CN113582549A - Microcrystalline glass and preparation method thereof - Google Patents
Microcrystalline glass and preparation method thereof Download PDFInfo
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- CN113582549A CN113582549A CN202110920609.0A CN202110920609A CN113582549A CN 113582549 A CN113582549 A CN 113582549A CN 202110920609 A CN202110920609 A CN 202110920609A CN 113582549 A CN113582549 A CN 113582549A
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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
- 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
- C03C10/0045—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 containing SiO2, Al2O3 and MgO as main constituents
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- 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
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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
- 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
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Abstract
The invention relates to microcrystalline glass and a preparation method thereof, belonging to the technical field of inorganic materials. The microcrystalline glass comprises the raw material components of feldspar, quartz sand, calcite, borax, barium carbonate, soda ash, zinc oxide and a binder. The preparation process is simple and easy to realize, the performance of the prepared microcrystalline glass meets most of the requirements of the market, the aspects of mechanical performance, chemical stability, acid-base corrosion resistance and the like are optimized, and the promotion range is about 10-15%.
Description
Technical Field
The invention relates to the technical field of inorganic materials, in particular to microcrystalline glass and a preparation method thereof.
Background
The microcrystal glass is also named glass ceramic and is prepared with base glass with specific composition and crystal nucleus agent added or not added and through controlled crystallization during heating. 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.
The existing microcrystalline glass still has the problem of insufficient mechanical strength in some environments with severe use conditions, and some solutions are also found, for example, a preparation method of high-strength anti-collision microcrystalline glass is proposed in Chinese patent CN109180005A, and the microcrystalline glass with good toughness and high strength is prepared by adding silica gel resin and glass fiber. As another example, a high-strength glass-ceramic-metal composite material disclosed in chinese patent CN109130362A is provided with a glass-ceramic layer, a nickel-based alloy layer, and a ceramic layer, so that the strength of the glass-ceramic-metal composite material is greatly improved. Although the methods can solve the problem of insufficient mechanical strength, the treatment process is complex, difficult to implement, low in chemical stability and high in cost.
Disclosure of Invention
In order to solve the technical problems, the invention provides microcrystalline glass and a preparation method thereof. The invention can prepare the microcrystalline glass with excellent mechanical property and good chemical stability by adding the binder and simple treatment.
The first purpose of the invention is to provide microcrystalline glass, which comprises the following raw material components in parts by mass: 40-60 parts of feldspar, 15-25 parts of quartz sand, 15-25 parts of calcite, 0.5-2 parts of borax, 1-3 parts of barium carbonate, 1-3 parts of soda ash, 1-3 parts of zinc oxide and 3-7 parts of binder.
Further, the binder is liquid sodium silicate.
Further, the modulus of the liquid sodium silicate is 2-3.
The second purpose of the invention is to provide a preparation method of microcrystalline glass, which comprises the following steps:
s1, mixing feldspar, quartz sand, calcite, borax, barium carbonate, soda ash and zinc oxide uniformly, melting, preserving heat, pouring into water, and stirring to obtain glass particles;
s2, drying and ball-milling the glass particles obtained in the step S1, adding a binder, and uniformly mixing to obtain a mixture;
and S3, filling the mixture obtained in the step S2 into a mold, pressing, and calcining to obtain the microcrystalline glass.
Further, in the step S1, the particle sizes of the feldspar, the quartz sand, the calcite, the borax, the barium carbonate, the soda ash and the zinc oxide are less than 60 meshes.
Further, in the step S1, the temperature of the molten material is 1450-; the heat preservation time is 2-3 h.
Further, in the step S1, the stirring speed is 100-120r/min, and the glass needs to be continuously stirred in the pouring process so as to be cooled as soon as possible, so that the obtained glass particles have uniform composition, no air holes and high density.
Further, in the step S2, in the ball milling process, the drying temperature is 100-120 ℃, and the time is 1-1.5 h; the ball-milling adopts a planetary ball mill, the ball-milling tank is made of nylon material, the ball stone is made of zirconia material, the ball-milling time is 15-30min, and the granularity after the ball-milling is 100-mesh and 200-mesh.
Further, in the step S3, the die is filled by laying a nickel mesh into the die, and laying a film, wherein the size of the nickel mesh is smaller than that of the die, the wire diameter of the nickel mesh is 0.2-0.5mm, and the mesh diameter is 1-2 mm. The mould is made of corundum, and the surface of the mould is paved with alumina fiber paper. And laying the mixture for 3-5mm in a mould, putting a nickel net, and laying for 3-5mm, wherein the nickel net is kept flat.
Further, in step S3, the pressure of the pressurizing is 1-3 MPa.
Further, in the step S3, the step of drying the mixture before calcining is further included, wherein the drying is carried out at the temperature of 80-120 ℃ for 1.5-2.5 h.
Furthermore, the temperature rise rate of the calcination is 5-8 ℃/min, and the calcination temperature is 1100-1200 ℃.
Further, in the step S3, the calcining further includes preserving heat of the mixture, wherein the heat preservation time is 90-110 min.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) the liquid sodium silicate of the invention has complex adsorption with minerals such as quartz, feldspar and the like. Alkali metal oxides such as sodium oxide and magnesium oxide in calcite and feldspar react with liquid sodium silicate to form hydrated calcium (magnesium) silicate gel. The surface of quartz and feldspar skeleton particle does not adsorb the position of cementing material, and the lattice defect of its surface has silicon-oxygen bond. The liquid sodium silicate also has silicon-oxygen bonds, and can be coated on the surfaces of quartz and feldspar skeleton particles through hydrogen bonding and adsorption.
(2) The microcrystalline glass prepared by the invention is CaO-MgO-Al2O3-SiO2Is a microcrystalline glass capable of precipitating diopside (CaMgSi)2O6) Anorthite (CaAl)2Si2O8) Cordierite (Mg)2Al4Si5O18) And mullite (Al)6Si2O13) Etc., wherein the diopside phase can make the microcrystalline glass have excellent mechanical properties. Because the material contains a large amount of microcrystalline phases and the porosity of the material is zero, the properties of surface hardness, breaking strength, acid and alkali resistance and the like of the material are greatly improved.
(3) The preparation of the microcrystalline glass adopts a sintering method, and a process of obtaining glass particles by water quenching exists. The proportion of the crystalline phase and the glass phase in the preparation process of the method can be randomly adjusted, and the melting temperature of the basic glass is lower than that of the integral crystallization method, so that the melting time period is short and the energy consumption is low; meanwhile, the crystallite dimension of the microcrystalline glass is easy to control, so that the structure and the performance of a sample can be well controlled.
(4) The preparation process is simple and easy to realize, the performance of the prepared microcrystalline glass meets most of the requirements of the market, the aspects of mechanical performance, chemical stability, acid-base corrosion resistance and the like are optimized, and the promotion range is about 10-15%.
Drawings
In order that the present disclosure may be more readily and clearly understood, reference is now made to the following detailed description of the present disclosure taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a conceptual diagram of an embodiment of the present invention.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Example 1
The microcrystalline glass and the preparation method thereof comprise the following steps:
(1) respectively sieving 54 parts of feldspar, 20 parts of quartz sand, 19 parts of calcite, 1 part of borax, 2 parts of barium carbonate, 2 parts of soda ash and 2 parts of zinc oxide to obtain particles with the granularity of less than 60 meshes;
(2) drying the raw materials and mixing;
(3) placing the mixture in a heating furnace to start heating;
(4) heating to 1450 ℃, and preserving heat for 2h to obtain molten glass;
(5) pouring the glass solution into water for water quenching, and stirring a water quenching tank in the water quenching process to obtain glass particles;
(6) putting the glass particles into an oven for drying at the drying temperature of 120 ℃ for 1 h;
(7) putting the dried glass particles into a ball milling tank for ball milling for 20min to obtain glass powder;
(8) adding 5 parts of liquid sodium silicate into the powder, and uniformly stirring;
(9) paving alumina fiber paper on the mould, paving powder with the thickness of 3-5mm, putting a 20-mesh nickel screen, and paving the powder with the thickness of 3-5 mm;
(10) pressurizing the powder under 1MPa, compacting, and drying in an oven at 100 ℃ for 2 h;
(11) placing the mould in a heating furnace, heating to 1150 ℃ at a heating rate of 7 ℃/min, preserving heat for 100min, and cooling along with the furnace;
(12) and cutting and polishing the sample to obtain the finished product of the microcrystalline glass.
Example 2
The microcrystalline glass and the preparation method thereof comprise the following steps:
(1) respectively sieving 52 parts of feldspar, 22 parts of quartz sand, 19 parts of calcite, 1 part of borax, 2 parts of barium carbonate, 2 parts of soda ash and 2 parts of zinc oxide to obtain particles with the granularity of less than 60 meshes;
(2) drying the raw materials and mixing;
(3) placing the mixture in a heating furnace to start heating;
(4) heating to 1450 ℃, and preserving heat for 2h to obtain molten glass;
(5) pouring the glass solution into water for water quenching, and stirring a water quenching tank in the water quenching process to obtain glass particles;
(6) putting the glass particles into an oven for drying at the drying temperature of 120 ℃ for 1 h;
(7) putting the dried glass particles into a ball milling tank for ball milling for 20min to obtain glass powder;
(8) adding 7 parts of liquid sodium silicate into the powder, and uniformly stirring;
(9) paving alumina fiber paper on the mould, paving powder with the thickness of 3-5mm, putting a 20-mesh nickel screen, and paving the powder with the thickness of 3-5 mm;
(10) pressurizing the powder under 1MPa, compacting, and drying in an oven at 100 ℃ for 2 h;
(11) placing the mould in a heating furnace, heating to 1150 ℃ at a heating rate of 7 ℃/min, preserving heat for 100min, and cooling along with the furnace;
(12) and cutting and polishing the sample to obtain the finished product of the microcrystalline glass.
Example 3
The microcrystalline glass and the preparation method thereof comprise the following steps:
(1) screening 56 parts of feldspar, 20 parts of quartz sand, 17 parts of calcite, 1 part of borax, 2 parts of barium carbonate, 2 parts of soda ash and 2 parts of zinc oxide respectively to obtain particles with the granularity lower than 60 meshes;
(2) drying the raw materials and mixing;
(3) placing the mixture in a heating furnace to start heating;
(4) heating to 1450 ℃, and preserving heat for 2h to obtain molten glass;
(5) pouring the glass solution into water for water quenching, and stirring a water quenching tank in the water quenching process to obtain glass particles;
(6) putting the glass particles into an oven for drying at the drying temperature of 120 ℃ for 1 h;
(7) putting the dried glass particles into a ball milling tank for ball milling for 20min to obtain glass powder;
(8) adding 3 parts of liquid sodium silicate into the powder, and uniformly stirring;
(9) paving alumina fiber paper on the mould, paving powder with the thickness of 3-5mm, putting a 20-mesh nickel screen, and paving the powder with the thickness of 3-5 mm;
(10) pressurizing the powder under 1MPa, compacting, and drying in an oven at 100 ℃ for 2 h;
(11) placing the mould in a heating furnace, heating to 1150 ℃ at a heating rate of 7 ℃/min, preserving heat for 100min, and cooling along with the furnace;
(12) and cutting and polishing the sample to obtain the finished product of the microcrystalline glass.
Comparative example
The method is basically the same as the method in the example 1, except that no liquid sodium silicate is added, and the specific steps are as follows:
(1) respectively sieving 54 parts of feldspar, 20 parts of quartz sand, 19 parts of calcite, 1 part of borax, 2 parts of barium carbonate, 2 parts of soda ash and 2 parts of zinc oxide to obtain particles with the granularity of less than 60 meshes;
(2) drying the raw materials and mixing;
(3) placing the mixture in a heating furnace to start heating;
(4) heating to 1450 ℃, and preserving heat for 2h to obtain molten glass;
(5) pouring the glass solution into water for water quenching, and stirring a water quenching tank in the water quenching process to obtain glass particles;
(6) putting the glass particles into an oven for drying at the drying temperature of 120 ℃ for 1 h;
(7) putting the dried glass particles into a ball milling tank for ball milling for 20min to obtain glass powder;
(8) paving alumina fiber paper on the mould, paving powder with the thickness of 3-5mm, putting a 20-mesh nickel screen, and paving the powder with the thickness of 3-5 mm;
(9) pressurizing the powder under 1MPa, compacting, and drying in an oven at 100 ℃ for 2 h;
(10) placing the mould in a heating furnace, heating to 1150 ℃ at a heating rate of 7 ℃/min, preserving heat for 100min, and cooling along with the furnace;
(11) and cutting and polishing the sample to obtain the finished product of the microcrystalline glass.
Test example
The microcrystalline glasses obtained in examples 1 to 3 of the present invention and the comparative example were tested for density, hardness, flexural strength, acid and alkali resistance.
(1) Density determination
The density was measured using archimedes drainage method, the principle of which is shown below:
where ρ represents the density of the glass-ceramic, M0Representing the mass of the measurement specimen, M1Representing the quality of the overflow water.
(2) Measurement of hardness
With reference to EN 843-4-2005, part 4 of mechanical properties of advanced ceramic monolithic ceramics at room temperature, Vickers, Nurse and Rockwell surface hardness tests, a Vickers hardness tester was used to test and ensure that the surface of the sample was planar.
(3) Measurement of bending Strength
With reference to GB/T6569-2006 Fine ceramic bending Strength test method, a three-point bending resistance test method using a universal tester was used to measure, and the sample was cut into strips of 3mm × 4mm × 40 mm.
(4) Determination of acid and alkali resistance
Refer to JC/T2138 and 2012, test method for acid and alkali corrosion resistance of fine ceramics. Sulfuric acid or sodium hydroxide solution is used as the etching solution. Preparing a sulfuric acid solution with the concentration of 3.0mol/L by adopting analytically pure sulfuric acid conforming to GB/T625 and distilled water or deionized water conforming to GB/T6682; the analytical pure sodium hydroxide meeting GB/T629 and the distilled water or the deionized water meeting GB/T6682 are adopted to prepare the sodium hydroxide solution with the concentration of 6.0 mol/L. A1L flask was charged with 0.5L of the test solution, heated to boiling, and then immersed by slowly placing a sample in the bottom of the flask. And keeping for 24 hours. After the corrosion test, the sample is taken out, fully washed by distilled water or deionized water and dried to constant weight.
Table 1 shows the relevant parameters of the finally measured glass ceramics:
TABLE 1
It can be seen from examples 1-3 that the effect obtained by adding liquid sodium silicate is different for microcrystalline glass with different proportions, wherein the proportion is the best in example 1. As can be seen from the embodiment 1 and the comparative example, the mechanical property and the chemical stability of the sample are remarkably improved after the liquid sodium silicate is added, the hardness is improved by about 20%, the breaking strength is improved by about 40%, and the acid and alkali corrosion resistance is also greatly improved.
Fig. 1 is a conceptual diagram of an embodiment of the present invention. Alkali metal oxides such as sodium oxide, magnesium oxide, etc. in calcite and feldspar react with liquid sodium silicate to form hydrated calcium (magnesium) silicate gel. The gel can be adsorbed on the surfaces of quartz and feldspar skeleton particles, the positions of the cementing materials are not adsorbed, and silicon-oxygen bonds exist in lattice defects on the surfaces of the gel. Liquid sodium silicate can wrap the surfaces of quartz and feldspar skeleton particles through hydrogen bonding and adsorption, and the interaction force among the particles is enhanced by adding the liquid sodium silicate, so that the mechanical properties of the microcrystalline glass, such as hardness, breaking strength and the like, can be improved. In addition, the generated hydrated calcium silicate (magnesium) gel can enable the interface structure of a diffusion layer between the microcrystalline glass and the erosion liquid to be more compact, the higher the activation energy is, and the number of ions or molecules which can smoothly pass through the diffusion layer is reduced, so that the acid-base erosion resistance of the microcrystalline glass is enhanced.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. The microcrystalline glass is characterized by comprising the following raw material components in parts by mass: 40-60 parts of feldspar, 15-25 parts of quartz sand, 15-25 parts of calcite, 0.5-2 parts of borax, 1-3 parts of barium carbonate, 1-3 parts of soda ash, 1-3 parts of zinc oxide and 3-7 parts of binder.
2. The glass-ceramic according to claim 1, characterized in that: the binder is liquid sodium silicate.
3. A glass-ceramic according to claim 2, characterized in that: the modulus of the liquid sodium silicate is 2-3.
4. The method for producing a glass-ceramic according to any one of claims 1 to 3, characterized by comprising the steps of:
s1, mixing feldspar, quartz sand, calcite, borax, barium carbonate, soda ash and zinc oxide uniformly, melting, preserving heat, pouring into water, and stirring to obtain glass particles;
s2, drying and ball-milling the glass particles obtained in the step S1, adding a binder, and uniformly mixing to obtain a mixture;
and S3, filling the mixture obtained in the step S2 into a mold, pressing, and calcining to obtain the microcrystalline glass.
5. The method for producing a crystallized glass according to claim 4, characterized in that: in the step S1, the temperature of the molten material is 1450-1550 ℃; the heat preservation time is 2-3 h.
6. The method for producing a crystallized glass according to claim 4, characterized in that: in the step S1, the stirring speed is 100-120 r/min.
7. The method for producing a crystallized glass according to claim 4, characterized in that: in step S3, the pressure of the pressurizing is 1-3 MPa.
8. The method for producing a crystallized glass according to claim 4, characterized in that: in the step S3, the mixed material is dried before calcination, wherein the drying is carried out at 80-120 ℃ for 1.5-2.5 h.
9. The method for producing a crystallized glass according to claim 4, characterized in that: in the step S3, the temperature rise rate of the calcination is 5-8 ℃/min, and the calcination temperature is 1100-1200 ℃.
10. The method for producing a crystallized glass according to claim 4, characterized in that: in the step S3, the step of calcining further comprises the step of preserving heat of the mixture, wherein the heat preservation time is 90-110 min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115636588A (en) * | 2022-10-26 | 2023-01-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing microcrystalline glass by extracting titanium tailings |
| CN117602837A (en) * | 2024-01-23 | 2024-02-27 | 内蒙古兴固科技有限公司 | Production process of corrosion-resistant nano microcrystalline building board |
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| CN101591144A (en) * | 2009-06-26 | 2009-12-02 | 武汉理工大学 | Slim CaO-Al 2O 3-SiO 2System glass ceramics and preparation |
| CN102219380A (en) * | 2011-05-03 | 2011-10-19 | 北京中伦基业科技发展有限公司 | Method for producing glass-ceramics plate by using construction waste |
| CN111039569A (en) * | 2019-12-19 | 2020-04-21 | 吉林省梓楗新型建材股份有限公司 | Black microcrystalline glass plate produced by utilizing lead-zinc-iron tailings and manufacturing method thereof |
| CN113233779A (en) * | 2021-05-28 | 2021-08-10 | 苏州大学 | Microcrystalline glass composite material and preparation method thereof |
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2021
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101591144A (en) * | 2009-06-26 | 2009-12-02 | 武汉理工大学 | Slim CaO-Al 2O 3-SiO 2System glass ceramics and preparation |
| CN102219380A (en) * | 2011-05-03 | 2011-10-19 | 北京中伦基业科技发展有限公司 | Method for producing glass-ceramics plate by using construction waste |
| CN111039569A (en) * | 2019-12-19 | 2020-04-21 | 吉林省梓楗新型建材股份有限公司 | Black microcrystalline glass plate produced by utilizing lead-zinc-iron tailings and manufacturing method thereof |
| CN113233779A (en) * | 2021-05-28 | 2021-08-10 | 苏州大学 | Microcrystalline glass composite material and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115636588A (en) * | 2022-10-26 | 2023-01-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing microcrystalline glass by extracting titanium tailings |
| CN117602837A (en) * | 2024-01-23 | 2024-02-27 | 内蒙古兴固科技有限公司 | Production process of corrosion-resistant nano microcrystalline building board |
| CN117602837B (en) * | 2024-01-23 | 2024-04-12 | 内蒙古兴固科技有限公司 | Production process of corrosion-resistant nano microcrystalline building board |
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Application publication date: 20211102 |