CN116813194A - Preparation method of photochromic phosphosilicate glass ceramic - Google Patents
Preparation method of photochromic phosphosilicate glass ceramic Download PDFInfo
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- CN116813194A CN116813194A CN202310825197.1A CN202310825197A CN116813194A CN 116813194 A CN116813194 A CN 116813194A CN 202310825197 A CN202310825197 A CN 202310825197A CN 116813194 A CN116813194 A CN 116813194A
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- 239000005360 phosphosilicate glass Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000919 ceramic Substances 0.000 title abstract description 16
- 239000002241 glass-ceramic Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 19
- 230000000694 effects Effects 0.000 claims abstract description 16
- 239000011521 glass Substances 0.000 claims abstract description 13
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 8
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 7
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 7
- 229910001369 Brass Inorganic materials 0.000 claims abstract description 6
- 239000010951 brass Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 15
- 238000005245 sintering Methods 0.000 claims description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 238000007578 melt-quenching technique Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 230000002441 reversible effect Effects 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims 2
- 230000003287 optical effect Effects 0.000 abstract description 9
- 238000003860 storage Methods 0.000 abstract description 8
- 230000008859 change Effects 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 3
- 229910010293 ceramic material Inorganic materials 0.000 abstract 1
- 238000005562 fading Methods 0.000 abstract 1
- 239000005365 phosphate glass Substances 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 238000002845 discoloration Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 230000000638 stimulation Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000002983 circular dichroism Methods 0.000 description 1
- 238000013500 data storage Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 231100000584 environmental toxicity Toxicity 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000004984 smart glass Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
The invention relates to a photochromic phosphosilicate glass ceramic and a preparation method thereof, belonging to the technical field of preparation and application of photochromic glass ceramic. A phosphosilicate glass ceramic material with photochromic effect, which is prepared at 1100 ℃. Firstly, weighing a proper amount of NH 4 H 2 PO 4 、SiO 2 、SrCO 3 、Al 2 O 3 、Cs 2 CO 3 、PbBr 2 Uniformly mixing KBr and AgBr, and doping a proper amount of AgBr and Cu 2 O is ground to obtain a mixed material. The molten phosphate glass ceramic was then poured onto a preheated brass mold and cooled to 30-40 ℃ to obtain a sample glass. The sample can generate photovariation under 365nm ultraviolet lightThe color phenomenon, and the corresponding color-changing area can be obtained according to the laser irradiation path, so that a clear pattern is formed, the initial state before the color change can be quickly faded back under the heating of 300 ℃, and the color-changing and fading process can be stably repeated for a plurality of times, so that the method has a certain prospect in the field of optical storage.
Description
Technical Field
The invention belongs to the technical field of functional glass ceramics, and particularly relates to a preparation method of photochromic phosphosilicate glass ceramics.
Technical Field
Optical storage technology has the advantages of high stability, fast reading speed, long lifetime, and has been used in the past few decades to prepare circular dichroism, DVD and blu-ray discs. With the further development of modern internet and smart devices, the storage capacity requirements for data storage devices are increasing. Thus, there is a higher demand for new optical storage media. Some special materials exhibit interesting color-changing reactions under light, thermal, electric and magnetic field stimuli. Photochromic materials are of great interest for their unique ability to reversibly change their optical properties in response to light stimuli. Particularly, photochromic glass has been widely used in various fields of optics, sensors, smart windows, etc., due to its excellent optical properties and ease of manufacturing. Currently, organic photochromic materials having photoluminescent properties are widely studied as optical storage media. However, poor thermal stability and high synthesis costs of organic photochromic materials are unavoidable. Therefore, a photochromic inorganic material may be more suitable as an optical storage medium than an organic photochromic material, and the inorganic photochromic material has been receiving attention as an optical information storage medium due to its high strength or mechanical resistance, good fatigue resistance and chemical stability, and low environmental toxicity.
Photochromism can be used to adjust the luminescence characteristics of active centers, and information readout can be achieved by monitoring changes in luminescence intensity. At present, reversible photoluminescence regulation and control of ceramics are researched based on a photochromic effect, and potential application prospects are shown in the fields of holographic storage, optical data processing and the like.
Disclosure of Invention
The invention aims to provide a preparation method of photochromic phosphosilicate glass ceramic with a photochromic effect by adopting inorganic AgBr phosphosilicate with the photochromic effect aiming at the problems that in the existing photochromic materials, the color body of an organic material is poor in light stability, fatigue resistance and service life, most of inorganic color-changing materials are poor in reversibility and repeatability. The photochromic phosphosilicate glass ceramic has high-efficiency response characteristic at 365nm ultraviolet light source: firstly, after it is sintered in an air atmosphere, the sample may show a light green color; in addition, clear patterns can be irradiated on the surface of a sample according to the photochromic phenomenon under the irradiation of a 365nm ultraviolet light source, the sample can be completely faded back to the original state under the thermal stimulation at 300 ℃, and the cycle can be repeated for a plurality of times.
The invention is realized by the following technical scheme.
A photochromic phosphosilicate glass ceramic comprises the following specific steps:
s1: NH is first of all 4 H 2 PO 4 、SiO 2 、SrCO 3 、Al 2 O 3 、Cs 2 CO 3 、PbBr 2 Mixing KBr and KBr, adding proper AgBr and Cu 2 O is ground to obtain a mixed material;
s2: NH is added to 4 H 2 PO 4 Conversion to P 2 O 5 Placing the ground mixed material into an alumina crucible, placing the alumina crucible into a muffle furnace, heating the alumina crucible at 200 ℃ for one hour, and discharging gaseous ammonia and water;
s3: sintering for 20min at 1100 ℃ in an air atmosphere by adopting a conventional melt quenching method;
s4: the molten phosphosilicate glass was poured onto a brass mold preheated to 350 c and cooled to 30-40 c to obtain a sample glass.
The beneficial effects of the invention are as follows:
1. after the sintered glass is irradiated by 365nm ultraviolet light, the surface of the sample is changed from light green to gray, the photochromic phenomenon is achieved, the sample is heated for 2 minutes at 300 ℃, and the gray completely fades back to a transparent light green state;
2. by 365nm ultraviolet irradiation, clear patterns can be irradiated on the surface of the sample according to the photochromic phenomenon.
3. The color of the sample is changed reversibly and can be repeated circularly for a plurality of times;
4. the change of the body color depth of the sample can be regulated by regulating the laser irradiation time;
5. the preparation process is simple and efficient, has low cost and is favorable for realizing industrialization.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention.
FIG. 1 is a light green photograph of a photochromic phosphosilicate glass-ceramic sample obtained in example 1 of the present invention, before irradiation with 365nm ultraviolet light.
FIG. 2 is a light green photograph of a photochromic phosphosilicate glass-ceramic sample obtained in example 2 of the present invention, prior to irradiation with 365nm ultraviolet light.
FIG. 3 is a light green photograph of a photochromic phosphosilicate glass-ceramic sample obtained in example 3 of the present invention, before irradiation with 365nm ultraviolet light.
FIG. 4 is a photograph of a sample of a photochromic phosphosilicate glass-ceramic according to example 3 of the present invention that exhibits a photochromic effect upon exposure to ultraviolet light at 365 nm.
FIG. 5 is an XRD pattern of an AgBr phosphosilicate glass ceramic sample obtained in examples 1,2,3 of the present invention before and after illumination with 365nm ultraviolet light source.
Description of the preferred embodiments
The present invention will be further described with reference to the following specific examples and drawings, but the present invention is not limited to the following examples.
Example 1
The photochromic phosphosilicate glass ceramic with the photochromic effect is prepared by adopting an air atmosphere as a sintering atmosphere, wherein the sintering temperature is 1100 ℃, and the color of a sample is light green glass state.
The preparation method of the photochromic phosphosilicate glass ceramic with the thermochromic effect comprises the following specific steps:
s1: first 80% NH 4 H 2 PO 4 、-10％SiO 2 、-6％SrCO 3 、-3.5％Al 2 O 3 、-15％Cs 2 CO 3 、-7.5％PbBr 2 Mixing well 15% KBr, adding 0.01g AgBr and 0.001g Cu 2 O is ground to obtain a mixed material;
s2: NH is added to 4 H 2 PO 4 Conversion to P 2 O 5 Placing the ground mixed material into an alumina crucible, placing the alumina crucible into a muffle furnace, heating the alumina crucible at 200 ℃ for one hour, and discharging gaseous ammonia and water;
s3: sintering for 20min at 1100 ℃ in an air atmosphere by adopting a conventional melt quenching method;
s4: the molten phosphosilicate glass was poured onto a brass mold preheated to 350 c and cooled to 30-40 c to obtain a sample glass.
The light green glass ceramic with the photochromic effect is obtained.
The photo of the photochromic glass-ceramic obtained in example 1 of the present invention is shown in FIG. 1, and the sample is seen to be pale green in color from FIG. 1. Under 365nm ultraviolet laser irradiation, ag is little precipitated, the sample is in a glass state, the photochromism phenomenon is weak, and the color-changing state of FIG. 2 can be returned to the original state of FIG. 1 under 300 ℃ heating. The color change reversibility of the sample is realized, and clear patterns cannot be obtained.
Example 2
The photochromic phosphosilicate glass ceramic with the photochromic effect is prepared by adopting an air atmosphere as a sintering atmosphere, wherein the sintering temperature is 1100 ℃, and the color of a sample is light green glass state.
The preparation method of the photochromic phosphosilicate glass ceramic with the thermochromic effect comprises the following specific steps:
s1: first 80% NH 4 H 2 PO 4 、-10％SiO 2 、-6％SrCO 3 、-3.5％Al 2 O 3 、-15％Cs 2 CO 3 、-7.5％PbBr 2 Mixing well 15% KBr, adding 0.02g AgBr and 0.002g Cu 2 O is ground to obtain a mixed material;
s2: NH is added to 4 H 2 PO 4 Conversion to P 2 O 5 Placing the ground mixed material into an alumina crucible, placing the alumina crucible into a muffle furnace, heating the alumina crucible at 200 ℃ for one hour, and discharging gaseous ammonia and water;
s3: sintering for 20min at 1100 ℃ in an air atmosphere by adopting a conventional melt quenching method;
s4: the molten phosphosilicate glass was poured onto a brass mold preheated to 350 c and cooled to 30-40 c to obtain a sample glass.
The light green glass ceramic with the photochromic effect is obtained.
The photo of the photochromic glass-ceramic obtained in example 2 of the present invention is shown in FIG. 2, and the sample color is seen as light green in FIG. 2. Ag begins to precipitate in a large amount, the Ag becomes deep gradually under 365nm ultraviolet laser irradiation, the sample is in a semitransparent glass state, the photochromic phenomenon is enhanced, and the color-changing state of FIG. 2 can be returned to the original state of FIG. 2 under 300 ℃ heating. The color change reversibility of the sample is realized, and clear patterns cannot be obtained.
Example 3
The photochromic phosphosilicate glass ceramic with the photochromic effect is prepared by adopting an air atmosphere as a sintering atmosphere, wherein the sintering temperature is 1100 ℃, and the color of a sample is light green glass state.
The preparation method of the photochromic phosphosilicate glass ceramic with the thermochromic effect comprises the following specific steps:
s1: first 80% NH 4 H 2 PO 4 、-10％SiO 2 、-6％SrCO 3 、-3.5％Al 2 O 3 、-15％Cs 2 CO 3 、-7.5％PbBr 2 Mixing well 15% KBr, adding 0.03g AgBr and 0.003g Cu 2 O is ground to obtain a mixed material;
s2: NH is added to 4 H 2 PO 4 Conversion to P 2 O 5 Placing the ground mixed material into an alumina crucible, placing the alumina crucible into a muffle furnace, heating the alumina crucible at 200 ℃ for one hour, and discharging gaseous ammonia and water;
s3: sintering for 20min at 1100 ℃ in an air atmosphere by adopting a conventional melt quenching method;
s4: the molten phosphosilicate glass was poured onto a brass mold preheated to 350 c and cooled to 30-40 c to obtain a sample glass.
The light green glass ceramic with the photochromic effect is obtained.
The photo of the photochromic glass-ceramic obtained in example 3 of the present invention is shown in FIG. 3, and the sample is seen to be pale green in color from FIG. 3. Ag begins to precipitate in a large amount, the Ag becomes deep gradually under 365nm ultraviolet irradiation, the sample is in a glass ceramic state, the photochromic phenomenon is enhanced, and the color-changing state of FIG. 4 can be returned to the original state of FIG. 3 under 300 ℃ heating. The color change reversibility of the sample is realized, and clear patterns can be obtained.
FIG. 5 is an XRD photograph of the photochromic glass-ceramic obtained in example 3 before and after discoloration, and it can be seen from FIG. 5 that AgBr crystals were precipitated in both the samples before and after discoloration. FIG. 5 shows XRD data of the photochromic glass-ceramic obtained in example 3 in the original state in a dark light environment and in the state after discoloration under irradiation of 365nm ultraviolet light source, respectively, and it can be seen from FIG. 5 that AgBr crystals were precipitated in the samples before and after discoloration. Indicating that discoloration is caused by Ag ions.
The photochromic glass-ceramic obtained in example 3 of the present invention was sintered in an air atmosphere to appear pale green; the color depth of the photochromic glass ceramic is gradually deepened under 365nm ultraviolet irradiation and is increased along with the increase of irradiation time, in addition, the color of the photochromic glass ceramic is changed from gray black to light green under 300 ℃ thermal stimulation, a template can be covered according to different patterns under 365nm ultraviolet irradiation, clear patterns can be printed, the pattern information can be recorded through a photochromic process, the reversibility and the repeatability of the process are good, the gradient change can be realized, the preparation process is simple and convenient, the cost is low, and the method has wide application prospect.
While there have been described and shown what are at present considered to be the primary examples of the invention, it will be understood by those skilled in the art that various changes, modifications and combinations may be made therein without departing from the spirit and scope of the invention as defined in the appended claims and their equivalents.
Claims (5)
1. The photochromic down-conversion phosphosilicate glass is characterized in that the reversible and repeatable sample color regulation and control are realized by utilizing the photochromic effect of AgBr.
2. A preparation method of photochromic phosphosilicate glass is characterized by comprising the following specific steps:
s1: firstly, raw materials are as follows: NH (NH) 4 H 2 PO 4 、SiO 2 、SrCO 3 、Al 2 O 3 、Cs 2 CO 3 、PbBr 2 Mixing KBr and KBr, adding proper AgBr and Cu 2 O is ground to obtain a mixed material;
s2: NH is added to 4 H 2 PO 4 Conversion to P 2 O 5 Placing the ground mixed material into an alumina crucible, placing the alumina crucible into a muffle furnace, heating the alumina crucible at 200 ℃ for one hour, and discharging gaseous ammonia and water;
s3: sintering under air atmosphere by adopting a conventional melt quenching method;
s4: the molten phosphosilicate glass was poured onto a brass mold preheated to 350 c and cooled to 30-40 c to obtain a sample glass.
3. The method for preparing a photochromic phosphosilicate glass-ceramic according to claim 2, wherein: in S1, the concentration of the raw material is (70-90)% NH 4 H 2 PO 4 、-10％SiO 2 、-6％SrCO 3 、-3.5％Al 2 O 3 、-15％Cs 2 CO 3 、-7.5％PbBr 2 、-15％KBr。
4. The method for preparing a photochromic phosphosilicate glass-ceramic according to claim 2, wherein: in S3, sintering is carried out under an air atmosphere at 1100 ℃ for 20min.
5. The method for preparing a photochromic phosphosilicate glass-ceramic according to claim 2, wherein: reversible and repeatable sample color regulation and control are realized by utilizing the photochromic effect of AgBr.
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| CN202310825197.1A CN116813194A (en) | 2023-07-06 | 2023-07-06 | Preparation method of photochromic phosphosilicate glass ceramic |
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| CN202310825197.1A CN116813194A (en) | 2023-07-06 | 2023-07-06 | Preparation method of photochromic phosphosilicate glass ceramic |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891387A (en) * | 2009-05-22 | 2010-11-24 | 宋沛 | Automotive color-changing glass product and preparation method thereof |
| CN103032018A (en) * | 2012-12-19 | 2013-04-10 | 绍兴文理学院 | Intelligent photochromic window and use method thereof |
| CN110903824A (en) * | 2019-12-27 | 2020-03-24 | 上海交通大学 | Composite luminescent material and preparation method thereof |
| CN112341003A (en) * | 2020-11-26 | 2021-02-09 | 中国建材国际工程集团有限公司 | Photochromic glass and preparation method thereof |
| CN115806385A (en) * | 2022-10-28 | 2023-03-17 | 华南农业大学 | High light stability and high heat stability CsPbBr 3 Perovskite quantum dot glass and preparation method and application thereof |
-
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- 2023-07-06 CN CN202310825197.1A patent/CN116813194A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891387A (en) * | 2009-05-22 | 2010-11-24 | 宋沛 | Automotive color-changing glass product and preparation method thereof |
| CN103032018A (en) * | 2012-12-19 | 2013-04-10 | 绍兴文理学院 | Intelligent photochromic window and use method thereof |
| CN110903824A (en) * | 2019-12-27 | 2020-03-24 | 上海交通大学 | Composite luminescent material and preparation method thereof |
| US20210198568A1 (en) * | 2019-12-27 | 2021-07-01 | Shanghai Jiao Tong University | Luminescent composite material and preparation method therefor |
| CN112341003A (en) * | 2020-11-26 | 2021-02-09 | 中国建材国际工程集团有限公司 | Photochromic glass and preparation method thereof |
| CN115806385A (en) * | 2022-10-28 | 2023-03-17 | 华南农业大学 | High light stability and high heat stability CsPbBr 3 Perovskite quantum dot glass and preparation method and application thereof |
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