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WO2018176995A1 - Procédé de préparation d'un transistor à effet de champ composite - Google Patents

Procédé de préparation d'un transistor à effet de champ composite Download PDF

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Publication number
WO2018176995A1
WO2018176995A1 PCT/CN2018/072964 CN2018072964W WO2018176995A1 WO 2018176995 A1 WO2018176995 A1 WO 2018176995A1 CN 2018072964 W CN2018072964 W CN 2018072964W WO 2018176995 A1 WO2018176995 A1 WO 2018176995A1
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WIPO (PCT)
Prior art keywords
polymer
graphene
composite
dispersion
effect transistor
Prior art date
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Ceased
Application number
PCT/CN2018/072964
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English (en)
Chinese (zh)
Inventor
吴雨辰
刘芸
江雷
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Beijing Scitech Nanotechnology Co Ltd
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Beijing Scitech Nanotechnology Co Ltd
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Filing date
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Publication of WO2018176995A1 publication Critical patent/WO2018176995A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/10—Organic polymers or oligomers
    • H10K85/111—Organic polymers or oligomers comprising aromatic, heteroaromatic, or aryl chains, e.g. polyaniline, polyphenylene or polyphenylene vinylene
    • H10K85/113—Heteroaromatic compounds comprising sulfur or selene, e.g. polythiophene
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K10/00—Organic devices specially adapted for rectifying, amplifying, oscillating or switching; Organic capacitors or resistors having potential barriers
    • H10K10/40—Organic transistors
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K10/00—Organic devices specially adapted for rectifying, amplifying, oscillating or switching; Organic capacitors or resistors having potential barriers
    • H10K10/40—Organic transistors
    • H10K10/46—Field-effect transistors, e.g. organic thin-film transistors [OTFT]
    • 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

Definitions

  • the invention belongs to the field of microelectronic devices. Specifically, a non-covalent adsorption between graphene and a polymer provides a simple and efficient method for preparing a high performance composite field effect transistor.
  • the organic-effect transistor based on conjugated polymer molecules has attracted wide attention in low-cost, flexible, large-area electrical devices such as integrated circuits, pressure sensors, organic memory components, etc.
  • the molecular chain of polymers is relatively Large, highly imaged liberalization and irregular interchain entanglement reduce their mobility and thus the electrical performance of the device.
  • the performance of polymer field effect transistors can be improved by optimizing their molecular structure, the effect is not significant.
  • molecules with high electric field mobility such as graphene, carbon nanotubes, and the like may be added thereto.
  • the valence band and the conduction band are symmetrically distributed above and below the Fermi level, and the intersection of the Dirac points coincides.
  • the transmission of electrons in the graphene follows the Dirac equation and the whole graphite.
  • Each ⁇ bond in the molecular structure of the olefin is conjugated to each other to form a large conjugated large ⁇ bond.
  • the electron or hole can move at a high electron Fermi rate in such a large conjugate system, exhibiting zero mass behavior.
  • the carrier mobility can reach 2 ⁇ 10 5 cm 2 V -1 s -1 , and it has electron conduction phenomena such as room temperature quantum echo effect and quantum tunneling effect.
  • the molecular chain of the polymer is large, the height of the conformation is liberalized, and the irregular interchain entanglement reduces the mobility, which in turn affects the electrical properties of the device.
  • the polymer molecules are adsorbed on the surface of the graphene molecules to form a polymer-graphene composite structure, and then
  • the silicon structure of the column structure can prepare a polymer-graphene composite structure nanowire with a large-area direction controllable and accurate positioning, and can be transferred to a specific substrate for device application.
  • the composite dispersion is added to a silicon wafer having a microcolumn structure and covered with a flat substrate, so that the polymer-graphene composite self-assembles into a regular one-dimensional array at the top of the microcolumn to form a polymerization.
  • Field effect transistor
  • step 2) after suction filtration, the filter residue is rinsed using the same organic solvent as in step 1), and then filtered again, and repeatedly filtered and rinsed to remove excess polymerization.
  • Object molecule the filter residue is rinsed using the same organic solvent as in step 1), and then filtered again, and repeatedly filtered and rinsed to remove excess polymerization.
  • the concentration of the polymer solution in step 1) is 0.01-0.05 Mg/mL; the mass ratio of graphene to polymer in the mixed dispersion is about 1:0.05 to 1:1.
  • the present invention is applicable to various polythiophene p-type conjugated polymers such as, but not limited to, polyalkylthiophene (P3AT); or polyacene compounds such as naphthalene and anthracene. , tetracene, pentacene, hexacene; or a conjugated system containing a hetero atom.
  • P3AT polyalkylthiophene
  • polyacene compounds such as naphthalene and anthracene.
  • tetracene pentacene, hexacene
  • conjugated system containing a hetero atom such as, but not limited to, polyalkylthiophene (P3AT)
  • P3AT polyalkylthiophene
  • acene compounds such as naphthalene and anthracene.
  • tetracene pentacene, hexacene
  • conjugated system containing a hetero atom
  • the organic solvent of the step 1) is one or more of o-dichlorobenzene, tetrahydrofuran, dichloromethane, N,N-dimethylformamide and chlorobenzene.
  • the organic solvent of the step 1) is one or more of o-dichlorobenzene, tetrahydrofuran, dichloromethane, N,N-dimethylformamide and chlorobenzene.
  • the filtration membrane of step 2) may be a cellulose acetate membrane having a pore diameter of preferably 0.2 to 0.45. Mm.
  • an alumina filter may be used, and its pore diameter is preferably 0.02 to 0.2 ⁇ m.
  • step 2) drying is to remove residual organic solvent.
  • the drying method can be in a manner well known in the art. For example, the filter residue is placed in an oven at 80-120 ° C for thorough drying.
  • the organic solvent of the step 3) is one or more of DMF, tetrahydrofuran, dichloromethane, o-dichlorobenzene, chlorobenzene and the like.
  • Step 3) The added concentration of the polymer (complex dispersion concentration) 0.01 -0.1 mg/mL.
  • the spacing between the microcolumns in step 4) is 5-20 ⁇ m
  • the width of the microcolumn (width and length of the rectangular section) is 2-10 ⁇ m.
  • step 4) is to apply a dispersion of the polymer-graphene composite to a silicon wafer having a micro-pillar structure, and to cover a layer of the substrate to form a "sandwich" assembly structure.
  • the solution forms a continuous liquid film on the surface of the microcolumn.
  • the liquid film first ruptures at the microcolumn groove, thereby forming a parallel liquid bridge between the top of the microcolumn and the substrate, and the liquid bridge Gradually shrinking, after the solvent is completely volatilized, it will be observed that the polymer-graphene compound self-assembles at the top of the silicon column to form a large-area micron-scale one-dimensional array of micrometer-scale nano-scale, realizing the polymer-graphene Patterned assembly of composite materials.
  • the flat substrate of the step 4) may use a glass substrate, ITO or a conductive silicon wafer.
  • the invention utilizes a conjugate interaction force between a polymer molecule having a benzene ring structure and a two-dimensional crystal having a large ⁇ -conjugated system such as graphene to obtain a composite structure in which a polymer molecule is adsorbed on the surface of the graphene, and then the graphite is washed away. Excess polymer molecules on the surface of the olefin ensure that there are only a few polymer molecules on the surface of the graphene.
  • Graphene molecules encapsulated by polymer molecules can be uniformly dispersed in an organic solvent, dropped on a silicon wafer with micropillars and covered with a substrate to form a "sandwich" assembly structure in a silicon column (microcolumn)
  • Auxiliary, liquid bridge induction allows the molecules to self-assemble at the top of the column, ultimately forming a regular array of nanowires that can be transferred to the desired substrate.
  • the performance of the polymer-graphene composite structure field effect transistor prepared by the invention is significantly improved compared with the simple polymer field effect transistor, and the method is simple and convenient, and the cost is low.
  • the invention saves the amount of organic matter, thereby reducing the cost, and at the same time, the directional assembly of the material improves the performance of the device. Moreover, there is a significant increase in switching ratio and electron/hole mobility.
  • FIG. 1 is a schematic view showing a method of preparing a composite field effect transistor according to the present invention
  • a is a schematic diagram of fully adsorbing the graphene powder in a dilute solution of the polymer
  • b is an optical photograph of the polymer-graphene composite after filtration on the filter
  • c is a schematic diagram of preparing a polymer-graphene composite dispersion after dispersing the composite in an organic solvent
  • d is a schematic diagram of an assembly structure in which a uniformly dispersed droplet of a polymer-graphene composite structure is applied to a silicon wafer having a microcolumn structure and covered with a layer of a substrate to form a "sandwich";
  • e is a schematic diagram of forming a continuous liquid film between the template silicon wafer and the substrate;
  • f is a schematic diagram of a liquid bridge formed at the top of the silicon column
  • g is a schematic representation of a regular nanowire array formed by self-assembly at the top of a silicon column, wherein the enlarged portion shows a layered stack configuration of the polymer-graphene composite.
  • Example 2 is a schematic view of a polymer solution according to Example 1 of the present invention; wherein a is a polymer solution, and b is a mixed dispersion obtained by adding graphene to a polymer solution.
  • Figure 3 is a polymer-graphene composite dispersion of Example 1 of the present invention.
  • FIG. 4 is a schematic view of a microcolumn according to Embodiment 1 of the present invention.
  • Example 5 is an infrared characterization diagram of a polymer molecule, a graphene, and a polymer-graphene composite according to Example 2 of the present invention.
  • Figure 6 is an optical photograph of a filtered polymer-graphene composite on a filter membrane according to Example 2 of the present invention.
  • Example 7 is a performance test curve of a polymer-graphene composite dispersion according to Example 2 of the present invention; wherein a is a transfer characteristic curve and b is an output curve.
  • Example 8 is an infrared characterization diagram of a polymer molecule, a graphene, and a polymer-graphene composite according to Example 3 of the present invention.
  • Example 9 is a performance test curve of the polymer-graphene composite dispersion of Example 3 of the present invention; wherein a is a transfer characteristic curve and b is an output curve.
  • Figure 10 is an infrared characterization diagram of a polymer molecule, graphene, polymer-graphene composite of Example 4 of the present invention.
  • Figure 11 is a performance test curve of the polymer-graphene composite dispersion of Example 4 of the present invention; wherein a is a transfer characteristic curve and b is an output curve.
  • the method controls the re-wetting of the liquid film by forming a liquid bridge between the top end of the micro-column structure of the template silicon wafer and the substrate, thereby forming a one-dimensional structure of regular arrangement.
  • the template wafer needs to be selectively modified to obtain a template wafer with asymmetric wettability: the liquid at the top of the silicon column, the side wall of the silicon column and the liquid in the trench.
  • a uniformly dispersed droplet of the polymer-graphene composite structure was applied to a silicon wafer having a microcolumn structure, and a flat substrate was covered to form a "sandwich" assembly structure (Fig. 1d). Since the top of the silicon column is liquid, the liquid first forms a continuous liquid film between the template wafer and the substrate (Fig. 1e). As the solvent gradually evaporates, the amount of liquid also decreases, and finally the liquid film ruptures and forms a plurality of regular liquid strip regions. Because of the asymmetric wetting characteristics of the template wafer, a uniform dispersion of the polymer-graphene composite structure is adhered to the top of the lyophilic portion of the silicon column and forms a regular liquid bridge at the top of the silicon column (Fig.
  • the method controls the re-wetting of the liquid film by forming a liquid bridge between the top end of the micro-column structure of the template silicon wafer and the substrate, thereby forming a one-dimensional structure of regular arrangement.
  • the template wafer needs to be selectively modified to obtain a template wafer with asymmetric wettability: the liquid at the top of the silicon column, the side wall of the silicon column and the liquid in the trench.
  • a uniformly dispersed droplet of the polymer-graphene composite structure was applied to a silicon wafer having a microcolumn structure, and a flat substrate was covered to form a "sandwich" assembly structure (Fig. 1d). Since the top of the silicon column is liquid, the liquid first forms a continuous liquid film between the template wafer and the substrate (Fig. 1e). As the solvent gradually evaporates, the amount of liquid also decreases, and finally the liquid film ruptures and forms a plurality of regular liquid strip regions. Because of the asymmetric wetting characteristics of the template wafer, a uniform dispersion of the polymer-graphene composite structure is adhered to the top of the lyophilic portion of the silicon column and forms a regular liquid bridge at the top of the silicon column (Fig.
  • the cellulose acetate membrane (pore size 0.2) ⁇ m) is subjected to suction filtration, and is repeatedly rinsed with o-dichlorobenzene and filtered to remove excess polymer molecules on the surface of graphene, ensuring that only a small number of polymer molecules are adsorbed on the surface of graphene (infrared is used to characterize the presence of polymer molecules) .
  • the obtained composite powder was sufficiently dried in an oven at 80 ° C to remove residual o-dichlorobenzene solvent, and uniformly dispersed in DMF after drying to prepare a polymer-graphene composite structure uniform dispersion (0.08 mg/mL). (Fig. 3) for the preparation of subsequent molecular devices.
  • FIG. 7 An optical photograph of the polymer-graphene complex on the filter after suction filtration is shown in FIG.
  • the obtained composite powder was sufficiently dried in an oven at 80 ° C to remove residual o-dichlorobenzene solvent, and uniformly dispersed in DMF after drying to prepare a polymer-graphene composite structure uniform dispersion (0.08 mg/mL). In order to prepare the subsequent molecular device.
  • the performance test curve is shown in Figure 7.
  • FIG. 5 illustrates that the polymer molecule CDTBTZ of the present embodiment is successfully adsorbed on the surface of graphene.
  • a is a transfer characteristic curve of a device constructed based on a polymer-graphene composite
  • Fig. 7b is an output curve.
  • Figure 7 illustrates that the polymer-graphene composite has excellent electrical properties.
  • the obtained composite powder is sufficiently dried in an oven at 120 ° C to remove the residual chlorobenzene solvent, and after drying, it can be uniformly dispersed in tetrahydrofuran to prepare a polymer-graphene composite structure uniform dispersion (0.01 mg/mL), so that Preparation of subsequent molecular devices.
  • the performance test curve is shown in Figure 9.
  • FIG. 8 illustrates that the polymer molecule P3HT is successfully adsorbed on the graphene surface.
  • Figure 9a is a transfer characteristic curve of a device constructed based on a polymer-graphene composite
  • Figure 9b is an output curve.
  • Figure 9 illustrates that the polymer-graphene composite has excellent electrical properties.
  • the obtained composite powder was sufficiently dried in an oven at 100 ° C to remove residual o-dichlorobenzene solvent, and uniformly dispersed in tetrahydrofuran after drying to prepare a polymer/graphene composite structure uniform dispersion (0.1 mg/mL). In order to prepare the subsequent molecular device.
  • the performance test curve is shown in Figure 11.
  • FIG. 10 illustrates that the polymer molecule P3HT is successfully adsorbed on the graphene surface.
  • Figure 11a is a transfer characteristic curve of a device constructed based on a polymer-graphene composite, and Figure 11b is an output curve.
  • Figure 11 illustrates that the polymer-graphene composite has excellent electrical properties.
  • the performance of the polymer-graphene composite structure field effect transistor prepared by the invention is significantly improved compared with the simple polymer field effect transistor, and the method is simple and convenient, and the cost is low.
  • the invention saves the amount of organic matter, thereby reducing the cost, and at the same time, the directional assembly of the material improves the performance of the device. Moreover, there is a significant increase in switching ratio and electron/hole mobility.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Thin Film Transistor (AREA)

Abstract

L'invention concerne un procédé de préparation d'un transistor à effet de champ composite, comprenant les étapes suivantes consistant à : 1) dissoudre des molécules de polymère dans un solvant organique pour obtenir une solution de polymère, et immerger du graphène dans la solution de polymère pour obtenir une dispersion mixte ; 2) filtrer par aspiration la dispersion mixte et la nettoyer pour obtenir un composite de graphène, le polymère étant adsorbé sur la surface de celui-ci ; 3) disperser de nouveau le composite de graphène dans le solvant organique pour obtenir une dispersion composite ; et 4) ajouter goutte à goutte la dispersion composite sur une tranche de silicium ayant une structure de microcolonne et la recouvrir avec un substrat de plaque, de telle sorte que le composite polymère-graphène s'auto-assemble en un réseau unidimensionnel régulier au niveau de la position de microcolonne sur la surface de la plaque, de manière à former un transistor à effet de champ composite. La performance du transistor à effet de champ préparé de la structure composite polymère-graphène est considérablement améliorée par rapport à celle du transistor à effet de champ avec seulement un polymère. Le procédé est simple et commode, et le coût est faible.
PCT/CN2018/072964 2017-03-28 2018-01-17 Procédé de préparation d'un transistor à effet de champ composite Ceased WO2018176995A1 (fr)

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CN201710192082.8 2017-03-28
CN201710192082.8A CN108666422B (zh) 2017-03-28 2017-03-28 一种制备复合物场效应晶体管的方法

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CN113483796A (zh) * 2021-06-15 2021-10-08 桂林理工大学 一种新型“三明治”结构柔性传感器复合膜的制备方法
CN115395351A (zh) * 2022-07-11 2022-11-25 北京仿生界面科学未来技术研究院 毛细聚集效应诱导限域重结晶制备异质图案化阵列的方法

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CN112851968A (zh) * 2021-01-11 2021-05-28 季华实验室 一种制备导电聚合物一维纳米阵列的方法
CN114808136B (zh) * 2021-01-19 2024-05-07 中国科学院理化技术研究所 一种基于液桥现象制备大面积有机单晶阵列的方法
CN116230543A (zh) * 2022-12-13 2023-06-06 北京中科纳通电子技术有限公司 一种晶体管的全印刷方法

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CN102320599A (zh) * 2011-08-02 2012-01-18 同济大学 一种纳米氧化石墨烯表面聚合物功能化的方法
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Cited By (3)

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CN113483796A (zh) * 2021-06-15 2021-10-08 桂林理工大学 一种新型“三明治”结构柔性传感器复合膜的制备方法
CN113483796B (zh) * 2021-06-15 2023-05-05 桂林理工大学 一种新型“三明治”结构柔性传感器复合膜的制备方法
CN115395351A (zh) * 2022-07-11 2022-11-25 北京仿生界面科学未来技术研究院 毛细聚集效应诱导限域重结晶制备异质图案化阵列的方法

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