阅读说明：本技术 一种玻璃晶化方法、玻璃板及隔离粉混合液 (Glass crystallization method, glass plate and isolating powder mixed solution ) 是由 邓双 黄昊 谈宝权 张延起 姜宏 胡伟 于 2021-01-15 设计创作，主要内容包括：本申请公开了一种玻璃晶化方法、玻璃板及隔离粉混合液,该玻璃晶化方法包括提供多片玻璃坯体,将至少部分玻璃坯体进行堆叠,并且在相邻的两层玻璃坯体之间设置由隔离粉混合液形成的隔离层,对堆叠的所述玻璃坯体进行晶化处理,得到晶化后的玻璃板。通过上述方式,本申请能够使隔离粉的分布更加均匀,提升隔离层的均匀性,从而增强晶化效果。(The application discloses a glass crystallization method, a glass plate and an isolation powder mixed solution, the glass crystallization method comprises the steps of providing a plurality of glass blanks, stacking at least part of the glass blanks, arranging an isolation layer formed by the isolation powder mixed solution between two adjacent layers of the glass blanks, and carrying out crystallization treatment on the stacked glass blanks to obtain the crystallized glass plate. Through the mode, the distribution that this application can make the isolation powder is more even, promotes the homogeneity of isolation layer to reinforcing crystallization effect.)

1. A method for crystallizing glass, which is characterized in that,

providing a plurality of glass blanks;

stacking at least part of the glass blanks, and arranging an isolation layer formed by isolation powder mixed liquor between two adjacent layers of the glass blanks;

and crystallizing the stacked glass body to obtain a crystallized glass plate.

2. The glass crystallization method according to claim 1,

set up the isolation layer that is formed by keeping apart the mixed liquid of powder between adjacent two-layer glass body and include:

coating the surface of the glass blank with an isolation powder mixed solution to form an isolation layer in a spraying, rolling or brushing mode, or forming the surface of the glass blank with an isolation layer in a soaking mode;

and stacking another glass body on the isolating layer.

3. The glass crystallization method according to claim 1,

the isolation powder mixed solution comprises 5-85 wt% of isolation powder, 8-12 wt% of dissolution promoter and 5-85 wt% of solvent.

4. The glass crystallization method according to claim 3,

the isolating powder comprises one or more of boron nitride, silicon nitride, aluminum oxide and magnesium oxide.

5. The glass crystallization method according to claim 3,

the particle size of the isolating powder is 0.3-1 μm.

6. The glass crystallization method according to claim 3,

the isolating powder comprises boron nitride, and the crystal structure of the boron nitride is a hexagonal crystal form.

7. The glass crystallization method according to claim 3,

the solvent is water, and the cosolvent comprises a surfactant and a water-soluble polymer.

8. The glass crystallization method according to claim 7,

the surfactant comprises one or more of cetyl trimethyl ammonium bromide, sodium dodecyl benzene sulfonate, calcium dodecyl benzene sulfonate and sodium dodecyl sulfate.

9. The glass crystallization method according to claim 7,

the water-soluble polymer comprises one or more of polyvinyl alcohol, polyacrylamide, polyvinylpyrrolidone, polyethylene glycol and hydroxypropyl methyl cellulose.

10. The glass crystallization method according to claim 1,

the usage amount of the isolation powder mixed solution for forming the isolation layer is 0.15-1.0mg/cm²。

11. The glass crystallization method according to claim 1,

the glass blank is a glass plate, and the thickness of the glass plate is 0.5-5 mm;

the total thickness of each group of stacked glass bodies is 1.5-50 mm.

12. The glass crystallization method according to claim 1,

every group glass body piles up between lower bolster and top board, and every group glass body total thickness that piles up is c, length is a, the width is b, the thickness of top board is greater than 2c/3 and is less than 3c/2, the length of top board is greater than a and is less than a +10mm, the width of top board is greater than b and is less than b +10mm, the thickness of lower bolster is greater than c and is less than 2c, the length of lower bolster is greater than a and is less than a +10mm, the width of lower bolster is greater than b and is less than b +10 mm.

13. The glass crystallization method according to claim 1,

the crystallizing the stacked glass bodies comprises:

carrying out nucleation treatment on the glass body, wherein the time of the nucleation treatment is 20-400min, and the temperature is 500-1000 ℃;

and carrying out crystallization treatment on the nucleated glass to obtain the microcrystalline glass, wherein the crystallization treatment time is 10-600min, and the temperature is 550-1100 ℃.

14. The glass crystallization method according to claim 13, further comprising:

and carrying out flat grinding and polishing treatment on the microcrystalline glass, wherein the minimum total thickness subtracted by the flat grinding and polishing is more than or equal to 0.5 time of the particle size of the isolation powder and less than or equal to 10 times of the particle size of the isolation powder.

15. The glass crystallization method according to claim 13,

the crystalline phase of the microcrystalline glass comprises one or more of lithium disilicate, petalite, beta-quartz, lithium silicate, a beta-quartz solid solution, beta-spodumene, spinel and eucryptite.

16. The glass crystallization method according to claim 13,

the transmittance of the microcrystalline glass to light with the wavelength of 360nm is more than 80%, the transmittance to light with the wavelength of 400nm is more than 84%, and the transmittance to light with the wavelength of 550nm is more than 85%;

the crystallinity of the microcrystalline glass is 10 wt% -100 wt%.

17. A glass sheet characterized in that it comprises,

the glass plate surface adheres to the isolation layer, the isolation layer is formed by isolation powder mixed liquid.

18. Glass sheet according to claim 17,

the isolation layer comprises 5-85 wt% of isolation powder, 8-12 wt% of dissolution promoter and 5-85 wt% of solvent.

19. A glass sheet characterized in that it comprises,

the glass plate is a glass plate obtained by crystallization using the glass crystallization method according to any one of claims 1 to 16.

20. Glass sheet according to claim 19,

the Wa value of the glass plate is 0.1-10 μm.

21. A mixed solution of isolating powder is characterized in that,

the isolation powder mixed solution comprises 5-85 wt% of isolation powder, 8-12 wt% of dissolution promoter and 5-85 wt% of solvent.

22. The dusting powder mixture of claim 21,

the isolating powder comprises boron nitride, the solvent is water, and the dissolution promoter comprises a surfactant and a water-soluble polymer.

Technical Field

The invention relates to the technical field of glass production and manufacturing, in particular to a glass crystallization method, a glass plate and an isolation powder mixed solution.

Background

With the development of glass production technology, transparent glass ceramics are widely applied to electronic products due to excellent optical properties and mechanical properties.

The production of the transparent glass ceramics needs to be processed by a crystallization process, the traditional crystallization process is that a glass blank is cut into plates, then the glass plates are stacked together layer by layer for crystallization, and in order to prevent the glass plates from being adhered, an isolating layer needs to be arranged between every two glass plates. In the long-term research and development process, the inventor of the application finds that the current isolating layer is easy to change the uniformity of the temperature field of the surface of the glass plate, thereby causing the uneven crystallization of the surface of the glass plate. Meanwhile, the conventional spacer is easily adsorbed on the surface of glass after being crystallized, so that the surface of the glass is not flat.

Disclosure of Invention

The invention mainly solves the technical problem of providing a glass crystallization method, a glass plate and an isolation powder mixed solution, which can improve the uniformity of an isolation layer so as to enhance the crystallization effect.

In order to solve the technical problems, the invention adopts a technical scheme that: the glass crystallization method comprises the steps of providing a plurality of glass blanks, stacking at least part of the glass blanks, arranging an isolating layer formed by isolating powder mixed liquid between two adjacent layers of the glass blanks, and carrying out crystallization treatment on the stacked glass blanks to obtain crystallized glass plates.

Wherein, set up the isolation layer that is formed by keeping apart the mixed liquid of powder between adjacent two-layer glass body and include: coating the surface of a glass blank with the isolating powder mixed solution in a spraying, rolling or brushing way to form an isolating layer, or forming the surface of the glass blank with the isolating layer in a soaking way; and stacking another glass body on the isolating layer.

The isolation powder mixed solution comprises 5-85 wt% of isolation powder, 8-12 wt% of dissolution promoter and 5-85 wt% of solvent.

The isolating powder comprises one or more of boron nitride, silicon nitride, aluminum oxide and magnesium oxide.

Wherein the particle size of the isolating powder is 0.3-1 μm.

The isolating powder comprises boron nitride, and the crystal structure of the boron nitride is a hexagonal crystal form.

Wherein, the solvent of the mixed solution of the isolating powder is water, and the dissolution promoter comprises a surfactant and a water-soluble polymer.

Wherein the surfactant comprises one or more of cetyl trimethyl ammonium bromide, sodium dodecyl benzene sulfonate, calcium dodecyl benzene sulfonate and sodium dodecyl sulfate.

Wherein the water-soluble polymer comprises one or more of polyvinyl alcohol, polyacrylamide, polyvinylpyrrolidone, polyethylene glycol and hydroxypropyl methyl cellulose.

Wherein the usage amount of the mixed solution of the isolation powder for forming the isolation layer is 0.15-1.0mg/cm²。

Wherein the glass body is a glass plate, the thickness of the glass body is 0.5-5mm, and the total thickness of each group of stacked glass bodies is 1.5-50 mm.

Each group of glass blanks are stacked between a lower cushion plate and an upper pressing plate, the total thickness of each group of stacked glass blanks is c, the length of each group of stacked glass blanks is a, the width of each group of stacked glass blanks is b, the thickness of each upper pressing plate is greater than 2c/3 and smaller than 3c/2, the length of each upper pressing plate is greater than a and smaller than a +10mm, the width of each upper pressing plate is greater than b and smaller than b +10mm, the thickness of each lower cushion plate is greater than c and smaller than 2c, the length of each lower cushion plate is greater than a and smaller than a +10mm, and the width of each lower cushion plate is greater.

Wherein crystallizing the stacked glass bodies comprises: carrying out nucleation treatment on the glass body, wherein the time of the nucleation treatment is 20-400min, and the temperature is 500-; and carrying out crystallization treatment on the nucleated glass to obtain the microcrystalline glass, wherein the crystallization treatment time is 10-600min, and the temperature is 550-1100 ℃.

And performing flat grinding and polishing treatment on the microcrystalline glass, wherein the minimum total thickness subtracted by the flat grinding and polishing is more than or equal to 0.5 time of the particle size of the isolation powder and less than or equal to 10 times of the particle size of the isolation powder.

Wherein the crystalline phase of the microcrystalline glass comprises one or more of lithium disilicate, petalite, beta-quartz, lithium silicate, a beta-quartz solid solution, beta-spodumene, spinel and eucryptite.

Wherein, the transmittance of the microcrystalline glass to light with the wavelength of 360nm is more than 80 percent, the transmittance to light with the wavelength of 400nm is more than 84 percent, the transmittance to light with the wavelength of 550nm is more than 85 percent, and the crystallinity of the microcrystalline glass is 10 to 100 percent by weight.

In order to solve the technical problem, the invention adopts another technical scheme that: a glass plate is provided, wherein an isolation layer is attached to the surface of the glass plate and is formed by an isolation powder mixed liquid.

The isolation layer comprises 5-85 wt% of isolation powder, 8-12 wt% of dissolution promoter and 5-85 wt% of solvent.

In order to solve the technical problem, the invention adopts another technical scheme that: a glass plate is provided, which is obtained by crystallization by the glass crystallization method.

Wherein the Wa value of the glass plate is 0.1 μm to 10 μm.

In order to solve the technical problem, the invention adopts another technical scheme that: the isolation powder mixed solution comprises 5-85 wt% of isolation powder, 8-12 wt% of dissolution promoter and 5-85 wt% of solvent.

The isolating powder comprises boron nitride, the solvent is water, and the dissolution promoter comprises a surfactant and a water-soluble polymer.

The invention has the beneficial effects that: be different from prior art's condition, this application provides the multi-disc glass body, stacks at least part of glass body to set up the isolation layer that is formed by keeping apart the mixed liquid of powder between adjacent two-layer glass body, can prevent to take place the adhesion between the glass body in the crystallization process. The isolating layer is formed between the two layers of glass bodies by the isolating powder in the form of mixed liquid, so that the dispersing capacity of the isolating powder can be improved, and the gaps among the glass bodies caused by the agglomeration of the powder are reduced, thereby enhancing the uniformity of the surface temperature field of the glass bodies and ensuring that the degree of uniform crystallization of the glass bodies is higher. Meanwhile, unevenness of the glass surface caused by adsorption of the spacer can be reduced to a certain extent.

Drawings

FIG. 1 is a schematic view of a stack of glass blanks according to an embodiment of the present application;

FIG. 2 is a schematic flow chart of a glass crystallization method according to an embodiment of the present application.

Detailed Description

In order to make the objects, technical solutions and effects of the present invention clearer and clearer, the present invention is further described in detail below with reference to the accompanying drawings and examples.

The application provides a crystallization method of microcrystalline glass, and the microcrystalline glass produced by the crystallization method can be used on a display cover plate of an electronic product, can also be used as a heating plate or a touch panel of an electromagnetic oven, a microwave oven, a gas furnace, a white household appliance and the like, and can also be applied to a windshield of an automobile and the like.

In a laboratory, only a single glass is generally crystallized in order to minimize interference from other conditions, but in an actual industrial production process, a plurality of glasses are simultaneously crystallized in consideration of production efficiency and cost, and thus, a plurality of glasses are generally stacked and then crystallized. To prevent the adhesion between the glass sheets, an insulating layer is required to be disposed between each glass sheet. The isolation pad can be used as the isolation layer, and the isolation powder can also be used as the isolation layer. The inventor of the present application has found that there is a problem when the barrier powder is selected to form the barrier layer. The main point is that the dispersion ability, heat conduction ability and particle size uniformity of the isolation powder all affect the crystallization uniformity of the glass plate. Also, unevenness of the glass surface may be caused.

First, when the spacer powder has low uniformity of particle size, minute gaps may exist between the glass plates, which may change the uniformity of the temperature field of the surface of the glass plates, resulting in non-uniform crystallization of the glass plates. Secondly, when the dispersing ability of the isolating powder is low, the powder can be agglomerated, so that gaps are generated among glass plates, and the glass plates are not uniformly crystallized. Finally, when the thermal conductivity of the spacer powder is low, the thermal transfer between the glass plates is affected, resulting in non-uniform crystallization of the glass plates. These problems are not readily apparent when the target glass sheet has low requirements for uniformity of crystallization, for example, a glass sheet in an opaque or translucent state has relatively low requirements for uniformity of crystallization. When the target glass plate has a high requirement for uniformity of crystallization, for example, when the target glass plate needs to maintain high optical uniformity, the requirement for uniformity of crystallization is high, and the problem of crystallization unevenness is more obviously reflected. The inventors of the present application further studied to find that the cause of the problem of the crystallization unevenness is, in addition to the characteristics of the separator itself, another main cause of the coating unevenness of the separator. When the coating of the spacer powder is not uniform, a minute gap exists between the glass plates, which affects heat transfer between the glass plates, resulting in non-uniform crystallization of the glass plates. Meanwhile, in the crystallization process of the glass, due to the action of high temperature, part of the spacers are adsorbed on the surface of the glass due to the softening of the glass, so that the surface of the glass is not flat.

In order to solve the technical problem, the application provides a mixed solution of isolating powder, which consists of a solvent, a dissolving promoter and isolating powder. The isolation powder forms an isolation layer between two layers of glass bodies in the form of mixed liquid, so that the dispersing capacity of the isolation powder can be improved, and gaps between the glass bodies caused by the agglomeration of the powder are reduced, thereby enhancing the uniformity of the surface temperature field of the glass bodies and ensuring that the degree of uniform crystallization of the glass bodies is higher. Meanwhile, the problem that the surface of the glass is not flat due to the adsorption effect of the spacer can be reduced to a certain degree.

In one embodiment, the isolation powder mixture includes a solvent, a dissolution promoter, and an isolation powder.

Specifically, the isolation powder may be magnesia powder, alumina powder, talc powder, silicon nitride, aluminum nitride, boron nitride, or the like. The magnesium oxide powder and the aluminum oxide powder have good thermal stability, but when the magnesium oxide powder and the aluminum oxide powder are used as crystallization isolation layers, certain adhesion can be generated with glass in the crystallization process, and when the thickness of the isolation layers is small, the separation difficulty of the glass plate can be increased due to the adhesion condition. This is usually due to the fact that at high temperatures, a certain chemical reaction takes place between the magnesia or alumina powder and the glass, which has the formula: MgO + SiO₂＝MgSiO₃，Al₂O₃+3SiO₂＝Al₂(SiO₃)₃. The melting point of the talcum powder is lower than that of other isolation powders, the main component of the talcum powder is hydrous magnesium silicate, and the talcum powder also contains impurities such as aluminum oxide and the like, which can cause adhesion in the crystallization process. Boron nitride is white loose powder with an ultrahigh melting point, the melting point of the boron nitride is up to 3000 ℃, and the boron nitride also has chemical erosion resistance and is not eroded by inorganic acid and water; besides, the boron nitride has the similar properties with graphite, has good electrical insulation and thermal conductivity, and can be used as a good isolation layer in the lamination crystallization process of the microcrystalline glass by combining the properties. Different isolation powders can be selected according to requirements, for example, when the requirement on the surface roughness of the glass is not high, magnesium oxide or alumina powder can be selected; when the crystallization temperature is not high, talcum powder can be selected; when the requirement on the precision of the glass is higher, boron nitride and the like can be selected. When the magnesium oxide powder, the aluminum oxide powder and the talcum powder are selected, the thickness of the isolation layer can be increased so as to reduce the adhesion. The following will describe the embodiments of the present application in detail by taking boron nitride as an example, but not limited thereto.

Further, boron nitride with a hexagonal crystal structure can be selected as the isolating powder. The boron nitride with the hexagonal crystal structure has good thermal conductivity and strong high-temperature stability, and can play a good isolation layer effect in the crystallization process of glass.

Further, the particle size of the dusting powder may be 0.3 to 1 μm. In the crystallization process, the isolating powder used as an isolating layer is embedded into the surface of the glass along with the softening of the glass, so that the flatness of the surface of the microcrystalline glass is influenced, the larger the isolating powder particle size is, the larger the surface roughness is, and the thicker the rough layer is, therefore, the microcrystalline glass after the crystallization of the lamination must be processed again to remove the surface roughness layer. The roughness of the glass surface and the thickness of the rough layer after crystallization can be reduced by controlling the isolation particle size within 0.3-1 μm, and the processing difficulty is reduced.

The solvent can be selected from water, organic solvent such as ethanol, etc. Since most of the isolating powder is inorganic, the dissolving capacities of different isolating powders in water or organic solvents are different, and the solvent can be selected according to the solubility of the isolating powder.

In one embodiment, the solvent of the mixed solution of the isolation powder is water, and in order to improve the solubility of the isolation powder in water, a dissolution promoter is further added to the mixed solution of the isolation powder. The dissolution promoting agent comprises a surfactant and a water-soluble polymer. The surfactant is a substance which can obviously reduce the surface tension of a target solution, has fixed hydrophilic and lipophilic groups, can be directionally arranged on the surface of the solution and can promote the dissolution of the substance. The surfactant can be one or more of cetyl trimethyl ammonium bromide, sodium dodecyl benzene sulfonate, calcium dodecyl benzene sulfonate, and sodium dodecyl sulfate. The water-soluble polymer is generally referred to as a water-soluble polymer, and a water-soluble polymer compound is also referred to as a water-soluble resin or a water-soluble polymer, and is a polymer material having a strong hydrophilic property, and can be dissolved or swollen in water to form an aqueous solution or a dispersion system, which can promote the dissolution of a substance. In one embodiment, the water soluble polymer may be one or more of polyvinyl alcohol, polyacrylamide, polyvinylpyrrolidone, polyethylene glycol, hydroxypropyl methylcellulose.

In one embodiment, the content of the isolation powder in the isolation powder mixture is in a range of 5 to 85 wt%, the content of the dissolution promoter is in a range of 8 to 12 wt%, and the content of the solvent is in a range of 5 to 85 wt%. For example, the content of the barrier powder may be 5 wt%, 8 wt%, 15 wt%, 23 wt%, 35 wt%, 41 wt%, 50 wt%, 62 wt%, 70 wt%, 77 wt%, 85 wt%, etc., the content of the dissolution promoting agent may be 8 wt%, 8.6 wt%, 9.3 wt%, 10 wt%, 10.5 wt%, 11.1 wt%, 12 wt%, etc., and the content of the solvent may be 5 wt%, 10 wt%, 15 wt%, 20 wt%, 35 wt%, 40 wt%, 50 wt%, 60 wt%, 70 wt%, 75 wt%, 85 wt%, etc. For example, the mixed solution of the barrier powder can be composed of 5 wt% of barrier powder, 10 wt% of dissolution promoter and 85 wt% of solvent. The specific components of each component may be within the above ranges, and are not particularly limited. The isolation powder in the isolation powder mixed liquid in the component range can be uniformly mixed with the solvent, and the distribution of the isolation powder in the formed isolation layer is uniform.

In the above embodiment, the isolating powder is prepared into the isolating powder mixed solution, so that the isolating powder is coated more uniformly, and is uniformly distributed on the surface of the glass, and the uniformity is higher; meanwhile, the gaps among the glass blanks caused by the agglomeration of the powder can be reduced, so that the uniformity of the surface temperature field of the glass blanks is enhanced, and the uniform crystallization degree of the glass blanks is higher. Meanwhile, unevenness of the glass surface caused by adsorption of the spacer can be reduced to a certain extent.

Referring to fig. 1 and fig. 2 in combination, fig. 1 is a schematic view of a stacked structure of glass blanks according to an embodiment of the present disclosure, and fig. 2 is a schematic view of a flow chart of a glass crystallization method according to an embodiment of the present disclosure. In this embodiment, the spacer between the glasses can be made by using a spacer powder mixture. The glass crystallization method comprises the following steps:

s201, providing a plurality of glass blanks.

The glass body is a glass body subjected to forming and annealing treatment. Specifically, weighing corresponding glass raw materials according to a glass formula, mixing the materials, and then carrying out glass melting molding, wherein the molding modes comprise a float method, an overflow method, a rolling method, a pouring method and the like; and annealing the formed glass plate to obtain a glass blank. The annealed glass body can be cut and inspected as required.

And S203, stacking at least part of the glass bodies.

And an isolating layer formed by isolating powder mixed liquid is arranged between two adjacent layers of glass blanks during stacking. As shown in fig. 1, a spacer 105 formed of a spacer powder mixture is disposed between the glass bodies 101 and 103. The stacking direction is generally along the vertical direction, the number of stacked glass layers can be three to ten, or can be other layers selected in combination with actual production conditions, and is not particularly limited here, and the isolating layer formed by the isolating powder mixed liquid can prevent the glass bodies from being in direct contact with each other, so that the glass bodies are prevented from being heated and adhered in the crystallization process.

A plurality of glass blanks are used as a group to be tiled and stacked, and in order to prevent the glass blanks from deforming, silicon carbide plates are respectively placed on the upper surface and the lower surface of the stacked glass blanks to be used as an upper pressing plate and a lower backing plate. And isolation layers formed by isolation powder mixed liquor are arranged between the glass blanks and the silicon carbide plate.

Specifically, the method comprises the steps of coating the surface of a glass blank with the mixed solution of the isolating powder in a spraying, rolling or brushing mode to form an isolating layer, or forming the surface of a glass blank with an isolating layer in a soaking mode, and then stacking another glass blank on the isolating layer. By the mode, the isolation powder can be uniformly distributed on the surface of the glass, and the uniformity of the isolation layer is improved.

In one embodiment, the amount of the mixed solution of the isolation powder in the isolation layer is in the range of 0.15-1.0mg/cm². In the process of glass crystallization, the use amount of the mixed liquid of the isolation powder in the isolation layer is too small, so that the isolation effect is difficult to achieve, and the use amount of the mixed liquid of the isolation powder is increased when the use amount of the mixed liquid of the isolation powder is too large, so that the production cost is increased. Controlling the usage amount of the mixed solution of the isolation powder in the isolation layer to be 0.15-1.0mg/cm²Within the range, a superior crystallization result can be achieved.

In one embodiment, a set of glass bodies can be 3 to 10 sheets. The production efficiency is reduced and the production cost is increased if the number of stacked glass blanks is too small, and the extrusion deformation is easily caused if the pressure between the glass blanks is too large if the number of stacked glass blanks is too large, and the optical performance of the finally crystallized glass is affected due to the fact that the glass blanks are heated unevenly.

In one embodiment, in order to achieve a better clamping effect of the silicon carbide plate, the sizes of the upper pressing plate and the lower backing plate need to be adjusted correspondingly according to the size of the stacked glass blanks. Setting the thickness of a group of stacked glass blanks as (c), the length as (a) and the width as (b), wherein the thickness of the upper pressing plate is more than 2c/3 and less than 3c/2, the length of the upper pressing plate is more than a and less than a +10mm, and the width of the upper pressing plate is more than b and less than b +10 mm; the thickness of the lower backing plate is larger than c and smaller than 2c, the length of the lower backing plate is larger than a and smaller than a +10mm, and the width of the lower backing plate is larger than b and smaller than b +10 mm.

In one embodiment, the glass used for the stack crystallization is ultra-thin glass sheets, the thickness of the single glass body is 0.5 to 5mm, and the total thickness of the glass sheets stacked in each group is 1.5 to 50 mm. Due to the unevenness of the glass sheets and the low thermal conductivity of the glass sheets themselves, there is an optimum thickness range during stacking, beyond which the quality of the glass sheet surface and its optical properties will be affected. The glass plate for stacking crystallization in the embodiment is an ultra-thin glass plate applied to a display cover plate of an electronic product, and the thickness of the ultra-thin glass plate is 0.5-5mm, and the total thickness of each group of stacked glass plates is 1.5-50 mm.

And S205, crystallizing the glass body.

The crystallization process is a key step for producing a predetermined crystal phase and a glass phase in the glass ceramics. After the composition is determined, the structure and the performance of the microcrystalline glass mainly depend on a crystallization treatment process (crystallization treatment temperature and heat preservation time). During the crystallization process, phase separation, nucleation, crystal growth, secondary crystallization, etc. may occur in the glass. The manner in which the above processes are performed differs for different types of crystallized glass. The crystallization process can be generally divided into two stages: the first stage is the fine tuning of the glass structure and nucleation, and the second stage is crystal growth. The nucleation and crystal growth of the glass-ceramic are generally carried out at a temperature higher than the transition temperature Tg and lower than the melting point of the main crystal phase. Generally, the nucleation is performed at a temperature corresponding to a viscosity of 10 to 10 pas for a predetermined time to form a predetermined number of uniformly distributed crystal nuclei in the mother glass. For glasses that are very susceptible to crystallization (e.g., systems with lower melt viscosity and higher alkali metal oxide content), the nucleation stage can also be omitted and the glasses can be heated directly to the crystal growth temperature, since these glasses can complete nucleation during the temperature rise process, resulting in a large number of nuclei. Generally, the crystal growth temperature is about 150-200 ℃ higher than the nucleation temperature.

In one embodiment, the crystallization process of the glass body is divided into two stages, wherein the first stage is a nucleation stage of the glass ceramics, i.e. a nucleation stage, the nucleation time is 20-400min, and the nucleation temperature range is 500-1000 ℃; the second stage is a crystallization stage of the glass ceramics, namely a crystallization treatment stage, wherein the crystallization treatment time is 10-600min, and the crystallization temperature range is 550-1100 ℃. Specifically, the nucleation treatment and the crystallization treatment can be performed in the same equipment, for example, in the same high temperature furnace, the temperature of the high temperature furnace is controlled to be raised to the nucleation treatment temperature, and the temperature is continuously raised to the crystallization treatment temperature after the nucleation treatment. The crystalline phase precipitated from the microcrystalline glass after the crystallization process treatment comprises one or more of lithium disilicate, petalite, beta-quartz, lithium silicate, beta-quartz solid solution, beta-spodumene, spinel, eucryptite and the like. Wherein the crystallinity of the crystallized glass is 10 wt% -100 wt%. The transmittance of the coating to light with the wavelength of 360nm is more than 80%, the transmittance to light with the wavelength of 400nm is more than 84%, and the transmittance to light with the wavelength of 550nm is more than 85%;

and S207, performing flat grinding and polishing treatment on the crystallized glass plate.

In the crystallization process, part of the components of the mixed solution of the isolating powder volatilizes at high temperature, and the other part of the components and the glass surface generate adsorption action, and the adsorbate has certain influence on the surface flatness and the optical performance of the glass. The adsorbate is because the release powder can be embedded into the surface of the glass along with the softening of the glass, thereby affecting the flatness of the surface of the microcrystalline glass, and the larger the release powder granularity is, the larger the surface roughness is, the thicker the rough layer is, therefore, the microcrystalline glass after the crystallization of the lamination must be processed again to remove the surface roughness layer, and the method for processing and removing the surface roughness layer is usually flat grinding and polishing treatment. Wherein, the flat grinding is to carry out surface treatment on the surface of the glass by utilizing the grinding action of the polishing powder and the hydration action of the surface of the glass and water. The glass flat grinding is divided into coarse grinding and fine grinding, wherein the coarse grinding is to grind the rough and uneven or excessive surface of the glass by using a coarse grinding material, so that the glass product has the required shape and size, but a pit and a crack layer are left on the surface of the glass, and the fine grinding is to be carried out by using a fine grinding material, so that the pit and the crack layer become thin and are also fine rough surfaces, and then the glass is changed into a transparent and smooth surface by a polishing process. The material of the grinding disc is generally cast iron, and a brass disc can also be used. The abrasive is essentially an aqueous suspension of free abrasive, the hardness of which must be greater than the hardness of the glass being ground. The grinding process of the glass is that the grinding disc and the glass surface move relatively, the free abrasive material scratches and peels the glass surface under the load of the grinding disc, and simultaneously microcracks are generated on the glass. The water used by the grinding material has a cooling effect and also generates a hydrolysis effect with a new stripping surface of the glass to generate silica gel which is beneficial to further stripping, so that the grinding process has a certain chemical effect besides a mechanical grinding effect, a sunk rough surface is formed on the surface of the glass in a cycle, and a crack layer with a certain depth is generated at the same time. The polishing of glass is to change the final rough surface into bright surface, and to remove the depressed layer and crack layer, the polishing plate is usually made of felt, hard asphalt, non-woven fabric, polyurethane, polytetrafluoroethylene, etc. The flexible polishing disk with thin asphalt layer is covered with nylon, aluminum, zinc and other sheets, and the polishing disk is always matched with the surface of the workpiece to be processed, and the foamed polyurethane polishing disk soaked with cerium oxide can realize high-efficiency polishing.

Wherein, the particle diameter d of the boron nitride and the minimum total thickness m subtracted by flat grinding and polishing when the crystallized glass plate reaches mirror surface level flatness have a certain functional relationship, and the expression is that m is more than 0.5d and less than 10 d. By the method, the surface roughness can be removed to a greater extent, the surface smoothness of the glass is improved, the loss of the glass plate can be reduced as little as possible, and the preparation of thinner glass plates is facilitated.

The application still provides a glass board, and the surface attachment of glass board has the isolation layer, and the isolation layer is formed by keeping apart the mixed liquid of powder, and this glass board can be the glass body before the crystallization, and the process material of keeping apart the mixed liquid of powder is gone up in the spraying promptly, and the isolation layer includes 5 ~ 85 wt% isolation powder, 8 ~ 12 wt% short solvent and 5 ~ 85 wt% solvent this moment, specifically can be the isolation layer that the mixed liquid of arbitrary one kind of isolation powder formed among the above-mentioned embodiment formed.

The application also provides a glass plate, which can also be a glass plate subjected to crystallization treatment, namely a microcrystalline glass plate, wherein the isolation layer at least comprises partial isolation powder, and also can comprise residual cosolvent molecules and solvent molecules, or a product formed by heating the cosolvent, or a product formed by heating the isolation powder, and the like.

In one embodiment, the glass plate after crystallization is cleaned and polished without polishing or grinding, and the Wa value (the arithmetic mean of the absolute values of the measured waviness profile offsets from the reference line in the sampling length) is measured after cleaning, and the Wa value of the glass plate is 0.1 μm to 10 μm.

The present application will now be illustrated and explained by means of several groups of specific examples, which should not be taken to limit the scope of the present application.

In the embodiment provided by the application, the glass plate is crystallized under different process conditions, and the performance of the obtained microcrystalline glass is tested, wherein the test method and the standard are as follows:

1. degree of crystallinity

And analyzing by an XRD diffractometer to obtain a diffraction peak curve, wherein the incidence angle range is 2Theta which is 10-50 degrees, the scanning speed is 6 degrees/min, and the equipment used in the embodiment is Shimadzu XRD-6000.

Fitting the glass diffraction peak curve in the XRD result by using JADE software, and calculating the crystal proportion contained in the glass.

2. Optical Properties

The transmittance and the b value of the glass under different wavelengths are respectively tested, the b value of the glass is a yellow blue value, the b value is tested as transmission light, the b value is positive and indicates that the transmission blue light is less, namely, the reflection blue light is more, and the larger the b value is, the more blue the glass is.

Optical properties were measured using a haze meter according to GB/T7962.12-2010 colorless optical glass test method part 12: spectral internal transmittance standard test, the device used in this example was a Konika minolta spectrocolorimeter CM-3600A, Japan.

Wa value

The Wa value is the arithmetic mean of the absolute values of the deviation of the measured ripple profile from the baseline within the sampling length.

The Wa value of the glass surface of the glass is tested by using a Tokyo precision roughness meter according to the standard test of GB/T32643-2016 testing method for the surface waviness of the glass of a flat-panel display substrate.

4. Vickers hardness

The Vickers hardness of the glass is tested by using a Vickers hardness tester according to the standard of GB/T37900-2019 test method for the ultra-thin glass hardness and the fracture toughness, namely a small-load Vickers hardness indentation method, in the embodiment, the digital display small-load Vickers hardness tester VTD405 (Beijing Wawei science and technology Co., Ltd.) is used.

In the embodiment provided by the application, the application condition of using the isolation powder mixed solution to manufacture the isolation layer is verified under different crystallization process conditions, and the details of the crystallization process conditions are shown in table 1.

TABLE 1 glass crystallization Process parameters

The embodiment that this application provided has made the mixed liquid of multiple isolation powder to be used for making the isolation layer, the preparation method of the mixed liquid of isolation powder is as follows:

the isolation powder, the solvent and the dissolution accelerator with corresponding components and dosage are respectively weighed and evenly mixed to obtain isolation powder mixed solution 1, isolation powder mixed solution 2 and isolation powder mixed solution 3, and the specific component proportion refers to table 2.

TABLE 2 ingredient table of mixed solution of isolating powder

This application has verified the application condition who uses the mixed liquid preparation isolation layer of isolation powder from different angles, specifically as follows:

(1) influence of different isolation layers on the crystallization process

Comparative examples 1 to 8

And directly laying a group of glass blanks in a single layer without using an isolation layer in a high-temperature furnace, and respectively crystallizing the glass under the same crystallization process conditions to obtain the microcrystalline glass. And carrying out flat grinding and polishing processing on the obtained microcrystalline glass, and carrying out performance test on the processed microcrystalline glass. See table 3 for specific experimental conditions and test results.

Comparative examples 9 to 16

Respectively using boron nitride powder with different amounts to manufacture isolating layers, stacking the glass blanks provided with the isolating layers, placing the glass blanks in a high-temperature furnace, and respectively crystallizing the glass under the same crystallization process conditions to obtain the microcrystalline glass. And carrying out flat grinding and polishing processing on the obtained microcrystalline glass, and carrying out performance test on the processed microcrystalline glass. See table 3 for specific experimental conditions and test results.

Examples 1 to 12

The isolating layers are manufactured by respectively using different amounts of isolating powder mixed liquid 1, isolating powder mixed liquid 2 and isolating powder mixed liquid 3, and a layer of isolating powder mixed liquid can be uniformly sprayed on the surface of the glass blank by a spray gun to form the isolating layer. And stacking the glass blanks provided with the isolating layers, placing the glass blanks in a high-temperature furnace, and respectively crystallizing the glass under the same crystallization process conditions to obtain the microcrystalline glass. And carrying out flat grinding and polishing processing on the obtained microcrystalline glass, and carrying out performance test on the processed microcrystalline glass. See table 3 for specific experimental conditions and test results.

TABLE 3 Property parameters of the glass ceramics obtained with different barrier layers

It can be seen from comparison of experimental examples 1 to 24 and comparative examples 1 to 16 that, in the same crystallization processes, the optical properties of the microcrystalline glass obtained without using the spacer layer are almost the same as those of the microcrystalline glass obtained with the spacer powder mixture, and the optical properties of the microcrystalline glass obtained with the boron nitride powder mixture are slightly inferior to those of the microcrystalline glass obtained without using the spacer layer. Therefore, the mixed solution of the isolation powder can be used for manufacturing the isolation layer between glass plates in the crystallization process, the performance of the obtained microcrystalline glass is basically not influenced, and meanwhile, the production efficiency of the microcrystalline glass can be improved and the production cost can be reduced.

(2) Influence of different usage of isolation layer on crystallization process

Examples 1 to 24

The isolating layers are manufactured by respectively using different amounts of isolating powder mixed liquid 1, isolating powder mixed liquid 2 and isolating powder mixed liquid 3, and a layer of isolating powder mixed liquid can be uniformly sprayed on the surface of the glass blank by a spray gun to form the isolating layer. And stacking the glass blanks provided with the isolating layers, placing the glass blanks in a high-temperature furnace, and respectively crystallizing the glass under the same crystallization process conditions to obtain the microcrystalline glass. And carrying out flat grinding and polishing processing on the obtained microcrystalline glass, and carrying out performance test on the processed microcrystalline glass. See table 3 for specific experimental conditions and test results.

In comparison with examples 1-24, under the same crystallization process conditions, the microcrystalline glass prepared by using the same spacer powder mixed solution with different amounts has better performance, and the performance of the microcrystalline glass cannot be affected by different amounts. Therefore, the influence of the use amount of the isolation powder mixed liquid on the crystallization treatment process is small, and in actual use, the isolation powder mixed liquid can be used as less as required, so that the use amount of the isolation powder is reduced, and the production cost is reduced.

(3) Influence of different crystallization process conditions on the crystallization process

Examples 25 to 45

The isolation layer is manufactured by respectively using the same amount of isolation powder mixed solution 1, isolation powder mixed solution 2 and isolation powder mixed solution 3, and specifically, a layer of isolation powder mixed solution can be uniformly sprayed on the surface of the glass blank by using a spray gun to form the isolation layer. And stacking the glass blanks provided with the isolating layers, placing the glass blanks in a high-temperature furnace, and respectively carrying out crystallization treatment on the glass under a plurality of different crystallization process conditions to obtain the microcrystalline glass. And carrying out flat grinding and polishing processing on the obtained microcrystalline glass, and carrying out performance test on the processed microcrystalline glass. See table 4 for specific experimental conditions and test results.

TABLE 4 Property parameters of the glass ceramics obtained under different crystallization process conditions

In comparative examples 25 to 45, the optical properties of the microcrystalline glasses prepared under the same crystallization process conditions were almost the same without any difference under the same amount of different spacer powder mixtures, and the performance of the microcrystalline glasses was not affected by the different crystallization processes. From this, the isolation powder mixed liquid that this application provided is applicable in multiple crystallization technology, and the content of isolating the powder in the isolation powder mixed liquid influences crystallization technology not very, in-service use, can prepare the isolation powder mixed liquid of appropriate concentration as required to follow-up spraying makes the spraying more even.

(4) Influence of different barrier layers on the surface of the glass

Comparative examples 17 to 28

Respectively using boron nitride powder with different amounts to manufacture isolating layers, stacking the glass blanks provided with the isolating layers, placing the glass blanks in a high-temperature furnace, and respectively crystallizing the glass under the same crystallization process conditions to obtain the microcrystalline glass. Cleaning the crystallized microcrystalline glass sheet by using an ultrasonic cleaning machine, wherein the cleaning conditions comprise that: cleaning time: 5-10 min; the used cleaning agents: diluting the common washing powder by 10 times; cleaning temperature: 45-65 ℃; cleaning frequency: 20KHZ-40 KHZ. After cleaning, the Wa value of the surface of the microcrystalline glass sheet is tested. See table 5 for specific experimental conditions and test results.

Examples 46 to 81

The isolating layers are manufactured by respectively using different amounts of isolating powder mixed liquid 1, isolating powder mixed liquid 2 and isolating powder mixed liquid 3, and a layer of isolating powder mixed liquid can be uniformly sprayed on the surface of the glass blank by a spray gun to form the isolating layer. And stacking the glass blanks provided with the isolating layers, placing the glass blanks in a high-temperature furnace, and respectively crystallizing the glass under the same crystallization process conditions to obtain the microcrystalline glass. Cleaning the crystallized microcrystalline glass sheet by using an ultrasonic cleaning machine, wherein the cleaning conditions comprise that: cleaning time: 5-10 min; the used cleaning agents: diluting the common washing powder by 10 times; cleaning temperature: 45-65 ℃; cleaning frequency: 20KHZ-40 KHZ. After cleaning, the Wa value of the surface of the microcrystalline glass sheet is tested. See table 5 for specific experimental conditions and test results.

TABLE 5 Property parameters (Wa values) of the devitrified glasses obtained with different barrier layers

Comparing the experimental examples 46-57 with the comparative examples 17-20, it can be seen that the use of the spacer powder mixture to make the spacer layer results in less adsorption of the spacer on the surface of the crystallized glass and a relatively flat glass surface. It can be seen from comparative examples 46 to 57 that as the amount of the spacer used increases, the amount of the spacer adsorbed remains increases, and the flatness of the glass surface decreases. Therefore, on the basis of the isolation effect, the using amount of the isolation layer can be reduced as much as possible, so that the adsorption after crystallization is reduced, the flatness of the surface of the glass is improved, and the separation and the subsequent treatment between the glass plates are facilitated.

(5) Effect of different barrier layers on the mechanical Properties of glass

The method also comprises the steps of carrying out chemical strengthening treatment on the crystallized microcrystalline glass, and carrying out mechanical property test on the strengthened microcrystalline glass.

Each sample batch comprises 5 microcrystalline glass sheet samples, the samples are microcrystalline glass sheets obtained after crystallization treatment under the same condition, and the Vickers hardness of the batch is an average value of all samples of the batch. Specific preparation experimental conditions and test results are detailed in table 6.

TABLE 6 Vickers hardness test results for microcrystalline glasses

As can be seen from the data in the table, the mechanical properties of the obtained glass ceramics are good when no isolation layer is used. The isolating layer is made of the isolating powder mixed liquid, the mechanical property of the obtained microcrystalline glass is almost the same as that of the microcrystalline glass without the isolating layer, the microcrystalline glass still has good mechanical property, and the mechanical property of the crystallized microcrystalline glass cannot be influenced by the isolating layer. The isolation layer is made of the isolation powder mixed liquid, the mechanical property of the obtained microcrystalline glass is almost the same as that of the isolation layer made of the boron nitride powder, the microcrystalline glass still has good mechanical property, and the mechanical property of the crystallized microcrystalline glass cannot be influenced by using different isolation layers. Therefore, the mixed solution of the isolation powder can be used for manufacturing the spacers between glass plates in the crystallization process, the mechanical property of the obtained microcrystalline glass cannot be influenced, and meanwhile, the production efficiency of the microcrystalline glass can be improved and the production cost can be reduced.

In the above embodiment, the mixed solution of the spacer powders with different concentrations, the usage amount of the mixed solution of the different spacer powders, and different crystallization processes are compared and analyzed, and the method is opposite to other types of isolation layers, so that the spacer powder mixed solution provided by the application is verified, can be applied to different glass crystallization processes, has no influence on the performance of crystallized glass, can improve the surface flatness of the crystallized glass plate, and is beneficial to subsequent processing.

Above scheme, the glass crystallization method that this application provided provides the multi-disc glass body, piles up at least part of glass body, and set up the isolation layer that is formed by keeping apart the powder mixed solution between adjacent two-layer glass body, can prevent to take place the adhesion between the glass body at the crystallization in-process, and will keep apart the powder and form the isolation layer with the form of mixed solution between two-layer glass body, can promote the dispersion ability who keeps apart the powder, reduce the space between the glass body because of the reunion of powder causes, thereby the homogeneity of reinforcing glass body surface temperature field, make the even crystallization degree of glass body higher. Meanwhile, unevenness of the glass surface caused by adsorption of the spacer can be reduced to a certain extent.

The above description is only an embodiment of the present application, and not intended to limit the scope of the present application, and all modifications of equivalent structures and equivalent processes, which are made by using the contents of the present specification and the accompanying drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.