CN114230182B - Rare earth doped transparent photoelectric niobate glass ceramic material and preparation method thereof - Google Patents
Rare earth doped transparent photoelectric niobate glass ceramic material and preparation method thereof Download PDFInfo
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- CN114230182B CN114230182B CN202111536211.3A CN202111536211A CN114230182B CN 114230182 B CN114230182 B CN 114230182B CN 202111536211 A CN202111536211 A CN 202111536211A CN 114230182 B CN114230182 B CN 114230182B
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- 239000006112 glass ceramic composition Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 7
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 10
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 10
- 239000013078 crystal Substances 0.000 claims abstract description 8
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 6
- 229910000906 Bronze Inorganic materials 0.000 claims abstract description 3
- 239000010974 bronze Substances 0.000 claims abstract description 3
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 claims abstract description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000010937 tungsten Substances 0.000 claims abstract description 3
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 3
- 239000011521 glass Substances 0.000 claims description 27
- 239000011159 matrix material Substances 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 8
- 239000010949 copper Substances 0.000 claims description 8
- 229910052802 copper Inorganic materials 0.000 claims description 8
- 239000000156 glass melt Substances 0.000 claims description 8
- 238000000137 annealing Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- 238000009529 body temperature measurement Methods 0.000 abstract description 15
- 230000003287 optical effect Effects 0.000 abstract description 9
- 238000002834 transmittance Methods 0.000 abstract description 8
- 238000004146 energy storage Methods 0.000 abstract description 5
- 239000002241 glass-ceramic Substances 0.000 description 22
- 239000000203 mixture Substances 0.000 description 18
- 230000035945 sensitivity Effects 0.000 description 12
- 238000004321 preservation Methods 0.000 description 7
- 230000005684 electric field Effects 0.000 description 6
- 239000004570 mortar (masonry) Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 239000000523 sample Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 3
- 238000000411 transmission spectrum Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- -1 rare earth ions Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000075 oxide glass Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000004861 thermometry Methods 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
Abstract
The invention discloses a rare earth doped transparent photoelectric niobate glass ceramic material and a preparation method thereof, wherein the glass ceramic material comprises RR 'with a tungsten bronze structure' 2 Nb 5 O 15 Crystal and R' Nb having orthogonal structure 2 O 6 Crystals (r=na, K; R' =ca, sr, ba) and Yb 2 O 3 、Tm 2 O 3 、Er 2 O 3 、Ho 2 O 3 、Tb 4 O 7 And Eu 2 O 3 Two or more rare earth oxides of (3). Wherein the proportion of each oxide is as follows: 8 to 15mol% of R 2 O,20 to 27mol percent of R' O,23 to 28mol percent of SiO 2 3 to 6mol% of Al 2 O 3 5 to 9 mol% of B 2 O 3 28 to 35mol% of Nb 2 O 5 Mixed rare earth oxide accounting for 0.3-3.1 mol% of the total oxide is added. The invention can solve the problem of realizing multi-mode temperature measurement in a wide temperature range, and has high light transmittance, optical temperature measurement and energy storage performance.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a multifunctional transparent niobate glass ceramic material with high light transmittance, optical temperature measurement property, dielectric property and energy storage property.
Background
The non-contact optical temperature measurement technology has the advantages of non-contact temperature measurement, high response speed, high sensitivity and the like, and is suitable for temperature measurement in various severe environments (including biological tissues, corrosion and high pressure) by measuring the change of the fluorescence property of the material along with the temperature to detect the temperature. Most of the fluorescent materials disclosed as temperature probes realize temperature measurement by using the fluorescence intensity ratio of a luminescence center based on the thermal coupling energy level, but the emission band at the non-thermal coupling energy level is not well utilized. If based on thermally and non-thermally coupled energy levels, multimode temperature measurements can be successfully achieved over a wide temperature range by calculation using the fluorescence intensity ratios of the multiple emission bands.
Disclosure of Invention
The invention aims to provide a novel niobate transparent glass ceramic material with high light transmittance, optical temperature measurement and energy storage performance, and solves the problem of realizing multi-mode temperature measurement in a wide temperature range. The glass ceramic material provided by the invention takes niobate glass as a matrix, and the oxide glass matrix comprises R 2 O（R=Na，K）、R′O(R′= Ca，Sr，Ba）、Al 2 O 3 、B 2 O 3 、SiO 2 And Nb (Nb) 2 O 5 And is doped with various rare earth ions (Yb 3+ 、Tm 3+ 、Er 3+ 、Ho 3+ 、Tb 3+ 、Dy 3+ And Eu 3+ Two or more of the following). The glass ceramic material mainly comprises RR 'with tungsten bronze structure' 2 Nb 5 O 15 (r=na, K, R' =ca, sr, ba) crystals, e.g. NaSr 2 Nb 5 O 15 、NaBa 2 Nb 5 O 15 And KSr 2 Nb 5 O 15 And R' Nb having an orthogonal structure 2 O 6 (R' =ca, sr, ba) crystals, e.g. CaNb 2 O 6 And BaNb 2 O 6 . These precipitated crystalsThe type and content have a direct impact on the optical, dielectric and energy storage properties of the glass-ceramic, where the rare earth species doped is critical to obtain multimode temperature measurements and has a direct impact on the optical temperature measurement sensitivity. The opposite temperature dependence of the rare earth ion emission band is utilized to obtain higher optical temperature measurement sensitivity, and the regulation of the grain size and crystallization number of the glass ceramic is a key for influencing the transparency of the glass ceramic and the electrical property of the glass ceramic.
The invention also provides a preparation method of the glass ceramic material.
In the preparation raw materials of the glass ceramic material, the preferable values of the proportions of the oxides are respectively as follows: 8 to 15mol% of R 2 O (r=na, K); 20-27 mol% of R 'O (R' =ca, sr, ba); 23 to 28mol% of SiO 2 The method comprises the steps of carrying out a first treatment on the surface of the 3 to 6mol% of Al 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the 5 to 9 mol% of B 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the 28 to 35mol% of Nb 2 O 5 . Adding mixed rare earth oxide accounting for 0.3-3.1 mol% of the total amount of the oxide, wherein the mixed rare earth oxide is prepared from Yb 2 O 3 、Tm 2 O 3 、Er 2 O 3 、Ho 2 O 3 、Tb 4 O 7 And Eu 2 O 3 Two or more of the above materials are mixed.
The preparation method of the glass ceramic material comprises the following steps: grinding and uniformly mixing all the powder raw materials, then placing the powder raw materials into a crucible, heating to 1400-1500 ℃, and preserving heat for 1-2 hours; then pouring the obtained glass melt into a copper mold preheated at 550-600 ℃ for molding and annealing to obtain matrix glass; cutting the substrate glass into glass flakes, and then carrying out heat preservation at 710-770 ℃ for 0.5-3 hours to obtain the glass ceramic material.
Drawings
FIG. 1 is an X-ray diffraction pattern of samples of examples 1, 2, 3, and 4 of the present invention; FIG. 2 is a graph showing the transmission spectrum of the sample of example 1 of the present invention; FIG. 3 is a graph showing the temperature dependent emission spectrum of the sample of example 1 of the present invention; FIG. 4 is a graph of optical thermometry sensitivity of a sample of example 1 of the invention; FIG. 5 is a graph of measured discharge energy density for a sample of example 1 of the present invention.
Detailed Description
The invention will be further illustrated with reference to specific examples.
Example 1:
na is mixed with 2 CO 3 、SrCO 3 、SiO 2 、H 3 BO 3 、Al 2 O 3 、Nb 2 O 5 、Yb 2 O 3 、Tm 2 O 3 、Er 2 O 3 Powder according to 15Na 2 O：20SrO：25SiO 2 ：5B 2 O 3 ：3Al 2 O 3 ：35Nb 2 O 5 (mole percent) plus 2.0Yb 2 O 3 、0.05Tm 2 O 3 、0.05Ho 2 O 3 The (mol percent) is calculated and weighed, then is placed in a mortar, ground for more than 0.5 hour to be uniformly mixed, then is placed in a crucible, and is heated to 1500 ℃ in a high-temperature resistance furnace and then is kept for 2 hours to be fully melted; then, rapidly pouring the glass melt into a copper mold preheated at 580 ℃ for forming; putting the formed glass into a muffle furnace with heat preservation at 580 ℃ for annealing for 10 hours, and then cooling along with the furnace to obtain matrix glass; placing the obtained matrix glass into a resistance furnace, and preserving heat at 750 ℃ for 0.5 hour to obtain NaSr 2 Nb 5 O 15 Transparent glass ceramics. The glass ceramic has a transmittance of 39% -75% in the range of 500-700 nm and a maximum relative sensitivity of 2.0% K in the temperature range of 298-698K -1 The method comprises the steps of carrying out a first treatment on the surface of the Applying 600KV/cm electric field at room temperature to obtain glass ceramic with measured discharge energy density up to 1.15J/cm 3 。
Example 2:
na is mixed with 2 CO 3 、BaCO 3 、SiO 2 、H 3 BO 3 、Al 2 O 3 、Nb 2 O 5 、Yb 2 O 3 、Er 2 O 3 Powder according to 13Na 2 O：27BaO：25SiO 2 ：9B 2 O 3 ：6Al 2 O 3 ：28Nb 2 O 5 (mole percent) plus 2.0Yb 2 O 3 、0.05Er 2 O 3 The (mol percent) is calculated and weighed, then is placed in a mortar, ground for more than 0.5 hour to be uniformly mixed, then is placed in a crucible, and is heated to 1500 ℃ in a high-temperature resistance furnace and then is kept for 2 hours to be fully melted; then, rapidly pouring the glass melt into a copper mold preheated at 550 ℃ for forming, and putting the formed glass into a muffle furnace with heat preservation at 550 ℃ for annealing for 10 hours and then cooling along with the furnace to obtain matrix glass; and placing the obtained matrix glass into a resistance furnace, and preserving heat for 3 hours at 760 ℃ to obtain the transparent glass ceramic. X-ray diffraction patterns indicate that NaBa is precipitated in a glass matrix 2 Nb 5 O 15 The crystal phase and the transmission spectrum diagram show that the glass ceramic is a transparent glass ceramic material, and the transmittance of the glass ceramic is not less than 30% within the range of 500-700 nm. The temperature-changing up-conversion emission spectrum is tested under the excitation of a 980nm laser, the luminous intensity of the three emission bands is reduced along with the temperature rise, a sensitivity curve is obtained by calculating the fluorescence intensity ratio, and the maximum relative sensitivity is 1.19% in the temperature range of 298-698K. Applying 600KV/cm electric field at room temperature to obtain glass ceramic with measured discharge energy density up to 1.53J/cm 3 。
Example 3:
will K 2 CO 3 、SrCO 3 、SiO 2 、H 3 BO 3 、Al 2 O 3 、Nb 2 O 5 、Yb 2 O 3 、Tm 2 O 3 Powder according to 8K 2 O：27SrO：25SiO 2 ：5B 2 O 3 ：4Al 2 O 3 ：32Nb 2 O 5 (mole percent) plus 1.5Yb 2 O 3 、0.05Tm 2 O 3 The mixture ratio of the (mole percent) is calculated and weighed, and then the mixture is placed in a mortar, and the mixture is ground for more than 0.5 hour to be uniformly mixed; then placing the mixture into a crucible, heating the mixture to 1500 ℃ in a high-temperature resistance furnace, and preserving heat for 2 hours to enable the mixture to be fully melted; then the glass melt is quickly poured into a copper mold preheated at 560 ℃ for forming; putting the formed glass into a muffle furnace with heat preservation at 560 ℃ for annealing for 10 hours, and then cooling along with the furnace to obtain matrix glass; placing the obtained matrix glass into a resistance furnace at 750Preserving the temperature for 1 hour at the temperature to obtain KSr 2 Nb 5 O 15 The transparent glass ceramic has a transmittance of not less than 32% in the range of 500-700 nm. The maximum relative sensitivity of the glass ceramic is 2.15% K when tested in the temperature range of 298-673K -1 . The measured discharge energy density of the glass ceramic under 600KV/cm electric field at room temperature reaches 1.32J/cm 3 。
Example 4:
will K 2 CO 3 、BaCO 3 、SiO 2 、H 3 BO 3 、Al 2 O 3 、Nb 2 O 5 、Yb 2 O 3 、Tm 2 O 3 、Er 2 O 3 Powder according to 13K 2 O：20BaO：25SiO 2 ：5B 2 O 3 ：4Al 2 O 3 ：32Nb 2 O 5 (mole percent) plus 2Yb 2 O 3 、0.05Tm 2 O 3 And 0.05Er 2 O 3 The mixture ratio of the (mole percent) is calculated and weighed, and then the mixture is placed in a mortar, and the mixture is ground for more than 1 hour to be uniformly mixed; then placing the mixture into a crucible, heating the mixture to 1500 ℃ in a high-temperature resistance furnace, and preserving heat for 2 hours to enable the mixture to be fully melted; then, rapidly pouring the glass melt into a copper mold preheated at 570 ℃ for forming; the formed glass is put into a muffle furnace with heat preservation at 570 ℃ for annealing for 10 hours and then cooled along with the furnace, so as to obtain matrix glass; placing the obtained matrix glass into a heat treatment resistance furnace, and preserving heat at 760 ℃ for 2 hours to obtain BaNb 2 O 6 The transparent glass ceramic has a transmittance of not less than 35% in the range of 500-700 nm. The sensitivity of the glass ceramic is 0.97% K in the temperature range 298-673K -1 The measured discharge energy density of the glass ceramic at room temperature under the electric field of 700kV/cm is 1.0J/cm 3 。
Example 5:
na is mixed with 2 CO 3 、CaCO 3 、SiO 2 、H 3 BO 3 、Al 2 O 3 、Nb 2 O 5 、Yb 2 O 3 、Er 2 O 3 Powder according to 13Na 2 O：21CaO：25SiO 2 ：5B 2 O 3 ：4Al 2 O 3 ：32Nb 2 O 5 (mole percent) plus 0.25Yb 2 O 3 、0.05Er 2 O 3 The (mol percent) is calculated and weighed, then is placed in a mortar, ground for more than 0.5 hour to be uniformly mixed, then is placed in a crucible, and is heated to 1500 ℃ in a high-temperature resistance furnace and then is kept for 2 hours to be fully melted; then, rapidly pouring the glass melt into a copper mold preheated at 560 ℃ for forming, and putting the formed glass into a muffle furnace with heat preservation at 560 ℃ for annealing for 10 hours and then cooling along with the furnace to obtain matrix glass; and placing the obtained matrix glass into a resistance furnace, and preserving heat for 2 hours at 760 ℃ to obtain the transparent glass ceramic. X-ray diffraction patterns indicate that NaBa is precipitated in a glass matrix 2 Nb 5 O 15 The crystal phase and the transmission spectrum chart show that the glass ceramic is a transparent glass ceramic material, the variable temperature up-conversion emission spectrum is tested under the excitation of a 980nm laser, the luminous intensity of the three emission bands is reduced along with the rising of the temperature, the sensitivity curve is obtained by calculating the fluorescence intensity ratio, and the maximum relative sensitivity is 1.21% in the temperature range of 298-698K. The measured energy density reaches 1.13J/cm under the electric field of 600KV/cm at room temperature 3 。
Example 6:
will K 2 CO 3 、SrCO 3 、SiO 2 、H 3 BO 3 、Al 2 O 3 、Nb 2 O 5 、Yb 2 O 3 、Tm 2 O 3 Powder according to 13K 2 O：21SrO：25SiO 2 ：5B 2 O 3 ：4Al 2 O 3 ：32Nb 2 O 5 (mole percent) plus 3Yb 2 O 3 、0.05Tm 2 O 3 、0.05Er 2 O 3 The mixture ratio of the (mole percent) is calculated and weighed, and then the mixture is placed in a mortar, and the mixture is ground for more than 0.5 hour to be uniformly mixed; then placing the mixture into a crucible, heating the mixture to 1500 ℃ in a high-temperature resistance furnace, and preserving heat for 2 hours to enable the mixture to be fully melted; then the glass melt is quickly poured into a copper mold preheated at 590 ℃ for forming; placing the shaped glass intoAnnealing in a muffle furnace with heat preservation at 590 ℃ for 10 hours, and cooling along with the furnace to obtain matrix glass; placing the obtained matrix glass into a heat treatment resistance furnace, and preserving the temperature at 710 ℃ for 2 hours to obtain KSr 2 Nb 5 O 15 The transparent glass ceramic has a transmittance of not less than 32% in the range of 500-700 nm. The maximum relative sensitivity of the glass ceramic is 2.1% K when tested in the temperature range of 298-698K -1 . The measured discharge energy density of the glass ceramic under 600KV/cm electric field at room temperature reaches 1.25J/cm 3 。
The invention has the beneficial effects that:
the glass ceramic material provided by the invention can solve the problem of realizing multi-mode temperature measurement in a wide temperature range, and has high light transmission, optical temperature measurement and energy storage performance.
Claims (1)
1. A rare earth doped transparent photoelectric niobate glass ceramic material is characterized in that the glass ceramic material comprises RR 'with tungsten bronze structure' 2 Nb 5 O 15 Crystal and R' Nb having orthogonal structure 2 O 6 A crystal, wherein r=na or K, R' =ca, sr or Ba; the proportion of each oxide in the glass ceramic material is as follows: 8 to 15mol% of R 2 O,20 to 27mol percent of R' O,23 to 28mol percent of SiO 2 3 to 6mol% of Al 2 O 3 5 to 9 mol% of B 2 O 3 28 to 35mol% of Nb 2 O 5 Adding mixed rare earth oxide accounting for 0.3-3.1 mol% of the total oxide; the mixed rare earth oxide is made of Yb 2 O 3 、Tm 2 O 3 、Er 2 O 3 、Ho 2 O 3 、Tb 4 O 7 And Eu 2 O 3 Two or more of them are mixed; the preparation method of the glass ceramic material comprises the following steps: grinding and uniformly mixing all powder raw materials, placing the powder raw materials into a crucible, heating to 1400-1500 ℃, and preserving heat for 1-2 hours; then pouring the obtained glass melt into a copper mold preheated at 550-600 ℃ for molding and annealing to obtain matrix glass; cutting the substrate glass into glass flakes, and then preserving the heat at 710-770 ℃ for 0.5-3 hoursAnd (5) treating to obtain the glass ceramic material.
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| Title |
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| Improvement in structural, dielectric and energy-storage properties of lead-free niobate glass-ceramic with Sm2O3;Yi Zhou等;《Journal of the European Ceramic Society》;第995-999页 * |
| Na_2O含量对BaO-SrO-Nb_2O_5-B_2O_3-SiO_2系玻璃陶瓷微结构和性能的影响;张文俊;陈国华;周昌荣;江民红;王华;刘心宇;;中国有色金属学报(06);第1-8页 * |
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