CN114920459A - Preparation method of lithium disilicate glass ceramic material - Google Patents
Preparation method of lithium disilicate glass ceramic material Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 28
- 239000003103 lithium disilicate glass Substances 0.000 title claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 70
- 239000011521 glass Substances 0.000 claims abstract description 33
- 239000011159 matrix material Substances 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 238000002844 melting Methods 0.000 claims abstract description 15
- 230000008018 melting Effects 0.000 claims abstract description 15
- 239000000155 melt Substances 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 239000006112 glass ceramic composition Substances 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 8
- 229920002635 polyurethane Polymers 0.000 claims description 30
- 239000004814 polyurethane Substances 0.000 claims description 30
- 239000000725 suspension Substances 0.000 claims description 30
- 235000015895 biscuits Nutrition 0.000 claims description 25
- 238000000137 annealing Methods 0.000 claims description 21
- 238000000498 ball milling Methods 0.000 claims description 16
- 238000005266 casting Methods 0.000 claims description 15
- 238000007599 discharging Methods 0.000 claims description 15
- 238000005303 weighing Methods 0.000 claims description 15
- 238000010304 firing Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 239000011812 mixed powder Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 10
- 239000012856 weighed raw material Substances 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 229920001971 elastomer Polymers 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- 239000011368 organic material Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 239000003292 glue Substances 0.000 claims description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 3
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 3
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- -1 ammonia inorganic acid Chemical class 0.000 claims description 2
- WVMPCBWWBLZKPD-UHFFFAOYSA-N dilithium oxido-[oxido(oxo)silyl]oxy-oxosilane Chemical compound [Li+].[Li+].[O-][Si](=O)O[Si]([O-])=O WVMPCBWWBLZKPD-UHFFFAOYSA-N 0.000 claims description 2
- 239000006136 disilicate glass ceramic Substances 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 238000002425 crystallisation Methods 0.000 abstract description 13
- 230000008025 crystallization Effects 0.000 abstract description 13
- 230000008439 repair process Effects 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 4
- 230000006911 nucleation Effects 0.000 abstract description 3
- 238000010899 nucleation Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000006060 molten glass Substances 0.000 abstract 2
- 239000002241 glass-ceramic Substances 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 11
- 235000012239 silicon dioxide Nutrition 0.000 description 6
- 229910052681 coesite Inorganic materials 0.000 description 5
- 229910052906 cristobalite Inorganic materials 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 229910052682 stishovite Inorganic materials 0.000 description 5
- 229910052905 tridymite Inorganic materials 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 239000000156 glass melt Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 239000002667 nucleating agent Substances 0.000 description 3
- 238000005191 phase separation Methods 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 description 2
- 229910052912 lithium silicate Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910018119 Li 3 PO 4 Inorganic materials 0.000 description 1
- 208000008312 Tooth Loss Diseases 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 210000000214 mouth Anatomy 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Ceramic Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Glass Compositions (AREA)
Abstract
The invention belongs to the technical field of glass ceramic materials, and particularly relates to a preparation method of a lithium disilicate glass ceramic material suitable for dental repair. The preparation method comprises the following steps: firstly preparing a glass ceramic framework material, then melting the prepared powder, pouring the melt into the framework, cooling to obtain matrix glass, and carrying out heat treatment on the matrix glass to obtain the lithium disilicate glass ceramic material. The invention changes surface crystallization into integral crystallization, accelerates the crystallization speed of the material and leads the glass ceramic material to form a uniform and compact microstructure. Secondly, the preparation method of the invention ensures that the framework material is biased to the Si-rich phase and the molten glass is biased to the Li-rich phase by adjusting the formulas of the framework material and the molten glass, thereby being more beneficial to phase splitting of the material and the nucleation and growth of subsequent crystals and ensuring that the mechanical property of the material is more outstanding.
Description
Technical Field
The invention belongs to the technical field of glass ceramic materials, and particularly relates to a preparation method of a lithium disilicate glass ceramic material suitable for dental repair.
Background
Teeth are important constituent organs of human oral cavity, and the maintenance of normal physiological functions of teeth is an important guarantee for maintaining human health. The total number of the patients with tooth defects and tooth loss in China is calculated to be 1/5-1/3 of the general population. With the gradual increase of the attention degree and the living quality requirement of people on oral health, the consumption demand of tooth restoration protection and dental restoration materials is further enhanced. Ceramic restorative materials have become the major development trend in current oral restorations. The lithium disilicate glass ceramic material is a brand new dental repair substitute material which is sold in the market in recent years abroad, has safe material performance and good biocompatibility, has moderate hardness compared with the existing ceramic material, and cannot cause abrasion to natural teeth; the semitransparent texture of the artificial tooth is closer to that of a natural tooth, the artificial tooth is easy to color and adjust, and the artificial tooth has excellent simulation and aesthetic effects and gradually becomes one of the main development trends of the current dental repair materials.
The preparation method of the lithium disilicate glass ceramic material mainly comprises a melting method and a sintering method.
Chinese patent CN200910043711.6 reports that P2O5 is taken as a nucleating agent by adopting a melting method, and B2O3 and La are added 2 O 3 And Y 2 O 3 The lithium disilicate glass ceramic material with the same auxiliary components and the preparation method thereof have the characteristics of: ball-milling, mixing and sieving the raw materials, putting the raw materials into a quartz crucible, heating the mixture to 1500 ℃ to obtain uniform glass melt, then quickly pouring the glass melt into a preheated stainless steel mold, annealing to obtain a colorless transparent ceramic block, and preparing the lithium disilicate glass ceramic material by a crystallization heat treatment process, wherein the maximum bending strength of the lithium disilicate glass ceramic material reaches 334MPa, and the maximum fracture toughness of the lithium disilicate glass ceramic material reaches 3.34 MPa.m 1 /2 . Chinese patent 201510246538.5 reports a method for preparing lithium disilicate glass ceramic material by sintering method, and the preparation process is characterized in that: the preparation method comprises the steps of mixing and melting raw materials of all components, then carrying out water quenching to obtain glass frit, grinding the glass frit into micron-sized glass powder, carrying out hot-pressing sintering on the glass powder to form a compact lithium metasilicate microcrystalline glass body, and then converting a lithium metasilicate crystal into a lithium disilicate glass ceramic material through a crystallization heat treatment process, wherein the highest bending strength reaches 300-400MPa, and the highest density reaches 99.1-99.7%. Inducing phase separation in the matrix glass to form a Si-rich phase and a Li-rich phase, and separating the matrix glass from the surfaceThe crystallization is changed into integral crystallization, the crystallization speed of the material is accelerated, and the glass ceramic material forms a uniform and compact microstructure. In the existing preparation method of the lithium disilicate glass ceramic material, no matter a sintering method or a melting method, the prepared matrix glass material has uniform integral components, and only phase separation can be induced in the matrix glass by a nucleating agent, so that the crystallization speed of the material is indirectly influenced.
Disclosure of Invention
The invention aims to provide a preparation method of a lithium disilicate glass ceramic material suitable for dental repair.
The technical scheme adopted by the invention is as follows:
the preparation method of the lithium disilicate glass ceramic material comprises the following steps
Step one, a framework material formula:
SiO 2 :75-85，LiO 2 :5-15，CaO:1-2，CeO 2 :1-3，B 2 O 3 3-5, dispersing agent: 0-8, ppi: 15-40 polyurethane sponge;
(2) the formula of the molten liquid is as follows:
SiO 2 :7-17，LiO 2 :50-75，P 2 O 5 :6-10，K 2 O:6-12，Al 2 O 3 :5-8，ZrO 2 :0-3；
second step, preparation of framework Material
(1) Preparing materials: weighing all components except the polyurethane sponge according to the prescription;
(2) ball milling: adding a proper amount of dispersing agent and distilled water into the weighed raw materials, ensuring that the solid content of the slurry is more than or equal to 65%, and performing ball milling for 30-150 minutes;
(3) sieving: enabling the slurry after ball milling to pass through a 300-400-mesh screen to obtain a filtered suspension;
(3) coating: filling the suspension into polyurethane sponge, and removing air bubbles in the suspension through vibration to obtain the polyurethane sponge filled with the suspension;
(4) and (3) drying: putting the polyurethane sponge filled with the suspension into an oven, drying at 80-120 ℃, and evaporating and discharging water in the suspension to obtain a framework blank;
(5) rubber discharging: placing the framework blank into a glue discharging furnace, preserving heat for 1-3 hours at 400-600 ℃, and decomposing and volatilizing the polyurethane sponge organic material in the blank to obtain a framework biscuit firing blank;
third step, preparation of matrix glass Material
(1) Weighing: weighing all raw materials according to a molten liquid formula;
(2) mixing materials: putting the weighed raw materials into a mixer, and mixing for 2-5 hours to obtain uniformly mixed powder;
(3) and (3) firing: putting the skeleton biscuit firing blank into a mold, putting the mold into a kiln, and preserving heat for 20-60 minutes at 1400-1700 ℃;
(4) melting: pouring the mixed powder into a crucible, putting the crucible into a kiln, melting the powder at 1300-1500 ℃, and preserving heat for 1-5 hours to obtain a melt with better fluidity;
(5) casting: taking out the fired framework biscuit from the kiln, casting the melt into the framework biscuit, putting the framework biscuit into the kiln again after casting, and preserving heat for 0.5-2 hours at the temperature of 1450 ℃ in 1300-;
(6) and (3) annealing: taking out the mold, putting the mold into an annealing furnace to anneal the material, wherein the annealing temperature is 350-500 ℃, the annealing time is 30-120 minutes, and cooling the mold along with the furnace to obtain a matrix glass material;
fourthly, preparation of glass ceramic material
(1) And (3) heat treatment: carrying out first heat treatment on the matrix glass material at 500-700 ℃ for 5-60 minutes, then carrying out second heat treatment on the heat-treated matrix glass material at 750-950 ℃ for 5-120 minutes, and cooling along with a furnace to obtain the lithium disilicate glass ceramic material.
In a further preferred mode of the above technical scheme, the dispersant is hydrochloric acid, ammonia inorganic acid alkali, or water glass, sodium tripolyphosphate inorganic salt or sodium stearate low-grade organic matter.
The invention has the beneficial effects that:
first, the lithium disilicate glass-ceramic material of the present inventionA small amount of P can be added in the preparation process of the material 2 O 5 As nucleating agent, P 2 O 5 Can induce phase separation in the matrix glass to form a "Si-rich phase" and a "Li-rich phase" with P in the Li-rich region 2 O 5 With Li 2 Reaction of O to form Li 3 PO 4 The nuclei act as non-uniform nucleation sites by means of which Li is present 2 SiO 3 The crystal begins to nucleate and grow, the crystallization mode of the matrix glass is changed from surface crystallization to integral crystallization, the crystallization speed of the material is accelerated, and the glass ceramic material forms a uniform and compact microstructure.
Secondly, according to the preparation method, the framework material is biased to the Si-rich phase and the glass melt is biased to the Li-rich phase by adjusting the formulas of the framework material and the glass melt, so that the phase splitting of the material and the subsequent nucleation and growth of crystals are facilitated, and the mechanical property of the material is more outstanding.
Detailed Description
Example 1
The preparation method of the lithium disilicate glass ceramic material comprises the following steps
Firstly, preparing a framework material formula:
the formula of the framework material is as follows: SiO2:75, LiO2:15, CaO:1, CeO2:1, B2O3:3, dispersant: 5, polyurethane sponge with ppi of 15;
(2) the melt formula is as follows:
SiO2:12，LiO2:70，P2O5:6，K2O:6，Al2O3:5，ZrO2:3；
second step, preparation of framework Material
(1) Preparing materials: weighing all components except the polyurethane sponge according to the prescription;
(2) ball milling: adding ammonia water and distilled water into the weighed raw materials, ensuring that the solid content of the slurry is more than or equal to 65 percent, and performing ball milling for 45 minutes;
(3) sieving: enabling the slurry after ball milling to pass through a 300-400-mesh screen to obtain a filtered suspension;
(3) coating: filling the suspension into polyurethane sponge, and removing air bubbles in the suspension through vibration to obtain the polyurethane sponge filled with the suspension;
(4) and (3) drying: putting the polyurethane sponge filled with the suspension into an oven, drying at 100 ℃, and evaporating and discharging water in the suspension to obtain a framework blank;
(5) rubber discharging: putting the skeleton blank into a glue discharging furnace, preserving heat for 3 hours at 450 ℃, and decomposing and volatilizing the polyurethane sponge organic material in the blank to obtain a skeleton biscuit blank;
third step, preparation of matrix glass material
(1) Weighing: weighing all raw materials according to a molten liquid formula;
(2) mixing materials: putting the weighed raw materials into a mixer, and mixing for 2 hours to obtain uniformly mixed powder;
(3) firing: putting the skeleton biscuit firing blank into a mold, putting the mold into a kiln, and keeping the temperature at 1400 ℃ for 60 minutes;
(4) melting: pouring the mixed powder into a crucible, putting the crucible into a kiln, melting the powder at 1480 ℃, and preserving heat for 4.5 hours to obtain a melt with better fluidity;
(5) casting: taking out the fired framework biscuit from the kiln, casting the melt into the framework biscuit, putting the framework biscuit into the kiln again after casting, and keeping the temperature of 1330 ℃ for 0.5 hour;
(6) annealing: taking out the mold, putting the mold into an annealing furnace to anneal the material, wherein the annealing temperature is 400 ℃, the annealing time is 30 minutes, and cooling along with the furnace to obtain a matrix glass material;
fourthly, preparation of glass ceramic material
And (3) heat treatment: carrying out first heat treatment on the matrix glass material at 550 ℃ for 10 minutes, then carrying out second heat treatment on the matrix glass material after heat treatment at 790 ℃ for 5 minutes, and cooling along with the furnace to obtain the lithium disilicate glass ceramic material.
Example 2
The preparation method of the lithium disilicate glass ceramic material comprises the following steps
Step one, a framework material formula:
the formula of the framework material comprises: SiO2 2 :80，LiO 2 :8，CaO:2，CeO 2 :2，B 2 O 3 4, dispersant: 4, a polyurethane sponge with ppi of 25;
(2) the melt formula is as follows:
SiO 2 :10，LiO 2 :66，P 2 O 5 :7，K 2 O:10，Al 2 O 3 :6，ZrO 2 :1；
second step, preparation of the framework Material
(1) Preparing materials: weighing all components except the polyurethane sponge according to the prescription;
(2) ball milling: adding a proper amount of sodium tripolyphosphate and distilled water into the weighed raw materials to ensure that the solid content of the slurry is more than or equal to 65 percent, and the ball milling time is 60 minutes;
(3) sieving: enabling the slurry after ball milling to pass through a 300-400-mesh screen to obtain a filtered suspension;
(3) coating: filling the suspension into polyurethane sponge, and removing air bubbles in the suspension through vibration to obtain the polyurethane sponge filled with the suspension;
(4) and (3) drying: putting the polyurethane sponge filled with the suspension into an oven, drying at 80 ℃, and evaporating and discharging water in the suspension to obtain a framework blank;
(5) rubber discharging: putting the skeleton blank into a glue discharging furnace, preserving heat for 1.5 hours at 500 ℃, and decomposing and volatilizing the polyurethane sponge organic material in the blank to obtain a skeleton biscuit blank;
third step, preparation of matrix glass material
(1) Weighing: weighing all raw materials according to a molten liquid formula;
(2) mixing materials: the weighed raw materials are loaded into a mixer, and the materials are mixed for 3 hours to obtain uniformly mixed powder;
(3) firing: putting the skeleton biscuit firing blank into a mold, putting the mold into a kiln, and keeping the temperature at 1470 ℃ for 30 minutes;
(4) melting: pouring the mixed powder into a crucible, putting the crucible into a kiln, melting the powder at 1420 ℃, and preserving heat for 3 hours to obtain a melt with better fluidity;
(5) casting: taking out the fired framework biscuit from the kiln, casting the melt into the framework biscuit, putting the framework biscuit into the kiln again after casting, and preserving heat at 1380 ℃ for 1 hour;
(6) annealing: taking out the mold, putting the mold into an annealing furnace to anneal the material, wherein the annealing temperature is 450 ℃, the annealing time is 80 minutes, and cooling the material along with the furnace to obtain a matrix glass material;
fourthly, preparation of glass ceramic material
And (3) heat treatment: carrying out first heat treatment on the matrix glass material at 600 ℃ for 25 minutes, then carrying out second heat treatment on the matrix glass material after heat treatment at 830 ℃ for 45 minutes, and cooling along with the furnace to obtain the lithium disilicate glass ceramic material.
Example 3
The preparation method of the lithium disilicate glass ceramic material comprises the following steps
Firstly, preparing a framework material formula:
the formula of the framework material is as follows: SiO2:82, LiO2:5, CaO:1, CeO2:2, B2O3:2, dispersant: 8, polyurethane sponge with ppi of 40;
(2) the formula of the molten liquid is as follows:
SiO2:7，LiO2:61，P2O5:10，K2O:12，Al2O3:7，ZrO2:2；
second step, preparation of framework Material
(1) Preparing materials: weighing all components except the polyurethane sponge according to the prescription;
(2) ball milling: adding a proper amount of sodium stearate and distilled water into the weighed raw materials to ensure that the solid content of the slurry is more than or equal to 65 percent, and the ball milling time is 120 minutes;
(3) sieving: enabling the slurry after ball milling to pass through a screen of 300-400 meshes to obtain a filtered suspension;
(3) coating: filling the suspension into polyurethane sponge, and removing air bubbles in the suspension through vibration to obtain the polyurethane sponge filled with the suspension;
(4) and (3) drying: putting the polyurethane sponge filled with the suspension into an oven, drying at 120 ℃, and evaporating and discharging water in the suspension to obtain a framework blank;
(5) rubber discharging: putting the framework blank into a gel discharging furnace, preserving heat for 1 hour at 600 ℃, and decomposing and volatilizing the polyurethane sponge organic material in the blank to obtain a framework biscuit firing blank;
third step, preparation of matrix glass Material
(1) Weighing: weighing all raw materials according to a molten liquid formula;
(2) mixing materials: the weighed raw materials are put into a mixer to be mixed for 4.5 hours to obtain uniformly mixed powder;
(3) firing: putting the skeleton biscuit firing blank into a mold, putting the mold into a kiln, and preserving heat for 20 minutes at 1550 ℃;
(4) melting: pouring the mixed powder into a crucible, putting the crucible into a kiln, melting the powder at 1320 ℃, and preserving heat for 4.5 hours to obtain a melt with better fluidity;
(5) casting: taking out the fired skeleton biscuit from the kiln, casting the melt into the skeleton biscuit, putting the skeleton biscuit into the kiln again after casting, and keeping the temperature of 1450 ℃ for 2 hours;
(6) annealing: taking out the mold, putting the mold into an annealing furnace to anneal the material, wherein the annealing temperature is 500 ℃, the annealing time is 120 minutes, and cooling the mold along with the furnace to obtain a matrix glass material;
fourthly, preparation of glass ceramic material
And (3) heat treatment: carrying out first heat treatment on the matrix glass material at 680 ℃ for 55 minutes, then carrying out second heat treatment on the matrix glass material after heat treatment at 930 ℃ for 110 minutes, and cooling along with the furnace to obtain the lithium disilicate glass ceramic material.
Claims (2)
1. The preparation method of the lithium disilicate glass ceramic material is characterized by comprising the following steps
Firstly, preparing a framework material formula:
SiO 2 :75-85，LiO 2 :5-15，CaO:1-2，CeO 2 :1-3，B 2 O 3 3-5, dispersing agent: 0-8, ppi: 15-40 polyurethane sponge;
(2) the melt formula is as follows:
SiO 2 :7-17，LiO 2 :50-75，P 2 O 5 :6-10，K 2 O:6-12，Al 2 O 3 :5-8，ZrO 2 :0-3；
second step, preparation of framework Material
(1) Preparing materials: weighing all components except the polyurethane sponge according to the prescription;
(2) ball milling: adding a proper amount of dispersing agent and distilled water into the weighed raw materials, ensuring that the solid content of the slurry is more than or equal to 65%, and performing ball milling for 30-150 minutes;
(3) sieving: enabling the slurry after ball milling to pass through a 300-400-mesh screen to obtain a filtered suspension;
(3) coating: filling the suspension into polyurethane sponge, and removing air bubbles in the suspension through vibration to obtain the polyurethane sponge filled with the suspension;
(4) and (3) drying: putting the polyurethane sponge filled with the suspension into an oven, drying at 80-120 ℃, and evaporating and discharging water in the suspension to obtain a framework blank;
(5) rubber discharging: placing the framework blank into a glue discharging furnace, preserving heat for 1-3 hours at 400-600 ℃, and decomposing and volatilizing the polyurethane sponge organic material in the blank to obtain a framework biscuit firing blank;
third step, preparation of matrix glass Material
(1) Weighing: weighing all raw materials according to a molten liquid formula;
(2) mixing materials: putting the weighed raw materials into a mixer, mixing for 2-5 hours to obtain uniformly mixed powder;
(3) and (3) firing: putting the skeleton biscuit firing blank into a mold, putting the mold into a kiln, and preserving heat for 20-60 minutes at 1400-1700 ℃;
(4) melting: pouring the mixed powder into a crucible, putting the crucible into a kiln, melting the powder at 1300-1500 ℃, and preserving heat for 1-5 hours to obtain a melt with better fluidity;
(5) casting: taking out the fired framework biscuit from the kiln, casting the melt into the framework biscuit, putting the framework biscuit into the kiln again after casting, and preserving heat for 0.5-2 hours at the temperature of 1450 ℃ in 1300-;
(6) annealing: taking out the mold, putting the mold into an annealing furnace to anneal the material, wherein the annealing temperature is 350-500 ℃, the annealing time is 30-120 minutes, and cooling the mold along with the furnace to obtain a matrix glass material;
fourthly, preparation of glass ceramic material
(1) And (3) heat treatment: carrying out first heat treatment on the matrix glass material at 500-700 ℃ for 5-60 minutes, then carrying out second heat treatment on the heat-treated matrix glass material at 750-950 ℃ for 5-120 minutes, and cooling along with a furnace to obtain the lithium disilicate glass ceramic material.
2. The method for preparing a lithium disilicate glass-ceramic material according to claim 1, wherein the dispersing agent is selected from hydrochloric acid, ammonia inorganic acid bases, or selected from water glass, sodium tripolyphosphate inorganic salts, or selected from sodium stearate low-grade organic substances.
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