CN116477838A - Lanthanum oxide modified high borosilicate glass and preparation method thereof - Google Patents
Lanthanum oxide modified high borosilicate glass and preparation method thereof Download PDFInfo
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- CN116477838A CN116477838A CN202310444706.6A CN202310444706A CN116477838A CN 116477838 A CN116477838 A CN 116477838A CN 202310444706 A CN202310444706 A CN 202310444706A CN 116477838 A CN116477838 A CN 116477838A
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- 239000005388 borosilicate glass Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 title claims description 8
- 238000000137 annealing Methods 0.000 claims abstract description 23
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 238000000465 moulding Methods 0.000 claims abstract description 15
- 238000003723 Smelting Methods 0.000 claims abstract description 12
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 9
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000011521 glass Substances 0.000 claims description 17
- 238000002844 melting Methods 0.000 claims description 17
- 230000008018 melting Effects 0.000 claims description 17
- 238000000498 ball milling Methods 0.000 claims description 13
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims description 10
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 239000011812 mixed powder Substances 0.000 claims description 9
- 239000006060 molten glass Substances 0.000 claims description 9
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 239000004615 ingredient Substances 0.000 claims description 7
- 239000000155 melt Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims 2
- 239000011734 sodium Substances 0.000 claims 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims 1
- 229910000019 calcium carbonate Inorganic materials 0.000 claims 1
- 239000013078 crystal Substances 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 claims 1
- 239000000843 powder Substances 0.000 claims 1
- 229910000029 sodium carbonate Inorganic materials 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000012545 processing Methods 0.000 abstract description 2
- 229910044991 metal oxide Inorganic materials 0.000 abstract 1
- 150000004706 metal oxides Chemical class 0.000 abstract 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 10
- 239000000156 glass melt Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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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
- C03C3/095—Glass compositions containing silica with 40% to 90% silica, by weight containing rare earths
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- 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
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
- Glass Compositions (AREA)
Abstract
本发明涉及一种氧化镧改性高硼硅玻璃及其制备方法，属于高硼硅玻璃制备生产的技术领域，本发明目的是优化现有高硼硅玻璃的组成，提供一种氧化镧改性高硼硅玻璃及其制备方法。本发明是在原有高硼硅玻璃组成的基础上掺杂金属氧化物，制备过程包括配料、熔炼、成型、退火、加工，本发明提供的方法制备的氧化镧改性高硼硅玻璃具有更优异的密度、折射率、化学稳定性和热膨胀系数。The invention relates to a lanthanum oxide-modified high borosilicate glass and a preparation method thereof, belonging to the technical field of preparation and production of high borosilicate glass. The purpose of the invention is to optimize the composition of the existing high borosilicate glass and provide a lanthanum oxide-modified high borosilicate glass and a preparation method thereof. The present invention is to dope metal oxides on the basis of the original high borosilicate glass composition. The preparation process includes batching, smelting, molding, annealing, and processing. The lanthanum oxide-modified high borosilicate glass prepared by the method provided by the present invention has more excellent density, refractive index, chemical stability and thermal expansion coefficient.
Description
技术领域technical field
本发明涉及玻璃制备生产的技术领域，具体涉一种氧化镧改性高硼硅玻璃及其制备方法。The invention relates to the technical field of glass preparation and production, in particular to a lanthanum oxide-modified high borosilicate glass and a preparation method thereof.
背景技术Background technique
高硼硅玻璃的耐火性能好，物理强度高，与普遍玻璃相比，无毒副作用，其机械性能，热稳定性能，抗水、抗碱、抗酸等性能大大提高。因此，可广泛用于化工、航天、军事、家庭、医院等各个领域，可制成灯具、餐具、标盘、望远镜片、洗衣机观察孔、微波炉盘、太阳能热水器等多种产品，具有良好的推广价值和社会效益。High borosilicate glass has good fire resistance and high physical strength. Compared with ordinary glass, it has no toxic side effects, and its mechanical properties, thermal stability, water resistance, alkali resistance, and acid resistance are greatly improved. Therefore, it can be widely used in various fields such as chemical industry, aerospace, military affairs, family, hospital, etc., and can be made into various products such as lamps, tableware, standard plates, telescope sheets, washing machine observation holes, microwave oven plates, solar water heaters, etc., and has good promotion value and social benefits.
但是，由于高硼硅玻璃熔化温度高、耗热量大、熔化率低、澄清均化困难，使高硼硅玻璃生产质量控制难度大。同时，高硼硅酸盐玻璃产品又要求具有良好的抗化学侵蚀性能、优异的抗热冲击性能、机械性能、较高的软化温度和良好的工艺性能等。因此，在选择高硼硅酸盐玻璃成分时，既要满足和达到以上要求，又要考虑到该玻璃在熔制、成型、退火、加工等工艺技术上的可行性。However, due to the high melting temperature of high borosilicate glass, high heat consumption, low melting rate and difficulty in clarification and homogenization, it is difficult to control the quality of high borosilicate glass production. At the same time, high borosilicate glass products are required to have good chemical corrosion resistance, excellent thermal shock resistance, mechanical properties, high softening temperature and good process performance. Therefore, when selecting high borosilicate glass components, it is necessary to meet and meet the above requirements, but also to consider the feasibility of the glass in melting, forming, annealing, processing and other technological processes.
基于以上原因，本发明设计了一种氧化镧改性高硼硅玻璃及其制备方法。Based on the above reasons, the present invention designs a lanthanum oxide modified high borosilicate glass and a preparation method thereof.
发明内容Contents of the invention
本发明目的是优化现有高硼硅玻璃的组成，提供一种氧化镧改性高硼硅玻璃及其制备方法，制备的高硼硅玻璃具有高折射率、高密度、优异的化学稳定性和低热膨胀系数等优点。本发明可以得到高折射率、高密度、优异的化学稳定性和低热膨胀系数的高硼硅玻璃。The purpose of the present invention is to optimize the composition of the existing high borosilicate glass, and provide a lanthanum oxide modified high borosilicate glass and its preparation method. The prepared high borosilicate glass has the advantages of high refractive index, high density, excellent chemical stability and low thermal expansion coefficient. The invention can obtain high borosilicate glass with high refractive index, high density, excellent chemical stability and low thermal expansion coefficient.
（1）配料：按照质量百分比称取制备高硼硅玻璃的原料，SiO279%、B2O312%、Na2O4%、CaO 3%、Al2O32%，掺杂的La2O3按质量百分数计分别为3%、6%、9%、12%和15%，将原料混合均匀得到混合粉体；(1) Ingredients: Weigh the raw materials for the preparation of high borosilicate glass according to the mass percentage, SiO 2 79%, B 2 O 3 12%, Na 2 O 4%, CaO 3%, Al 2 O 3 2%, and the doped La 2 O 3 are 3%, 6%, 9%, 12% and 15% in mass percentage, and mix the raw materials evenly to obtain a mixed powder;
（2）熔炼：将步骤（1）的混合粉体在1600°C熔炼3小时，直至溶体澄清匀化，得到玻璃熔融液；(2) Melting: melting the mixed powder in step (1) at 1600°C for 3 hours until the melt is clarified and homogenized to obtain molten glass;
（3）成型：将步骤（2）所得玻璃熔融液倒入已预热到560°C的石墨模具中成型；(3) Molding: Pour the molten glass obtained in step (2) into a graphite mold preheated to 560°C for molding;
（4）退火：将步骤（3）初步成型后的玻璃放入已经加热到560°C的退火炉中退火1小时，然后随炉自然冷却至室温；(4) Annealing: Put the preliminarily formed glass in step (3) into an annealing furnace heated to 560°C for annealing for 1 hour, and then naturally cool to room temperature with the furnace;
（5）将步骤（4）所得玻璃进行打磨、清洗、烘干，得到本发明La2O3改性的高硼硅玻璃。(5) Grinding, cleaning and drying the glass obtained in step (4) to obtain the La 2 O 3 modified high borosilicate glass of the present invention.
本发明可以得到高折射率、高密度、优异的化学稳定性和低热膨胀系数的高硼硅玻璃。The invention can obtain high borosilicate glass with high refractive index, high density, excellent chemical stability and low thermal expansion coefficient.
具体实施方式Detailed ways
实例1:Example 1:
（1）配料：按照质量百分比称取制备高硼硅玻璃的原料至球磨罐中，SiO279%、B2O312%、Na2O 4%、CaO 3%、Al2O32%，掺杂的La2O3质量分数为3%；采用无水乙醇为球磨介质，以280 rpm的转速球磨8小时，将混合料烘干、粉碎，得到混合粉体；(1) Ingredients: Weigh the raw materials for the preparation of high borosilicate glass into a ball milling tank according to the mass percentage, SiO 2 79%, B 2 O 3 12%, Na 2 O 4%, CaO 3%, Al 2 O 3 2%, and the mass fraction of doped La 2 O 3 is 3%; use absolute ethanol as the ball milling medium, ball mill at a speed of 280 rpm for 8 hours, dry and pulverize the mixture to obtain a mixed powder;
（2）熔炼：将步骤（1）的混合料进行熔炼，熔炼控温程序为熔炼控温程序为室温到400℃升温速率2℃/min，400℃到1200℃升温速率5℃/min，1200℃到1600℃升温速率1℃/min并保温3小时，直至溶体澄清匀化，得到玻璃熔融液；(2) Melting: Melting the mixture in step (1), the smelting temperature control program is the smelting temperature control program is room temperature to 400 °C heating rate 2 °C/min, 400 °C to 1200 °C heating rate 5 °C/min, 1200 °C to 1600 °C heating rate 1 °C/min and keep warm for 3 hours until the melt is clarified and homogenized to obtain a glass melt;
（3）成型：将步骤（2）所得玻璃熔融液倒入已预热到560°C的石墨模具中成型；(3) Molding: Pour the molten glass obtained in step (2) into a graphite mold preheated to 560°C for molding;
（4）退火：将步骤（3）初步成型后的玻璃放入已经加热到560°C的退火炉中退火1小时，然后随炉自然冷却至室温；(4) Annealing: Put the preliminarily formed glass in step (3) into an annealing furnace heated to 560°C for annealing for 1 hour, and then naturally cool to room temperature with the furnace;
（5）将步骤（4）所得玻璃进行打磨、清洗、烘干，得到本发明ZrO2改性的高硼硅玻璃。(5) Grinding, cleaning and drying the glass obtained in step (4) to obtain the ZrO2 modified borosilicate glass of the present invention.
本发明可以得到高折射率、高密度、优异的化学稳定性和低热膨胀系数的高硼硅玻璃。The invention can obtain high borosilicate glass with high refractive index, high density, excellent chemical stability and low thermal expansion coefficient.
实例2：Example 2:
（1）配料：按照质量百分比称取制备高硼硅玻璃的原料至球磨罐中，SiO279%、B2O312%、Na2O 4%、CaO 3%、Al2O32%，掺杂的La2O3质量分数为6%；采用无水乙醇为球磨介质，以280 rpm的转速球磨8小时，将混合料烘干、粉碎，得到混合粉体；(1) Ingredients: Weigh the raw materials for the preparation of high borosilicate glass into a ball milling tank according to the mass percentage, SiO 2 79%, B 2 O 3 12%, Na 2 O 4%, CaO 3%, Al 2 O 3 2%, and the mass fraction of doped La 2 O 3 is 6%; use absolute ethanol as the ball milling medium, ball mill at a speed of 280 rpm for 8 hours, dry and pulverize the mixture to obtain a mixed powder;
（2）熔炼：将步骤（1）的混合料进行熔炼，熔炼控温程序为熔炼控温程序为室温到400℃升温速率2℃/min，400℃到1200℃升温速率5℃/min，1200℃到1600℃升温速率1℃/min并保温3小时，直至溶体澄清匀化，得到玻璃熔融液；(2) Melting: Melting the mixture in step (1), the smelting temperature control program is the smelting temperature control program is room temperature to 400 °C heating rate 2 °C/min, 400 °C to 1200 °C heating rate 5 °C/min, 1200 °C to 1600 °C heating rate 1 °C/min and keep warm for 3 hours until the melt is clarified and homogenized to obtain a glass melt;
（3）成型：将步骤（2）所得玻璃熔融液倒入已预热到560°C的石墨模具中成型；(3) Molding: Pour the molten glass obtained in step (2) into a graphite mold preheated to 560°C for molding;
（4）退火：将步骤（3）初步成型后的玻璃放入已经加热到560°C的退火炉中退火1小时，然后随炉自然冷却至室温；(4) Annealing: Put the preliminarily formed glass in step (3) into an annealing furnace heated to 560°C for annealing for 1 hour, and then naturally cool to room temperature with the furnace;
（5）将步骤（4）所得玻璃进行打磨、清洗、烘干，得到本发明ZrO2改性的高硼硅玻璃。(5) Grinding, cleaning and drying the glass obtained in step (4) to obtain the ZrO2 modified borosilicate glass of the present invention.
本发明可以得到高折射率、高密度、优异的化学稳定性和低热膨胀系数的高硼硅玻璃。The invention can obtain high borosilicate glass with high refractive index, high density, excellent chemical stability and low thermal expansion coefficient.
实例3：Example 3:
（1）配料：按照质量百分比称取制备高硼硅玻璃的原料至球磨罐中，SiO279%、B2O312%、Na2O 4%、CaO 3%、Al2O32%，掺杂的La2O3质量分数为9%；采用无水乙醇为球磨介质，以280 rpm的转速球磨8小时，将混合料烘干、粉碎，得到混合粉体；(1) Ingredients: Weigh the raw materials for preparing high borosilicate glass into a ball milling tank according to the mass percentage, SiO 2 79%, B 2 O 3 12%, Na 2 O 4%, CaO 3%, Al 2 O 3 2%, and the mass fraction of doped La 2 O 3 is 9%; use absolute ethanol as the ball milling medium, ball mill at a speed of 280 rpm for 8 hours, dry and pulverize the mixture to obtain a mixed powder;
（2）熔炼：将步骤（1）的混合料进行熔炼，熔炼控温程序为熔炼控温程序为室温到400℃升温速率2℃/min，400℃到1200℃升温速率5℃/min，1200℃到1600℃升温速率1℃/min并保温3小时，直至溶体澄清匀化，得到玻璃熔融液；(2) Melting: Melting the mixture in step (1), the smelting temperature control program is the smelting temperature control program is room temperature to 400 °C heating rate 2 °C/min, 400 °C to 1200 °C heating rate 5 °C/min, 1200 °C to 1600 °C heating rate 1 °C/min and keep warm for 3 hours until the melt is clarified and homogenized to obtain a glass melt;
（3）成型：将步骤（2）所得玻璃熔融液倒入已预热到560°C的石墨模具中成型；(3) Molding: Pour the molten glass obtained in step (2) into a graphite mold preheated to 560°C for molding;
（4）退火：将步骤（3）初步成型后的玻璃放入已经加热到560°C的退火炉中退火1小时，然后随炉自然冷却至室温；(4) Annealing: Put the preliminarily formed glass in step (3) into an annealing furnace heated to 560°C for annealing for 1 hour, and then naturally cool to room temperature with the furnace;
（5）将步骤（4）所得玻璃进行打磨、清洗、烘干，得到本发明ZrO2改性的高硼硅玻璃。(5) Grinding, cleaning and drying the glass obtained in step (4) to obtain the ZrO2 modified borosilicate glass of the present invention.
本发明可以得到高折射率、高密度、优异的化学稳定性和低热膨胀系数的高硼硅玻璃。The invention can obtain high borosilicate glass with high refractive index, high density, excellent chemical stability and low thermal expansion coefficient.
实例4：Example 4:
（1）配料：按照质量百分比称取制备高硼硅玻璃的原料至球磨罐中，SiO279%、B2O312%、Na2O 4%、CaO 3%、Al2O32%，掺杂的La2O3质量分数为12%；采用无水乙醇为球磨介质，以280 rpm的转速球磨8小时，将混合料烘干、粉碎，得到混合粉体；(1) Ingredients: Weigh the raw materials for the preparation of high borosilicate glass into a ball milling tank according to the mass percentage, SiO 2 79%, B 2 O 3 12%, Na 2 O 4%, CaO 3%, Al 2 O 3 2%, and the mass fraction of doped La 2 O 3 is 12%; use absolute ethanol as the ball milling medium, ball mill at a speed of 280 rpm for 8 hours, dry and pulverize the mixture to obtain a mixed powder;
（2）熔炼：将步骤（1）的混合料进行熔炼，熔炼控温程序为熔炼控温程序为室温到400℃升温速率2℃/min，400℃到1200℃升温速率5℃/min，1200℃到1600℃升温速率1℃/min并保温3小时，直至溶体澄清匀化，得到玻璃熔融液；(2) Melting: Melting the mixture in step (1), the smelting temperature control program is the smelting temperature control program is room temperature to 400 °C heating rate 2 °C/min, 400 °C to 1200 °C heating rate 5 °C/min, 1200 °C to 1600 °C heating rate 1 °C/min and keep warm for 3 hours until the melt is clarified and homogenized to obtain a glass melt;
（3）成型：将步骤（2）所得玻璃熔融液倒入已预热到560°C的石墨模具中成型；(3) Molding: Pour the molten glass obtained in step (2) into a graphite mold preheated to 560°C for molding;
（4）退火：将步骤（3）初步成型后的玻璃放入已经加热到560°C的退火炉中退火1小时，然后随炉自然冷却至室温；(4) Annealing: Put the preliminarily formed glass in step (3) into an annealing furnace heated to 560°C for annealing for 1 hour, and then naturally cool to room temperature with the furnace;
（5）将步骤（4）所得玻璃进行打磨、清洗、烘干，得到本发明ZrO2改性的高硼硅玻璃。(5) Grinding, cleaning and drying the glass obtained in step (4) to obtain the ZrO2 modified borosilicate glass of the present invention.
本发明可以得到高折射率、高密度、优异的化学稳定性和低热膨胀系数的高硼硅玻璃。The invention can obtain high borosilicate glass with high refractive index, high density, excellent chemical stability and low thermal expansion coefficient.
实例5：Example 5:
（1）配料：按照质量百分比称取制备高硼硅玻璃的原料至球磨罐中，SiO279%、B2O312%、Na2O 4%、CaO 3%、Al2O32%，掺杂的La2O3质量分数为15%；采用无水乙醇为球磨介质，以280 rpm的转速球磨8小时，将混合料烘干、粉碎，得到混合粉体；(1) Ingredients: Weigh the raw materials for preparing high borosilicate glass into a ball milling tank according to the mass percentage, SiO 2 79%, B 2 O 3 12%, Na 2 O 4%, CaO 3%, Al 2 O 3 2%, and the mass fraction of doped La 2 O 3 is 15%; use absolute ethanol as the ball milling medium, ball mill at a speed of 280 rpm for 8 hours, dry and pulverize the mixture to obtain a mixed powder;
（2）熔炼：将步骤（1）的混合料进行熔炼，熔炼控温程序为熔炼控温程序为室温到400℃升温速率2℃/min，400℃到1200℃升温速率5℃/min，1200℃到1600℃升温速率1℃/min并保温3小时，直至溶体澄清匀化，得到玻璃熔融液；(2) Melting: Melting the mixture in step (1), the smelting temperature control program is the smelting temperature control program is room temperature to 400 °C heating rate 2 °C/min, 400 °C to 1200 °C heating rate 5 °C/min, 1200 °C to 1600 °C heating rate 1 °C/min and keep warm for 3 hours until the melt is clarified and homogenized to obtain a glass melt;
（3）成型：将步骤（2）所得玻璃熔融液倒入已预热到560°C的石墨模具中成型；(3) Molding: Pour the molten glass obtained in step (2) into a graphite mold preheated to 560°C for molding;
（4）退火：将步骤（3）初步成型后的玻璃放入已经加热到560°C的退火炉中退火1小时，然后随炉自然冷却至室温；(4) Annealing: Put the preliminarily formed glass in step (3) into an annealing furnace heated to 560°C for annealing for 1 hour, and then naturally cool to room temperature with the furnace;
（5）将步骤（4）所得玻璃进行打磨、清洗、烘干，得到本发明ZrO2改性的高硼硅玻璃。(5) Grinding, cleaning and drying the glass obtained in step (4) to obtain the ZrO2 modified borosilicate glass of the present invention.
本发明可以得到高折射率、高密度、优异的化学稳定性和低热膨胀系数的高硼硅玻璃。The invention can obtain high borosilicate glass with high refractive index, high density, excellent chemical stability and low thermal expansion coefficient.
表1 本发明制备的高硼硅玻璃性能测试结果Table 1 Performance test results of borosilicate glass prepared by the present invention
Claims (7)
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| JP2008297162A (en) * | 2007-05-31 | 2008-12-11 | Ｈｏｙａ Ｃａｎｄｅｏ Ｏｐｔｒｏｎｉｃｓ株式会社 | Glass composition for joining quartz glass body, glass paste for joining quartz glass body and method for joining quartz glass body |
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| CN110191865A (en) * | 2016-12-29 | 2019-08-30 | 广东东阳光药业有限公司 | The borosilicate glass of high chemical resistance and its application |
| CN111018347A (en) * | 2020-01-07 | 2020-04-17 | 山东理工大学 | A kind of lanthanum oxide-based lead-free crystal glass and preparation method thereof |
| CN112811813A (en) * | 2021-01-15 | 2021-05-18 | 河北光兴半导体技术有限公司 | Borosilicate glass composition, borosilicate glass, and preparation method and application thereof |
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| JP2008297162A (en) * | 2007-05-31 | 2008-12-11 | Ｈｏｙａ Ｃａｎｄｅｏ Ｏｐｔｒｏｎｉｃｓ株式会社 | Glass composition for joining quartz glass body, glass paste for joining quartz glass body and method for joining quartz glass body |
| CN110191865A (en) * | 2016-12-29 | 2019-08-30 | 广东东阳光药业有限公司 | The borosilicate glass of high chemical resistance and its application |
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| CN111018347A (en) * | 2020-01-07 | 2020-04-17 | 山东理工大学 | A kind of lanthanum oxide-based lead-free crystal glass and preparation method thereof |
| CN112811813A (en) * | 2021-01-15 | 2021-05-18 | 河北光兴半导体技术有限公司 | Borosilicate glass composition, borosilicate glass, and preparation method and application thereof |
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