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Glass ceramic containing fluorine phosphorus lithium aluminium silican and its preparation method

A glass-ceramic, fluorine-phosphorus-containing lithium technology, which is applied in the field of fluorine-phosphorus-lithium-aluminosilicate glass-ceramic and its preparation, can solve the problems of grain size growth, affecting the structure and performance of glass-ceramic, and achieves good comprehensive performance, fine The effect of comprehensive performance of crystal microstructure and low cost of raw materials

Inactive Publication Date: 2007-05-16
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, if the measures to control the heat treatment process are not effective, the grain size will grow too much, which will affect the structure and performance of glass ceramics.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1, a kind of fluorine-containing phosphorus lithium aluminum silicon glass ceramics, it is made up of the composition of following weight percent:

[0019] SiO 2 70%, Li 2 O 4.0%, Al 2 o 3 15%, MgO 0.7%, ZnO 0.8%, CaO 0.7%, B 2 o 3 0.2%, TiO 2 2.5%, ZrO 2 2.1%, Na 2 O 1.0%, K 2 O 1.0%, P 2 o 5 1.0%, LiF 0.1%, Sb 2 o 3 0.5%, As 2 o 3 0.4%.

[0020] Grind the above-mentioned glass-ceramic components evenly and prepare a mixture, melt at 1550-1610°C, shape and anneal; then nucleate at 700°C for 1.5 hours, and then heat up to 800°C for 2 hours to crystallize to obtain the flexural strength 130-160MPa, expansion coefficient 5-15×10 -7 / °C glass ceramics, the primary and secondary crystal phases are β-spodumene and anorthite, and the grain size is between 20 and 100nm.

Embodiment 2

[0021] Embodiment 2, a kind of fluorine-containing phosphorus lithium aluminum silicon glass-ceramic, it is made up of the composition of following percentage by weight:

[0022] SiO 2 70%, Li 2 O 3.9%, Al 2 o 3 15%, MgO 0.7%, ZnO 0.8%, CaO 0.7%, B 2 o 3 0.2%, TiO 2 2.5%, ZrO 22.0%, Na 2 O 1.0%, K 2 O 1.0%, P 2 o 5 0.8%, LiF 0.5%, Sb 2 o 3 0.5%, As 2 o 3 0.4%.

[0023] Grind the above-mentioned glass-ceramic components evenly and prepare a mixture, melt at 1550-1600°C, shape, and anneal; then nucleate at 680°C for 1 hour, and then heat up to 780°C for 4 hours to obtain the flexural strength 130-160MPa, expansion coefficient 5-15×10 -7 / °C glass ceramics, the primary and secondary crystal phases are β-spodumene and anorthite, and the grain size is between 20 and 100nm.

Embodiment 3

[0024] Embodiment 3, a kind of fluorine-containing phosphorus lithium aluminum silicon glass-ceramic, it is made up of the composition of following percentage by weight:

[0025] SiO 2 70%, Li 2 O 3.8%, Al 2 o 3 15%, MgO 0.7%, ZnO 0.8%, CaO 0.7%, B 2 o 3 0.2%, TiO 2 2.5%, ZrO 2 1.9%, Na 2 O 1.1%, K 2 O 1.0%, P 2 o 5 0.4%, LiF 1%, Sb 2 o 3 0.5%, As 2 o 3 0.4%.

[0026] Grind the above-mentioned glass-ceramic components evenly and prepare a mixture, melt at 1550-1600°C, shape, and anneal; then nucleate at 660°C for 1 hour, and then heat up to 760°C for 4 hours to obtain a flexural strength of 130 -160MPa, expansion coefficient 5-15×10 -7 / °C glass ceramics, the primary and secondary crystal phases are β-spodumene and anorthite, and the grain size is between 20 and 100 nm.

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Abstract

The present invention relates to a glass ceramic containing fluorine, phosphorus, lithium aluminium and silicone. Its composition contains: (by wt%) 70% of silicone dioxide, 3.8%-4% of lithium oxide, 15% of aluminium oxide, 0.7% of magnesium oxide, 0.8% of zinc oxide, 0.7% of calcium oxide, 0.2% of boron oxide, 2.5% of titanium oxide, 1.9%-2.1% of zirconium oxide, 2%-2.1% of mixture of potassium oxide and sodium oxide, 0.4%-1% of phosphorus pentoxide, 0.07%-1% of lithium fluoride and 0.9% of mixture of arsenium oxide and antimony oxide. Its preparation method includes the following steps: grinding the above-mentioned components, uniformly mixing them to obtain mixed material, melting at 1550-1610deg.C, forming, annealing nucleating for 1-4 hr at 600-800deg.C, then heating to 700-905deg.C and crystallizing for 1-12hr so as to obtain the invented product.

Description

technical field [0001] The invention relates to a glass ceramic and a preparation method thereof, in particular, a fluorine-containing phosphorous lithium aluminum silicon glass ceramic and a preparation method thereof. Background technique [0002] Glass ceramics are polycrystalline solid materials made 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-al...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C03C10/00C03B32/02
Inventor 郭兴忠陈明形潘颐韩陈宋芳芳
Owner ZHEJIANG UNIV
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