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Glass ceramic containing phosphorus lithium aluminium silicon and its preparation method

A technology of glass ceramics and lithium aluminum silicon, which is applied in the field of glass ceramics containing phosphorus lithium aluminum silicon and its preparation, can solve the problems of lowering the quality of color, increasing the thermal expansion coefficient of glass-ceramic, affecting the structure and performance of glass ceramics, and achieving Effect of low thermal expansion coefficient and high mechanical strength

Active Publication Date: 2007-12-05
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But when TiO 2 When the mass fraction is too large, coarse grains may be produced, which increases the thermal expansion coefficient of the glass-ceramic; and TiO 2 Will cause the color of glass ceramics to turn yellow, resulting in a loss of color quality
[0005] There are also TiO 2 and ZrO 2 As a mixed crystal nucleating agent, the research results found that the glass ceramics prepared by using either of the two alone has a finer grain size and higher mechanical strength, but due to ZrO 2 It has a high melting point and low solubility in glass, which limits its role as an improvement in nucleation
[0006] In recent years, fluoride has also been added as a crystal nucleus agent or a crystal nucleus growth accelerator to promote the nucleation and crystallization process of the glass, which can significantly reduce the crystallization temperature and crystallization power of the glass, but it is also easy to cause crystallization. Excessive growth and affect the structure and properties of glass ceramics

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1: a kind of phosphorus-containing lithium aluminum silicon glass-ceramic, its weight percentage is composed of:

[0017] SiO 2 70%, Li 2 O 4%, Al 2 o 3 1 5%, MgO 1%, ZnO 1.1%, CaO 0.5%, B 2 o 3 0.2%, TiO 2 3.2%, ZrO 2 2%, K 2 O 1.1%, Na 2 O 1.0%, P 2 o 5 0.1%, As 2 o 3 0.4%, Sb 2 o 3 0.4%.

[0018] Grind the above-mentioned glass-ceramic components evenly and prepare a mixture, melt at 1550-1650°C, shape, and anneal; then nucleate at 720°C for 1.5 hours, and then heat up to 810°C for 4 hours to crystallize; obtain the flexural strength 110~150MPa, expansion coefficient 5~21×10 -7 / °C glass ceramics, the spherical grain size is between 20 and 100nm.

Embodiment 2

[0019] Embodiment 2: a kind of phosphorus-containing lithium aluminum silicon glass-ceramic, its weight percentage is composed of:

[0020] SiO 2 70%, Li 2 O 4%, Al 2 o 3 15%, MgO 0.9%, ZnO 1.1%, CaO 0.5%, B 2 o 3 0.2%, TiO 2 2.5%, ZrO 2 2.1%, K 2 O 1.1%, Na 2 O 1.0%, P 2 o 5 0.8%, As 2 o 3 0.4%, Sb 2 o 3 0.4%.

[0021] Prepare the mixture according to the above components, melt at 1550-1650°C, shape, anneal, nucleate at 740°C for 1.5 hours, and then heat up to 870°C for 8 hours to obtain a flexural strength of 110-150MPa. Expansion coefficient 5~21×10 -7 / °C glass ceramics, the spherical grain size is between 20 and 100nm.

Embodiment 3

[0022] Embodiment 3: a kind of phosphorus-containing lithium aluminum silicon glass-ceramic, its weight percentage is composed of:

[0023] SiO 2 70%, Li 2 O 4%, Al 2 o 3 15%, MgO 0.9%, ZnO 1%, CaO 0.4%, B 2 o 3 0.2%, TiO 2 1.8%, ZrO 2 2.3%, K 2 O 1.0%, Na 2 O 1.0%, P 2 o 5 1.6%, As 2 o 3 0.4%, Sb 2 o 3 0.4%.

[0024] Prepare the mixture according to the above components, melt at 1550-1650°C, shape, anneal, nucleate at 760°C for 1.5 hours, and then heat up to 950°C for 4 hours to crystallize to obtain a flexural strength of 110-150MPa, Expansion coefficient 5~21×10 -7 / °C glass ceramics, the spherical grain size is between 20 and 100nm.

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Abstract

The present invention discloses a glass ceramic containing phosphorus, lithium, aluminium and silicone. Its composition contains: (by wt%) 70% of silicone dioxide, 4% of lithium oxide, 15% of aluminium oxide, 0.9%-1% of magnesium oxide, 1%-1.1% of zinc oxide, 0.4%-0.5% of calcium oxide, 0.2% of boron oxide, 1.8%-3.2% of titanium oxide, 2.0%-2.3% of zirconium oxide, 2%-2.1% of mixture of potassium oxide and sodium oxide, 0.1%-1.6% of phosphorus pentoxide and 0.8% of mixture of arsenium oxide and antimony oxide. Its preparation method includes the following steps: grinding all the above-mentioned components, uniformly mixing them to obtain mixed material, melting at 1550-1650deg.C, forming, annealing, nucleating for 1-4hr at 600-800deg.C, then heating to 700-1000deg.C, crystallizing for 1-12hr so as to obtain the invented product.

Description

technical field [0001] The present invention relates to a kind of glass ceramics and its preparation method, specifically, glass ceramics containing phosphorous lithium aluminum silicon and its preparation method. Background technique [0002] Glass-ceramic is a polycrystalline solid material prepared by controlled crystallization of LAS glass, in which lithium-aluminum-silicon (Li 2 O-Al 2 o 3 -SiO 2 , referred to as LAS) is the main glass ceramics, because of its ultra-low expansion, high strength, high thermal shock resistance, it is widely used in the manufacture of astronomical telescopes, cooking utensils, tableware, induction cooker panels, high-temperature electric light source glass, Substrates for microelectronics technology, heating appliances for laboratories, high-temperature heat exchangers, substitute quartz glass, high-temperature windows, radar radomes and other products. [0003] Regarding the lithium-aluminum-silicon-based glass ceramics, lithium-alumi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C03C10/12C03C3/097C03B32/02
CPCC03C3/097
Inventor 郭兴忠陈明形潘颐韩陈宋芳芳
Owner ZHEJIANG UNIV