CN117550801A - Lithium aluminosilicate glass and preparation method and application thereof - Google Patents
Lithium aluminosilicate glass and preparation method and application thereof Download PDFInfo
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- CN117550801A CN117550801A CN202310697841.1A CN202310697841A CN117550801A CN 117550801 A CN117550801 A CN 117550801A CN 202310697841 A CN202310697841 A CN 202310697841A CN 117550801 A CN117550801 A CN 117550801A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
- C03C14/002—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of fibres, filaments, yarns, felts or woven material
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
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Abstract
The invention discloses lithium aluminum silicon glass and a preparation method and application thereof. The preparation method of the lithium aluminum silicon glass comprises the following steps: the solution for synthesizing copper whisker forms a wire grid structure which is periodically distributed on lithium aluminum silicon base glass, and is heated and reduced under a parallel electric field. According to the method, copper whiskers are grown on the surface of base glass in situ, the adhesion force of the copper whiskers on the surface of the glass is improved by using alkali metal ion diffusion in the base glass, and the copper whiskers are aligned and orderly by combining an auxiliary electric field with a temperature field. The method can simplify the preparation process of the polarized glass and solve the problem of limited size of the polarized glass, thereby obtaining the lithium aluminum silicon-based polarized glass with large size and excellent polarization performance.
Description
Technical Field
The invention relates to the technical field of lithium aluminum silicon glass, in particular to lithium aluminum silicon glass and a preparation method and application thereof.
Background
Light can be used as an information carrier, so that the optoelectronics technology is developed, and the optoelectronics information technology is developed vigorously. Light will be the choice for technological development as a carrier of information, but it is obviously not enough to have only excellent light sources, and efficient light control means are needed. The optical polarization glass has the characteristics of compact structure, stable performance and good heat resistance, and is an important material for manufacturing components for controlling the light propagation state, and the optical polarization glass is widely applied to a plurality of fields such as optical display, optical communication, optical detection and the like. With the unprecedented development of photoelectric technology, these fields put forward requirements on polarization devices, such as excellent optical performance, low cost, large-scale production, stable physicochemical properties, etc.
Conventional polarized glass is a glass-based composite material in which long particulate metal nanoparticles are uniformly distributed in a glass matrix in an oriented arrangement. The key to affecting the polarization properties of polarized glass is the generation of long grains in the glass matrix and the directional alignment in the glass. The conventional preparation method of the optical polarization glass still takes the way of the traditional manufacturing process, and is characterized in that the melted glass containing metal elements is subjected to crystallization treatment, then is subjected to stretching or rolling treatment, and is then placed in strong reducing gas for reduction or is subjected to exposure to form the long granular metal nano structure in directional distribution.
However, the polarizing glass prepared by the process has the problem of small size, can only be applied to the fields of optical communication and the like, can not meet the use requirements in the fields of three-dimensional display screens, vehicle glare cancellers and the like, has the defects of complex process, difficult control of polarizing effect, low yield and the like, and seriously affects the wide application of the polarizing glass. Therefore, research into the preparation technology of large-sized polarizing glass is urgently required.
Disclosure of Invention
In view of the above, the main purpose of the invention is to provide a lithium aluminum silicon glass, a preparation method and application thereof, and the technical problem to be solved is to break the limit of the prior art on the size of the polarized glass, realize the production of large-size lithium aluminum silicon-based polarized glass with the size of more than a meter, and simultaneously maintain excellent optical performance, thereby meeting the requirements of industry development on the polarization performance of the glass.
The aim of the invention and the solution of the technical problems are achieved by adopting the following technical proposal. The preparation method of the lithium aluminum silicon glass provided by the invention comprises the following steps:
the solution for synthesizing the copper whisker forms a wire grid structure which is periodically distributed on lithium aluminum silicon base glass, and the lithium aluminum silicon base glass is obtained by heating and reducing the solution under a parallel electric field.
The aim and the technical problems of the invention can be further realized by adopting the following technical measures.
Preferably, the preparation method of the lithium aluminum silicon glass comprises the following steps:
1) Preparing the solution for synthesizing the copper whisker by a soft template method;
2) Arranging a wire grid die on the surface of the lithium aluminum silicon base glass;
3) Coating the solution on the surface of glass provided with the wire grid die;
4) Heating the glass obtained in the step 3) in an oven with the parallel electric field;
5) And (3) placing the glass obtained in the step (4) in a reducing atmosphere for reduction to obtain the lithium aluminum silicon glass.
Preferably, in the foregoing method for preparing lithium aluminum silicon glass, in the step 2), the lithium aluminum silicon base glass contains alkali metal ions, and the content of the alkali metal ions is 5 to 20wt% based on the total weight of the lithium aluminum silicon base glass.
Preferably, in the foregoing method for preparing lithium aluminum silicate glass, in the step 2), the alkali metal ion includes Li + 。
Preferably, the preparation of the lithium aluminum silicon glassThe method, wherein in the step 2), the alkali metal ions further comprise Na + 、K + At least one of them.
Preferably, in the foregoing method for preparing lithium aluminosilicate glass, in the step 2), the period of the wire grid mold is 100-500nm, and the width is 100-300nm.
Preferably, in the method for preparing lithium aluminum silicon glass, in step 4), the parallel electric field is an electrostatic field parallel to a surface of the glass.
Preferably, in the above preparation method of lithium aluminum silicon glass, in the step 4), the electrostatic field intensity of the parallel electric field loading is 500-800V/mm, and the time is 30-60min.
Preferably, in the foregoing method for preparing lithium aluminum silicon glass, in the step 4), the heating temperature is 200-300 ℃ and the time is 30-60min.
Preferably, in the foregoing method for preparing lithium aluminosilicate glass, in step 5), the reducing atmosphere is at least one gas selected from hydrogen and carbon monoxide or a mixed gas of the hydrogen and carbon monoxide with an inert gas.
Preferably, in the method for preparing lithium aluminum silicon glass, in the step 5), the pressure of the gas is 0.3-1.0Mpa, and the time of the reduction is 3-6h.
The aim of the invention and the technical problems are also achieved by adopting the following technical proposal. According to the invention, a lithium aluminum silicon glass comprises:
lithium aluminum silicon base glass; and
copper whiskers grown on the lithium aluminum silicon base glass, the copper whiskers having a periodically distributed wire grid structure.
The aim and the technical problems of the invention can be further realized by adopting the following technical measures.
Preferably, the aforementioned lithium aluminosilicate glass, wherein the lithium aluminosilicate glass is prepared by any one of the methods described above.
Preferably, the aforementioned lithium aluminum silicate glass, wherein the length and width of the lithium aluminum silicate glass are independently 1mm or more.
Preferably, the aforementioned lithium aluminum silicate glass, wherein the extinction ratio of the lithium aluminum silicate glass is 60dB or more, and the transmittance of the lithium aluminum silicate glass for light in the wavelength range of 190-1100nm is 76% or more.
The aim of the invention and the technical problems are also achieved by adopting the following technical proposal. According to the invention, the polarizing device comprises a polarizer, an analyzer or an attenuator, wherein the polarizer, the analyzer or the attenuator comprises any one of the lithium aluminum silicon glass.
The aim and the technical problems of the invention can be further realized by adopting the following technical measures.
Preferably, the polarizing device is an optical isolator, an optical disk signal detection sensor, an optical voltage sensor, an optical fiber connector or a liquid crystal display.
By means of the technical scheme, the lithium aluminum silicon glass and the preparation method and application thereof have at least the following beneficial effects:
the preparation method of the lithium aluminum silicon glass comprises the steps of firstly preparing a solution for synthesizing copper whiskers, then coating the solution on the surface of glass with a wire grid die, loading a parallel electric field and a temperature field, and carrying out in-situ growth and directional arrangement of the copper whiskers on the surface of the glass after reduction, thereby greatly simplifying the subsequent treatment process of basic glass, effectively reducing the complexity of preparation, avoiding the difficulties in the high-temperature stretching process of the glass and shortening the time consumption of the process. And, alkali metal ions (e.g., li + 、Na + 、K + ) Can diffuse into copper whisker to anchor the whisker on the glass surface and improve the adhesive force of the copper whisker on the glass surface, thereby realizing the preparation of the lithium aluminum silicon-based polarized glass with controllable polarization performance under the low temperature condition. In addition, by introducing the metallic copper element in directional arrangement on the lithium aluminum silicon base glass through in-situ growth, the problem of turbidity or coloration of the base glass caused by introducing the metallic copper element in the process of preparing the base glass can be avoided. In particular, the method can solve the difficult problem of small preparation size of the traditional polarized glass, and can obtain large-size and high-polarizationThe application field of the lithium aluminum silicon glass is greatly expanded by the vibratile lithium aluminum silicon glass.
According to the preparation method of the lithium aluminum silicon glass, a soft template method can be adopted to prepare a solution for synthesizing the copper whisker so as to grow the copper whisker on the surface of the glass in situ, so that the length-diameter ratio of the copper whisker can be adjusted by controlling the solution proportion, and the copper whisker can show selective absorption on light waves vibrating in different directions by utilizing plasma resonance absorption, wherein the light waves vibrating in the direction parallel to the long axis are absorbed by metal particles, and the light waves vibrating in the direction perpendicular to the long axis are weaker in absorption.
The preparation method of the lithium aluminum silicon glass can add an electrostatic field in the process of growing copper whiskers, and compared with a temperature field, the control of the electrostatic field loading intensity and time is easier and more accurate, so that the arrangement of the copper whiskers on the surface of the glass can be controlled by using the loading electrostatic field under the action of an auxiliary electric field parallel to the surface of the glass, the ordered chain-shaped directional arrangement structure is formed along the direction of the electric field, and the size of the chain-shaped arrangement structure is adjusted by controlling the intensity of the electric field and the loading time, so that the high order degree is realized, and the lithium aluminum silicon-based polarized glass with high extinction ratio is obtained.
The lithium aluminum silicon glass provided by the invention has the advantages that the size is not limited by the conventional polarized glass manufacturing process, the size can be controllably realized in a wide range from a few millimeters to hundreds of meters, the extinction ratio can reach more than 60dB, and the transmittance of light with the wavelength within the range of 190-1100nm can reach more than 76%.
The foregoing description is only an overview of the present invention, and is intended to provide a more clear understanding of the technical means of the present invention, and is to be implemented in accordance with the teachings of the present invention, as set forth in detail in the following description of the preferred embodiments of the present invention.
Detailed Description
In order to further describe the technical means and effects adopted for achieving the preset aim of the present invention, the following describes the specific implementation, structure, characteristics and effects of the polarizing glass and the preparation method and application thereof according to the present invention in detail with reference to the preferred embodiments. In the following description, reference to "an embodiment" or "an embodiment" does not necessarily refer to the same embodiment. Furthermore, the particular features, structures, or characteristics of one or more embodiments may be combined in any suitable manner.
In the examples of the present invention, unless otherwise specified, materials, reagents, etc. are commercially available products well known to those skilled in the art; unless otherwise indicated, all methods referred to are known in the art. Unless defined otherwise, technical or scientific terms used should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs.
The invention provides a preparation method of lithium aluminum silicon glass, which comprises the following steps:
the solution for synthesizing the copper whisker forms a wire grid structure which is periodically distributed on lithium aluminum silicon base glass, and the lithium aluminum silicon base glass is obtained by heating and reducing the solution under a parallel electric field.
In the prior art, metal elements are introduced into glass components in advance for preparing polarized glass, crystallization heat treatment is carried out after fusion forming, and finally, a directional arrangement structure containing rod-shaped silver nano particles is formed through a drawing process. However, in the silver-containing polarized glass drawn by the technology, the problems of uneven distribution of silver colloidal particles, difficult regulation and control of the particle size ratio, wide range and the like exist, so that the extinction ratio of the glass is low, the polarization performance is poor, the subsequent treatment process consumes long time and energy consumption is large; at the same time, the glass produced is small in size, typically on the order of millimeters only. In view of this, the invention grows copper whisker on the base glass without introducing metal element in advance by soft template method, etc., so that the glass has plasma oscillation absorption effect, and the lithium aluminum silicon base glass contains alkali metal, and since alkali metal ion is very active, it is easy to move, so it can diffuse into copper whisker and fill into the gap of copper structure, so that the binding force between copper whisker and glass surface is improved, thus solving the problem of insufficient adhesion of whisker on glass surface. Meanwhile, the preparation process does not need a drawing process, and the glass size is not limited, so that the rice-grade polarized glass can be prepared under the low-temperature condition, the preparation problem of large-size and high-polarization-performance lithium aluminum silicon glass is solved, and the requirements of industry development on the polarization performance of the glass can be met.
In some embodiments, the method comprises the steps of:
1) Preparing the solution for synthesizing the copper whisker by a soft template method;
2) Arranging a wire grid die on the surface of the lithium aluminum silicon base glass;
3) Coating the solution on the surface of glass provided with the wire grid die;
4) Heating the glass obtained in the step 3) in an oven with the parallel electric field;
5) And (3) placing the glass obtained in the step (4) in a reducing atmosphere for reduction to obtain the lithium aluminum silicon glass.
In step 1) of some embodiments, the solution for synthesizing copper whiskers is formulated by a soft template method. The soft template method can be implemented by the following steps: 1) Dissolving 50-75g of copper sulfate, 100g of sodium hydroxide and 50g of polyvinylpyrrolidone in 100ml of a mixed solvent of deionized water and ethanol, and carrying out ultrasonic treatment for 10-15min; 2) Adding 1-50g of surfactant cetyl trimethyl ammonium bromide, and stirring for 30-60min; 3) Adding 40-80ml of hydrazine hydrate, and continuously stirring for 30min to obtain a solution for synthesizing copper whiskers. In addition to the above-described method, the solution for synthesizing copper whiskers according to the present invention may be prepared by other methods as long as a copper whisker precursor solution suitable for the subsequent step of the method according to the present invention can be prepared, which is not particularly limited by the present invention.
In step 2) of some embodiments, the lithium aluminum silicon base glass comprises alkali metal ions including Li + And may also include Na + 、K + At least one of them. In the method according to the invention, alkali metal ions (e.g. Li + 、Na + 、K + ) And the copper whisker is diffused into the copper whisker under a proper temperature field, so that the copper whisker is anchored on the surface of the glass, and the adhesion of the copper whisker on the surface of the glass is improved. The alkali metal ion content is 5-20wt%, based on the total weight of the lithium aluminum silicon base glass. If it isThe content of alkali metal ions is lower than 5wt%, so that the anchoring effect of the alkali metal ions on the copper whisker is not obvious, and the expected adhesive force improving effect cannot be achieved; if the content of the alkali metal ion is more than 20wt%, the thermal expansion coefficient of the glass is increased, and the thermal stability, chemical stability and mechanical strength of the glass are lowered. In this regard, the alkali ion content ranges described herein may be applicable to existing lithium aluminum silicate glass compositions. Thus, the method of the present invention can be realized skillfully using known conventional lithium aluminum silicate glasses without particularly changing the alkali metal ion content of the glass.
In step 2) of some embodiments, the alkali metal ion further comprises Na + 、K + At least one of them. When 2 or 3 alkali metals are added into the glass, a mixed alkali effect is generated, and the mixed alkali effect is used for reducing the thermal expansion coefficient of the glass and improving the chemical stability.
In step 2) of some embodiments, the wire grid mold has a period of 100-500nm and a width of 100-300nm. The wire grid mold is arranged to enable the copper whiskers to grow on the surface of glass to form a periodically distributed copper whisker body wire grid. Because copper is a metal material with higher light activity, when light irradiates on a copper whisker wire grid, electrons in the wire grid can only move along the whisker direction, the vibration direction of the light wave electric vector is parallel to the whisker direction and can be absorbed by electrons in the wire grid whisker, and the vibration direction of the light wave electric vector is perpendicular to the whisker direction and can penetrate lithium aluminum silicon glass. If the period of the wire grid mold is more than 500nm or the width is less than 100nm, the formed copper whisker wire grid is too thin, and the polarization performance is low; if the period of the wire grid mold is smaller than 100nm or the width is larger than 300nm, the formed copper whisker wire grid is too dense, and the light transmission performance of the glass is affected.
In step 2) of some embodiments, the wire grid mold is covered on the surface of the lithium aluminum silicon base glass.
In step 4) of some embodiments, the parallel electric field is an electrostatic field parallel to the surface of the glass, the parallel electric field is loaded with an electrostatic field strength of 500-800V/mm for 30-60min. Under the action of electrostatic field parallel to glass surface, the direction of copper whisker growth and arrangement on glass surface is controlled by using the loaded electrostatic field. If the electrostatic field strength is lower than 500V/mm, the copper whiskers in the glass cannot be arranged along the electric field direction; if the electrostatic field strength is higher than 800V/mm, copper whiskers in the glass are agglomerated rather than orderly arranged, so that the polarization effect cannot be realized. If the loading time is less than 30min, the copper whiskers are not sufficiently aligned; if the loading time is longer than 60min, the copper whisker is arranged completely, and energy waste can be caused by continuously increasing the time.
In step 4) of some embodiments, the heating is at a temperature of 200-300 ℃ for a time of 30-60 minutes. The heating is performed to promote the formation of copper whiskers and to remove ethanol from the solution so that the copper whiskers can be immobilized on the glass surface. If the heating temperature is lower than 200 ℃, the growth of copper whisker cannot be promoted at too low a temperature, and the volatilization rate of ethanol is too slow, and at the same time, alkali metal ions (Li + 、Na + And K + ) Difficult to diffuse into copper whiskers; if the heating temperature is higher than 300 ℃, the copper whisker grows too fast to influence the expected length-diameter ratio, and alkali metal ions diffuse too fast to influence the plasma oscillation effect of the copper whisker. If the heating time is less than 30min, the copper whisker is not grown completely, the ethanol is not removed completely, and the diffusion of alkali metal ions is insufficient; if the heating time is more than 60 minutes, the reaction is completed, and the energy waste is caused by continuously increasing the time.
In step 4) of some embodiments, the oven is a vacuum oven.
In step 5) of some embodiments, the reducing atmosphere is derived from at least one gas of hydrogen, carbon monoxide or a mixture thereof with an inert gas, the pressure of the gas being in the range of 0.3 to 1.0Mpa, the time of the reduction being in the range of 3 to 6 hours. The whiskers synthesized by, for example, a soft template method are cuprous oxide whiskers, which are reduced to copper whiskers using a reducing gas. If the gas pressure is less than 0.3MPa, the reduction reaction is performed to a low degree, and the number of generated copper whiskers is small; if the gas pressure is higher than 1.0MPa, the reduction reaction speed is too high, the copper whisker grows too fast, the reduction quality of the copper whisker is affected, the equipment requirement is increased, and the preparation cost is increased. If the reduction time is less than 3 hours, the reduction of the copper whisker is incomplete; if the reduction time is more than 6 hours, the reaction is already completed, and further increase in time leads to a decrease in efficiency.
The invention also provides lithium aluminum silicon glass, which comprises lithium aluminum silicon base glass and copper whiskers growing on the lithium aluminum silicon base glass, wherein the copper whiskers have a periodically distributed wire grid structure.
In some embodiments, the lithium aluminum silicate glass is prepared by any of the methods described above.
In some embodiments, the lithium aluminum silicate glass has a extinction ratio of 60dB or greater and a transmittance of 76% or greater for light in the wavelength range of 190-1100 nm.
As described above, the method for preparing lithium aluminum silicon glass according to the present invention is performed by in-situ directional growth of copper whiskers on the surface of lithium aluminum silicon base glass, and thus the lithium aluminum silicon glass prepared by the method is not limited by the size of glass by conventional polarizing glass preparation processes. In other words, by allowing the use of ready-made base glass, the lithium aluminosilicate glass produced by the method of the invention can reach dimensions comparable to those of the base glass, i.e. it is possible to achieve the controlled production of polarizing glasses ranging from millimeter to meter or even from hundred meter dimensions.
Thus, the length and width of the lithium aluminosilicate glass of the invention can be independently controllably adjusted, for example, in the range of 0.1-100000 mm. For example, upper limit values for the length and width of the lithium aluminum silicate glass include, but are not limited to 100000mm, 80000mm, 50000mm, 30000mm, 10000mm, 8000mm, 5000mm, 3000mm, 1000mm, 800mm, 500mm, 300mm, 100mm, 80mm, 50mm, 30mm, 10mm, 8mm, 5mm, 3mm, 1mm, 0.8mm, 0.5mm, and 0.3mm; lower limits for the length and width of the lithium aluminosilicate glass include, but are not limited to, 80000mm, 50000mm, 30000mm, 10000mm, 8000mm, 5000mm, 3000mm, 1000mm, 800mm, 500mm, 300mm, 100mm, 80mm, 50mm, 30mm, 10mm, 8mm, 5mm, 3mm, 1mm, 0.8mm, 0.5mm, 0.3mm, and 0.1mm.
In addition, the thickness of the lithium aluminosilicate glass can be controllably adjusted in the range of, for example, 15-60 mm. For example, upper limit values for the thickness of the lithium aluminosilicate glass include, but are not limited to, 60mm, 55mm, 50mm, 45mm, 40mm, 35mm, 30mm, 25mm, and 20mm; lower limits of the thickness of the lithium aluminosilicate glass include, but are not limited to, 55mm, 50mm, 45mm, 40mm, 35mm, 30mm, 25mm, 20mm, and 15mm.
In some embodiments, the length and width of the lithium aluminum silicate glass are independently 1mm or more.
In some specific embodiments, the lithium aluminum silicate glass has dimensions such as 1500mm length by 1500mm width by (25-50) mm thickness.
The invention also provides a polarizing device, which comprises a polarizer, an analyzer or an attenuator, wherein the polarizer, the analyzer or the attenuator comprises any one of the lithium aluminum silicon glass.
In some embodiments, the polarizing device is an opto-isolator, an opto-magnetic disk signal detection sensor, an opto-voltage sensor, a fiber optic connector, a liquid crystal display, or the like. The optical isolator can be used in the fields of optical fiber communication, optical fiber sensing systems and the like; the photovoltage sensor can be used in the fields of electric energy metering and relay protection in an electric power system; the magneto-optical disk signal detection sensor can be used in the field of high-voltage high-current measurement or electronic anti-theft detectors in an electric power system.
The invention will be further described in connection with specific examples which are not to be construed as limiting the scope of the invention. Some insubstantial modifications and adaptations of the invention as described above would be within the scope of the invention.
Extinction ratio test: the semiconductor laser fiber collimator of each wavelength was made into parallel light, which was vertically incident on the lithium aluminum silicon-based polarizing glass prepared in each of the following examples via a phase compensator and a gram-thompson prism, and the lithium aluminum silicon-based polarizing glass was rotated in a plane perpendicular to the optical axis. First, the minimum transmitted light quantity P is measured 1 Then the lithium aluminum silicon-based polarized glass is rotated by 90 degrees to determine the maximum transmitted light quantity P 2 Calculating the extinction ratio by using the formula: extinction methodRatio (dB) = -10Log (P 1 /P 2 )。
Transmittance test: and testing the luminous flux or the light energy of the incident light after passing through the object, and comparing the test value with the total luminous flux or the light energy of the incident light, thereby obtaining the transmittance of the object. Firstly, directly testing the luminous flux or the light energy of incident light without passing through a sample to obtain reference illumination data; and then testing the luminous flux or the light energy of the incident light after passing through the object to obtain test illumination data. Specifically, incident light was irradiated onto the lithium aluminum silicon based polarizing glass prepared in each example covering the light inlet, light transmitted through each lithium aluminum silicon based polarizing glass was collected, and then entered into the detector through the detection port, and outgoing light data was detected using the detector, wherein the wavelength of the incident light for the test was in the range of 190-1100 nm.
The lithium aluminum silicon base glass used in each of the following examples and comparative examples had the following chemical composition: 62wt% SiO 2 15wt% of Al 2 O 3 10wt% of Li 2 O,5wt% of B 2 O 3 4wt% Na 2 O,3wt% ZnO 2 And 1wt% of Sb 2 O 3 。
Example 1
Weighing copper sulfate, sodium hydroxide and polyvinylpyrrolidone, wherein the mass ratio of the copper sulfate to the sodium hydroxide is 50g to 100g to 50g, dissolving the copper sulfate, the sodium hydroxide and the polyvinylpyrrolidone in 100ml of deionized water/ethanol mixed solvent (50:50), and carrying out ultrasonic treatment for 10min; 20g of cetyltrimethylammonium bromide was added and stirred for 30min; then 40ml of hydrazine hydrate is added and stirred for 30min to prepare a solution for synthesizing copper whiskers. And attaching a wire grid die with the period of 100nm and the width of 300nm on the surface of lithium aluminum silicon base glass, coating the prepared solution on the surface of the lithium aluminum silicon base glass with the wire grid die, then placing the glass in an oven with the parallel electric field intensity of 500V/mm, heating for 30min at 200 ℃, and finally reducing for 3h in a hydrogen atmosphere with the gas pressure of 0.3MPa to obtain the lithium aluminum silicon base polarized glass. The test shows that the prepared lithium aluminum silicon-based polarized glass has the dimensions of 1500mm long by 1500mm wide by 25mm thick, the extinction ratio of 62dB and the light transmittance of 78% in the wavelength range of 190-1100 nm. The prepared lithium aluminum silicon-based polarized glass can be used for a polarizer, an analyzer or an attenuator of an optical isolator.
Example 2
Weighing copper sulfate, sodium hydroxide and polyvinylpyrrolidone, wherein the mass ratio of the copper sulfate to the sodium hydroxide is 75g to 100g to 50g, dissolving the copper sulfate, the sodium hydroxide and the polyvinylpyrrolidone in 100ml of deionized water/ethanol mixed solvent (50 to 50), and carrying out ultrasonic treatment for 10min; 20g of cetyltrimethylammonium bromide was added and stirred for 30min; then 40ml of hydrazine hydrate is added and stirred for 30min to prepare a solution for synthesizing copper whiskers. And attaching a wire grid die with the period of 100nm and the width of 300nm on the surface of lithium aluminum silicon base glass, coating the prepared solution on the surface of the lithium aluminum silicon base glass with the wire grid die, then placing the glass in an oven with the parallel electric field intensity of 500V/mm, heating for 30min at 200 ℃, and finally reducing for 3h in a hydrogen atmosphere with the gas pressure of 0.3MPa to obtain the lithium aluminum silicon base polarized glass. The test shows that the prepared lithium aluminum silicon-based polarized glass has the dimensions of 1500mm long by 1500mm wide by 25mm thick, the extinction ratio of 64dB and the light transmittance of 78% in the wavelength range of 190-1100 nm. The prepared lithium aluminum silicon-based polarized glass can be used for a polarizer, an analyzer or an attenuator of an optical isolator.
Example 3
Weighing copper sulfate, sodium hydroxide and polyvinylpyrrolidone, wherein the mass ratio of the copper sulfate to the sodium hydroxide is 50g to 100g to 50g, dissolving the copper sulfate, the sodium hydroxide and the polyvinylpyrrolidone in 100ml of deionized water/ethanol mixed solvent (50:50), and carrying out ultrasonic treatment for 10min; 20g of cetyltrimethylammonium bromide was added and stirred for 30min; then 40ml of hydrazine hydrate is added and stirred for 30min to prepare a solution for synthesizing copper whiskers. And attaching a wire grid die with the period of 500nm and the width of 300nm on the surface of lithium aluminum silicon base glass, coating the prepared solution on the surface of the lithium aluminum silicon base glass with the wire grid die, then placing the glass in an oven with the parallel electric field intensity of 500V/mm, heating for 30min at 200 ℃, and finally reducing for 3h in a hydrogen atmosphere with the gas pressure of 0.3MPa to obtain the lithium aluminum silicon base polarized glass. The test shows that the prepared lithium aluminum silicon-based polarized glass has the dimensions of 1500mm long by 1500mm wide by 25mm thick, the extinction ratio of 61dB and the light transmittance of 79% in the wavelength range of 190-1100 nm. The prepared lithium aluminum silicon-based polarized glass can be used for a polarizer, an analyzer or an attenuator of an optical isolator.
Example 4
Weighing copper sulfate, sodium hydroxide and polyvinylpyrrolidone, wherein the mass ratio of the copper sulfate to the sodium hydroxide is 50g to 100g to 50g, dissolving the copper sulfate, the sodium hydroxide and the polyvinylpyrrolidone in 100ml of deionized water/ethanol mixed solvent (50:50), and carrying out ultrasonic treatment for 10min; 20g of cetyltrimethylammonium bromide was added and stirred for 30min; then 40ml of hydrazine hydrate is added and stirred for 30min to prepare a solution for synthesizing copper whiskers. And attaching a wire grid die with the period of 100nm and the width of 100nm on the surface of lithium aluminum silicon base glass, coating the prepared solution on the surface of the lithium aluminum silicon base glass with the wire grid die, then placing the glass in an oven with the parallel electric field intensity of 500V/mm, heating for 30min at 300 ℃, and finally reducing for 3h in a hydrogen atmosphere with the gas pressure of 0.3MPa to obtain the lithium aluminum silicon base polarized glass. The test shows that the prepared lithium aluminum silicon-based polarized glass has the dimensions of 1500mm long by 1500mm wide by 25mm thick, the extinction ratio of 60dB and the light transmittance of 79% in the wavelength range of 190-1100 nm. The prepared lithium aluminum silicon-based polarized glass can be used for a polarizer, an analyzer or an attenuator of an optical isolator.
Example 5
Weighing copper sulfate, sodium hydroxide and polyvinylpyrrolidone, wherein the mass ratio of the copper sulfate to the sodium hydroxide is 50g to 100g to 50g, dissolving the copper sulfate, the sodium hydroxide and the polyvinylpyrrolidone in 100ml of deionized water/ethanol mixed solvent (50:50), and carrying out ultrasonic treatment for 10min; 20g of cetyltrimethylammonium bromide was added and stirred for 30min; then 40ml of hydrazine hydrate is added and stirred for 30min to prepare a solution for synthesizing copper whiskers. And attaching a wire grid die with a period of 100nm and a width of 300nm on the surface of the lithium aluminum silicon base glass, coating the prepared solution on the surface of the lithium aluminum silicon base glass with the wire grid die, then placing the glass in an oven with a parallel electric field intensity of 800V/mm, heating at 300 ℃ for 30min, and finally reducing for 3h in a hydrogen atmosphere with a gas pressure of 0.3MPa to obtain the lithium aluminum silicon base polarized glass. The test shows that the prepared lithium aluminum silicon-based polarized glass has the dimensions of 1500mm long by 1500mm wide by 25mm thick, the extinction ratio of 66dB and the light transmittance of 78% in the wavelength range of 190-1100 nm. The prepared lithium aluminum silicon-based polarized glass can be used for a polarizer, an analyzer or an attenuator of an optical isolator.
Example 6
Weighing copper sulfate, sodium hydroxide and polyvinylpyrrolidone, wherein the mass ratio of the copper sulfate to the sodium hydroxide is 50g to 100g to 50g, dissolving the copper sulfate, the sodium hydroxide and the polyvinylpyrrolidone in 100ml of deionized water/ethanol mixed solvent (50:50), and carrying out ultrasonic treatment for 10min; 20g of cetyltrimethylammonium bromide was added and stirred for 30min; then 40ml of hydrazine hydrate is added and stirred for 30min to prepare a solution for synthesizing copper whiskers. And attaching a wire grid die with the period of 100nm and the width of 300nm on the surface of lithium aluminum silicon base glass, coating the prepared solution on the surface of the lithium aluminum silicon base glass with the wire grid die, then placing the glass in an oven with the parallel electric field intensity of 500V/mm, heating at 300 ℃ for 60min, and finally reducing for 3h in a hydrogen atmosphere with the gas pressure of 0.3MPa to obtain the lithium aluminum silicon base polarized glass. The test shows that the prepared lithium aluminum silicon-based polarized glass has the dimensions of 1500mm long by 1500mm wide by 25mm thick, the extinction ratio of 67dB and the light transmittance of 77% in the wavelength range of 190-1100 nm. The prepared lithium aluminum silicon-based polarized glass can be used for a polarizer, an analyzer or an attenuator of an optical isolator.
Example 7
Weighing copper sulfate, sodium hydroxide and polyvinylpyrrolidone, wherein the mass ratio of the copper sulfate to the sodium hydroxide is 50g to 100g to 50g, dissolving the copper sulfate, the sodium hydroxide and the polyvinylpyrrolidone in 100ml of deionized water/ethanol mixed solvent (50:50), and carrying out ultrasonic treatment for 10min; 20g of cetyltrimethylammonium bromide was added and stirred for 30min; then 40ml of hydrazine hydrate is added and stirred for 30min to prepare a solution for synthesizing copper whiskers. And attaching a wire grid die with a period of 100nm and a width of 300nm on the surface of the lithium aluminum silicon base glass, coating the prepared solution on the surface of the lithium aluminum silicon base glass with the wire grid die, then placing the glass in an oven with a parallel electric field intensity of 500V/mm, heating for 30min at 300 ℃, and finally reducing for 3h in a hydrogen atmosphere with a gas pressure of 1.0MPa to obtain the lithium aluminum silicon base polarized glass. The test shows that the prepared lithium aluminum silicon-based polarized glass has the dimensions of 1500mm long by 1500mm wide by 25mm thick, the extinction ratio of 64dB and the light transmittance of 80% in the wavelength range of 190-1100 nm. The prepared lithium aluminum silicon-based polarized glass can be used for a polarizer, an analyzer or an attenuator of an optical isolator.
Example 8
Weighing copper sulfate, sodium hydroxide and polyvinylpyrrolidone, wherein the mass ratio of the copper sulfate to the sodium hydroxide is 50g to 100g to 50g, dissolving the copper sulfate, the sodium hydroxide and the polyvinylpyrrolidone in 100ml of deionized water/ethanol mixed solvent (50:50), and carrying out ultrasonic treatment for 10min; 20g of cetyltrimethylammonium bromide was added and stirred for 30min; then 40ml of hydrazine hydrate is added and stirred for 30min to prepare a solution for synthesizing copper whiskers. And attaching a wire grid die with a period of 100nm and a width of 300nm on the surface of the lithium aluminum silicon base glass, coating the prepared solution on the surface of the lithium aluminum silicon base glass with the wire grid die, then placing the glass in an oven with a parallel electric field intensity of 500V/mm, heating for 30min at 300 ℃, and finally reducing for 6h in a hydrogen atmosphere with a gas pressure of 1.0MPa to obtain the lithium aluminum silicon base polarized glass. The test shows that the prepared lithium aluminum silicon-based polarized glass has the dimensions of 1500mm long by 1500mm wide by 25mm thick, the extinction ratio of 64dB and the light transmittance of 78% in the wavelength range of 190-1100 nm. The prepared lithium aluminum silicon-based polarized glass can be used for a polarizer, an analyzer or an attenuator of an optical isolator.
Example 9
Weighing copper sulfate, sodium hydroxide and polyvinylpyrrolidone, wherein the mass ratio of the copper sulfate to the sodium hydroxide is 50g to 100g to 50g, dissolving the copper sulfate, the sodium hydroxide and the polyvinylpyrrolidone in 100ml of deionized water/ethanol mixed solvent (50:50), and carrying out ultrasonic treatment for 10min; 20g of cetyltrimethylammonium bromide was added and stirred for 30min; then 40ml of hydrazine hydrate is added and stirred for 30min to prepare a solution for synthesizing copper whiskers. And attaching a wire grid die with a period of 100nm and a width of 300nm on the surface of the lithium aluminum silicon base glass, coating the prepared solution on the surface of the lithium aluminum silicon base glass with the wire grid die, then placing the glass in an oven with a parallel electric field intensity of 500V/mm, heating for 30min at 300 ℃, and finally reducing for 6h in a hydrogen atmosphere with a gas pressure of 0.3MPa to obtain the lithium aluminum silicon base polarized glass. The test shows that the prepared lithium aluminum silicon-based polarized glass has the dimensions of 1500mm long by 1500mm wide by 25mm thick, the extinction ratio of 63dB and the light transmittance of 79% in the wavelength range of 190-1100 nm. The prepared lithium aluminum silicon-based polarized glass can be used for a polarizer, an analyzer or an attenuator of an optical isolator.
Example 10
Weighing copper sulfate, sodium hydroxide and polyvinylpyrrolidone, wherein the mass ratio of the copper sulfate to the sodium hydroxide is 50g to 100g to 50g, dissolving the copper sulfate, the sodium hydroxide and the polyvinylpyrrolidone in 100ml of deionized water/ethanol mixed solvent (50:50), and carrying out ultrasonic treatment for 10min; 20g of cetyltrimethylammonium bromide was added and stirred for 30min; then 40ml of hydrazine hydrate is added and stirred for 30min to prepare a solution for synthesizing copper whiskers. And attaching a wire grid die with a period of 100nm and a width of 300nm on the surface of the lithium aluminum silicon base glass, coating the prepared solution on the surface of the lithium aluminum silicon base glass with the wire grid die, then placing the glass in an oven with a parallel electric field intensity of 500V/mm, heating for 30min at 300 ℃, and finally reducing for 3h in a hydrogen atmosphere with a gas pressure of 0.3MPa to obtain the lithium aluminum silicon base polarized glass. The test shows that the prepared lithium aluminum silicon-based polarized glass has the dimensions of 1500mm long by 1500mm wide by 50mm thick, the extinction ratio of 64dB and the light transmittance of 76% in the wavelength range of 190-1100 nm. The prepared lithium aluminum silicon-based polarized glass can be used for a polarizer, an analyzer or an attenuator of an optical isolator.
Comparative example 1
This comparative example differs from example 1 in that: the lithium aluminum silicon base glass was not attached with a wire grid mold, and the rest was the same as in example 1. The test shows that the prepared lithium aluminum silicon-based glass has the dimensions of 1500mm long by 1500mm wide by 25mm thick, the extinction ratio of 19dB and the light transmittance of 68% in the wavelength range of 190-1100 nm.
Comparative example 2
This comparative example differs from example 1 in that: no parallel electric field was applied, and the rest was the same as in example 1. The test shows that the prepared lithium aluminum silicon-based glass has the dimensions of 1500mm long by 1500mm wide by 25mm thick, the extinction ratio of 13dB and the light transmittance of 70% in the wavelength range of 190-1100 nm.
Comparative example 3
This comparative example differs from example 1 in that: the heating treatment was not performed, and the rest was the same as in example 1. The test shows that the prepared lithium aluminum silicon-based glass has the dimensions of 1500mm long by 1500mm wide by 25mm thick, the extinction ratio of 31dB and the light transmittance of 71% in the wavelength range of 190-1100 nm.
Comparative example 4
This comparative example differs from example 1 in that: the reduction treatment was not performed, and the rest was the same as in example 1. The test shows that the prepared lithium aluminum silicon-based glass has the dimensions of 1500mm long by 1500mm wide by 25mm thick, the extinction ratio of 34dB and the light transmittance of 72% in the wavelength range of 190-1100 nm.
As can be seen from the test data of the above examples 1 to 10, the size of the lithium aluminum silicon-based polarized glass prepared by the method of the invention can reach 1500mm in length, 1500mm in width and 20-50 mm in thickness, the extinction ratio can reach more than 60dB, and the light transmittance in the wavelength range of 190-1100nm can reach more than 76%.
As is clear from the test data of the above comparative examples 1 to 4, comparative example 1 was not attached with a wire grid mold, and the extinction ratio of the prepared lithium aluminum silicon-based glass was 19dB, and the light transmittance in the wavelength range of 190-1100nm was 68%. In comparative example 2, the extinction ratio of the prepared lithium aluminum silicon-based glass was 13dB, and the light transmittance in the wavelength range of 190-1100nm was 70%. In comparative example 3, the extinction ratio of the prepared lithium aluminum silicon-based glass was 31dB and the light transmittance in the wavelength range of 190-1100nm was 71%. The lithium aluminum silicon-based glass prepared in comparative example 4 was not subjected to reduction treatment, and had a extinction ratio of 34dB and a light transmittance of 72% in the wavelength range of 190-1100 nm.
In comparison with the above comparative examples, in the examples of the present invention (e.g., example 1), after a solution for synthesizing copper whiskers was coated on a lithium aluminum silicon base glass provided with a wire grid mold, a lithium aluminum silicon base polarizing glass was prepared by a synergistic effect of heating, an auxiliary electric field and a reduction compounding process. The extinction ratio of the prepared lithium aluminum silicon-based polarized glass is 62dB, the light transmittance in the wavelength range of 190-1100nm is 78%, and the optical performance is greatly improved.
The technical features of the claims and/or the description of the present invention may be combined in a manner not limited to the combination of the claims by the relation of reference. The technical solutions obtained by combining the technical features in the claims and/or the description are also within the scope of the invention.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention in any way. Any simple modification, equivalent variation and modification of the above embodiments according to the technical substance of the present invention still fall within the scope of the technical solution of the present invention.
Claims (15)
1. The preparation method of the lithium aluminum silicon glass is characterized by comprising the following steps of:
the solution for synthesizing the copper whisker forms a wire grid structure which is periodically distributed on lithium aluminum silicon base glass, and the lithium aluminum silicon base glass is obtained by heating and reducing the solution under a parallel electric field.
2. The method according to claim 1, comprising the steps of:
1) Preparing the solution for synthesizing the copper whisker by a soft template method;
2) Arranging a wire grid die on the surface of the lithium aluminum silicon base glass;
3) Coating the solution on the surface of glass provided with the wire grid die;
4) Heating the glass obtained in the step 3) in an oven with the parallel electric field;
5) And (3) placing the glass obtained in the step (4) in a reducing atmosphere for reduction to obtain the lithium aluminum silicon glass.
3. The method according to claim 2, characterized in that in step 2) the lithium aluminum silicon base glass comprises alkali metal ions in an amount of 5-20 wt. -%, based on the total weight of the lithium aluminum silicon base glass.
4. A method according to claim 3, wherein in step 2) the alkali metal ions comprise Li + 。
5. The method according to claim 4, wherein the method comprises,characterized in that in step 2), the alkali metal ions further comprise Na + 、K + At least one of them.
6. A method as recited in claim 2, wherein in step 2), the wire grid mold has a period of 100-500nm and a width of 100-300nm.
7. The method according to claim 2, wherein in step 4), the parallel electric field is an electrostatic field parallel to the surface of the glass, and the parallel electric field is applied at an electrostatic field strength of 500-800V/mm for 30-60min.
8. The method according to claim 2, wherein in step 4), the heating is performed at a temperature of 200-300 ℃ for a time of 30-60min.
9. The method according to claim 2, wherein in step 5), the reducing atmosphere is derived from at least one gas selected from hydrogen and carbon monoxide or a mixed gas thereof with an inert gas, the pressure of the gas is 0.3-1.0Mpa, and the time of the reduction is 3-6h.
10. A lithium aluminum silicon glass, comprising:
lithium aluminum silicon base glass; and
copper whiskers grown on the lithium aluminum silicon base glass, the copper whiskers having a periodically distributed wire grid structure.
11. The lithium aluminosilicate glass according to claim 10, wherein the glass is prepared by the method according to any one of claims 1-9.
12. The lithium aluminosilicate glass according to claim 11, wherein the length and width of the lithium aluminosilicate glass are independently 1mm or more.
13. The lithium aluminum silicate glass according to claim 11, wherein the extinction ratio of the lithium aluminum silicate glass is 60dB or more, and the transmittance of the lithium aluminum silicate glass to light in a wavelength range of 190 to 1100nm is 76% or more.
14. A polarizing device comprising a polarizer, analyzer or attenuator comprising the lithium aluminum silicate glass of any one of claims 10-13.
15. The polarizing device of claim 14, wherein the polarizing device is an opto-isolator, an opto-magnetic disc signal detection sensor, an opto-voltage sensor, a fiber optic connector, or a liquid crystal display.
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|---|---|---|---|---|
| WO1999056332A1 (en) * | 1998-04-24 | 1999-11-04 | Hitachi, Ltd. | Lithium secondary cell |
| US20090190215A1 (en) * | 2008-01-29 | 2009-07-30 | Nicholas Francis Borrelli | Polarizing photorefractive glass |
| CN101959816A (en) * | 2008-01-29 | 2011-01-26 | 康宁股份有限公司 | Polarizing photoreactive glass |
| CN113880445A (en) * | 2021-11-17 | 2022-01-04 | 中国建筑材料科学研究总院有限公司 | Polarizing glass and preparation method and application thereof |
| CN115403270A (en) * | 2022-09-21 | 2022-11-29 | 中国建筑材料科学研究总院有限公司 | A kind of lithium aluminum silicon polarizing glass and its preparation method and application |
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2023
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999056332A1 (en) * | 1998-04-24 | 1999-11-04 | Hitachi, Ltd. | Lithium secondary cell |
| US20090190215A1 (en) * | 2008-01-29 | 2009-07-30 | Nicholas Francis Borrelli | Polarizing photorefractive glass |
| CN101959816A (en) * | 2008-01-29 | 2011-01-26 | 康宁股份有限公司 | Polarizing photoreactive glass |
| CN113880445A (en) * | 2021-11-17 | 2022-01-04 | 中国建筑材料科学研究总院有限公司 | Polarizing glass and preparation method and application thereof |
| CN115403270A (en) * | 2022-09-21 | 2022-11-29 | 中国建筑材料科学研究总院有限公司 | A kind of lithium aluminum silicon polarizing glass and its preparation method and application |
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