CN113233779A - Microcrystalline glass composite material and preparation method thereof - Google Patents
Microcrystalline glass composite material and preparation method thereof Download PDFInfo
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- CN113233779A CN113233779A CN202110590719.5A CN202110590719A CN113233779A CN 113233779 A CN113233779 A CN 113233779A CN 202110590719 A CN202110590719 A CN 202110590719A CN 113233779 A CN113233779 A CN 113233779A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
- C03C14/002—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of fibres, filaments, yarns, felts or woven material
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C10/00—Devitrified 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
- C03C10/0036—Devitrified 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 a divalent metal oxide as main constituents
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C12/00—Powdered glass; Bead compositions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C2214/00—Nature of the non-vitreous component
- C03C2214/08—Metals
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C2214/00—Nature of the non-vitreous component
- C03C2214/20—Glass-ceramics matrix
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C2214/00—Nature of the non-vitreous component
- C03C2214/30—Methods of making the composites
Abstract
The invention discloses a microcrystalline glass composite material and a preparation method thereof. The preparation method comprises the following steps: providing glass powder; uniformly stirring the glass powder and liquid sodium silicate to obtain a mixed material; the mass percentage of the liquid sodium silicate in the mixed material is 3-5 wt%; laying the mixed material in a mould, putting a nickel net into the mould, and then continuously laying the mixed material on the nickel net; and compacting and drying the mixed material in the mould, and then heating for crystallization. The strength of the microcrystalline glass composite material is greatly improved.
Description
Technical Field
The invention relates to a microcrystalline glass composite material and a preparation method thereof.
Background
The microcrystal glass is also called glass ceramic and is a composite material containing a large amount of microcrystal phase and glass phase which are uniformly distributed. The microcrystalline glass has the characteristics of no brittleness, high strength, good chemical stability, high thermal stability and hardness and the like, and becomes a unique novel material.
However, the strength of the microcrystalline glass still needs to be further improved.
Disclosure of Invention
In view of the above disadvantages, it is necessary to provide a new method for preparing a glass-ceramic composite material.
A preparation method of a microcrystalline glass composite material comprises the following steps:
providing glass powder;
uniformly stirring the glass powder and liquid sodium silicate to obtain a mixed material; the mass percentage of the liquid sodium silicate in the mixed material is 3-5 wt%;
laying the mixed material in a mould, putting a nickel net into the mould, and then continuously laying the mixed material on the nickel net;
and compacting and drying the mixed material in the mould, and then heating for crystallization.
The strength of the microcrystalline glass composite material obtained by the preparation method is greatly increased.
Preferably, the modulus of the liquid sodium silicate is 2-3.
Preferably, the components of the glass frit include:
60 to 75 wt% of SiO215 to 20 wt% of CaO, 5 to 10 wt% of Al2O31 to 3 wt% of BaO, 3 to 5 wt% of Na2O, 1-3 wt% of ZnO, 1-3 wt% of B2O3。
Preferably, the granularity of the glass powder is 100 meshes to 200 meshes.
Preferably, the glass frit is obtained by the following steps:
mixing and heating the raw materials according to a proportion to obtain molten glass; the raw materials comprise 40-60 wt% of feldspar, 15-25 wt% of quartz sand, 15-25 wt% of calcite, 0.5-2 wt% of borax, 1-3 wt% of barium carbonate, 1-3 wt% of soda ash and 1-3 wt% of zinc oxide;
water quenching the molten glass to obtain glass particles;
and ball-milling the glass particles to obtain glass powder.
Preferably, the wire diameter of the nickel screen is 0.2-0.5 mm, and the screen aperture is 1-2 mm.
Preferably, the laying thickness of the upper and lower mixed materials of the nickel screen is 3-5 mm.
Preferably, the compaction pressure is 1-3 MPa; the drying temperature is 90-100 ℃, and the drying time is 2-2.5 hours.
Preferably, the heating crystallization comprises raising the temperature to 1150 ℃ at a temperature raising speed of 5-8 ℃/min, and keeping the temperature for 100 min.
The invention also provides a microcrystalline glass composite material.
The invention provides a microcrystalline glass composite material, which is obtained by the preparation method provided by the invention.
The strength of the microcrystalline glass composite material is greatly increased.
Drawings
Fig. 1 is a schematic cross-sectional view of a crystallized glass composite material according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to specific embodiments. It should be understood that the detailed description and specific examples, while indicating the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
A preparation method of a microcrystalline glass composite material comprises the following steps:
s1, providing glass powder;
s2, uniformly stirring the glass powder and liquid sodium silicate to obtain a mixed material; the mass percentage of the liquid sodium silicate in the mixed material is 3-5 wt%;
s3, laying the mixed material in a mould, putting a nickel net in the mould, and then continuously laying the mixed material on the nickel net;
and S4, compacting and drying the mixed material in the mould, and then heating for crystallization.
In step S1, the glass frit preferably has a composition comprising:
60 to 75 wt% of SiO215 to 20 wt% of CaO, 5 to 10 wt% of Al2O31 to 3 wt% of BaO, 3 to 5 wt% of Na2O, 1-3 wt% of ZnO, 1-3 wt% of B2O3。
Preferably, the granularity of the glass powder is 100 meshes to 200 meshes. Therefore, the glass powder can be better mixed with sodium silicate, and the dried mixed material in the mold can have good strength at normal temperature, so that the mold can be conveniently transferred into a heating furnace.
Preferably, the glass frit is obtained by the following steps:
s11, weighing raw materials according to a weight ratio, wherein the raw materials comprise 40-60 wt% of feldspar, 15-25 wt% of quartz sand, 15-25 wt% of calcite, 0.5-2 wt% of borax, 1-3 wt% of barium carbonate, 1-3 wt% of soda ash and 1-3 wt% of zinc oxide;
s12, mixing and heating the raw materials to obtain molten glass;
s13, water quenching the glass melt to obtain glass particles;
s14, ball-milling the glass particles to obtain the glass powder.
In step S11, the feedstock particle size is preferably less than 60 mesh; therefore, the uniformity of the melting process is ensured, and the strength of the microcrystalline glass composite material is further improved.
In step S12, the heating temperature of the raw material is preferably 1450-1550 ℃; this can sufficiently melt the raw materials. In the melting process, the heat preservation time is preferably 2-3 hours. Thus, the uniformity of the melting process can be improved.
In step S13, preferably, the glass melt is poured into water for water quenching; in the water quenching process, the water temperature is normal temperature, and the molten glass is poured into the water pool to be continuously stirred so as to cool the molten glass as soon as possible; after water quenching is finished, filtering out solids and then drying, wherein the drying temperature is 120 ℃, and the drying time is 1 hour; drying to obtain glass particles.
In step S14, ball-milling the glass particles with a planetary ball mill, wherein the ball-milling tank is made of nylon, the ball stone is made of zirconia, and the ball-milling time is 15-30 minutes; obtaining the glass powder.
In step S2, the liquid sodium silicate solidifies after drying, so that the mixed material has better strength and is convenient for transferring the mold; meanwhile, the liquid sodium silicate enables the powder particles to be combined more tightly, and is beneficial to firing the microcrystalline glass composite material with smaller porosity.
The chemical formula of sodium silicate can be expressed as Na2O·nSiO2. The modulus in sodium silicate is SiO2With Na2The molar ratio of O, i.e., the value of n in the formula. Preferably, the modulus of the liquid sodium silicate is 2-3. Thus, the cost is further reduced while the strength is ensured. The mass percentage of the liquid sodium silicate in the mixed material is 3-5 wt%; therefore, the cold strength can be satisfied, the transfer is convenient, and the cost is reduced.
In step S3, the nickel mesh serves as a skeleton to reinforce the strength of the glass-ceramic composite material.
Preferably, the wire diameter of the nickel screen is 0.2-0.5 mm, and the screen aperture is 1-2 mm. Therefore, the nickel screen can be ensured to be kept at the middle position of the microcrystalline glass composite material, the strength is better, and the cost of the microcrystalline glass composite material is effectively reduced.
Preferably, the laying thickness of the upper and lower mixed materials of the nickel screen is 3-5 mm.
In step S4, preferably, the compaction pressure is 1-3 MPa; the drying temperature is 90-100 ℃, and the drying time is 2-2.5 hours. By compacting, the problem that the mixed material shrinks seriously during crystallization heating is avoided, so that the nickel net cannot be well kept in the microcrystalline plate; meanwhile, the cost can be effectively reduced.
In step S4, preferably, the heating crystallization includes raising the temperature to 1150 ℃ at a rate of 5-8 ℃/min, and maintaining the temperature for 100 min. Therefore, the oxidation of the nickel net in heating crystallization can be effectively inhibited, and the uniform temperature and uniform crystallization are ensured.
The strength of the microcrystalline glass composite material obtained by the preparation method is greatly increased.
The invention also provides a microcrystalline glass composite material.
The invention provides a microcrystalline glass composite material, which is obtained by the preparation method provided by the invention.
Referring to fig. 1, the glass-ceramic composite material includes a nickel mesh 2, and glass-ceramic layers 1 on both sides of the nickel mesh 2.
The strength of the microcrystalline glass composite material is greatly increased.
The invention is further illustrated with reference to the following specific examples.
Example 1
Respectively sieving feldspar, quartz sand, calcite, borax, barium carbonate, sodium carbonate and zinc oxide to obtain particles with the particle size of less than 60 meshes; drying the screened particles, weighing, and mixing according to the proportion in the table 1; putting the obtained mixture into a heating furnace for heating; heating to 1450 deg.C, and maintaining the temperature for 2 hr to obtain molten glass.
Pouring the molten glass into normal-temperature water for water quenching, continuously stirring a water quenching tank in the water quenching process, and filtering out solids; putting the filtered solid into an oven for drying at the drying temperature of 120 ℃ for 1 hour; and (3) putting the dried glass particles into a nylon ball milling tank of a planetary ball mill for ball milling, wherein ball stones are made of zirconia, and carrying out ball milling for 20 minutes to obtain glass powder.
Adding liquid sodium silicate into the glass powder, and uniformly stirring to obtain a mixed material.
Paving alumina fiber paper in a mould, then paving a mixed material with the thickness of 4mm, then putting a 20-mesh nickel screen, and then paving the mixed material with the thickness of 4 mm; pressurizing the powder under 1MPa to compact the powder, putting the powder into an oven to dry the powder at the drying temperature of 100 ℃ for 2 hours; after drying, placing the die in a heating furnace, heating to 1150 ℃ at the heating rate of 6 ℃/min, preserving the temperature for 100min, and then cooling along with the furnace; and cutting and polishing the cooled product to obtain the finished product of the microcrystalline glass.
Example 2
The difference from example 1 is that the mass parts of the raw materials are different, and the mass parts of the raw materials are shown in table 1. The other portions are the same as in example 1.
Example 3
The difference from example 1 is that the mass parts of the raw materials are different, and the mass parts of the raw materials are shown in table 1. The other portions are the same as in example 1.
Comparative example 1
Unlike example 1, no nickel mesh was placed. The other portions are the same as in example 1.
TABLE 1
| Raw materials in parts by mass | Feldspar | Quartz sand | Calcite | Borax | Barium carbonate | Soda ash | Zinc oxide |
| Example 1 | 54 | 20 | 19 | 1 | 2 | 2 | 2 |
| Example 2 | 52 | 22 | 19 | 1 | 2 | 2 | 2 |
| Example 3 | 56 | 20 | 17 | 1 | 2 | 2 | 2 |
Performance testing
The microcrystalline glasses of examples 1 to 3 and comparative example 1 were subjected to a strength test, and the test results are shown in table 2.
TABLE 2
| Examples | Example 1 | Example 2 | Example 3 | Comparative example 1 |
| Strength of | 228MPa | 246MPa | 217Mpa | 155MPa |
As can be seen from Table 2, the strength of examples 1-3 was greatly improved relative to that of comparative example 1. Therefore, the strength of the microcrystalline glass composite material is greatly improved.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The preparation method of the microcrystalline glass composite material is characterized by comprising the following steps of:
providing glass powder;
uniformly stirring the glass powder and liquid sodium silicate to obtain a mixed material; the mass percentage of the liquid sodium silicate in the mixed material is 3-5 wt%;
laying the mixed material in a mould, putting a nickel net into the mould, and then continuously laying the mixed material on the nickel net;
and compacting and drying the mixed material in the mould, and then heating for crystallization.
2. The preparation method of the glass-ceramic composite material according to claim 1, wherein the modulus of the liquid sodium silicate is 2-3.
3. The method for preparing the glass-ceramic composite material according to claim 1, wherein the glass frit comprises the following components:
60 to 75 wt% of SiO215 to 20 wt% of CaO, 5 to 10 wt% of Al2O31 to 3 wt% of BaO, 3 to 5 wt% of Na2O, 1-3 wt% of ZnO, 1-3 wt% of B2O3。
4. The method for preparing a glass-ceramic composite material according to claim 1, wherein the particle size of the glass powder is 100-200 meshes.
5. The method for preparing the glass-ceramic composite material according to claim 1, wherein the glass frit is obtained by the steps of:
mixing and heating the raw materials according to a proportion to obtain molten glass; the raw materials comprise 40-60 wt% of feldspar, 15-25 wt% of quartz sand, 15-25 wt% of calcite, 0.5-2 wt% of borax, 1-3 wt% of barium carbonate, 1-3 wt% of soda ash and 1-3 wt% of zinc oxide;
water quenching the molten glass to obtain glass particles;
and ball-milling the glass particles to obtain glass powder.
6. The method for preparing the microcrystalline glass composite material according to claim 1, wherein the wire diameter of the nickel mesh is 0.2-0.5 mm, and the mesh aperture is 1-2 mm.
7. The preparation method of the microcrystalline glass composite material as claimed in claim 1, wherein the laying thickness of the upper and lower mixed materials of the nickel mesh is 3-5 mm.
8. The preparation method of the microcrystalline glass composite material as claimed in claim 1, wherein the compaction pressure is 1-3 MPa; the drying temperature is 90-100 ℃, and the drying time is 2-2.5 hours.
9. The preparation method of the microcrystalline glass composite material as claimed in claim 1, wherein the heating crystallization comprises raising the temperature to 1150 ℃ at a temperature raising speed of 5-8 ℃/min, and keeping the temperature for 100 min.
10. A glass-ceramic composite material, characterized in that it is obtained by the production method of any one of claims 1 to 9.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113582549A (en) * | 2021-08-11 | 2021-11-02 | 苏州大学 | Microcrystalline glass and preparation method thereof |
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| CN111423127A (en) * | 2020-04-21 | 2020-07-17 | 北京北旭电子材料有限公司 | Preparation method of glass powder and glass powder |
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2021
- 2021-05-28 CN CN202110590719.5A patent/CN113233779A/en active Pending
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| JPH04193742A (en) * | 1990-11-27 | 1992-07-13 | Nippon Electric Glass Co Ltd | Manufacture of porous crystallized glass |
| CN101928108A (en) * | 2009-09-25 | 2010-12-29 | 韦鸿雁 | High-strength and low-cost reinforced structure distribution of reinforced glass matrix |
| CN103641314A (en) * | 2013-12-16 | 2014-03-19 | 福州大学 | ZnO-containing sealing microcrystalline glass, and preparation and using methods thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113582549A (en) * | 2021-08-11 | 2021-11-02 | 苏州大学 | Microcrystalline glass and preparation method thereof |
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