Transparent microcrystalline glass with high elastic modulus and high hardness and preparation method

A glass-ceramic, high-hardness technology, used in glass manufacturing equipment, glass molding, manufacturing tools, etc., can solve the problems of reduced production efficiency, low elastic modulus, and high cost, and achieve improved structure, elastic modulus and Low hardness and low impact

Active Publication Date: 2022-05-13
GLASS TECH RES INST OF SHAHE CITY OF HEBEI PROVINCE
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Problems solved by technology

[0007] CN1275542A relates to a high-rigidity glass-ceramic substrate, with enstatite, enstatite solid solution, magnesium titanate and magnesium titanate solid solution as the main crystal phase, with high elastic modulus, specifically greater than 115GPa, and Al 2 o 3 The content is not less than 20%, mainly used in hard disk substrates, in the embodiment involves the introduction of more Y 2 o 3 , the glass composition does not contain Li due to the need for higher precision and better quality magnetized films 2 O / Na 2 O / K 2 O component, containing 8-12% TiO as a nucleating agent 2 , and completely different from the present invention in terms of crystal phase, belonging to a different glass-ceramic system, in addition, it cannot form compressive stress by ion exchange
The main components include TiO 2 16~36mol%, ZrO 2 5~25mol%, Y 2 o 3 2~22mol%, Al 2 o 3 30-55mol%, other fifth oxides 0-30mol%, including 0mol%, said other fifth oxides include beryllium oxide, calcium oxide, gallium oxide, vanadium oxide, iron oxide, strontium oxide, tantalum oxide, chromium oxide , barium oxide, lanthanum oxide, samarium oxide or gadolinium oxide, or a combination of at least two; although it has high hardness and elastic modulus, it contains more TiO 2 Seriously affects the coloring, but does not contain alkali metal oxides, and glass melting becomes very difficult. As mentioned, it uses suspension melting and enters the atmosphere protection, which greatly reduces production efficiency, and the cost is extremely high, which does not meet the actual mass production requirements.
[0009] In view of the problems existing in the prior art, it is reflected in the following aspects, one is that although it contains more Y 2 o 3 and Al 2 o 3 , some containing alkali metal oxides such as Na 2 O is for chemical strengthening, but the elastic modulus is not high, about 90GPa. The second is that it does not contain alkali metal oxides, which can have high hardness and elastic modulus, but contains more TiO 2 The optical properties are seriously affected, or the preparation method is relatively difficult, and it cannot be chemically strengthened without alkali metal, and the result is that the drop resistance is not ideal

Method used

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  • Transparent microcrystalline glass with high elastic modulus and high hardness and preparation method
  • Transparent microcrystalline glass with high elastic modulus and high hardness and preparation method
  • Transparent microcrystalline glass with high elastic modulus and high hardness and preparation method

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Experimental program
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Effect test

Embodiment 1

[0043] Raw material (wt%): 32% SiO 2 ;29%Al 2 o 3 ;31%Y 2 o 3 ;4%ZrO 2 ; 1%Na 2 O; 2% Li 2 O; 1% B 2 o 3 ;Accurately weigh various raw materials according to the designed glass composition, mix and stir the batch materials evenly, put them into a platinum crucible and melt them at 1560°C for 24 hours, heat preservation and annealing at 650°C for 5 hours after casting and cooling with the furnace, the heat treatment process is : The nucleation temperature is 750°C, the nucleation time is 6h, the crystallization temperature is 810°C, and the crystallization time is 2h. After the heat treatment, it is cooled with the furnace to obtain glass-ceramics.

[0044] The main crystal phase Y of the obtained glass-ceramic 2 Zr 2 o 7 , the elastic modulus is 130GPa, the microhardness is 860MPa, and the visible light transmittance at 300-780nm of the glass-ceramic with a thickness of 0.65mm is 90%.

[0045] After further chemical strengthening, the depth of the stress layer is 1...

Embodiment 2

[0047] Raw material (wt%): 29% SiO 2 ;30%Al 2 o 3 ;31%Y 2 o 3 ;4%ZrO 2 ;2%Na 2 O; 3% Li 2 O; 1% B 2 o 3Accurately weigh various raw materials according to the designed glass composition, mix and stir the batch materials evenly, put them into a platinum crucible for melting at 1580°C for 20 hours, heat preservation and annealing at 650°C for 3 hours after casting and cooling in the furnace. The heat treatment process is: nucleation temperature 780°C, nucleation time 10h, crystallization temperature 860°C, crystallization time 1h, after the heat treatment is completed, it is cooled in the furnace to obtain glass-ceramics.

[0048] The main crystal phase Y of the obtained glass-ceramic 2 Zr 2 o 7 , the elastic modulus is 125GPa, the microhardness is 876MPa, and the visible light transmittance of the glass-ceramic with a thickness of 0.65mm is 89.5% at 300-800nm.

[0049] After further chemical strengthening, the depth of the stress layer is 108μm, the surface compress...

Embodiment 3

[0051] Raw material (wt%): 30% SiO 2 ;29%Al 2 o 3 ;30%Y 2 o 3 ;5% ZrO 2 ;2%Na 2 O; 3.5% Li 2 O; 0.5% B 2 o 3 ;Accurately weigh various raw materials according to the designed glass composition, mix and stir the batch materials evenly, put them into a platinum crucible for melting at 1580°C for 20 hours, heat preservation and annealing at 650°C for 2 hours after casting and cooling in the furnace. The heat treatment process is: nucleation temperature 760°C, nucleation time 10h, crystallization temperature 860°C, crystallization time 1h, after the heat treatment is completed, it is cooled in the furnace to obtain glass-ceramics.

[0052] The main crystal phase Y of the obtained glass-ceramic 2 Zr 2 o 7 , the elastic modulus is 125GPa, the microhardness is 874MPa, and the visible light transmittance of 0.65mm-thick glass-ceramics at 300-800nm ​​is 89.3%.

[0053] After further chemical strengthening, the depth of the stress layer is 118μm, the surface compressive stre...

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Abstract

The invention relates to the technical field of glass ceramics, and provides transparent glass ceramics with high elasticity modulus and high hardness, which comprises the following components in percentage by mass: 25 to 40 percent of SiO2, 23 to 36 percent of Al2O3, 25 to 35 percent of Y2O3, 2 to 5 percent of ZrO2, 1 to 4 percent of Na2O, 2 to 6 percent of Li2O and 0.5 to 4 percent of B2O3. According to the technical scheme, the problem that chemical strengthening, elastic modulus and optical performance of microcrystalline glass in the prior art cannot be considered at the same time is solved.

Description

technical field [0001] The invention relates to the technical field of glass-ceramic, in particular to a transparent glass-ceramic with high elastic modulus and high hardness and a preparation method thereof. Background technique [0002] Materials with high elastic modulus and high hardness, such as sapphire or zirconia ceramics, can be used as the protective layer of electronic equipment, which can be used as cover glass or display window of electronic consumer equipment or can be used as protective material for the backplane of electronic equipment, or coated on the surface of the used material Applying a layer of high elastic modulus and high hardness coating increases hardness and improves scratch resistance, but this coating is easy to contact with the outside world during use, and there is a risk of delamination, resulting in failure of the protective function. [0003] In response to the required high hardness and high elastic modulus glass materials, the intrinsic m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C10/02C03C10/04C03B19/02C03B25/00C03B32/02
CPCC03C10/0009C03B19/02C03B25/00C03B32/02
Inventor 彭志钢袁坚杜晓欧张茂森郑伟宏田培静薛瑞锋史连莹
Owner GLASS TECH RES INST OF SHAHE CITY OF HEBEI PROVINCE
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