CN110577364A - Lithium-aluminum silicate nanocrystalline glass ceramic and preparation method thereof - Google Patents

Lithium-aluminum silicate nanocrystalline glass ceramic and preparation method thereof Download PDF

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Publication number
CN110577364A
CN110577364A CN201910848520.0A CN201910848520A CN110577364A CN 110577364 A CN110577364 A CN 110577364A CN 201910848520 A CN201910848520 A CN 201910848520A CN 110577364 A CN110577364 A CN 110577364A
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lithium aluminosilicate
oxide
nanocrystalline glass
glass ceramic
nanocrystalline
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Inventor
张月皎
姚全星
罗恺
袁晓波
刘庆
李军旗
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Shenzhen Jingshi Yun Chuang Technology Co Ltd
Shenzhen Jingjiang Yunchuang Technology Co Ltd
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Shenzhen Jingshi Yun Chuang Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00Other methods of shaping glass
    • C03B19/02Other methods of shaping glass by casting molten glass, e.g. injection moulding
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B25/00Annealing glass products
    • C03B25/02Annealing glass products in a discontinuous way
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C10/00Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0009Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing silica as main constituent
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C10/00Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0018Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and monovalent metal oxide as main constituents
    • C03C10/0027Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and monovalent metal oxide as main constituents containing SiO2, Al2O3, Li2O as main constituents

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Dispersion Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Glass Compositions (AREA)

Abstract

The invention provides a lithium aluminosilicate nanocrystalline glass ceramic, which comprises the following components in percentage by weight: 5% -15% of lithium oxide (Li)2o), 40% -80% of silicon dioxide (SiO)2) And 10% -35% of alumina (Al)2O3) Wherein the lithium oxide is used for reducing the expansion coefficient of the lithium aluminosilicate nanocrystalline glass ceramic, the silicon dioxide is used for forming the framework of the lithium aluminosilicate nanocrystalline glass ceramic, and the aluminum oxide is used for enhancing the mechanical strength of the lithium aluminosilicate nanocrystalline glass ceramic. The invention also provides a preparation method of the lithium aluminosilicate nanocrystalline glass ceramic.

Description

Lithium-aluminum silicate nanocrystalline glass ceramic and preparation method thereof
Technical Field
The invention relates to the field of chemical industry, in particular to a lithium-aluminum silicate nanocrystalline glass ceramic and a preparation method thereof.
Background
Nanocrystalline glass-ceramics are a multiphase composite material that combines a dense nanocrystalline phase (crystalline phase) with a glassy phase. After the base glass with specific composition is heat treated, the glass liquid phase generates nucleus and grows crystal, and the composite material with homogeneous nanometer crystal phase and glass phase is further produced. The nano-crystalline glass ceramic has excellent performance, on one hand, the nano-crystalline glass ceramic has the characteristics of high strength, high hardness and the like of the ceramic, and the nano-crystalline glass ceramic has good wear resistance and corrosion resistance, strong impact resistance and stable chemical performance; on the other hand, the nanocrystalline glass ceramic has high permeability of glass, and can realize curved surface molding by using a thermal molding process. The nanocrystalline glass ceramic can be widely applied to screen cover plates and back plates of intelligent products such as smart phones, smart watches, tablet computers, automobile central control protection screens and the like, and can also be widely applied to microscopes, digital cameras, projectors and various optical lenses.
The performance of the nanocrystalline glass ceramic is greatly influenced by the component proportion, and the existing nanocrystalline glass ceramic has certain expansion coefficient and is not suitable for some fields. It is considered by those skilled in the art how to provide a novel nanocrystalline glass-ceramic and a method for preparing the same.
Disclosure of Invention
In view of this, the present invention provides a lithium aluminosilicate nanocrystalline glass ceramic and a method for preparing the same.
The invention provides a lithium aluminosilicate nanocrystalline glass ceramic, which comprises the following components in percentage by weight: 5% -15% of lithium oxide (Li)2O), 40% -80% of silicon dioxide (SiO)2) And 10% -35% of alumina (Al)2O3) Wherein the lithium oxide is used for reducing the expansion coefficient of the lithium aluminosilicate nanocrystalline glass ceramic, the silicon dioxide is used for forming the framework of the lithium aluminosilicate nanocrystalline glass ceramic, and the aluminum oxide is used for enhancing the mechanical strength of the lithium aluminosilicate nanocrystalline glass ceramic.
Further, the paint also comprises the following components in percentage by weight: 0% -10% potassium oxide (K)2O), 0% -15% of sodium oxide (Na)2O), 0-5% of calcium oxide (CaO) and 0-5% of niobium pentoxide (Nb)2O5) Wherein, the potassium oxide, the sodium oxide, the calcium oxide, the ferric oxide and the niobium pentoxide are taken as cosolvents.
Further, the paint also comprises the following components in percentage by weight: 0% -5% of chromium oxide (Cr)2O3) 0% -5% of ferric oxide (Fe)2O3) 0% -10% of phosphorus oxide (P)2O5) 0% -15% of titanium dioxide (TiO)2) 0% -10% of zirconium dioxide (ZrO)2) The lithium aluminosilicate nanocrystalline glass ceramic is characterized by comprising chromium sesquioxide, iron sesquioxide, phosphorus oxide, titanium dioxide and zirconium dioxide, wherein the chromium sesquioxide, the iron sesquioxide, the phosphorus oxide, the titanium dioxide and the zirconium dioxide are used as nucleating agents, and the nucleating agents promote the formation and growth of crystal nuclei in the melting process of the lithium aluminosilicate nanocrystalline glass ceramic.
Further, the composition of the crystal nucleus agent may further include silver (Ag).
Further, the paint also comprises the following components in percentage by weight: 0% -5% of stannic oxide (SnO)2) 0% -5% of antimony oxide (Sb)2O3) And 0% -5% of arsenic trioxide (As)2O3) Wherein the tin dioxide, antimony oxide and arsenic trioxide are used as clarifying agents, and the clarifying agents promote bubble removal in the melting process of the lithium aluminosilicate nanocrystalline glass ceramic.
Further, the paint also comprises the following components in percentage by weight: 0% -10% of magnesium oxide (MgO) and 0% -10% of zinc oxide (ZnO), wherein the magnesium oxide and the zinc oxide are used for enhancing the mechanical strength and the chemical stability of the lithium aluminosilicate nanocrystalline glass ceramic.
further, the paint also comprises the following components in percentage by weight: 0% -5% barium oxide (BaO), wherein said barium oxide is used to increase the refractive index, density, gloss and chemical stability of said lithium aluminosilicate nanocrystalline glass ceramic.
The invention also provides a preparation method of the lithium aluminosilicate nanocrystalline glass ceramic, which comprises the following steps:
Providing raw materials with the components, mixing the raw materials, placing the mixture into a first reaction kettle, and heating the first reaction kettle until the raw materials are molten to obtain a first mixture;
Providing a mould, and injecting the first mixture into the mould for cooling and forming to obtain a lithium aluminosilicate nanocrystalline glass ceramic semi-finished product;
Placing the lithium aluminosilicate nanocrystalline glass ceramic semi-finished product into a second reaction kettle, keeping the temperature of the second reaction kettle within the range of 500-800 ℃, and preserving heat for 2-10 hours to obtain a second mixture; and
And adjusting the temperature of the second reaction kettle to be 650-1050 ℃, and preserving the heat for 2-12 hours to obtain the lithium aluminosilicate nanocrystalline glass ceramic.
Further, cutting, surface treatment and strengthening are carried out on the lithium aluminosilicate nanocrystalline glass ceramic.
Further, the grain size in the lithium aluminosilicate nanocrystalline glass ceramic ranges from 1nm to 100 nm.
The lithium aluminosilicate nanocrystalline glass ceramic material has excellent mechanical strength and chemical stability and a low expansion coefficient.
Drawings
Fig. 1 is a schematic flow chart of a method for preparing a lithium aluminosilicate nanocrystalline glass ceramic according to an embodiment of the present invention.
Description of the main elements
step (ii) of S1~S5
The following detailed description will further illustrate the invention in conjunction with the above-described figures.
Detailed Description
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention and the scope of the present invention is therefore not limited to the specific embodiments disclosed below.
The lithium aluminosilicate nanocrystalline glass ceramic of the invention comprises the following raw materials by weight percent:
Lithium oxide (Li)2O) 5% -15%, silicon dioxide (SiO)2) 40-80% of aluminum oxide (Al)2O3) 10-35 percent of magnesium oxide (MgO), 0-20 percent of zinc oxide (ZnO), 0-10 percent of potassium oxide (K)2O) 0% -10%, sodium oxide (Na)20 to 15 percent of O), 0 to 5 percent of calcium oxide (CaO), and ferric oxide (Fe)2O3) 0% -5% of chromium oxide (Cr)2O3)0-5 percent of nickel oxide (NiO), 0-5 percent of phosphorus oxide (P)2O5) 0% -10% of titanium dioxide (TiO)2) 0% -15% of zirconium dioxide (ZrO)2) 0% -10% of tin dioxide (SnO)2) 0% -5% of niobium pentoxide (Nb)2O5) 0% -5%, antimony oxide (Sb)2O3) 0% -5% of arsenic trioxide (As)2O3) 0-5%, barium oxide (BaO) 0-5% and trace silver (Ag).
Wherein Li2O is used for replacing potassium oxide or sodium oxide in the traditional nanocrystalline glass ceramic, and Li2O can adjust the thermal expansion coefficient of the material to manufacture the low-expansion or zero-expansion nanocrystalline glass ceramics for special optical products. Li2The content of O can also control the crystallization tendency of the material, Li2O may also be in oneThe melting temperature and viscosity of the material are reduced to a certain degree, so that the difficulty of subsequent curved surface forming of the material is reduced, and Li2The percentage by weight of O may be between 5% and 15%.
Wherein, SiO2SiO, the basic skeleton for forming lithium aluminosilicate nanocrystalline glass ceramics2Too low a content may destabilize or coarsen the crystalline phase generated in the lithium aluminosilicate nanocrystalline glass ceramic and may cause the lithium aluminosilicate nanocrystalline glass ceramic to lack gloss or even to devitrify, while SiO2too high a content may make the raw material difficult to melt, so that the preparation process of the lithium aluminosilicate nanocrystalline glass ceramic requires a higher melting temperature, and therefore, SiO2The weight percentage of the components is controlled to be between 40 and 80 percent.
Among them, BaO can be used to increase the refractive index, density, gloss and chemical stability of the lithium aluminosilicate nanocrystalline glass ceramic, but when the BaO content is too high, it may cause the lithium aluminosilicate nanocrystalline glass ceramic material to be not clear, and therefore, the weight percentage of BaO should be controlled between 0% and 5%.
Wherein, Al2O3Can be used to increase the mechanical strength and stability of lithium aluminosilicate nanocrystalline glass ceramics, however, when Al is used2O3Too high a content may cause difficulty in the melting process of the lithium aluminosilicate nanocrystalline glass ceramic or a decrease in devitrification resistance thereof, and therefore, Al2O3The weight percentage of the components is controlled to be between 10 and 35 percent.
The MgO can be used for enabling the lithium aluminosilicate nanocrystalline glass ceramic to form a high-strength stable crystalline phase, and the proper amount of the MgO can be added to enhance the mechanical strength and the chemical stability of the lithium aluminosilicate nanocrystalline glass ceramic, so that the weight percentage of the MgO can be between 0 and 20 percent.
Wherein, ZnO can be used for improving the chemical stability of the lithium aluminosilicate nanocrystalline glass ceramic, and can be used for reducing the softening point temperature of the lithium aluminosilicate nanocrystalline glass ceramic, which is beneficial to the melting preparation process of the lithium aluminosilicate nanocrystalline glass ceramic, but the high ZnO content can cause the crystal phase variety to change greatly, further leading the stable crystal grain not to be formed, therefore, the weight percentage of ZnO should be controlled between 0 percent and 10 percent.
Wherein, K2O、Na2O can be used as a good cosolvent, can be an oxide outside a lithium aluminosilicate nanocrystalline glass ceramic structure network, and can effectively reduce the viscosity of the lithium aluminosilicate nanocrystalline glass ceramic so as to reduce the melting temperature. However, excessive Na2The thermal expansion coefficient of the lithium aluminosilicate nanocrystalline glass ceramic is increased by O, and the mechanical strength and the chemical stability of the lithium aluminosilicate nanocrystalline glass ceramic are reduced; k2O can increase the transparency and gloss of lithium aluminosilicate nanocrystalline glass ceramics, but the content of K is too high2O reduces the devitrification ability of the lithium aluminosilicate nanocrystalline glass ceramic, and thus, K2The weight percentage of O is controlled between 0 percent and 10 percent, Na2The weight percentage of O is controlled between 0% and 15%.
Wherein, CaO can be used as a good cosolvent and a stabilizer, can be an oxide outside a lithium aluminosilicate nanocrystalline glass ceramic structure network, and can effectively reduce the viscosity of the lithium aluminosilicate nanocrystalline glass ceramic so as to reduce the melting temperature. However, excessive CaO may lead to a reduction in glass fritness, an increase in brittleness, and an increase in crystallization tendency of the lithium aluminosilicate nanocrystalline glass ceramic, and thus the weight percentage of CaO should be controlled between 0% and 5%.
Wherein Nb2O5can be used as good cosolvent and stabilizer, can be used for improving the chemical stability of lithium aluminosilicate nanocrystalline glass ceramic and the thermal stability of glass ceramic, and simultaneously can reduce the softening point, so that Nb2O5The weight percentage of the components is controlled to be between 0 and 5 percent.
Wherein, Fe2O3Can be used as a crystal nucleus agent, Fe2O3Precipitation and formation of nanocrystalline phases may be promoted, however, Fe2O3Too high a content may result in a deterioration of the compactness of the material and a decrease in the chemical stability of the material, and therefore, Fe2O3The weight percentage of the components is controlled to be between 0 and 5 percent.
Wherein, Cr2O3Can be used as a crystal nucleus agent, Cr2O3Precipitation and formation of nanocrystalline phases may be promoted, however, Cr2O3The inclusion of chromium has a coloring effect which affects the transparency of the lithium aluminosilicate nanocrystalline glass ceramic, and therefore, Cr2O3the weight percentage of the components is controlled to be between 0 and 5 percent.
Wherein, P2O5Can be used as a crystal nucleus agent, P2O5Can promote the precipitation and formation of nanocrystalline phase and prevent excessive grain growth, and can improve the dispersion coefficient and transmittance of lithium aluminosilicate nanocrystalline glass ceramic, but with excessive content of P2O5The material thermal expansion coefficient is increased because the lithium aluminosilicate nanocrystalline glass ceramic generates a white turbidity phenomenon and is devitrified, so that P2O5The weight percentage of the components is controlled to be between 0 and 10 percent.
Wherein, TiO2Can be used as a crystal nucleus agent, TiO2Can promote the precipitation and formation of nanocrystalline phase and increase the uniformity of the lithium aluminosilicate nanocrystalline glass ceramic, but contains too much TiO2May cause devitrification of the lithium aluminosilicate nanocrystalline glass ceramic and, therefore, of the TiO2The weight percentage of the components is controlled to be between 0 and 15 percent.
Wherein, ZrO2Can be used as a nucleating agent, ZrO2Can promote the precipitation and formation of nanocrystalline phase and make the crystal grain fine, further can increase the mechanical strength and chemical stability of the lithium aluminosilicate nanocrystalline glass ceramic, but the content of TiO is too high2May cause difficulty in melting the raw material, and thus, ZrO2The weight percentage of the components is controlled to be between 0 and 10 percent.
Wherein Sb2O3、As2O3、SnO2can be used as clarifier, Sb2O3、As2O3、SnO2Is favorable for promoting the discharge of bubbles in the process of melting raw materials, further improves the compactness of the lithium aluminosilicate nanocrystalline glass ceramic, and Sb2O3、As2O3、SnO2In percentage by weight ofCan be between 0% and 5%.
Wherein Ag can be used as a crystal nucleus agent.
In one embodiment, the lithium aluminosilicate nanocrystalline glass ceramic may be LiO-containing2LiO of (2)2-Al2O3-SiO2The nanocrystalline glass-ceramic of the system, the crystalline phase of the lithium aluminosilicate nanocrystalline glass-ceramic may comprise 2SiO2-Li2Lithium O-disilicate, nepheline, spinel, cordierite, beta-quartz, beta-spodumene, and the like.
The raw materials can be mixed according to the proportion to prepare the lithium aluminosilicate nanocrystalline glass ceramic, and the prepared lithium aluminosilicate nanocrystalline glass ceramic can be strengthened by a strengthening method to enhance the performance of the lithium aluminosilicate nanocrystalline glass ceramic.
As shown in fig. 1, the preparation method of the lithium aluminosilicate nanocrystalline glass ceramic provided by the invention comprises the following steps:
Step S1: mixing the raw materials of the components, placing the mixture into a first reaction kettle, and heating the first reaction kettle until the raw materials are melted to obtain a first mixture;
Specifically, the raw materials of the components are placed in a first reaction kettle, which can be a smelting furnace, to be fully mixed and uniformly stirred, the first reaction kettle is heated to enable the temperature of the first reaction kettle to range from 950 ℃ to 1700 ℃, and the raw materials are fully melted to obtain the first mixture.
During the melting process, the gap channel between the raw materials is gradually reduced into a single gap, or the air in the gap is removed in the form of bubbles, and a glassy molten substance is formed.
Step S2: and providing a mould, and injecting the first mixture into the mould for cooling and forming to obtain a lithium aluminosilicate nanocrystalline glass ceramic semi-finished product.
Specifically, the first mixture in a molten state is injected into the mold from the first reaction kettle, and the lithium aluminosilicate nanocrystalline glass ceramic semi-finished product is obtained after cooling. In one embodiment, the first mixture may be rolled or pressed to obtain a sheet-like semifinished lithium aluminosilicate nanocrystalline glass ceramic product with a thickness ranging from 0.2 to 5 mm; in other embodiments, the lithium aluminosilicate nanocrystalline glass ceramic blank may be a rectangular parallelepiped spindle. Step S3: and placing the lithium aluminosilicate nanocrystalline glass ceramic semi-finished product into a second reaction kettle, keeping the temperature of the second reaction kettle within the range of 500-800 ℃, and preserving the heat for 2-10 hours to obtain a second mixture.
Specifically, a second reaction kettle is provided, which can be an annealing furnace, the lithium aluminosilicate nanocrystalline glass ceramic semi-finished product is placed in the annealing furnace, the temperature of the annealing furnace is kept at 500-800 ℃, and the temperature is kept for 2-10 hours to obtain the second mixture.
Step S4: and adjusting the temperature of the second reaction kettle to be 650-1050 ℃, and preserving the heat for 2-12 hours to obtain the lithium aluminosilicate nanocrystalline glass ceramic.
Specifically, the temperature of the annealing furnace is adjusted to enable the temperature range of the annealing furnace and the second mixture in the annealing furnace to be 650-1050 ℃, and the temperature is kept for 2-12 hours in the temperature range, so that nanocrystal nuclei grow to obtain the lithium aluminosilicate nanocrystal glass ceramic. The type, the grain size and the content of a nanocrystalline phase in the nano glass ceramic can be controlled by adjusting different crystal nucleus growth temperatures and heat preservation time, so that the lithium aluminosilicate nano glass ceramic with specific performance is obtained.
Step S3 and step S4 are annealing processes, and adjusting the temperature in the annealing furnace can control the formation of nanocrystalline phases to obtain different lithium aluminosilicate nanocrystalline glass ceramics. The grain size in the lithium aluminosilicate nanocrystalline glass ceramic is smaller, and the grain size in the lithium aluminosilicate nanocrystalline glass ceramic is 1nm to 100 nm.
step S5: cutting, surface treatment and strengthening are carried out on the lithium aluminosilicate nanocrystalline glass ceramic.
Specifically, the lithium aluminosilicate nanocrystalline glass ceramic is cut to obtain a certain shape, and then the lithium aluminosilicate nanocrystalline glass ceramic is subjected to treatments such as grinding and polishing to remove impurities on the surface of the lithium aluminosilicate nanocrystalline glass ceramic and material defects (point defects, line defects or surface defects) on the surface.
Furthermore, the lithium aluminosilicate nanocrystalline glass ceramic can be subjected to chemical strengthening treatment in an ion exchange mode to enhance the material performance of the lithium aluminosilicate nanocrystalline glass ceramic.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (10)

1. The lithium aluminosilicate nanocrystalline glass ceramic is characterized by comprising the following components in percentage by weight: 5% -15% of lithium oxide (Li)2O), 40% -80% of silicon dioxide (SiO)2) And 10% -35% of alumina (Al)2O3) Wherein the lithium oxide is used for reducing the expansion coefficient of the lithium aluminosilicate nanocrystalline glass ceramic, the silicon dioxide is used for forming the framework of the lithium aluminosilicate nanocrystalline glass ceramic, and the aluminum oxide is used for enhancing the mechanical strength of the lithium aluminosilicate nanocrystalline glass ceramic.
2. The lithium aluminosilicate nanocrystalline glass-ceramic according to claim 1, further comprising the following components in weight percent: 0% -10% potassium oxide (K)2O), 0% -15% of sodium oxide (Na)2O), 0-5% of calcium oxide (CaO) and 0-5% of niobium pentoxide (Nb)2O5) Wherein, the potassium oxide, the sodium oxide, the calcium oxide, the ferric oxide and the niobium pentoxide are taken as cosolvents.
3. The lithium aluminosilicate nanocrystalline glass-ceramic according to claim 2, further comprising the following components in weight percent: 0% -5% of chromium oxide (Cr)2O3) 0% -5% of ferric oxide (Fe)2O3) 0% -10% of phosphorus oxide (P)2O5) 0% -15% of titanium dioxide (TiO)2) 0% -10% of zirconium dioxide (ZrO)2) The lithium aluminosilicate nanocrystalline glass ceramic is characterized by comprising chromium sesquioxide, iron sesquioxide, phosphorus oxide, titanium dioxide and zirconium dioxide, wherein the chromium sesquioxide, the iron sesquioxide, the phosphorus oxide, the titanium dioxide and the zirconium dioxide are used as nucleating agents, and the nucleating agents promote the formation and growth of crystal nuclei in the melting process of the lithium aluminosilicate nanocrystalline glass ceramic.
4. The lithium aluminosilicate nanocrystalline glass-ceramic according to claim 3, characterized in that the composition of the nucleating agent may also include silver (Ag).
5. The lithium aluminosilicate nanocrystalline glass-ceramic according to claim 3, further comprising the following components in weight percent: 0% -5% of stannic oxide (SnO)2) 0% -5% of antimony oxide (Sb)2O3) And 0% -5% of arsenic trioxide (As)2O3) Wherein the tin dioxide, antimony oxide and arsenic trioxide are used as clarifying agents, and the clarifying agents promote bubble removal in the melting process of the lithium aluminosilicate nanocrystalline glass ceramic.
6. The lithium aluminosilicate nanocrystalline glass-ceramic according to claim 5, further comprising the following components in weight percent: 0% -10% of magnesium oxide (MgO) and 0% -10% of zinc oxide (ZnO), wherein the magnesium oxide and the zinc oxide are used for enhancing the mechanical strength and the chemical stability of the lithium aluminosilicate nanocrystalline glass ceramic.
7. The lithium aluminosilicate nanocrystalline glass-ceramic according to claim 6, further comprising the following components in weight percent: 0% -5% barium oxide (BaO), wherein said barium oxide is used to increase the refractive index, density, gloss and chemical stability of said lithium aluminosilicate nanocrystalline glass ceramic.
8. The preparation method of the lithium aluminosilicate nanocrystalline glass ceramic is characterized by comprising the following steps:
Providing raw materials of the components of any one of claims 1 to 7, mixing the raw materials, placing the mixture in a first reaction kettle, and heating the first reaction kettle until the raw materials are molten to obtain a first mixture;
Providing a mould, and injecting the first mixture into the mould for cooling and forming to obtain a lithium aluminosilicate nanocrystalline glass ceramic semi-finished product;
placing the lithium aluminosilicate nanocrystalline glass ceramic semi-finished product into a second reaction kettle, keeping the temperature of the second reaction kettle within the range of 500-800 ℃, and preserving heat for 2-10 hours to obtain a second mixture; and
And adjusting the temperature of the second reaction kettle to be 650-1050 ℃, and preserving the heat for 2-12 hours to obtain the lithium aluminosilicate nanocrystalline glass ceramic.
9. The method of making lithium aluminosilicate nanocrystalline glass-ceramic according to claim 8, further comprising the steps of:
Cutting, surface treatment and strengthening are carried out on the lithium aluminosilicate nanocrystalline glass ceramic.
10. The method of producing lithium aluminosilicate nanocrystalline glass-ceramic according to claim 8, wherein the grain size in the lithium aluminosilicate nanocrystalline glass-ceramic ranges from 1nm to 100 nm.
CN201910848520.0A 2019-09-09 2019-09-09 Lithium-aluminum silicate nanocrystalline glass ceramic and preparation method thereof Pending CN110577364A (en)

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CN114790083A (en) * 2022-05-05 2022-07-26 山东国瓷功能材料股份有限公司 Glass ceramic and preparation method and application thereof
CN115667168A (en) * 2020-04-29 2023-01-31 康宁公司 Composition and method for making glass-ceramic articles
CN115893851A (en) * 2023-01-16 2023-04-04 清远南玻节能新材料有限公司 Microcrystalline glass and preparation method thereof

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