CN104355545A - Transparent glass ceramic having double-frequency light absorption and conversion capability and preparation method for transparent glass ceramic - Google Patents
Transparent glass ceramic having double-frequency light absorption and conversion capability and preparation method for transparent glass ceramic Download PDFInfo
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- CN104355545A CN104355545A CN201410494802.2A CN201410494802A CN104355545A CN 104355545 A CN104355545 A CN 104355545A CN 201410494802 A CN201410494802 A CN 201410494802A CN 104355545 A CN104355545 A CN 104355545A
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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
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0009—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing silica as main constituent
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Abstract
The invention discloses transparent glass ceramic having double-frequency light joint absorption and conversion capability and a preparation method for the transparent glass ceramic. The transparent glass ceramic can absorb ultraviolet light and infrared light simultaneously, and convert the light into visible light, is prepared from cheap silicate and aluminate as a base material, and Er<3+> ions as ions activating luminescence centers; the preparation method comprises the following steps: fully grinding and mixing raw materials in proportion; melting the raw materials at a high temperature; pouring and cooling; conducting annealing at an appropriate temperature, The transparent glass ceramic is high in transparency and rigidity, and environment-friendly, and can be produced in a large area.
Description
Technical field
The present invention relates to transparent glass ceramics synthesis technical field, particularly relate to a kind of novel double frequency and turn optical property and relevant transparent glass ceramics field.
Background technology
Sun power is as renewable energy source, inexhaustible.In the solar spectrum of ground, the solar radiation energy of about 99% is distributed in 220 ~ 2500 nanometer broadband wave bands, wherein visible ray (400 ~ 700nm) accounts for 71% of sunlight total radiation, and infrared light (700 ~ 2500nm) accounts for 22% of total radiation.But present various photoelectric devices all can only realize absorption and the conversion of greater efficiency to the light of respective specific spectral range.The characteristic of this selective use luminous energy of photoelectric device, has had a strong impact on the abundant absorption to sunlight and utilization.
It is reported, frequency inverted illumination mode is divided into conversion and lower conversion two kinds (F.Auzel, Chem.Rev., 2004,104,139).Upper transformation energy is converted to visible ray infrared light; Lower transformation energy is converted to visible ray UV-light.Till now, also do not have a kind of material can turn light mode these two kinds and combine, have no idea to change to visible ray while of realizing infrared light and UV-light yet.
Summary of the invention
Goal of the invention: the solution upper conversion of infrared light and the lower conversion two kinds of UV-light turn combining of light mode, and realize transparent glass ceramics of this combination and preparation method thereof.
Technical scheme: the technical problem that the present invention solves be disclose a kind of can the preparation method of transparent glass ceramics of simultaneously stability and conversion UV-light and infrared light double frequency light.
Simultaneously stability prepared by the present invention is analytically pure oxide compound with the matrix starting material of the transparent glass ceramics changing UV-light and infrared light double frequency light, borate, one or more mixtures in carbonate, crystallite forming core material is one or more mixtures in chemical pure fluorochemical, and matrix starting material are cheap Al
2o
3, Na
2cO
3, SiO
2, CaCO
3one or more mixtures, crystallite forming core material is YF
3, LaF
3, LuF
3, PbF
2, BaF
2in one or more mixtures, doping luminescent center ion is Er
3+ion.Consist of 15%-25%Al
2o
3, 10%-19%Na
2cO
3, 41%-60%SiO
2, 4%CaCO
3, 8%YF
3, 15%LaF
3, 8%-10%LuF
3, 50%PbF
2, 18%-20%BaF
2, 18%NaF, 20%ZnF
2, 1%-5%ErF
3.
Transparent glass ceramics of the present invention adopts melt supercooled method and subsequent heat treatment preparation.
The melt supercooled method that the present invention adopts and subsequent heat treatment comprise preparation and Crystallizing treatment two steps subsequently of forerunner's glass.The preparation temperature of forerunner's glass is 1000 DEG C-1500 DEG C; The temperature range of Crystallizing treatment is 471 DEG C-680 DEG C.
By changing the doping content of rare earth ion, control fluorescent emission intensity.
The preparation method of the transparent glass ceramics that the present invention relates to comprises the following steps:
Choosing of (a) raw material
Glass-ceramic raw material is mainly oxide compound and fluorochemical.
The mixing of (b) glass-ceramic admixtion
Take raw material accurately according to proportioning, put into mortar and add dehydrated alcohol and fully grind 0.5 hour.
C () glass-ceramic is founded
What glass smelting adopted is corundum crucible, has then carried out thermal treatment and annealing.
Beneficial effect:
(1) preparation method of the present invention is easy, is applicable to industrial mass manufacture.
(2) transparent glass ceramics that the present invention obtains has good thermostability and chemical stability compared with fluorescent material.
(3) transparent glass ceramics of the present invention can realize the upper conversion of infrared light and the lower conversion of UV-light simultaneously, launches visible ray.
Accompanying drawing explanation
Fig. 1 is the emmission spectrum of sample under 378nm and 980nm excites of embodiment 1.
Fig. 2 is the emmission spectrum of sample under 378nm and 980nm excites of embodiment 2.
Fig. 3 is the emmission spectrum of sample under 378nm and 980nm excites of embodiment 3.
Fig. 4 is the emmission spectrum of sample under 378nm and 980nm excites of embodiment 4.
Fig. 5 is the emmission spectrum of sample under 378nm and 980nm excites of embodiment 5.
Fig. 6 is the emmission spectrum of sample under 378nm and 980nm excites of embodiment 6.
Embodiment:
Embodiment 1-4
Al selected by matrix starting material
2o
3, Na
2cO
3, SiO
2, CaCO
3, crystallite forming core Material selec-tion is YF
3and NaF, doping luminescent center ion is chosen as ErF
3.Proportion of raw material is 15%Al
2o
3, 10%Na
2cO
3, 45%SiO
2, 4%CaCO
3, (8%-x) YF
3and 18%NaF, xErF
3, x=1%, 1.5%.Above-mentioned powder raw material is weighed, is placed on and mixes in agate mortar and to add alcohol 2 milliliters grinding, be then placed in corundum crucible, put into electric furnace be heated to 1500 DEG C after insulation 1 hour, make it abundant melting.Afterwards, glass solution is taken out and pours into fast shapingly in copper mold obtain block forerunner's glass, the block forerunner's glass obtained is put into 660 DEG C, electric furnace annealing 1 hour to eliminate internal stress and promotion microcrystallization.Sample, through surface finish, obtains green glow and red emission under 378nm and 980nm excites, and the emmission spectrum of embodiment 1 as shown in Figure 1.
The devitrified glass composition of table 1 embodiment 1-4
| Sequence number | Al 2O 3(g) | Na 2CO 3(g) | SiO 2(g) | CaCO 3(g) | YF 3(g) | NaF(g) | ErF 3(g) |
| 1 | 2.9316 | 2.0316 | 5.1827 | 0.7674 | 2.2150 | 1.4477 | 0.0345 |
| 2 | 4.3974 | 3.0474 | 7.7741 | 1.1511 | 3.3225 | 2.1716 | 0.0518 |
| 3 | 5.8632 | 4.0632 | 10.3654 | 1.5348 | 4.4300 | 2.8954 | 0.069 |
| 4 | 7.3290 | 5.0790 | 12.9568 | 1.9185 | 5.5375 | 3.6192 | 0.0863 |
Embodiment 5-8
Al selected by matrix starting material
2o
3, Na
2cO
3, SiO
2, CaCO
3, crystallite forming core Material selec-tion is LuF
3and NaF, doping luminescent center ion is chosen as ErF
3.Proportion of raw material is 15%Al
2o
3, 10%Na
2cO
3, 45%SiO
2, 4%CaCO
3, (8%-x) LuF
3and 18%NaF, xErF
3, x=1%, 1.5%.Above-mentioned powder raw material is weighed, is placed on and mixes in agate mortar and to add alcohol 2 milliliters grinding, be then placed in corundum crucible, put into electric furnace be heated to 1500 DEG C after insulation 1 hour, make it abundant melting.Afterwards, glass solution is taken out and pours into fast shapingly in copper mold obtain block forerunner's glass, the block forerunner's glass obtained is put into 650 DEG C, electric furnace annealing 2 hours to eliminate internal stress and promotion microcrystallization.Sample, through surface finish, obtains green glow and red emission under 378nm and 980nm excites, and the emmission spectrum of embodiment 5 as shown in Figure 2.
The devitrified glass composition of table 2 embodiment 5-8
| Sequence number | Al 2O 3(g) | Na 2CO 3(g) | SiO 2(g) | CaCO 3(g) | LuF 3(g) | NaF(g) | ErF 3(g) |
| 5 | 2.7624 | 1.9143 | 4.8835 | 0.7231 | 3.3182 | 1.3651 | 0.0324 |
| 6 | 4.1436 | 2.8715 | 7.3253 | 1.0847 | 4.9773 | 2.0477 | 0.0486 |
| 7 | 5.5248 | 3.8286 | 9.7670 | 1.4462 | 6.6364 | 2.7302 | 0.0648 |
| 8 | 6.9060 | 4.7858 | 12.2086 | 1.8078 | 8.2955 | 3.4128 | 0.0810 |
Embodiment 9-12
Al selected by matrix starting material
2o
3, Na
2cO
3, SiO
2, crystallite forming core Material selec-tion is LaF
3, doping luminescent center ion is chosen as ErF
3.Proportion of raw material is 25%Al
2o
3, 19%Na
2cO
3, 41%SiO
2, (15%-x) LaF
3, xErF
3, x=1%, 1.5%.Above-mentioned powder raw material is weighed, is placed on and mixes in agate mortar and to add alcohol 2 milliliters grinding, be then placed in corundum crucible, put into electric furnace be heated to 1500 DEG C after insulation 1 hour, make it abundant melting.Afterwards, glass solution is taken out and pours into fast shapingly in copper mold obtain block forerunner's glass, the block forerunner's glass obtained is put into 680 DEG C, electric furnace annealing 2 hours to eliminate internal stress and promotion microcrystallization.Sample, through surface finish, obtains green glow and red emission under 378nm and 980nm excites, and the emmission spectrum of embodiment 9 as shown in Figure 3.
The devitrified glass composition of table 3 embodiment 9-12
| Sequence number | Al 2O 3(g) | Na 2CO 3(g) | SiO 2(g) | LaF 3(g) | ErF 3(g) |
| 9 | 6.2790 | 4.9605 | 5.9202 | 7.7161 | 0.0829 |
| 10 | 9.4185 | 4.3073 | 8.8803 | 11.5742 | 0.1244 |
| 11 | 12.5580 | 9.9210 | 11.8404 | 15.4322 | 0.1658 |
| 12 | 15.6975 | 12.4013 | 14.8005 | 19.2903 | 0.2073 |
Embodiment 13-16
SiO selected by matrix starting material
2, crystallite forming core Material selec-tion is PbF
2, doping luminescent center ion is chosen as ErF
3.Proportion of raw material is 50%SiO
2, (50%-x) PbF
2, xErF
3, x=1%, 1.5%.Above-mentioned powder raw material is weighed, is placed on and mixes in agate mortar and to add alcohol 2 milliliters grinding, be then placed in corundum crucible, put into electric furnace be heated to 1000 DEG C after insulation 1 hour, make it abundant melting.Afterwards, glass solution is taken out and pours into fast shapingly in copper mold obtain block forerunner's glass, the block forerunner's glass obtained is put into 470 DEG C, electric furnace annealing 8 hours to eliminate internal stress and promotion microcrystallization.Sample, through surface finish, obtains green glow and red emission under 378nm and 980nm excites, and the emmission spectrum of embodiment 13 as shown in Figure 4.
The devitrified glass composition of table 4 embodiment 13-16
| Sequence number | SiO 2(g) | PbF 2(g) | ErF 3(g) |
| 13 | 2.9581 | 11.9511 | 0.1104 |
| 14 | 2.9581 | 11.9511 | 0.1656 |
| 15 | 4.4372 | 17.9267 | 0.1656 |
| 16 | 5.9162 | 23.9022 | 0.2208 |
Embodiment 17-20
SiO selected by matrix starting material
2, crystallite forming core Material selec-tion is BaF
2and ZnF
2, doping luminescent center ion is chosen as ErF
3.Proportion of raw material is 60%SiO
2, 20%BaF
2, 20%ZnF
2, doping ErF
3amount be total mass 2.5% and 5%.Above-mentioned powder raw material is weighed, is placed on and mixes in agate mortar and to add alcohol 2 milliliters grinding, be then placed in corundum crucible, put into electric furnace be heated to 1500 DEG C after insulation 30 minutes, make it abundant melting.Afterwards, glass solution is taken out and pours into fast shapingly in copper mold obtain block forerunner's glass, the block forerunner's glass obtained is put into 660 DEG C, electric furnace annealing 4 hours to eliminate internal stress and promotion microcrystallization.Sample, through surface finish, obtains green glow and red emission under 378nm and 980nm excites, and the emmission spectrum of embodiment 17 as shown in Figure 5.
The devitrified glass composition of table 5 embodiment 17-20
| Sequence number | BaF 2(g) | SiO 2(g) | ZnF 2(g) | ErF 3(g) |
| 17 | 5.5931 | 5.7504 | 3.2988 | 0.3577 |
| 18 | 5.5931 | 5.7504 | 3.2988 | 0.7154 |
| 19 | 8.8397 | 8.6256 | 4.9482 | 0.5366 |
| 20 | 11.1862 | 11.5008 | 6.5976 | 0.7154 |
Embodiment 21-24:
Al selected by matrix starting material
2o
3, Na
2cO
3, SiO
2, CaCO
3, crystallite forming core Material selec-tion is LuF
3and BaF
2, doping luminescent center ion is chosen as ErF
3.Proportion of raw material is 15%Al
2o
3, 10%Na
2cO
3, 43%SiO
2, 4%CaCO
3, (10%-x) LuF
3and 18%BaF
2, xErF
3, x=1%, 1.5%.Above-mentioned powder raw material is weighed, is placed on and mixes in agate mortar and to add alcohol 2 milliliters grinding, be then placed in corundum crucible, put into electric furnace be heated to 1500 DEG C after insulation 45 minutes, make it abundant melting.Afterwards, glass solution is taken out and pours into fast shapingly in copper mold obtain block forerunner's glass, the block forerunner's glass obtained is put into 640 DEG C, electric furnace annealing 2 hours to eliminate internal stress and promotion microcrystallization.Sample, through surface finish, obtains green glow and red emission under 378nm and 980nm excites, and the emmission spectrum of embodiment 21 as shown in Figure 6.
The devitrified glass composition of table 6 embodiment 21-24
| Sequence number | Al 2O 3(g) | Na 2CO 3(g) | SiO 2(g) | CaCO 3(g) | LuF 3(g) | BaF 2(g) | ErF 3(g) |
| 21 | 2.2941 | 1.5900 | 4.0554 | 0.6005 | 2.7562 | 4.7331 | 0.0271 |
| 22 | 2.2941 | 1.5900 | 4.0554 | 0.6005 | 2.7562 | 4.7331 | 0.0407 |
| 23 | 3.4412 | 2.3850 | 6.0831 | 0.9008 | 4.1343 | 7.1000 | 0.0407 |
| 24 | 4.5882 | 3.1800 | 8.1108 | 1.2010 | 5.5124 | 9.4662 | 0.0542 |
Claims (9)
1. one kind can simultaneously stability and conversion UV-light and the transparent glass ceramics of infrared light double frequency light, it is characterized in that, comprise substrate material, microcrystals material, doping luminescent center ion, matrix starting material are one or more mixtures in analytically pure oxide compound, borate, carbonate, crystallite forming core material is chemical pure fluorochemical, and doping luminescent center ion is Er
3+ion.
2. according to claim 1 can simultaneously stability and conversion UV-light and the transparent glass ceramics of infrared light double frequency light, it is characterized in that, matrix starting material are cheap Al
2o
3, Na
2cO
3, SiO
2, CaCO
3one or more mixtures, crystallite forming core material is YF
3, LaF
3, LuF
3, PbF
2, BaF
2in one or more mixtures.
3. according to claim 2 can simultaneously stability and conversion UV-light and the transparent glass ceramics of infrared light double frequency light, it consists of 15%-25%Al
2o
3, 10%-19%Na
2cO
3, 41%-60%SiO
2, 4%CaCO
3, 8%YF
3, 15%LaF
3, 8%-10%LuF
3, 50%PbF
2, 18%-20%BaF
2, 18%NaF, 20%ZnF
2, 1%-5%ErF
3.
4. according to claim 1 can simultaneously stability and conversion UV-light and the transparent glass ceramics preparation method of infrared light double frequency light, it is characterized in that, its preparation method comprises the following steps:
(a) raw material choose the mixing with glass batch
Silicate glass raw material is mainly analytically pure oxide compound, borate, one or more mixtures in carbonate, chemical pure fluorochemical; Rare earth ion selects the fluorochemical of purity 99.99%; Accurately take glass batch, ground and mixed in mortar;
B () glass smelting comprises the Crystallizing treatment of forerunner's glass melt chilling and forerunner's glass;
C material is positioned in crucible and processes glass melting temperature by () is 1000-1500 DEG C, and the time is 0.5-1 hour; Annealing temperature is 470-680 DEG C, insulation 1-8 hour.
5. according to claim 4 can simultaneously stability and conversion UV-light and the transparent glass ceramics preparation method of infrared light double frequency light, it is characterized in that, step (a) matrix starting material are cheap Al
2o
3, Na
2cO
3, SiO
2, CaCO
3one or more mixtures, crystallite forming core material is YF
3, LaF
3, LuF
3, PbF
2, BaF
2in one or more mixtures.
6. according to claim 5 can simultaneously stability and conversion UV-light and the transparent glass ceramics preparation method of infrared light double frequency light, it is characterized in that, consist of 15%-25%Al
2o
3, 10%-19%Na
2cO
3, 41%-60%SiO
2, 4%CaCO
3, 8%YF
3, 15%LaF
3, 8%-10%LuF
3, 50%PbF
2, 18%-20%BaF
2, 18%NaF, 20%ZnF
2, 1%-5%ErF
3.
7. according to claim 4 can simultaneously stability and conversion UV-light and the transparent glass ceramics preparation method of infrared light double frequency light, it is characterized in that, the crucible used in step (c) preparation process is platinum crucible or corundum crucible.
8. according to claim 4 can simultaneously stability and conversion UV-light and the transparent glass ceramics preparation method of infrared light double frequency light, it is characterized in that, step (a) is adulterated luminescence center Er
3+the quality of ion is 0.0271 gram-0.2208 gram.
9. according to claim 4 can simultaneously stability and conversion UV-light and the transparent glass ceramics preparation method of infrared light double frequency light, it is characterized in that, in the ground and mixed process of step (a) admixtion, add 2 ml ethanols.
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| CN104961343A (en) * | 2015-06-26 | 2015-10-07 | 中国计量学院 | Rare-earth-doped microcrystalline glass separating out NaYF4 nanocrystalline and manufacturing method thereof |
| CN105481254A (en) * | 2015-11-27 | 2016-04-13 | 南京邮电大学 | Transparent glass ceramic with functions of light conversion and light and temperature sensing and preparation method thereof |
| CN114716148A (en) * | 2021-01-05 | 2022-07-08 | 长春理工大学 | Visible light/laser/infrared/radar compatible stealth material and preparation method thereof |
| CN116477930A (en) * | 2023-03-17 | 2023-07-25 | 江苏师范大学 | Method for preparing large-size nanocrystalline transparent ceramic through nano metal nucleating agent |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104961343A (en) * | 2015-06-26 | 2015-10-07 | 中国计量学院 | Rare-earth-doped microcrystalline glass separating out NaYF4 nanocrystalline and manufacturing method thereof |
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| CN114716148A (en) * | 2021-01-05 | 2022-07-08 | 长春理工大学 | Visible light/laser/infrared/radar compatible stealth material and preparation method thereof |
| CN116477930A (en) * | 2023-03-17 | 2023-07-25 | 江苏师范大学 | Method for preparing large-size nanocrystalline transparent ceramic through nano metal nucleating agent |
| CN116477930B (en) * | 2023-03-17 | 2024-07-05 | 江苏师范大学 | Method for preparing large-size nanocrystalline transparent ceramic through nano metal nucleating agent |
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