FIG. 11 is a schematic structural view of a quantum dot light emitting diode according to Embodiment 40 of the present invention.
  • FIG. 12 is a schematic structural view of a quantum dot light emitting diode according to Embodiment 41 of the present invention.
  • FIG. 13 is a schematic structural view of a quantum dot light emitting diode according to Embodiment 42 of the present invention.
  • the present invention provides a quantum dot film and a preparation method thereof.
  • the present invention will be further described in detail below. It is understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
  • Quantum dot 0.01-40.0%; the quantum dot includes at least one quantum dot structural unit sequentially arranged in a radial direction, the quantum dot structural unit being a graded alloy composition structure in which a change in energy level width in a radial direction Or a uniform composition of uniform energy levels in the radial direction;
  • the semiconductor device made of the above quantum dot film of the present invention has excellent optical and electrical device properties.
  • the medium comprises at least one polymeric material.
  • the quantum dot film of the present invention comprises quantum dots and one or more polymer materials.
  • the polymer material may be, but not limited to, one of a phenol resin, polyethylene, polydimethylsiloxane (PDMS), polystyrene, polymethacrylate, polyacrylate, polycarbonate, and the like.
  • the medium comprises at least one polymeric prepolymer material.
  • the quantum dot film of the present invention comprises quantum dots and one or more polymeric prepolymer materials.
  • the polymeric prepolymer material may be, but not limited to, a methyl methacrylate prepolymer, a polyester prepolymer formed from phthalic acid and glycerin, an epoxy resin prepolymer, pyromellitic dianhydride, and One of an aromatic diamine prepolymer, a phenolic resin prepolymer, and the like.
  • the medium comprises at least one oligomeric material.
  • the quantum dot film of the present invention comprises quantum dots and one or more oligomer materials.
  • the oligomeric material may be, but not limited to, including dimers, trimers, tetramers, etc., such as unsaturated polyesters, low molecular weight polyethers, acrylate oligomers, carbonate oligomers, low molecular weight One of polyamide, low molecular weight polyurea, and the like.
  • the medium comprises at least one small molecule material.
  • the quantum dot film of the present invention includes quantum dots and one or more small molecule materials.
  • the small molecule material may be, but not limited to, an organic small molecule material such as tris(8-hydroxyquinoline)aluminum, alpha-NPD (bis[N-(1-naphthyl)-N-phenyl-amino]biphenyl), oil An acid, a 1-octaene or the like, and one of inorganic small molecular materials such as metal aluminum, metallic silver, zinc oxide, molybdenum oxide, cerium chloride, lithium carbonate or the like.
  • the medium comprises at least one inorganic material.
  • the quantum dot film of the present invention comprises quantum dots and one or more inorganic materials.
  • the inorganic material may be, but not limited to, one of metal aluminum, metallic silver, indium tin oxide, zinc oxide, molybdenum oxide, cerium chloride, lithium carbonate, quantum dots, nanorods, nanowires, nanosheets, glass, and the like. .
  • the medium comprises at least one body dielectric material. That is, the quantum dot film of the present invention comprises quantum dots and one or more host dielectric materials. More preferably, the body medium The material comprises at least one organic material, which may be, but not limited to, tris(8-hydroxyquinoline)aluminum, polymethyl methacrylate, polydimethylsiloxane, TFB (Poly[(9,9) -dioctylfluorenyl ⁇ 2,7 ⁇ diyl) ⁇ co ⁇ (4,4′ ⁇ (N ⁇ (4 ⁇ sec-butylphenyl)diphenylamine)]), ⁇ NPD(bis[N ⁇ (1 ⁇ naphthyl) ⁇ N ⁇ phenyl One of -amino]biphenyl), oleic acid, 1-octadecene, trioctylphosphine, etc.
  • organic material which may be, but not limited to, tris(8-hydroxyquinoline)aluminum, polymethyl meth
  • the host dielectric material comprises at least one inorganic material, which may be but not It is limited to one of metal aluminum, metallic silver, indium tin oxide, zinc oxide, molybdenum oxide, barium chloride, lithium carbonate, quantum dots, nanorods, nanowires, nanosheets, glass, and the like.
  • the medium comprises at least one non-polar liquid.
  • the quantum dot film of the present invention comprises quantum dots and one or more non-polar liquids, which may be, but not limited to, toluene, chloroform, n-hexane, n-octane, tridecane, oleic acid. One of 1-tenhene and the like.
  • the medium comprises at least one polar liquid.
  • the quantum dot film of the present invention comprises quantum dots and one or more polar liquids, which may be, but not limited to, water, methanol, ethanol, butanol, octanol, dimethylformamide, One of methyl sulfoxide and the like.
  • the quantum dot provided by the present invention comprises at least one quantum dot structural unit sequentially arranged in a radial direction, wherein the quantum dot structural unit is a graded alloy composition structure or a radial direction in which a width of the energy level changes in a radial direction.
  • each quantum dot structural unit has an alloy within a single atomic layer or more than one layer of a single atomic layer at any position in the radial direction from the inside to the outside.
  • the structure of the components is to say, in the quantum dots provided by the present invention.
  • the quantum dot structural unit contains Group II and Group VI elements.
  • the Group II elements include, but are not limited to, Zn, Cd, Hg, Cn, etc.; the Group VI elements include, but are not limited to, O, S, Se, Te, Po, Lv, and the like.
  • the alloy composition of each quantum dot structural unit is Cd x Zn 1 ⁇ x Se y S 1 ⁇ y , where 0 ⁇ x ⁇ 1, 0 ⁇ y ⁇ 1, and x and y are not 0 at the same time and At the same time it is 1. It should be noted that the above situation is preferred.
  • the components thereof are all alloy components; and for a quantum component structural unit of a uniform composition structure, the components thereof It may be an alloy component or a non-alloy component, but the present invention is preferably an alloy component, that is, the uniform component structure is a uniform alloy component structure, and more preferably, it comprises a Group II and VI group element,
  • the subsequent embodiments of the present invention are all described by taking the structure of the uniform alloy composition as an example, but it is obvious that the uniform composition of the non-alloy can also be carried out.
  • the radial direction here refers to the direction from the center of the quantum dot, for example, assuming that the quantum dot of the present invention is a spherical or spherical-like structure, then the radial direction refers to the center of the quantum dot in the direction of the radius (or Internal) refers to the center of its physical structure, and the surface (or exterior) of a quantum dot refers to the surface of its physical structure.
  • the present invention provides a quantum dot having a funnel-type energy level structure, and a quantum dot structure unit alloy component located inside the quantum dot has a corresponding energy level width smaller than a quantum dot structure located outside.
  • the unit alloy composition component corresponds to the energy level width; specifically, the quantum dot provided by the present invention includes at least one quantum dot structure unit sequentially arranged in the radial direction, and the quantum dot structural unit is radially outward in the radial direction.
  • the graded alloy composition structure has a wider width, and the energy level of the quantum dot structural unit of the graded alloy composition structure adjacent in the radial direction is continuous; the structure of the quantum dot shown in FIG. 1 in the subsequent embodiment Called the specific structure 1.
  • the energy level width of each adjacent quantum dot structural unit has a continuous structure, that is, the energy level width of each adjacent quantum dot structural unit has a continuous change characteristic, that is, a mutant structure, that is,
  • the alloy composition of the quantum dots is also continuous, and the subsequent continuous structure is the same.
  • the energy level width of the quantum dot structural unit near the center is smaller than the energy level width of the quantum dot structural unit away from the center; that is, in the quantum dot
  • the width of the energy level from the center to the surface is gradually widened, thereby forming a funnel-shaped structure in which the opening gradually becomes larger, wherein the opening gradually becomes larger, which means that the energy level structure shown in FIG. 1 is from the center of the quantum dot to
  • the energy levels of the quantum dot surface are continuous.
  • the energy levels of the adjacent quantum dot structural units are continuous, that is, the synthesized components of the quantum dots also have a continuously changing characteristic, which is more advantageous for achieving high light emission. effectiveness.
  • the specific structure 1 of the quantum dot is a quantum dot structure having a continuous gradual alloy composition from the inside to the outside in the radial direction; the quantum dot structure has a composition from the inside to the outside.
  • the quantum dot of the invention not only facilitates more efficient luminous efficiency, but also satisfies the comprehensive performance requirements of the quantum device and the corresponding display technology for the quantum dot.
  • An ideal quantum dot luminescent material suitable for semiconductor devices and display technologies.
  • the alloy composition of the point A is Cd x0 A Zn 1 - x0 A Se y0 A S 1 - y0 A
  • the alloy composition of the point B is Cd x0 B Zn 1 - x0 B Se y0 B S 1 ⁇ y0 B
  • point A is closer to the center of the quantum dot than point B
  • the composition of point A and point B satisfies: x0 A > x0 B , y0 A > y0 B .
  • a gradation structure is formed in the radial direction, and the lower the Cd and Se contents are, the more outward (i.e., away from the center of the quantum dot) in the radial direction, the more the Zn and S contents are. High, then according to the characteristics of these elements, the width of the energy level will be wider.
  • the alloy composition is preferably Cd x0 Zn 1 ⁇ x0 Se y0 S 1 ⁇ y0 , wherein the alloy composition of point A is Cd x0 A Zn 1 ⁇ x0 A Se y0 A S 1 ⁇ y0 A , and the alloy composition of point B is Cd x0 B Zn 1 ⁇ x0 B Se y0 B S 1 ⁇ y0 B , where point A is closer to the center of the quantum dot relative to point B, and the composition of points A and B satisfies: x0 A > x0 B , y0 A > y0 B .
  • the alloy composition is preferably Cd x0 Zn 1 ⁇ x0 Se y0 S 1 ⁇ y0 , wherein point C
  • the alloy composition is Cd x0 C Zn 1 ⁇ x0 C Se y0 C S 1 ⁇ y0 C
  • the alloy composition at point D is Cd x0 D Zn 1 ⁇ x0 D Se y0 D S 1 ⁇ y0 D , where point C is relative to Point D is closer to the center of the quantum dot, and the composition of point C and point D satisfies: x0 C ⁇ x0 D , y0 C ⁇ y0 D .
  • the present invention further provides that the internal alloy composition has a corresponding energy level width not greater than a corresponding energy level width of the outer alloy composition component, and the quantum dot structure has at least one layer between the most central and outermost regions.
  • a quantum dot of a quantum dot structural unit of a homogeneous alloy composition structure that is, the quantum dot provided by the present invention includes at least three quantum dot structural units arranged in a radial direction, wherein the at least three quantum In the dot structure unit, the quantum dot structural unit located at the center and the surface is a graded alloy composition structure in which the width of the outer level is wider in the radial direction, and the quantum structure of the graded alloy component adjacent in the radial direction is quantum.
  • the energy level of the point structural unit is continuous, and a quantum dot structural unit between the central and surface quantum dot structural units is a uniform alloy composition structure.
  • the structure of the quantum dot shown in FIG. 2 is referred to as a specific structure 2 in the subsequent embodiments.
  • the alloy composition at any point is Cd x1 Zn 1 ⁇ x1 Se y1 S 1 ⁇ y1 , where 0 ⁇ x1 ⁇ 1, 0 ⁇ y1 ⁇ 1, and x1 and y1 are not 0 at the same time and 1 at the same time, and x1 and y1 are fixed values.
  • the alloy composition at a certain point is Cd 0.5 Zn 0.5 Se 0.5 S 0.5
  • the alloy composition at another point in the radial direction should also be Cd 0.5 Zn 0.5 Se 0.5 S 0.5
  • the structure of a homogeneous alloy composition A group of points in a quantum dot structure unit is divided into Cd 0.7 Zn 0.3 S
  • the alloy composition of another point in the quantum dot structure unit should also be Cd 0.7 Zn 0.3 S
  • a uniform alloy composition structure A group of points in a quantum dot structure unit is divided into CdSe
  • the alloy composition of another point in the unit of the quantum dot structure should also be CdSe.
  • the quantum dot structural units located at the center and the surface are both graded alloy composition structures having a wider outer-level width in the radial direction, and adjacent gradients in the radial direction.
  • the energy level of the quantum dot structural unit of the alloy component structure is continuous; that is, in the quantum dot structural unit having the structure of the graded alloy component, the energy level corresponding to the alloy composition at any point in the radial direction is An energy level width corresponding to an alloy composition that is adjacent to and closer to another point in the center of the quantum dot structure.
  • the composition of the alloy component in the quantum dot structural unit having the structure of the graded alloy component is Cd x2 Zn 1 -x2 Se y2 S 1 ⁇ y2 , where 0 ⁇ x2 ⁇ 1, 0 ⁇ y2 ⁇ 1, and x2 and y2 are not It is 0 at the same time and 1 at the same time.
  • the alloy composition at a certain point is Cd 0.5 Zn 0.5 Se 0.5 S 0.5
  • the alloy composition at another point is Cd 0.3 Zn 0.7 Se 0.4 S 0.6 .
  • the present invention also provides a quantum dot having a fully graded alloy composition of a quantum well structure; that is, the quantum dot provided by the present invention includes two types of quantum dot structural units (A1 type) And A2 type), wherein the quantum dot structure unit of the A1 type is a graded alloy composition structure in which the width of the outer level is wider in the radial direction, and the quantum dot structure unit of the A2 type has a larger outer diameter level in the radial direction.
  • a narrow graded alloy composition structure in which the two quantum dot structural units are alternately arranged in the radial direction, and the energy levels of the adjacent quantum dot structural units in the radial direction are continuous.
  • the quantum dot structure unit distribution of the quantum dots may be: A1, A2, A1, A2, A1, ..., or A2, A1, A2, A1, A2, ..., that is, the initial quantum dot structural unit. It can be of type A1 or type A2.
  • the width of the energy level is wider toward the outside.
  • the width of the energy level is narrower toward the outside, and the two energy levels are as if The form of the wavy line extends in the radial direction, and the structure of the quantum dot shown in FIG. 3 is referred to as a specific structure 3 in the subsequent embodiment.
  • the present invention also provides a quantum dot of an alloy composition of a quantum well structure having a sudden change in energy level.
  • the quantum dot structural unit has a width in the radial direction.
  • the quantum dot described in FIG. 4 is a square that is mutated by a plurality of quantum dot structural units.
  • the formulas are arranged in order, and the quantum dot structural units are all graded alloy composition structures in which the width of the outer level is wider in the radial direction.
  • the energy level width of the quantum dot structural unit near the center is smaller than the energy level width of the quantum dot structural unit away from the center. That is to say, in the quantum dots, the width of the energy level from the center to the surface is gradually widened, thereby forming a funnel-shaped structure in which the intermittent opening is gradually enlarged.
  • the quantum dots are not The method is limited to the above manner, that is, the energy level width of the quantum dot structural unit away from the center may also be smaller than the energy level width of the quantum dot structural unit near the center. In this structure, the energy level widths of adjacent quantum dot structural units are staggered. The place.
  • the present invention also provides another quantum dot of an alloy composition of a quantum well structure having a sudden change in energy level.
  • the quantum dot structural unit has an outer level in the radial direction.
  • the quantum dots described in FIG. 5 are sequentially arranged by a plurality of quantum dot structural units by abrupt changes, and the quantum dot structural units are all graded alloy groups in which the width of the outer energy level is narrower in the radial direction. Substructure. Further, in the quantum dots, the energy level width of the quantum dot structural unit near the center is larger than the energy level width of the quantum dot structural unit away from the center. That is to say, in the quantum dots, the energy level width from the center to the surface is gradually narrowed, thereby forming a funnel-shaped structure in which the intermittent opening gradually becomes smaller.
  • the quantum dots are not The method is limited to the above manner, that is, the energy level width of the quantum dot structural unit far from the center may also be larger than the energy level width of the quantum dot structural unit near the center. In this structure, the energy level widths of adjacent quantum dot structural units are staggered. The place.
  • the present invention further provides a quantum dot, wherein an energy level width of an alloy component located inside the quantum dot gradually increases from a center to an outer portion, and an outermost region of the quantum dot structure is a uniform alloy group.
  • the quantum dot includes two quantum dot structural units (A3) Type and A4 type), wherein the quantum dot structural unit of the A3 type is a graded alloy composition structure in which the width of the outer level is wider in the radial direction, and the quantum dot structural unit of the A4 type is a uniform alloy composition structure,
  • the interior of the quantum dot includes quantum dot structural units including one or more graded alloy composition structures, and the energy levels of the quantum dot structural units of the graded alloy composition structures adjacent in the radial direction are continuous;
  • the outer portion of the quantum dot includes one or more quantum dot structural units of a uniform alloy composition structure; in the subsequent embodiment, the structure of the quantum dot shown in FIG. 6 is referred to as a specific structure 6.
  • the distribution of the quantum dot structural units is A3...A3A4...A4, that is, the inside of the quantum dots is composed of A3 type quantum dot structural units, the quantum dots The outer portion is composed of A4 type quantum dot structural units, and the number of A3 type quantum dot structural units and the number of A4 type quantum dot structural units are both greater than or equal to one.
  • the present invention further provides another quantum dot, wherein the alloy composition inside the quantum dot has a uniform energy level width, and the energy level width of the alloy composition outside the quantum dot is uniform. From the center to the outside, it gradually becomes larger; specifically, the quantum dot includes two kinds of quantum dot structural units (A5 type and A6 type), wherein the A5 type quantum dot structural unit is a uniform alloy composition structure, and the A6 type
  • the quantum dot structural unit is a graded alloy composition structure in which the width of the outer level is wider in the radial direction, and the inside of the quantum dot includes one or more quantum dot structural units of a uniform alloy composition structure; the quantum dot
  • the outer portion includes one or more quantum dot structural units of a graded alloy composition structure, and the energy levels of the quantum dot structural units of the graded alloy composition structures adjacent in the radial direction are continuous; in subsequent embodiments
  • the structure of the quantum dots shown in Fig. 7 is referred to as a specific structure 7.
  • the distribution of the monoatomic layers is A5...A5A6...A6, that is, the inside of the quantum dots is composed of A5 type quantum dot structural units, and the outside of the quantum dots It is composed of A6 type quantum dot structural units, and the number of A5 type quantum dot structural units and the number of A6 type quantum dot structural units are both greater than or equal to 1.
  • the quantum dot structural unit provided by the present invention comprises a 2-20 layer monoatomic layer.
  • the quantum dot structural unit comprises 2-5 monoatomic layers, and the preferred number of layers can ensure that the quantum dots achieve good luminescence quantum yield and efficient charge injection efficiency.
  • the quantum dot light emitting unit comprises 1-10 layer cell layers, preferably 2-5 layer cell layers; the cell layer is the smallest structural unit, that is, the cell layer of each layer has an alloy composition of Fixed, that is, each cell layer has the same lattice parameter and element, and each quantum dot structural unit is a closed cell surface formed by connecting the cell layers, and the energy level width between adjacent cell layers has Continuous structure or mutant structure.
  • the present invention adopts the quantum dots of the above structure, and can realize the luminescence quantum yield ranging from 1% to 100%, and the preferred luminescence quantum yield ranges from 30% to 100%, and the quantum dot can be ensured within the preferred luminescence quantum yield range. Good applicability.
  • the quantum dot wherein the quantum dot has an emission peak wavelength ranging from 400 nm to 700 nm.
  • the quantum dots of the above structure can realize the luminescence peak wavelength range of 400 nm to 700 nm, and the preferred luminescence peak wavelength range is 430 nm to 660 nm, and the preferred quantum dot luminescence peak wavelength range can ensure quantum dots here.
  • a luminescence quantum yield of greater than 30% is achieved in the range.
  • the half peak width of the luminescence peak of the quantum dot is from 12 nm to 80 nm.
  • the quantum dots provided by the invention have the following beneficial effects: firstly, it helps to minimize the lattice tension between quantum dot crystals of different alloy compositions and alleviate lattice mismatch, thereby reducing the formation of interface defects, The luminous efficiency of quantum dots is improved. Secondly, the energy level structure formed by the quantum dots provided by the invention is more favorable for the effective binding of electron clouds in the quantum dots, greatly reducing the probability of diffusion of the surface of the electron cloud vector sub-points, thereby greatly suppressing the quantum dots without radiation. The Auger recombination loss of the transition reduces the quantum dot flicker and improves the luminous efficiency of the quantum dots.
  • the energy level structure formed by the quantum dots provided by the present invention is more advantageous for improving the injection efficiency and transmission efficiency of the quantum dot light-emitting layer charge in the semiconductor device; at the same time, the charge accumulation and the resulting charge can be effectively avoided.
  • the excitons are quenched.
  • the easily controllable multi-level structure formed by the quantum dots provided by the present invention can fully satisfy and match the energy level structure of other functional layers in the device, so as to achieve matching of the overall energy level structure of the device, thereby contributing to realization. Efficient semiconductor devices.
  • the present invention further provides a method for preparing a quantum dot film according to any one of the above, comprising the steps of: first dispersing a quantum dot in a medium, and then stirring for 20 to 40 minutes to obtain a quantum dot film.
  • the quantum dot includes at least one quantum dot structural unit sequentially arranged in a radial direction, the quantum dot structural unit being a graded alloy composition structure or a radial direction level in a change in energy level width in a radial direction A uniform composition of uniform width.
  • the quantum dot film obtained by the present invention has good film forming properties and workability, particularly printability. Moreover, the semiconductor device made of the quantum dot film of the present invention has excellent optical and electrical properties.
  • the present invention also provides a method for preparing a quantum dot as described above, comprising the steps of:
  • a cation exchange reaction occurs between the first compound and the second compound to form a quantum dot material, and the luminescence peak wavelength of the quantum dot exhibits one or more of blue shift, red shift, and constant.
  • the preparation method of the invention combines the quantum dot SILAR synthesis method with the quantum dot one-step synthesis method to generate quantum dots, specifically, the quantum dot SILAR synthesis method is used to precisely control the quantum dot layer-by-layer growth and the quantum dot one-step synthesis method is used to form the graded component transition shell. That is, two thin layers of a compound having different alloy compositions are successively formed at a predetermined position, and a distribution of alloy components at a predetermined position is achieved by causing a cation exchange reaction between the two layers of compounds. Repeating the above process can continuously achieve the distribution of the alloy composition at a predetermined position in the radial direction.
  • the first compound and the second compound may be binary or binary compounds.
  • the wavelength of the luminescence peak of the quantum dot appears blue shift, it indicates that the luminescence peak shifts toward the short wavelength direction, and the energy level width becomes wider; when the luminescence peak wavelength of the quantum dot appears red shift, the generation The luminescence peak of the table moves toward the long wave direction, and the energy level width is narrowed; when the luminescence peak wavelength of the quantum dot is constant, the energy level width is unchanged.
  • the cationic precursor of the first compound and/or the second compound includes: a precursor of Zn, the precursor of the Zn is derived from dimethyl zinc (inc), diethyl zinc (diethyl) Zinc), Zinc acetate, Zinc acetylacetonate, Zinc iodide, Zinc bromide, Zinc chloride, Zinc fluoride, Zinc carbonate, Zinc cyanide, Zinc nitrate, Zinc oxide, Zinc peroxide, Zinc perchlorate, Zinc sulfate At least one of sulfate, zinc oleate or zinc stearate, but is not limited thereto.
  • the cationic precursor of the first compound and/or the second compound includes a precursor of Cd, and the precursor of the Cd is dimethyl cadmium, diethyl cadmium, Cadmium acetate, cadmium acetylacetonate, cadmium iodide, cadmium bromide, cadmium chloride, cadmium fluoride, cadmium carbonate Cadmium carbonate), cadmium nitrate, cadmium oxide, cadmium perchlorate, cadmium phosphide, cadmium sulfate, cadmium oleate or hard At least one of cadmium stearate and the like, but is not limited thereto.
  • the anion precursor of the first compound and/or the second compound includes a precursor of Se, such as a compound formed by any combination of Se and some organic substances, specifically Se ⁇ TOP (selenium ⁇ trioctylphosphine), Se ⁇ TBP (selenium-tributylphosphine), Se ⁇ TPP (selenium ⁇ triphenylphosphine), Se ⁇ ODE (selenium ⁇ 1 ⁇ octadecene), Se ⁇ OA (selenium ⁇ oleic acid), Se ⁇ ODA (selenium ⁇ octadecylamine), Se ⁇ TOA ( At least one of selenium-trioctylamine), Se ⁇ ODPA (selenium ⁇ octadecylphosphonic acid) or Se ⁇ OLA (selenium ⁇ oleylamine), and the like, but is not limited thereto.
  • Se ⁇ TOP senium ⁇ trioctylphosphine
  • Se ⁇ TBP senium-tribut
  • the anion precursor of the first compound and/or the second compound includes a precursor of S, such as a compound formed by any combination of S and some organic substances, specifically S-TOP (sulfur-trioctylphosphine), S ⁇ TBP(sulfur-tributylphosphine), S ⁇ TPP(sulfur ⁇ triphenylphosphine), S ⁇ ODE(sulfur ⁇ 1 ⁇ octadecene), S ⁇ OA(sulfur ⁇ oleic acid), S ⁇ ODA(sulfur ⁇ octadecylamine), S ⁇ TOA At least one of (sulfur-trioctylamine), S-ODPA (sulfur-octadecylphosphonic acid) or S-OLA (sulfur-oleylamine), etc., but is not limited thereto; the precursor of the S is an alkylthiol (alkyl thiol) The alkyl mercaptan is hexanethiol
  • the anion precursor of the first compound and/or the second compound further includes a precursor of Te, and the precursor of the Te is Te ⁇ TOP, Te ⁇ TBP, Te ⁇ TPP, Te ⁇ ODE, Te At least one of ⁇ OA, Te ⁇ ODA, Te ⁇ TOA, Te ⁇ ODPA, or Te ⁇ OLA.
  • the cation exchange reaction is carried out under the conditions of a heating reaction, for example, a heating temperature of between 100 ° C and 400 ° C, and a preferred heating temperature of between 150 ° C and 380 ° C.
  • the heating time is between 2 s and 24 h, and the preferred heating time is between 5 min and 4 h.
  • the above cationic precursor and anionic precursor may be determined according to the final nanocrystal composition to determine one or more of them: for example, when it is required to synthesize a nanocrystal of Cd x Zn 1 ⁇ x Se y S 1 ⁇ y , Cd is required.
  • Precursor, precursor of Zn, precursor of Se, precursor of S if it is necessary to synthesize nanocrystals of Cd x Zn 1 -x S, a precursor of Cd, a precursor of Zn, and a precursor of S are required;
  • a precursor of Cd, a precursor of Zn, and a precursor of Se are required.
  • the molar ratio of the cationic precursor to the anionic precursor may be from 100:1 to 1:50 (specifically, the molar ratio of the cation to the anion), for example, when forming the first layer of the compound, the cationic precursor The molar ratio to the anion precursor is from 100:1 to 1:50; in forming the second layer compound, the molar ratio of the cationic precursor to the anionic precursor is from 100:1 to 1:50, and the preferred ratio is 20:1.
  • 1:10 the preferred molar ratio of cationic precursor to anionic precursor ensures that the reaction rate is within an easily controllable range.
  • the quantum dots prepared by the above preparation method have a luminescence peak wavelength ranging from 400 nm to 700 nm, and a preferred luminescence peak wavelength range is from 430 nm to 660 nm.
  • the preferred quantum dot luminescence peak wavelength range can ensure quantum dots in this range.
  • a luminescence quantum yield of greater than 30% is achieved within.
  • the quantum dots prepared by the above preparation method have a luminescence quantum yield ranging from 1% to 100%, and the preferred luminescence quantum yield ranges from 30% to 100%, and the preferred luminescent quantum yield range can ensure good application of quantum dots. Sex.
  • the half peak width of the luminescence peak of the quantum dot is from 12 nm to 80 nm.
  • the present invention also provides another method for preparing quantum dots as described above, which comprises the steps of:
  • the difference between this method and the former method is that the former one forms two layers of compounds one after another, and then a cation exchange reaction occurs to achieve the distribution of the alloy components required by the present invention, and the latter method is directly controlled at a predetermined position.
  • a cationic precursor to which the desired synthetic alloy component is added The anion precursor is reacted to form quantum dots to achieve the desired alloy component distribution of the present invention.
  • the reaction principle is that the highly reactive cationic precursor and the anionic precursor react first, the reactive precursor with low reactivity and the anionic precursor react, and during the reaction, different cations undergo cations. The reaction is exchanged to achieve the desired alloy component distribution of the present invention.
  • the types of cationic precursors and anionic precursors are detailed in the foregoing methods.
  • the reaction temperature, the reaction time, the ratio, and the like may be different depending on the specific quantum dots to be synthesized, which are substantially the same as the former method described above, and will be described later in the specific examples.
  • the present invention also provides a semiconductor device comprising the quantum dot film of any of the above.
  • the semiconductor device is any one of an electroluminescent device, a photoluminescence device, a solar cell, a display device, a photodetector, a bioprobe, and a nonlinear optical device.
  • a quantum dot electroluminescent device which is a material of a light-emitting layer is composed of the quantum dots described in the present invention.
  • Such quantum dot electroluminescent devices are capable of achieving: 1) high efficiency charge injection, 2) high luminance, 3) low drive voltage, 4) high device efficiency and the like.
  • the quantum dots of the present invention have the characteristics of easy control and multi-level structure, and can fully satisfy and match the energy level structure of other functional layers in the device, so as to achieve matching of the overall energy level structure of the device, thereby contributing to A highly efficient and stable semiconductor device is realized.
  • the photoluminescent device refers to a device that relies on an external light source to obtain energy, thereby generating excitation and causing light emission, and ultraviolet radiation, visible light, and infrared radiation can cause photoluminescence, such as phosphorescence and fluorescence.
  • the nanocrystal of the present invention can be used as a light-emitting material of a photoluminescent device.
  • the solar cell is also called a photovoltaic device, and the nanocrystal of the invention can be used as a light absorbing material of a solar cell, thereby effectively improving various performances of the photovoltaic device.
  • the display device refers to a backlight module or a display panel to which the backlight module is applied, and the display panel can be applied to various products, such as a display, a tablet, a mobile phone, a notebook computer, a flat-panel TV, and a wearable display. Equipment or other products that contain different sized display panels.
  • the photodetector refers to a device capable of converting an optical signal into an electrical signal, the principle of which is The radiation causes the conductivity of the irradiated material to change, and the quantum dot is applied to the photodetector. It has the following advantages: sensitivity to normal incident light, high photoconductivity, high detection ratio, continuous detection wavelength, and low temperature preparation. .
  • the photogenerated electron-hole pairs generated by the quantum dot photosensitive layer ie, using the nanocrystal of the present invention
  • the built-in electric field which makes the photodetector
  • the structured photodetector has a lower drive voltage and can operate with low applied bias or even 0 applied bias and is easy to control.
  • the bioprobe refers to a device that modifies a certain type of material to have a labeling function, for example, coating the nanocrystal of the present invention to form a fluorescent probe, which is used in the field of cell imaging or substance detection, as opposed to
  • the traditional organic fluorescent dye probe adopts the biological probe prepared by the nanocrystal of the invention, and has the characteristics of high fluorescence intensity, good chemical stability and strong anti-photobleaching ability, and has wide application.
  • the nonlinear optical device belongs to the field of optical laser technology and is widely used, for example, for electro-optic light-on and laser modulation, for laser frequency conversion, laser frequency tuning, optical information processing, image quality improvement and beam quality; As a nonlinear etalon and bistable device; study the high-excited state of the material as well as the high-resolution spectrum and the internal energy and excitation transfer process of the material and other relaxation processes.
  • Example 1 The formulation and preparation process of the quantum dot film is as follows:
  • the medium in which the quantum dots are dispersed contains a non-polar liquid.
  • Quantum dot film 100 mg of quantum dots (surface ligand is oleic acid), 10 mL of decalin-non-polar liquid, and the mixture was stirred for 30 minutes. Quantum dot film.
  • Example 2 The formulation and preparation process of the quantum dot film is as follows:
  • the medium in which the quantum dots are dispersed contains two non-polar liquids.
  • the following components were added to a 500 mL single-necked flask with uniform stirring in the order of: 100 mg of quantum dots (surface ligand is octyl mercaptan), 2.5 mL of dodecane non-polar liquid, 2.5 mL of decalin non-polar liquid, and the mixture was stirred for 30 minutes to obtain a quantum dot film.
  • Example 3 The formulation and preparation process of the quantum dot film is as follows:
  • the medium in which the quantum dots are dispersed contains a polar liquid.
  • Example 4 The formulation and preparation process of the quantum dot film is as follows:
  • the medium in which the quantum dots are dispersed contains two polar liquids.
  • the following components were added to a 500 mL single-necked flask with uniform stirring in the order of: 100 mg of quantum dots (surface ligand is PEG), 2.0 mL of ethylene glycol-butyl ether polar liquid, 3.0 mL of two A polar liquid of ethylene glycol ether was stirred and the mixture was stirred for 30 minutes to obtain a quantum dot film.
  • 100 mg of quantum dots surface ligand is PEG
  • 2.0 mL of ethylene glycol-butyl ether polar liquid 3.0 mL of two A polar liquid of ethylene glycol ether was stirred and the mixture was stirred for 30 minutes to obtain a quantum dot film.
  • a precursor of a cationic Cd, a precursor of a cationic Zn, a precursor of an anion Se, and a precursor of an anion S are injected into a reaction system to form a Cd y Zn 1 ⁇ y Se b S 1 ⁇ b layer (where 0 ⁇ y) ⁇ 1,0 ⁇ b ⁇ 1); the precursor of the cationic Cd, the precursor of the cationic Zn, the precursor of the anion Se, and the precursor of the anion S are continuously injected into the reaction system, in the above Cd y Zn 1 ⁇ y Se b
  • the surface of the S 1 - b layer forms a layer of Cd z Zn 1 ⁇ z Se c S 1 ⁇ c (where 0 ⁇ z ⁇ 1, and z is not equal to y, 0 ⁇ c ⁇ 1); at a certain heating temperature and heating time Under the same reaction conditions, the exchange of Cd and Zn ions in the inner and outer nanocrystals (ie, the above two layers of compounds) occurs;
  • the precursor of the cationic Cd, the precursor of the cationic Zn, and the precursor of the anion S are injected into the reaction system to form a Cd y Zn 1 -y S layer (where 0 ⁇ y ⁇ 1 ); the precursor of the cationic Cd is continued.
  • the precursor of the bulk, cationic Zn and the precursor of the anion S are injected into the reaction system to form a Cd z Zn 1 ⁇ z S layer on the surface of the above Cd y Zn 1 ⁇ y S layer (where 0 ⁇ z ⁇ 1, and z Not equal to y); under certain reaction conditions such as heating temperature and heating time, the exchange of Cd and Zn ions in the inner and outer nanocrystals (ie, the above two layers of compounds) occurs; due to the limited migration distance of the cations and the further migration The smaller the probability of migration, the gradient alloy composition distribution of Cd content and Zn content near the interface between Cd y Zn 1 ⁇ y S layer and Cd z Zn 1 ⁇ z S layer, ie Cd x Zn 1 ⁇ x S, where 0 ⁇ x ⁇ 1.
  • the precursor of the cationic Cd, the precursor of the cationic Zn, and the precursor of the anion Se are injected into the reaction system to form a layer of Cd y Zn 1 ⁇ y Se (where 0 ⁇ y ⁇ 1 ); the precursor of the cation Cd is continued.
  • the precursor of the cationic Zn and the precursor of the anion Se are injected into the reaction system to form a Cd z Zn 1 ⁇ z Se layer on the surface of the above Cd y Zn 1 ⁇ y Se layer (where 0 ⁇ z ⁇ 1, and z does not Equivalent to y); under certain reaction conditions such as heating temperature and heating time, the exchange of Cd and Zn ions in the inner and outer nanocrystals occurs; the probability of migration due to the limited migration distance of the cation and the farther migration distance is smaller.
  • a graded alloy composition distribution of Cd content and Zn content is formed near the interface between the Cd y Zn 1 ⁇ y Se layer and the Cd z Zn 1 ⁇ z Se layer, that is, Cd x Zn 1 ⁇ x Se, where 0 ⁇ x ⁇ 1.
  • Example 8 Preparation based on CdS/ZnS quantum dots
  • the precursor of the cationic Cd and the precursor of the anion S are injected into the reaction system to form a CdS layer; the precursor of the cationic Zn and the precursor of the anion S are continuously injected into the reaction system to form on the surface of the CdS layer.
  • ZnS layer under certain reaction conditions such as heating temperature and heating time, the Zn cation of the outer layer will gradually migrate to the inner layer and undergo cation exchange reaction with Cd cation, that is, Cd ion migrates to the outer layer, and Cd and Zn occur.
  • the precursor of the cationic Cd and the precursor of the anion Se are first injected into the reaction system to form a CdSe layer; the precursor of the cationic Zn and the precursor of the anion Se are continuously injected into the reaction system to form ZnSe on the surface of the CdSe layer.
  • the Zn cation of the outer layer gradually migrates to the inner layer and undergoes cation exchange reaction with Cd cations, that is, Cd ions migrate to the outer layer, and Cd and Zn ions occur.
  • the interchangeability of the cations due to the limited migration distance of the cations and the migration distance of the migration distance is smaller.
  • the Cd content near the interface between the CdSe layer and the ZnSe layer is gradually decreased along the radial direction, and the Zn content is gradually decreased.
  • the distribution of the graded alloy composition gradually increasing radially outward that is, Cd x Zn 1 - x Se, where 0 ⁇ x ⁇ 1 and x is monotonously decreasing from 1 to 0 from the inside to the outside (radial direction).
  • Example 10 Preparation based on CdSeS/ZnSeS quantum dots
  • the precursor of the cationic Cd, the precursor of the anion Se, and the precursor of the anion S are injected into the reaction system to form a CdSe b S 1 -b layer (where 0 ⁇ b ⁇ 1); the precursor of the cationic Zn is continued,
  • the precursor of the anion Se and the precursor of the anion S are injected into the reaction system to form a layer of ZnSe c S 1 -c on the surface of the above CdSe b S 1 -b layer (where 0 ⁇ c ⁇ 1); at a certain heating temperature
  • the Zn cation of the outer layer gradually migrates to the inner layer and undergoes cation exchange reaction with the Cd cation, that is, the Cd ion migrates to the outer layer, and the exchange of Cd and Zn ions occurs;
  • the migration distance is limited and the migration distance of the migration distance is smaller.
  • the Cd content in the vicinity of the interface between the CdSe b S 1 ⁇ b layer and the ZnSe c S 1 ⁇ c layer gradually decreases along the radial direction.
  • Example 11 Preparation based on ZnS/CdS quantum dots
  • the precursor of the cationic Zn and the precursor of the anion S are first injected into the reaction system to form a ZnS layer; the precursor of the cationic Cd and the precursor of the anion S are continuously injected into the reaction system to form a CdS on the surface of the ZnS layer.
  • the Cd cation of the outer layer gradually migrates to the inner layer and undergoes cation exchange reaction with the Zn cation, that is, Zn ions migrate to the outer layer, and Cd and Zn ions occur.
  • Example 12 Preparation based on ZnSe/CdSe quantum dots
  • a precursor of a cationic Zn and a precursor of an anion Se are injected into the reaction system to form a ZnSe layer; and a precursor of a cationic Cd and a precursor of an anion Se are continuously injected into the reaction system to form a CdSe on the surface of the ZnSe layer.
  • the Cd cation of the outer layer gradually migrates to the inner layer and undergoes cation exchange reaction with the Zn cation, that is, Zn ions migrate to the outer layer, and Cd and Zn ions occur.
  • the interchangeability of the cations due to the limited migration distance of the cations and the migration distance of the migration distance is smaller.
  • the Zn content near the interface between the ZnSe layer and the CdSe layer gradually decreases along the radial direction, and the Cd content decreases.
  • Example 13 Preparation based on ZnSeS/CdSeS quantum dots
  • a precursor of a cationic Zn, a precursor of an anion Se, and a precursor of an anion S are first injected into a reaction system to form a ZnSe b S 1 -b layer (where 0 ⁇ b ⁇ 1); the precursor of the cationic Cd is continued, The precursor of the anion Se and the precursor of the anion S are injected into the reaction system to form a layer of CdSe c S 1-c on the surface of the above ZnSebS1 ⁇ b layer (where 0 ⁇ c ⁇ 1); at a certain heating temperature and heating time Under the same reaction conditions, the Cd cation of the outer layer will gradually migrate to the inner layer and undergo cation exchange reaction with the Zn cation, that is, the Zn ion migrates to the outer layer, and the exchange of Cd and Zn ions occurs; the migration distance of the cation is limited.
  • the Zn content in the vicinity of the interface between the ZnSe b S 1 ⁇ b layer and the CdSe c S 1 ⁇ c layer will gradually decrease along the radial direction, and the Cd content will decrease.
  • cadmium oleate and zinc oleate precursor 1 mmol of cadmium oxide (CdO), 9 mmol of zinc acetate [Zn(acet) 2 ], 8 mL of oleic acid (Oleic acid), and 15 mL of octadecene (1 -Octadecene) were placed.
  • vacuum degassing was carried out at 80 ° C for 60 min. It is then switched to a nitrogen atmosphere and stored at this temperature for use.
  • 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleic acid) and 5.4 mL of octadecene (1 -Octadecene) were placed in a 100 mL three-necked flask, and heated under reflux in a nitrogen atmosphere at 250 ° C for 120 min to obtain a transparent oleic acid.
  • Cadmium precursor 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleic acid) and 5.4 mL of octadecene (1 -Octadecene)
  • the cadmium oleate and zinc oleate precursors were heated to 310 ° C under a nitrogen atmosphere, and the thiooctadecene precursor was rapidly injected into the reaction system. After 10 minutes of reaction, the trioctylphosphine sulfide precursor and cadmium oleate were sulfided. The precursor was added dropwise to the reaction system at a rate of 3 mL/h and 10 mL/h, respectively.
  • cadmium oleate and zinc oleate precursor 0.4 mmol of cadmium oxide (CdO), 8 mmol of zinc acetate [Zn(acet) 2 ], and 10 mL of oleic acid (Oleic acid) were placed in a 100 mL three-necked flask at 80 ° C. Vacuum degassing for 60 min. It is then switched to a nitrogen atmosphere and stored at this temperature for use.
  • CdO cadmium oxide
  • Zn(acet) 2 zinc acetate
  • Oleic acid 10 mL
  • trioctylphosphine sulfide precursor Dissolve 2mmol of sulfur powder (Sulfur powder) in 2mL of trioctylphosphine In (Trioctylphosphine), a trioctylphosphine sulfide precursor is obtained.
  • the cadmium oleate and zinc oleate precursors were heated to 310 ° C under a nitrogen atmosphere, and the trioctylphosphine trisulfide sulfide trioctylphosphine precursor was rapidly injected into the reaction system to form Cd x Zn 1 ⁇ x.
  • Se y S 1 ⁇ y after reacting for 10 min, 2 mL of the trioctylphosphine sulfide precursor was added dropwise to the reaction system at a rate of 8 mL/h until the precursor was injected.
  • the product is repeatedly dissolved and precipitated with toluene and anhydrous methanol, and purified by centrifugation to obtain a green quantum dot having a specific structure (Cd x Zn 1 -x Se y S 1 ⁇ y /Cd z Zn 1 ⁇ z S), where the front of "/" represents the composition of the interior of the prepared green quantum dot, and the end of "/" represents the composition outside the prepared green quantum dot, and "/" It is not the obvious boundary, but the structure that changes from the inside to the outside.
  • the subsequent quantum dot representation has the same meaning.
  • cadmium oleate and zinc oleate precursor 0.8 mmol of cadmium oxide (CdO), 12 mmol of zinc acetate [Zn(acet) 2 ], and 14 mL of oleic acid (Oleic acid) were placed in a 100 mL three-necked flask at 80 ° C. Vacuum degassing for 60 min. It is then switched to a nitrogen atmosphere and stored at this temperature for use.
  • the cadmium oleate and zinc oleate precursors were heated to 310 ° C under a nitrogen atmosphere, and the trioctylphosphine precursor was quickly injected into the reaction system to form Cd x Zn 1 -x Se. After 10 minutes of reaction, 2 mL of a trioctylphosphine selenide-trioctylphosphine sulfide precursor was added dropwise to the reaction system at a rate of 4 mL/h.
  • Example 17 Effect of cadmium oleate injection rate on blue quantum dot synthesis with specific structure 1
  • the slope of the gradient change of the quantum dot component can be controlled, thereby affecting the energy level structure, and finally the regulation of the quantum dot emission wavelength is realized.
  • cadmium oleate and zinc oleate precursor 1 mmol of cadmium oxide (CdO), 9 mmol of zinc acetate [Zn(acet) 2 ], 8 mL of oleic acid (Oleic acid), and 15 mL of octadecene (1 -Octadecene) were placed.
  • vacuum degassing was carried out at 80 ° C for 60 min. It is then switched to a nitrogen atmosphere and stored at this temperature for use.
  • 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleic acid) and 5.4 mL of octadecene (1 -Octadecene) were placed in a 100 mL three-necked flask, and heated under reflux in a nitrogen atmosphere at 250 ° C for 120 min to obtain a transparent oleic acid.
  • Cadmium precursor 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleic acid) and 5.4 mL of octadecene (1 -Octadecene)
  • the cadmium oleate and zinc oleate precursors were heated to 310 ° C under a nitrogen atmosphere, and the thiooctadecene precursor was rapidly injected into the reaction system to form Cd x Zn 1 -x S. After 10 minutes of reaction, the sulfide was vulcanized.
  • the trioctylphosphine precursor was added dropwise to the reaction system at a rate of 3 mL/h, while the cadmium oleate precursor was added dropwise to the reaction system at different injection rates.
  • quantum dot emission wavelength modulation Based on the same core (alloy quantum dot luminescence peak 447nm) and the injection rate of different oleic acid cadmium precursors, the list of quantum dot emission wavelength modulation is as follows:
  • Cadmium oleate injection rate (mmol/h) Luminous wavelength (nm)
  • Example 18 Effect of cadmium oleate injection on the synthesis of blue quantum dots with specific structure 1
  • Example 14 and Example 17 by adjusting the injection amount of the cadmium oleate precursor, the interval of the gradient change of the composition of the quantum dot can be controlled, thereby affecting the change of the energy level structure, and finally realizing the quantum dot luminescence.
  • Wavelength regulation Based on the same core (alloy quantum dot luminescence peak 447 nm) and different oleic acid cadmium precursor injection rates (1 mmol/h at the same injection rate), the quantum dot emission wavelength modulation is listed below.
  • Cadmium oleate injection amount (mmol) Luminous wavelength (nm) 0.4 449 0.5 451 0.6 453 0.8 454 1.0 455
  • cadmium oleate and zinc oleate precursor 1 mmol of cadmium oxide (CdO), 9 mmol of zinc acetate [Zn(acet) 2 ], 8 mL of oleic acid (Oleic acid) and 15 mL of octadecene (1 -Octadecene) were placed in 100 mL In a three-necked flask, vacuum degassing was carried out at 80 ° C for 60 min. It is then switched to a nitrogen atmosphere and stored at this temperature for use.
  • CdO cadmium oxide
  • Zn(acet) 2 zinc acetate
  • Oleic acid oleic acid
  • octadecene 1 -Octadecene
  • trioctylphosphine sulfide precursor Dissolve 6mmol of sulfur powder (Sulfur powder) in 3mL of trioctylphosphine In (Trioctylphosphine), a trioctylphosphine sulfide precursor is obtained.
  • 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleic acid) and 5.4 mL of octadecene (1 -Octadecene) were placed in a 100 mL three-necked flask, and heated under reflux in a nitrogen atmosphere at 250 ° C for 120 min to obtain a transparent oleic acid.
  • Cadmium precursor 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleic acid) and 5.4 mL of octadecene (1 -Octadecene)
  • the cadmium oleate and zinc oleate precursors were heated to 310 ° C under a nitrogen atmosphere, and the thiooctadecene precursor was rapidly injected into the reaction system to form Cd x Zn 1 -x S. After 10 minutes of reaction, the reaction was carried out. The temperature of the system was lowered to 280 ° C, and then 2 mL of a trioctylphosphine sulfide precursor and 6 mL of a cadmium oleate precursor were simultaneously injected into the reaction system at a rate of 3 mL/h and 10 mL/h, respectively.
  • the temperature of the reaction system was raised to 310 ° C, and 1 mL of the trioctylphosphine sulfide precursor was injected into the reaction system at a rate of 3 mL/h.
  • the reaction solution was cooled to room temperature, and then toluene and no.
  • the product was repeatedly dissolved and precipitated by water methanol, and purified by centrifugation to obtain a blue quantum dot of the specific structure 2.
  • cadmium oleate and zinc oleate precursor 0.4 mmol of cadmium oxide (CdO), 8 mmol of zinc acetate [Zn(acet) 2], 10 mL of oleic acid (Oleic acid) and 20 mL of octadecene (1 -Octadecene) were placed. In a 100 mL three-necked flask, vacuum degassing was carried out at 80 ° C for 60 min. It is then switched to a nitrogen atmosphere and stored at this temperature for use.
  • CdO cadmium oxide
  • Zn(acet) 2 zinc acetate
  • 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleic acid) and 5.4 mL of octadecene (1 -Octadecene) were placed in a 100 mL three-necked flask, and heated under reflux in a nitrogen atmosphere at 250 ° C for 120 min to obtain a transparent oleic acid.
  • Cadmium precursor 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleic acid) and 5.4 mL of octadecene (1 -Octadecene)
  • the cadmium oleate and zinc oleate precursors were heated to 310 ° C under a nitrogen atmosphere, and the trioctylphosphine trisulfide sulfide trioctylphosphine precursor was rapidly injected into the reaction system to form Cd x Zn 1 ⁇ x.
  • Se y S 1 ⁇ y after reacting for 10 min, the temperature of the reaction system was lowered to 280 ° C, and then 1.2 mL of the trioctylphosphine sulfide precursor and 6 mL of the cadmium oleate precursor were respectively at a rate of 2 mL/h and 10 mL/h. Inject into the reaction system until the precursor is injected.
  • the temperature of the reaction system was raised to 310 ° C, and 0.8 mL of a trioctylphosphine sulfide precursor was injected into the reaction system at a rate of 2 mL/h. After completion of the reaction, after the reaction solution was cooled to room temperature, the product was repeatedly dissolved and precipitated with toluene and anhydrous methanol, and purified by centrifugation to obtain a green quantum dot having a specific structure 2.
  • cadmium oleate and zinc oleate precursor 0.8 mmol of cadmium oxide (CdO), 12 mmol of zinc acetate [Zn(acet) 2 ], 14 mL of oleic acid (Oleic acid) and 20 mL of octadecene (1 -Octadecene) were placed.
  • vacuum degassing was carried out at 80 ° C for 60 min. It is then switched to a nitrogen atmosphere and stored at this temperature for use.
  • Cadmium precursor 0.3 mmol of cadmium oxide (CdO), 0.3 mL of oleic acid (Oleic acid) and 2.7 mL of octadecene (1 -Octadecene) were placed in a 50 mL three-necked flask, and heated under reflux in a nitrogen atmosphere at 250 ° C for 120 min to obtain a transparent oleic acid.
  • Cadmium precursor 0.3 mmol of cadmium oxide (CdO), 0.3 mL of oleic acid (Oleic acid) and 2.7 mL of octadecene (1 -Octadecene) were placed in a 50 mL three-necked flask, and heated under reflux in a nitrogen atmosphere at 250 ° C for 120 min to obtain a transparent oleic acid.
  • Cadmium precursor 0.3 mmol of cadmium oxide (CdO)
  • oleic acid
  • the cadmium oleate and zinc oleate precursors were heated to 310 ° C under a nitrogen atmosphere, and the trioctylphosphine precursor was quickly injected into the reaction system to form Cd x Zn 1 -x Se. After 10 minutes of reaction, The temperature of the reaction system was lowered to 280 ° C, and then 1 mL of a trioctylphosphine sulfide-trioctylphosphine sulfide precursor and 3 mL of a cadmium oleate precursor were injected into the reaction system at a rate of 2 mL/h and 6 mL/h, respectively.
  • the temperature of the reaction system was raised to 310 ° C, and 1 mL of a trioctylphosphine selenide-trioctylphosphine sulfide precursor was injected into the reaction system at a rate of 4 mL/h. After completion of the reaction, after the reaction solution was cooled to room temperature, the product was repeatedly dissolved and precipitated with toluene and anhydrous methanol, and purified by centrifugation to obtain a red quantum dot having a specific structure 2.
  • cadmium oleate and zinc oleate precursor 1 mmol of cadmium oxide (CdO), 9 mmol of zinc acetate [Zn(acet) 2 ], 8 mL of oleic acid (Oleic acid), and 15 mL of octadecene (1 -Octadecene) were placed.
  • vacuum degassing was carried out at 80 ° C for 60 min. It is then switched to a nitrogen atmosphere and stored at this temperature for use.
  • 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleic acid) and 5.4 mL of octadecene (1 -Octadecene) were placed in a 100 mL three-necked flask, and heated under reflux in a nitrogen atmosphere at 250 ° C for 120 min to obtain a transparent oleic acid.
  • Cadmium precursor 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleic acid) and 5.4 mL of octadecene (1 -Octadecene)
  • the cadmium oleate and zinc oleate precursors were heated to 310 ° C under a nitrogen atmosphere, and the thiooctadecene precursor was rapidly injected into the reaction system to form Cd x Zn 1 -x S. After 10 minutes of reaction, the oil was oiled.
  • the cadmium acid precursor and the trioctylphosphine sulfide precursor were continuously injected into the reaction system at a rate of 0.6 mmol/h and 4 mmol/h, respectively, for 20 min.
  • the cadmium oleate precursor, the trioctylphosphine sulfide precursor and the trioctylphosphine selenide precursor were successively injected into the reaction system at a rate of 0.4 mmol/h, 0.6 mmol/h and 0.2 mmol/h, respectively, for 1 h.
  • the reaction solution was cooled to room temperature, the product was repeatedly dissolved and precipitated with toluene and anhydrous methanol, and purified by centrifugation to obtain a blue quantum dot (CdZnS/CdZnS/) having a quantum well level structure (specific structure 3). CdZnSeS 3 ).
  • cadmium oleate and zinc oleate precursor 0.4 mmol of cadmium oxide (CdO), 6 mmol of zinc acetate [Zn(acet) 2 ], 10 mL of oleic acid (Oleic acid) and 20 mL of octadecene (1 -Octadecene)
  • CdO cadmium oxide
  • Zn(acet) 2 zinc acetate
  • 10 mL of oleic acid (Oleic acid) and 20 mL of octadecene (1 -Octadecene) In a 100 mL three-necked flask, vacuum degassing was carried out at 80 ° C for 60 min. It is then switched to a nitrogen atmosphere and stored at this temperature for use.
  • Trioctylphosphine 0.1 mmol of Selenium powder and 0.3 mmol of sulfur powder (Sulfur powder) were dissolved in 2 mL of Trioctylphosphine to obtain trioctylphosphine selenide-trioctylphosphine sulfide precursor 2.
  • 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleic acid) and 5.4 mL of octadecene (1 -Octadecene) were placed in a 100 mL three-necked flask, and heated under reflux in a nitrogen atmosphere at 250 ° C for 120 min to obtain a transparent oleic acid.
  • Cadmium precursor 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleic acid) and 5.4 mL of octadecene (1 -Octadecene)
  • trioctylphosphine trisulfide sulfide trioctylphosphine precursor 1 was quickly injected into the reaction system to form Cd x Zn 1 ⁇ x SeyS 1 -y , after reacting for 5 min, 2 mL of trioctylphosphine selenide-trioctylphosphine sulfide precursor 2 was added dropwise to the reaction system at a rate of 6 mL/h.
  • trioctylphosphine selenide-trioctylphosphine sulfide precursor 3 and 6 mL of the cadmium oleate precursor were continuously added dropwise to the reaction system at a rate of 3 mL/h and 6 mL/h, respectively.
  • the product was repeatedly dissolved and precipitated with toluene and anhydrous methanol, and purified by centrifugation to obtain a green quantum dot (CdZn 3 SeS 3 /Zn 4 SeS 3 /Cd 3 having a specific structure 3). Zn 5 Se 4 S 4 ).
  • cadmium oleate and zinc oleate precursor 0.8 mmol of cadmium oxide (CdO), 12 mmol of zinc acetate [Zn(acet) 2 ], 14 mL of oleic acid (Oleic acid) and 20 mL of octadecene (1 -Octadecene) were placed.
  • vacuum degassing was carried out at 80 ° C for 60 min. It is then switched to a nitrogen atmosphere and stored at this temperature for use.
  • CdO cadmium oxide
  • Oleic acid oleic acid
  • octadecene octadecene
  • the cadmium oleate and zinc oleate precursors were heated to 310 ° C under a nitrogen atmosphere, and the trioctylphosphine precursor was quickly injected into the reaction system to form Cd x Zn 1 -x Se. After 10 minutes of reaction, 2 mL of a trioctylphosphine selenide-trioctylphosphine sulfide precursor was added dropwise to the reaction system at a rate of 2 mL/h. When injected for 30 min, 3 mL of a cadmium oleate precursor was simultaneously added dropwise to the reaction system at a rate of 6 mL/h.
  • cadmium oleate and zinc oleate precursor 1 mmol of cadmium oxide (CdO), 9 mmol of zinc acetate [Zn(acet) 2 ], 8 mL of oleic acid (Oleic acid), and 15 mL of octadecene (1 -Octadecene) were placed.
  • vacuum degassing was carried out at 80 ° C for 60 min. It is then switched to a nitrogen atmosphere and stored at this temperature for use.
  • trioctylphosphine selenide precursor Dissolve 0.2 mmol of Selenium powder in 1 mL of trioctylphosphine In (Trioctylphosphine), a trioctylphosphine selenide precursor is obtained.
  • 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleic acid) and 5.4 mL of octadecene (1 -Octadecene) were placed in a 100 mL three-necked flask, and heated under reflux in a nitrogen atmosphere at 250 ° C for 120 min to obtain a transparent oleic acid.
  • Cadmium precursor 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleic acid) and 5.4 mL of octadecene (1 -Octadecene)
  • the cadmium oleate and zinc oleate precursors were heated to 310 ° C under a nitrogen atmosphere, and the thiooctadecene precursor was rapidly injected into the reaction system to form Cd x Zn 1 -x S. After 10 minutes of reaction, the oil was oiled.
  • the cadmium acid precursor and the trioctylphosphine selenide precursor were continuously injected into the reaction system at a rate of 0.6 mmol/h and 0.6 mmol/h, respectively, for 20 min.
  • the cadmium oleate precursor and the trioctylphosphine sulfide precursor were continuously injected into the reaction system at a rate of 0.4 mmol/h and 6 mmol/h, respectively, for 1 hour.
  • the reaction solution was cooled to room temperature, the product was repeatedly dissolved and precipitated with toluene and anhydrous methanol, and purified by centrifugation to obtain a blue quantum dot (CdZnS/CdZnSe/) having a quantum well level structure (specific structure 4).
  • CdZnS blue quantum dot
  • cadmium oleate and zinc oleate precursor 1 mmol of cadmium oxide (CdO), 9 mmol of zinc acetate [Zn(acet) 2 ], 8 mL of oleic acid (Oleic acid), and 15 mL of octadecene (1 -Octadecene) were placed.
  • vacuum degassing was carried out at 80 ° C for 60 min. It is then switched to a nitrogen atmosphere and stored at this temperature for use.
  • Cadmium precursor 0.8 mmol of cadmium oxide (CdO), 1.2 mL of oleic acid (Oleic acid) and 4.8 mL of octadecene (1 -Octadecene) were placed in a 100 mL three-necked flask, and heated under reflux in a nitrogen atmosphere at 250 ° C for 120 min to obtain a transparent oleic acid.
  • Cadmium precursor 0.8 mmol of cadmium oxide (CdO), 1.2 mL of oleic acid (Oleic acid) and 4.8 mL of octadecene (1 -Octadecene) were placed in a 100 mL three-necked flask, and heated under reflux in a nitrogen atmosphere at 250 ° C for 120 min to obtain a transparent oleic acid.
  • Cadmium precursor 0.8 mmol of cadmium oxide (CdO)
  • oleic acid
  • the cadmium oleate and zinc oleate precursors were heated to 310 ° C under a nitrogen atmosphere, and the thiooctadecene precursor was rapidly injected into the reaction system to form Cd x Zn 1 -x S. After 10 minutes of reaction, the oil was oiled.
  • the cadmium acid precursor and the trioctylphosphine selenide precursor were continuously injected into the reaction system at a rate of 0.6 mmol/h and 0.6 mmol/h, respectively, for 40 min.
  • the cadmium oleate precursor and the trioctylphosphine sulfide precursor were continuously injected into the reaction system at a rate of 0.4 mmol/h and 6 mmol/h, respectively, for 1 hour.
  • the reaction solution was cooled to room temperature, the product was repeatedly dissolved and precipitated with toluene and anhydrous methanol, and purified by centrifugation to obtain a green quantum dot (CdZnS/CdZnSe/CdZnS having a quantum well level structure (specific structure 4). ).
  • cadmium oleate and zinc oleate precursor 0.8 mmol of cadmium oxide (CdO), 12 mmol of zinc acetate [Zn(acet) 2 ], 14 mL of oleic acid (Oleic acid) and 20 mL of octadecene (1 -Octadecene) were placed.
  • vacuum degassing was carried out at 80 ° C for 60 min. It is then switched to a nitrogen atmosphere and stored at this temperature for use.
  • the cadmium oleate and zinc oleate precursors were heated to 310 ° C under a nitrogen atmosphere, and the trioctylphosphine selenide-trioctylphosphine sulfide precursor 1 was injected into the reaction system to form Cd x Zn 1 ⁇ x. Se, after reacting for 10 min, 2 mL of a trioctylphosphine selenide precursor and 3 mL of a cadmium oleate precursor were added dropwise to the reaction system at a rate of 4 mL/h and 6 mL/h, respectively.
  • trioctylphosphine selenide-trioctylphosphine sulfide precursor 2 and 3 mL of cadmium oleate precursor were added dropwise to the reaction system at a rate of 2 mL/h and 3 mL/h, respectively.
  • the reaction solution is cooled to room temperature, the product is repeatedly dissolved and precipitated with toluene and anhydrous methanol, and purified by centrifugation to obtain a red quantum dot of specific structure 4 (Cd x Zn 1 -x Se/CdZnSe/Cd z Zn 1 ⁇ z SeS).
  • cadmium oleate and zinc oleate precursor 1 mmol of cadmium oxide (CdO), 9 mmol of zinc acetate [Zn(acet) 2 ], 8 mL of oleic acid (Oleic acid), and 15 mL of octadecene (1 -Octadecene) were placed.
  • vacuum degassing was carried out at 80 ° C for 60 min. It is then switched to a nitrogen atmosphere and stored at this temperature for use.
  • 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleic acid) and 5.4 mL of octadecene (1 -Octadecene) were placed in a 100 mL three-necked flask, and heated under reflux in a nitrogen atmosphere at 250 ° C for 120 min to obtain a transparent oleic acid.
  • Cadmium precursor 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleic acid) and 5.4 mL of octadecene (1 -Octadecene)
  • the cadmium oleate and zinc oleate precursors were heated to 310 ° C under a nitrogen atmosphere, and the thiooctadecene precursor was rapidly injected into the reaction system to form Cd x Zn 1 -x S. After 10 minutes of reaction, 3 mL was obtained.
  • the trioctylphosphine sulfide precursor was continuously injected into the reaction system at a rate of 3 mL/h for 1 h. When the trioctylphosphine sulfide precursor was injected for 20 min, 2 mL of the cadmium oleate precursor was injected into the reaction system at 6 mL/h.
  • cadmium oleate and zinc oleate precursor 0.4 mmol of cadmium oxide (CdO), 6 mmol of zinc acetate [Zn(acet) 2 ], 10 mL of oleic acid (Oleic acid) and 20 mL of octadecene (1 -Octadecene) were placed. In a 100 mL three-necked flask, vacuum degassing was carried out at 80 ° C for 60 min. It is then switched to a nitrogen atmosphere and stored at this temperature for use.
  • CdO cadmium oxide
  • Zn(acet) 2 zinc acetate
  • 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleic acid) and 5.4 mL of octadecene (1 -Octadecene) were placed in a 100 mL three-necked flask, and heated under reflux in a nitrogen atmosphere at 250 ° C for 120 min to obtain a transparent oleic acid.
  • Cadmium precursor 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleic acid) and 5.4 mL of octadecene (1 -Octadecene)
  • the cadmium oleate and zinc oleate precursors were heated to 310 ° C under a nitrogen atmosphere, and the trioctylphosphine trisulfide sulfide trioctylphosphine precursor was rapidly injected into the reaction system to form Cd x Zn 1 ⁇ x.
  • Se y S 1 ⁇ y after reacting for 10 min, 3 mL of the trioctylphosphine sulfide precursor was continuously injected at a rate of 3 mL/h for 1 h into the reaction system.
  • the trioctylphosphine sulfide precursor was injected for 20 min, 2 mL of oleic acid was added.
  • the cadmium precursor was injected into the reaction system at 6 mL/h.
  • the trioctylphosphine sulfide precursor was injected for 40 min, 4 mL of the cadmium oleate precursor was injected into the reaction system at 12 mL/h.
  • the product is repeatedly dissolved and precipitated with toluene and anhydrous methanol, and purified by centrifugation to obtain a green quantum dot (CdZnSeS/ZnS/CdZnS having a quantum well level structure (specific structure 5). ).
  • cadmium oleate and zinc oleate precursor 0.8 mmol of cadmium oxide (CdO), 12 mmol of zinc acetate [Zn(acet) 2 ], 14 mL of oleic acid (Oleic acid) and 20 mL of octadecene (1 -Octadecene) were placed.
  • vacuum degassing was carried out at 80 ° C for 60 min. It is then switched to a nitrogen atmosphere and stored at this temperature for use.
  • 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleic acid) and 5.4 mL of octadecene (1 -Octadecene) were placed in a 100 mL three-necked flask, and heated under reflux in a nitrogen atmosphere at 250 ° C for 120 min to obtain a transparent oleic acid.
  • Cadmium precursor 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleic acid) and 5.4 mL of octadecene (1 -Octadecene)
  • the cadmium oleate and zinc oleate precursors were heated to 310 ° C under a nitrogen atmosphere, and the trioctylphosphine precursor was quickly injected into the reaction system to form Cd x Zn 1 -x Se. After 10 minutes of reaction, The trioctylphosphine sulfide precursor was continuously injected into the reaction system at a rate of 6 mmol/h for 1 h. When S-TOP was injected for 20 min, 0.2 mmol of cadmium oleate precursor was injected into the reaction system at 0.6 mmol/h.
  • cadmium oleate and zinc oleate precursor 1 mmol of cadmium oxide (CdO), 9 mmol of zinc acetate [Zn(acet) 2 ], 8 mL of oleic acid (Oleic acid), and 15 mL of octadecene (1 -Octadecene) were placed.
  • vacuum degassing was carried out at 80 ° C for 60 min. It is then switched to a nitrogen atmosphere and stored at this temperature for use.
  • the cadmium oleate and zinc oleate precursors were heated to 310 ° C under a nitrogen atmosphere, and the thiooctadecene precursor was rapidly injected into the reaction system to form Cd x Zn 1 -x S. After 10 minutes of reaction, the sulfide was vulcanized.
  • the trioctylphosphine precursor and the cadmium oleate precursor were added dropwise to the reaction system at a rate of 6 mmol/h and 0.6 mmol/h, respectively.
  • cadmium oleate and zinc oleate precursor 0.4 mmol of cadmium oxide (CdO), 8 mmol of zinc acetate [Zn(acet) 2 ], and 10 mL of oleic acid (Oleic acid) were placed in a 100 mL three-necked flask at 80 ° C. Vacuum degassing for 60 min. It is then switched to a nitrogen atmosphere and stored at this temperature for use.
  • CdO cadmium oxide
  • Zn(acet) 2 zinc acetate
  • Oleic acid 10 mL
  • the cadmium oleate and zinc oleate precursors were heated to 310 ° C under a nitrogen atmosphere, and the trioctylphosphine trisulfide sulfide trioctylphosphine precursor was rapidly injected into the reaction system to form Cd x Zn 1 ⁇ x.
  • SeyS 1 ⁇ y after reacting for 10 min, the temperature of the reaction system was lowered to 280 ° C, and the trioctylphosphine sulfide precursor was added dropwise to the reaction system at a rate of 4 mL/h.
  • cadmium oleate and zinc oleate precursor 0.8 mmol of cadmium oxide (CdO), 12 mmol of zinc acetate [Zn(acet) 2 ], and 14 mL of oleic acid (Oleic acid) were placed in a 100 mL three-necked flask at 80 ° C. Vacuum degassing for 60 min. It is then switched to a nitrogen atmosphere and stored at this temperature for use.
  • the cadmium oleate and zinc oleate precursors were heated to 310 ° C under a nitrogen atmosphere, and the trioctylphosphine precursor was quickly injected into the reaction system to form Cd x Zn 1 -x Se. After 10 minutes of reaction, The temperature of the reaction system was lowered to 280 ° C, and a trioctylphosphine selenide-trioctylphosphine sulfide precursor was added dropwise to the reaction system at a rate of 4 mL/h.
  • cadmium oleate first precursor 1 mmol of cadmium oxide (CdO), 1 mL of oleic acid (Oleic acid) and 5 mL of octadecene (1 -Octadecene) were placed in a 100 mL three-necked flask and vacuum degassed at 80 ° C for 60 mins. . It is then switched to a nitrogen atmosphere and stored at this temperature for use.
  • CdO cadmium oxide
  • Oleic acid oleic acid
  • octadecene 1 -Octadecene
  • cadmium oleate second precursor 0.6 mmol of cadmium oxide (CdO), 0.6 mL of oleic acid (Oleicacid) and 5.4 mL of octadecene (1 -Octadecene) were placed in a 100 mL three-necked flask and heated at 250 ° C under a nitrogen atmosphere. After refluxing for 120 mins, a transparent second precursor of cadmium oleate was obtained.
  • CdO cadmium oxide
  • Oleicacid oleic acid
  • octadecene octadecene
  • the first precursor of cadmium oleate was heated to 310 ° C under nitrogen atmosphere, and the thiooctadecene precursor was rapidly injected into the reaction system to rapidly form CdS. After 10 mins of reaction, the zinc oleate precursor was completely injected into the reaction system. Subsequently, 3 mL of the trioctylphosphine sulfide precursor and 6 mL of the cadmium oleate precursor were simultaneously injected into the reaction system at a rate of 3 mL/h and 10 mL/h, respectively.
  • cadmium oleate precursor 0.4 mmol of cadmium oxide (CdO), 1 mL of oleic acid (Oleic acid) and 5 mL of octadecene (1 -Octadecene) were placed in a 100 mL three-necked flask and vacuum degassed at 80 ° C for 60 mins. It was then heated to reflux at 250 ° C under a nitrogen atmosphere and stored at this temperature for use.
  • CdO cadmium oxide
  • Oleic acid oleic acid
  • octadecene 1 -Octadecene
  • the cadmium oleate precursor was heated to 310 ° C under a nitrogen atmosphere, and the trioctylphosphine precursor was selenized.
  • the body was quickly injected into the reaction system to rapidly form CdSe. After reacting for 5 mins, all the zinc oleate precursors were injected into the reaction system, and 2 mL of the trioctylphosphine selenide-trioctylphosphine sulfide precursor was 2 mL/h. The rate is added dropwise to the reaction system until the precursor is injected.
  • the product was repeatedly dissolved and precipitated with toluene and anhydrous methanol, and purified by centrifugation to obtain a green fluorescent quantum dot having a quantum well level structure.
  • cadmium oleate precursor 0.8 mmol of cadmium oxide (CdO), 4 mL of oleic acid (Oleic acid) and 10 mL of octadecene (1 -Octadecene) were placed in a 100 mL three-necked flask and vacuum degassed at 80 ° C for 60 mins. It was then heated to reflux at 250 ° C under a nitrogen atmosphere and stored at this temperature for use.
  • CdO cadmium oxide
  • Oleic acid oleic acid
  • octadecene 1 -Octadecene
  • Zinc oleate precursor preparation 12mmol zinc acetate [Zn(acet) 2 ], 10mL oleic acid (Oleic acid) and 10mL octadecene (1 ⁇ Octadecene) were placed in a 100mL three-necked flask and vacuum degassed at 80 ° C 60mins.
  • the cadmium oleate precursor was heated to 310 ° C under nitrogen atmosphere, and the trioctylphosphine precursor was quickly injected into the reaction system to rapidly form CdSe. After 10 mins of reaction, the zinc oleate precursor was injected into the reaction. In the system, 2 mL of a trioctylphosphine selenide-trioctylphosphine sulfide precursor was added dropwise to the reaction system at a rate of 4 mL/h.
  • the product was repeatedly dissolved and precipitated with toluene and anhydrous methanol, and purified by centrifugation to obtain a red fluorescent quantum dot having a quantum well level structure.
  • the quantum dot light emitting diode of this embodiment includes: ITO lining from bottom to top. Bottom 11, bottom electrode 12, PEDOT: PSS hole injection layer 13, poly-TPD hole transport layer 14, quantum dot light-emitting layer 15, ZnO electron transport layer 16, and Al top electrode 17.
  • a quantum dot light-emitting layer is prepared on the poly-TPD hole transport layer 14. 15. The thickness was 20 nm, and then a 40 nm ZnO electron transport layer 16 and a 100 nm Al top electrode 17 were prepared on the quantum dot light-emitting layer 15.
  • the quantum dot material of the quantum dot light-emitting layer 15 is a quantum dot film as described in the examples.
  • the quantum dot light-emitting diodes include, in order from bottom to top, an ITO substrate 21, a bottom electrode 22, a PEDOT: PSS hole injection layer 23, and a poly(9-vinylcarbazole) (PVK) space.
  • a quantum dot light-emitting layer 25 is prepared on the PVK hole transport layer 24, and the thickness is At 20 nm, a 40 nm ZnO electron transport layer 26 and a 100 nm Al top electrode 27 were subsequently prepared on the quantum dot light-emitting layer 25.
  • the quantum dot material of the quantum dot light-emitting layer 25 is a quantum dot film as described in the examples.
  • the quantum dot light emitting diode of this embodiment includes an ITO substrate 31, a bottom electrode 32, a PEDOT: PSS hole injection layer 33, a poly-TPD hole transport layer 34, and a quantum dot in this order from bottom to top.
  • a quantum dot light-emitting layer is prepared on the poly-TPD hole transport layer 34.
  • 35 the thickness is 20 nm, and then pass through the quantum dot light-emitting layer 35
  • the 30 nm TPBi electron transport layer 36 and the 100 nm Al top electrode 37 were prepared by an air evaporation method.
  • the quantum dot material of the quantum dot light-emitting layer 35 is a quantum dot film as described in the examples.
  • the quantum dot light-emitting diode of this embodiment includes an ITO substrate 41, a bottom electrode 42, a ZnO electron transport layer 43, a quantum dot light-emitting layer 44, an NPB hole transport layer 45, and a MoO in this order from bottom to top. 3 hole injection layer 46 and Al top electrode 47.
  • a bottom electrode 42 and a 40 nm ZnO electron transport layer 43 are sequentially prepared on the ITO substrate 41, and a quantum dot light-emitting layer 44 is formed on the ZnO electron transport layer 43 to a thickness of 20 nm, and then a 30 nm NPB space is prepared by a vacuum evaporation method.
  • the quantum dot material of the quantum dot light-emitting layer 44 is a quantum dot film as described in the examples.
  • the quantum dot light-emitting diode of this embodiment includes, in order from bottom to top, a glass substrate 51, an Al electrode 52, a PEDOT: PSS hole injection layer 53, a poly-TPD hole transport layer 54, and a quantum dot.
  • a 100 nm Al electrode 52 was prepared on the glass substrate 51 by a vacuum evaporation method, and then a 30 nm PEDOT:PSS hole injection layer 53 and a 30 nm poly-TPD hole transport layer 54 were sequentially prepared, followed by a poly-TPD hole transport layer 54.
  • a quantum dot light-emitting layer 55 was prepared to have a thickness of 20 nm, and then a 40 nm ZnO electron transport layer 56 was prepared on the quantum dot light-emitting layer 55. Finally, 120 nm of ITO was prepared as a top electrode 57 by a sputtering method.
  • the quantum dot material of the quantum dot light-emitting layer 55 is a quantum dot film as described in the examples.
  • the quantum dot light-emitting diode of this embodiment includes, in order from bottom to top, a glass substrate 61, an Al electrode 62, a ZnO electron transport layer 63, a quantum dot light-emitting layer 64, an NPB hole transport layer 65, and a MoO. 3 hole injection layer 66 and ITO top electrode 67.
  • a 100 nm Al electrode 62 is prepared on the glass substrate 61 by a vacuum evaporation method, and then a 40 nm ZnO electron transport layer 63, a 20 nm quantum dot light emitting layer 64 is sequentially prepared, and then a 30 nm NPB hole transport layer 65 is prepared by a vacuum evaporation method. 5 nm MoO 3 hole injection layer 66, and finally 120 nm ITO was prepared as a top electrode 67 by a sputtering method.
  • the quantum dot material of the quantum dot light-emitting layer is a quantum dot film as described in the examples.

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Abstract

La présente invention concerne un film à points quantiques et un procédé de fabrication associé. Le film à points quantiques comprend, en pourcentage en poids, les constituants suivants : 0,01 à 40,0 % de points quantiques, les points quantiques comprenant une ou plusieurs unités de structure à points quantiques disposées séquentiellement dans une direction radiale, et les unités de structure à points quantiques forment une structure d'alliage à composition graduelle présentant une largeur de niveau d'énergie variée dans la direction radiale ou une structure de composition uniforme présentant une largeur de niveau d'énergie cohérente dans la direction radiale; et 60,0 à 99,99 % d'un milieu de dispersion pour les points quantiques. Un dispositif à semi-conducteur fabriqué en utilisant le film à points quantiques de la présente invention présente des propriétés optiques et électriques supérieures, etc.
PCT/CN2017/080607 2016-12-30 2017-04-14 Film à points quantiques et procédé de fabrication associé Ceased WO2018120511A1 (fr)

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WO2020147125A1 (fr) * 2019-01-18 2020-07-23 京东方科技集团股份有限公司 Structure de point quantique et procédé de fabrication correspondant, film optique et procédé de fabrication correspondant, et dispositif d'affichage
CN111647224B (zh) * 2019-03-04 2023-03-31 苏州星烁纳米科技有限公司 量子点-聚合物复合体的制备方法
CN110564404A (zh) * 2019-08-30 2019-12-13 苏州星烁纳米科技有限公司 量子点的制备方法及量子点、量子点组合物和彩膜

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CN104736234A (zh) * 2012-08-30 2015-06-24 应用纳米技术中枢(Can)有限公司 核-壳纳米颗粒的制备方法和核-壳纳米颗粒
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