CN112341003A - Photochromic glass and preparation method thereof - Google Patents

Photochromic glass and preparation method thereof Download PDF

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Publication number
CN112341003A
CN112341003A CN202011356933.6A CN202011356933A CN112341003A CN 112341003 A CN112341003 A CN 112341003A CN 202011356933 A CN202011356933 A CN 202011356933A CN 112341003 A CN112341003 A CN 112341003A
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China
Prior art keywords
glass
silver halide
temperature
melting
photochromic
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CN202011356933.6A
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Chinese (zh)
Inventor
彭寿
周文彩
魏晓俊
于浩
齐帅
王伟
曾红杰
张纲
李一哲
张正
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China Triumph International Engineering Co Ltd
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China Triumph International Engineering Co Ltd
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Priority to CN202011356933.6A priority Critical patent/CN112341003A/en
Publication of CN112341003A publication Critical patent/CN112341003A/en
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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
    • C03C14/006—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 microcrystallites, e.g. of optically or electrically active material
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
    • 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
    • C03C4/04—Compositions for glass with special properties for photosensitive glass
    • C03C4/06—Compositions for glass with special properties for photosensitive glass for phototropic or photochromic glass

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Glass Compositions (AREA)

Abstract

The invention provides photochromic glass and a preparation method thereof, wherein the photochromic glass comprises borate glass and a photosensitizer, the photosensitizer is silver halide nanocrystalline, and the melting point of the borate glass is lower than the volatilization temperature or decomposition temperature of the silver halide. The preparation method comprises the following steps: preparing borate glass; crushing borate glass to form glass powder, and uniformly mixing the glass powder with silver halide nanocrystals to form mixed powder; and melting the mixed powder at a temperature lower than the volatilization temperature or the decomposition temperature of the silver halide to obtain the photochromic glass. The melting temperature is lower than the volatilization temperature or the decomposition temperature of the silver halide, so that the waste of photosensitizer raw materials in the high-temperature melting process is avoided, and the cost is reduced; in addition, the preparation method introduces silver halide in a nanocrystalline mode, does not need an additional heat treatment process to crystallize the photosensitizer, effectively saves energy and further reduces cost.

Description

Photochromic glass and preparation method thereof
Technical Field
The invention relates to the technical field of glass, in particular to photochromic glass and a preparation method thereof.
Background
Photochromic glass refers to optical functional glass which can be colored after being irradiated by light with a certain wavelength and can be restored to an original state after being irradiated by removing the light or being irradiated by light with another wavelength for a period of time. Photochromic glasses can be used in photochromic glasses, display devices, holographic storage media, and advanced buildings and vehicles.
The traditional photochromic glass is a borosilicate system which mostly uses silver halide as a photosensitizer, and the preparation method comprises the steps of directly adding the photosensitizer into a matrix glass batch, melting and casting the mixture into sheet glass by adopting a high-temperature melting process, and then carrying out sectional heat treatment to enable the silver halide to form microcrystals with a certain size. Although the method is successfully applied to the photochromic glass lens, the required melting temperature is higher, so that the active ingredients are seriously volatilized in the melting process of the raw materials, particularly, the volatilization of silver salt can reach 50%, the price is high, the raw materials need to be supplemented in time, and the cost is increased. In addition, the traditional preparation method also needs to accurately control the heat treatment process, so that the silver halide crystals grow into particles with specific sizes, and the glass is prevented from softening and crystallizing, thereby increasing the difficulty and further increasing the cost.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the technical problem to be solved by the present invention is to provide a photochromic glass which is low in production cost.
In order to achieve the above object, the present invention provides a photochromic glass comprising a borate glass and a photosensitizer, wherein the photosensitizer is a silver halide nanocrystal, and the melting point of the borate glass is lower than the volatilization temperature or decomposition temperature of silver halide.
Further, the chemical general formula of the borate glass is B2O3-Li2O-MeO, where Me is Be, Mg, Ca, Zn, or Ba, or the chemical formula of the borate glass is B2O3-BeO-MgO、B2O3-Li2O-SnO, or B2O3-Na2O-Al2O3。
Further, the mass fraction of the silver halide nanocrystals is 0.1% -1%.
Further, the silver halide nanocrystalline is one or a mixture of AgCl, AgBr and AgI.
Further, the size of the silver halide nanocrystalline particles is 5 nm-30 nm.
As described above, the photochromic glass according to the present invention has the following advantageous effects:
according to the photochromic glass, the borate glass is used as the matrix, the silver halide nanocrystalline is used as the photosensitizer, and the melting point of the borate glass is lower than the volatilization temperature or decomposition temperature of the silver halide, so that the melting temperature can be lower than the volatilization temperature or decomposition temperature of the silver halide in the preparation process of the photochromic glass, particularly in the melting treatment process of the mixture of the borate glass and the silver halide nanocrystalline, a large amount of silver salt volatilization and the like in the melting process can be effectively avoided, the waste of photosensitizer raw materials in the high-temperature melting process is avoided, and the cost is reduced.
The invention aims to solve another technical problem of providing a preparation method with lower cost.
In order to achieve the above object, the present invention provides a method for preparing the photochromic glass, comprising the following steps:
preparing borate glass;
crushing borate glass to form glass powder, and uniformly mixing the glass powder with silver halide nanocrystals to form mixed powder;
and melting the mixed powder at a temperature lower than the volatilization temperature or the decomposition temperature of the silver halide to obtain the photochromic glass.
Further, when the mixed powder is melted, the melting temperature is 380-550 ℃, and the heat preservation time is 30 min-2 h.
Furthermore, in the process of preparing the borate glass, the melting temperature is 1000-1280 ℃, and the melting time is 20-60 min.
Further, in the process of melting the mixed powder, the mixed powder is firstly put into a crucible, and then the crucible is put into a muffle furnace for firing.
Further, the silver halide nanocrystalline is prepared by an ion precipitation reaction method, a complex precipitation method, a reversible micelle method, an electrolysis method or an in-situ semi-solid reaction method.
As described above, the preparation method according to the present invention has the following advantageous effects:
according to the preparation method, when the mixed powder formed by the glass powder and the silver halide nanocrystalline is subjected to melting treatment, the melting temperature is lower than the volatilization temperature or decomposition temperature of the silver halide, so that the conditions of volatilization and the like of a large amount of silver salt in the melting process are effectively avoided, the waste of a photosensitizer raw material in the high-temperature melting process is avoided, and the cost is reduced; in addition, the preparation method introduces silver halide in a nanocrystalline mode, does not need an additional heat treatment process to crystallize the photosensitizer, effectively saves energy and further reduces cost.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
The invention provides photochromic glass, which comprises borate glass and a photosensitizer, wherein the photosensitizer is silver halide nanocrystal, and the melting point of the borate glass is lower than the volatilization temperature or the decomposition temperature of silver halide. According to the photochromic glass, the borate glass is used as the matrix, the silver halide nanocrystalline is used as the photosensitizer, and the melting point of the borate glass is lower than the volatilization temperature or decomposition temperature of the silver halide, so that the melting temperature can be lower than the volatilization temperature or decomposition temperature of the silver halide in the preparation process of the photochromic glass, particularly in the melting treatment process of the mixture of the borate glass and the silver halide nanocrystalline, a large amount of silver salt volatilization and the like in the melting process can be effectively avoided, the waste of photosensitizer raw materials in the high-temperature melting process is avoided, and the cost is reduced.
In some embodiments of the invention the borate glass has the chemical formula B2O3-Li2O-MeO, where Me is Be, Mg, Ca, Zn, or Ba, or borate glass of formula B2O3-BeO-MgO、B2O3-Li2O-SnO, or B2O3-Na2O-Al2O3。
Meanwhile, the invention provides a preparation method of the photochromic glass, which comprises the following steps:
preparing borate glass;
crushing borate glass to form glass powder; uniformly mixing the glass powder and the silver halide nanocrystalline to form mixed powder;
and melting the mixed powder at a temperature lower than the volatilization temperature or the decomposition temperature of the silver halide to obtain the photochromic glass.
According to the preparation method, when the mixed powder formed by the glass powder and the silver halide nanocrystalline is subjected to melting treatment, the melting temperature is lower than the volatilization temperature or decomposition temperature of the silver halide, so that the conditions of volatilization and the like of a large amount of silver salt in the melting process are effectively avoided, the waste of a photosensitizer raw material in the high-temperature melting process is avoided, and the cost is reduced; in addition, the preparation method introduces silver halide in a nanocrystalline mode, does not need an additional heat treatment process to crystallize the photosensitizer, effectively saves energy and further reduces cost.
Example one
Photochromic glass in this exampleThe glass is concretely B2O3-Li2The preparation method of the photochromic glass of the O-CaO system comprises the following steps:
1. preparation of Borate glasses, in particular Li2CO3、CaCO3And H3BO3Mixing and grinding the raw materials according to a certain proportion, putting the mixture into a crucible, putting the crucible into a muffle furnace, heating the crucible to 1180 ℃, preserving the heat for 50min to obtain molten glass, pouring the molten glass on a mold to obtain B2O3-Li2O-CaO borate glass, which is a transparent bulk matrix glass;
2. preparing silver halide nanocrystals, specifically preparing AgCl/AgBr mixed nanocrystals by using a complex precipitation method, wherein the size of crystal grains is 20 nm;
3. grinding the obtained borate glass into glass powder, fully grinding the glass powder and AgCl/AgBr mixed nanocrystalline to realize uniform mixing of the glass powder and the AgCl/AgBr mixed nanocrystalline to form mixed powder;
4. melting the mixed powder, specifically putting the ground mixed powder into a crucible, sintering the crucible in a muffle furnace at 450 ℃, keeping the temperature for 2h, cooling and forming to obtain the product B2O3-Li2Photochromic glasses of the O-CaO system.
The mass fraction of the silver halide nanocrystals in the photochromic glass obtained in this example was 1%.
The photochromic glass prepared in this example is a low-melting glass whose matrix is a low-melting borate glass. The preparation method is simple to operate, the required melting temperature is lower when the mixed powder is melted, and the melting temperature is lower than the volatilization temperature or the decomposition temperature of the silver halide, so that the waste of the raw material of the photosensitizer in the high-temperature melting process is effectively avoided, and the cost is reduced. In addition, the silver halide is introduced in a nanocrystalline mode, an additional heat treatment process is not needed to crystallize the photosensitizer, and energy is effectively saved.
Example two
In the present example, the photochromic glass is specifically B2O3-Na2O-Al2O3The preparation method of the photochromic glass of the system comprises the following steps:
1. preparation of Borate glasses, in particular Na2CO3、Al(OH)3And H3BO3Mixing and grinding the raw materials according to a certain proportion, placing the mixture into a crucible, placing the crucible into a muffle furnace, heating the crucible to 1200 ℃, preserving the heat for 30min to obtain molten glass, pouring the molten glass on a mold to obtain B2O3-Na2O-Al2O3A borate glass which is a transparent bulk matrix glass;
2. preparing silver halide nanocrystals, specifically AgBr nanocrystals by using an ion precipitation reaction method, wherein the grain size is 15 nm;
3. grinding the obtained borate glass into glass powder, fully grinding the glass powder and AgBr nanocrystalline to realize uniform mixing of the glass powder and the AgBr nanocrystalline to form mixed powder;
4. melting the mixed powder, specifically putting the ground mixed powder into a crucible, sintering the crucible in a muffle furnace at 500 ℃, keeping the temperature for 2h, cooling and forming to obtain the product B2O3-Na2O-Al2O3Photochromic glasses of the system.
The mass fraction of the silver halide nanocrystals in the photochromic glass obtained in this example was 0.1%.
EXAMPLE III
In this embodiment, based on the first embodiment, the reversible micelle method is specifically used to prepare the AgI nanocrystals, and the grain size is 5 nm. In the embodiment, when the mixed powder formed by the glass powder and the AgI nanocrystalline is subjected to melting treatment, the melting temperature is 380 ℃, and the heat preservation time is 1.5 h.
In the process of preparing the borate glass in the embodiment, the melting temperature is 1000 ℃ and the melting time is 60 min.
The mass fraction of the silver halide nanocrystals in the photochromic glass obtained in this example was 0.5%.
Example four
In this embodiment, on the basis of the first embodiment, the AgCl nanocrystals were prepared by an electrolytic method or an in-situ semi-solid reaction method, and the grain size was 30 nm. In the embodiment, when the mixed powder formed by the glass powder and the AgCl nanocrystals is melted, the melting temperature is 550 ℃, and the heat preservation time is 30 min.
In the process of preparing the borate glass in the embodiment, the melting temperature is 1280 ℃, and the melting time is 20 min.
In conclusion, the present invention effectively overcomes various disadvantages of the prior art and has high industrial utilization value.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.

Claims (10)

1. The photochromic glass is characterized by comprising borate glass and a photosensitizer, wherein the photosensitizer is silver halide nanocrystal, and the melting point of the borate glass is lower than the volatilization temperature or the decomposition temperature of silver halide.
2. The photochromic glass of claim 1, wherein the borate glass has the chemical formula B2O3-Li2O-MeO, where Me is Be, Mg, Ca, Zn, or Ba, or the chemical formula of the borate glass is B2O3-BeO-MgO、B2O3-Li2O-SnO, or B2O3-Na2O-Al2O3。
3. The photochromic glass of claim 1 wherein the silver halide nanocrystals are present at a mass fraction of 0.1 to 1%.
4. The photochromic glass of claim 1 wherein the silver halide nanocrystals are any mixture of one or more of AgCl, AgBr and AgI.
5. The photochromic glass of claim 1 wherein the silver halide nanocrystalline particles have a size of 5nm to 30 nm.
6. A method for preparing the photochromic glass of claim 1 comprising the steps of:
preparing borate glass;
crushing borate glass to form glass powder, and uniformly mixing the glass powder with silver halide nanocrystals to form mixed powder;
and melting the mixed powder at a temperature lower than the volatilization temperature or the decomposition temperature of the silver halide to obtain the photochromic glass.
7. The preparation method according to claim 6, wherein the melting temperature is 380-550 ℃ and the holding time is 30 min-2 h when the mixed powder is melted.
8. The method according to claim 6, wherein the melting temperature is 1000 to 1280 ℃ and the melting time is 20 to 60 minutes in the process of preparing the borate glass.
9. The production method according to claim 6, wherein the mixed powder is charged into a crucible in the melting treatment of the mixed powder, and the crucible is fired in a muffle furnace.
10. The method according to claim 6, wherein the silver halide nanocrystals are prepared by an ion precipitation reaction method, a complex precipitation method, a reversible micelle method, an electrolysis method or an in-situ semi-solid reaction method.
CN202011356933.6A 2020-11-26 2020-11-26 Photochromic glass and preparation method thereof Pending CN112341003A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114573231A (en) * 2022-03-24 2022-06-03 中国科学院西安光学精密机械研究所 AgI-AgPO3-MpOqPreparation method of system transparent conductive glass and electromagnetic shielding application
CN116813194A (en) * 2023-07-06 2023-09-29 昆明理工大学 Preparation method of photochromic phosphosilicate glass ceramic

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US5430573A (en) * 1993-12-15 1995-07-04 Corning Incorporated UV-absorbing, polarizing glass article
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114573231A (en) * 2022-03-24 2022-06-03 中国科学院西安光学精密机械研究所 AgI-AgPO3-MpOqPreparation method of system transparent conductive glass and electromagnetic shielding application
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CN116813194A (en) * 2023-07-06 2023-09-29 昆明理工大学 Preparation method of photochromic phosphosilicate glass ceramic

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Application publication date: 20210209