CN114920459B - Preparation method of lithium disilicate glass ceramic material - Google Patents
Preparation method of lithium disilicate glass ceramic material Download PDFInfo
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- CN114920459B CN114920459B CN202210675438.4A CN202210675438A CN114920459B CN 114920459 B CN114920459 B CN 114920459B CN 202210675438 A CN202210675438 A CN 202210675438A CN 114920459 B CN114920459 B CN 114920459B
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 26
- 239000003103 lithium disilicate glass Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 58
- 239000011521 glass Substances 0.000 claims abstract description 32
- 239000011159 matrix material Substances 0.000 claims abstract description 27
- 239000000155 melt Substances 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 238000002844 melting Methods 0.000 claims abstract description 15
- 230000008018 melting Effects 0.000 claims abstract description 15
- 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
- 239000004814 polyurethane Substances 0.000 claims description 30
- 229920002635 polyurethane Polymers 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
- 238000010304 firing Methods 0.000 claims description 15
- 238000005303 weighing Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 239000003292 glue Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 239000011812 mixed powder Substances 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
- 238000002156 mixing Methods 0.000 claims description 7
- 239000002994 raw material 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
- 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
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 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
- 239000004115 Sodium Silicate Substances 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
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims 1
- 150000007522 mineralic acids Chemical class 0.000 claims 1
- 238000002425 crystallisation Methods 0.000 abstract description 14
- 230000008025 crystallization Effects 0.000 abstract description 14
- 239000000156 glass melt Substances 0.000 abstract description 6
- 238000005191 phase separation Methods 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 3
- 230000008439 repair process Effects 0.000 abstract description 3
- 230000006911 nucleation Effects 0.000 abstract description 2
- 238000010899 nucleation Methods 0.000 abstract description 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 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 239000002667 nucleating agent Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 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
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 230000001939 inductive effect 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
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 229910018068 Li 2 O Inorganic materials 0.000 description 1
- 229910018119 Li 3 PO 4 Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 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
- 229910017053 inorganic salt Inorganic materials 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 performing heat treatment on the matrix glass to obtain the lithium disilicate glass ceramic material. The invention changes surface crystallization into integral crystallization, quickens the crystallization speed of the material and leads the glass ceramic material to form a uniform and compact microstructure. Secondly, according to the preparation method disclosed by the invention, the skeleton 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 skeleton material and the glass melt, so that the phase separation of the material and the nucleation and growth of subsequent crystals are facilitated, and the mechanical properties of the material are better.
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 the oral cavity of a human body, and maintaining normal physiological functions of the teeth is an important guarantee for maintaining the health of the human body. The total number of patients with tooth defects and missing in China is up to 1/5-1/3 of the total population. With the gradual increase of the demands of people on oral health and quality of life, the consumption demands of dental restoration protection and dental restoration materials are further increased. Ceramic restorative materials have become the main trend of current oral restoration. The lithium disilicate glass ceramic material is a brand new dental restoration substitute material which is marketed in recent foreign countries, has safe material property and good biocompatibility, has moderate hardness compared with the existing ceramic material, and can not abrade natural teeth; the translucency texture of the dental restoration material is more similar to that of natural teeth, is easy to color and adjust, has excellent simulation and beautiful effects, and gradually becomes one of the main development trends of the current dental restoration 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 a melting method using P2O5 as a nucleating agent, adding B2O3, la 2 O 3 And Y 2 O 3 The lithium disilicate glass ceramic material with auxiliary components and the preparation method thereof are characterized in that: ball milling, mixing and sieving the raw materials of each component, putting into a quartz crucible, heating to 1500 ℃ to obtain uniform glass melt, then rapidly pouring the glass melt into a preheated stainless steel mold, annealing to obtain colorless transparent ceramic blocks, and preparing the lithium disilicate glass ceramic material by a crystallization heat treatment process, wherein the highest bending strength reaches 334MPa, and the highest fracture toughness reaches 3.34 MPa.m 1 /2 . Chinese patent 201510246538.5 reports a method for preparing lithium disilicate glass ceramic material by sintering, which is characterized in that: the method comprises the steps of mixing and melting raw materials of all the components, performing water quenching to obtain glass frit, grinding the glass frit into micron-sized glass powder, performing hot-pressing sintering on the glass powder to form a compact lithium metasilicate microcrystalline glass body, and then converting the 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 compactness reaches 99.1% -99.7%. 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. In the existing preparation method of the lithium disilicate glass ceramic material, whether a sintering method or a melting method is adopted, the prepared matrix glass material is uniform in overall components, and the crystallization speed of the material is indirectly influenced only by inducing phase separation in the matrix glass through a nucleating agent.
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 of
First, 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 parts of dispersing agent: 0-8, ppi:15-40 parts of polyurethane sponge;
(2) The formula of the melt 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, preparing skeleton material
(1) And (3) batching: weighing all components except the polyurethane sponge according to 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 percent, and performing ball milling for 30 to 150 minutes;
(3) Sieving: the slurry after ball milling is passed through a 300-400 mesh screen to obtain a filtered suspension;
(3) Coating: filling the suspension into polyurethane sponge, and removing bubbles in the suspension through vibration to obtain polyurethane sponge filled with the suspension;
(4) And (3) drying: placing polyurethane sponge filled with the suspension into an oven, drying at 80-120 ℃, and evaporating and discharging water in the suspension to obtain a skeleton blank;
(5) And (3) glue discharging: placing the skeleton blank into a glue discharging furnace, preserving heat for 1-3 hours at 400-600 ℃, and decomposing and volatilizing polyurethane sponge organic materials in the blank to obtain a skeleton biscuit firing blank;
third step, preparing the matrix glass material
(1) Weighing: weighing all raw materials according to a melt formula;
(2) Mixing: the weighed raw materials are put into a mixer, and mixed for 2 to 5 hours to obtain evenly mixed powder;
(3) Firing: placing the skeleton biscuit firing blank into a mould, placing the mould 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 the temperature for 1-5 hours to obtain a melt with better fluidity;
(5) Casting: taking out the framework biscuit which is being fired from the kiln, casting the melt into the framework biscuit, putting the framework biscuit into the kiln again after casting, and preserving the temperature for 0.5-2 hours at 1300-1450 ℃;
(6) Annealing: taking out the die, putting the die into an annealing furnace to anneal the material, wherein the annealing temperature is 350-500 ℃, the annealing time is 30-120 minutes, and cooling along with the furnace to obtain a matrix glass material;
fourth step, preparation of glass ceramic material
(1) And (3) heat treatment: and (3) performing primary heat treatment on the matrix glass material at 500-700 ℃ for 5-60 minutes, performing secondary 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 preferable mode of the technical scheme, the dispersing agent is hydrochloric acid or ammonia water inorganic acid-base, or sodium silicate or sodium tripolyphosphate inorganic salt or sodium stearate lower organic matter.
The beneficial effects of the invention are as follows:
first, the lithium disilicate glass ceramic material of the present invention may have a small amount of P added during the preparation process 2 O 5 As a nucleating agent, P 2 O 5 Is capable of inducing phase separation in the matrix glass to form a 'Si-rich phase' and a 'Li-rich phase', P in the-Li-rich region 2 O 5 With Li 2 O reacts to form Li 3 PO 4 The nuclei act as heterogeneous nuclei by means of these sites Li 2 SiO 3 The crystallization mode of the matrix glass is changed from surface crystallization to integral crystallization, so that 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 disclosed by the invention, the skeleton 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 skeleton material and the glass melt, so that the phase separation of the material and the nucleation and growth of subsequent crystals are facilitated, and the mechanical properties of the material are better.
Detailed Description
Example 1
The preparation method of the lithium disilicate glass ceramic material comprises the following steps of
First, a framework material formula:
the formula of the framework material comprises: siO2:75, liO2:15, caO:1, ceO2:1, B2O3:3, dispersant: 5, a polyurethane sponge having ppi of 15;
(2) The formula of the melt is as follows:
SiO2:12，LiO2:70，P2O5:6，K2O:6，Al2O3:5，ZrO2:3；
second step, preparing skeleton material
(1) And (3) batching: weighing all components except the polyurethane sponge according to 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%, and ball milling for 45 minutes;
(3) Sieving: the slurry after ball milling is passed through a 300-400 mesh screen to obtain a filtered suspension;
(3) Coating: filling the suspension into polyurethane sponge, and removing bubbles in the suspension through vibration to obtain polyurethane sponge filled with the suspension;
(4) And (3) drying: placing polyurethane sponge filled with the suspension into an oven, drying at 100 ℃, and evaporating and discharging water in the suspension to obtain a skeleton blank;
(5) And (3) glue discharging: placing the skeleton blank into a glue discharging furnace, preserving heat for 3 hours at 450 ℃, and decomposing and volatilizing polyurethane sponge organic materials in the blank to obtain a skeleton biscuit firing blank;
third step, preparing the matrix glass material
(1) Weighing: weighing all raw materials according to a melt formula;
(2) Mixing: the weighed raw materials are put into a mixer, and mixed for 2 hours to obtain evenly mixed powder;
(3) Firing: placing the skeleton biscuit firing blank into a mould, placing the mould into a kiln, and preserving 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 the heat for 4.5 hours to obtain a melt with better fluidity;
(5) Casting: taking out the framework biscuit which is being fired from the kiln, casting the melt into the framework biscuit, putting the framework biscuit into the kiln again after casting, and preserving the temperature at 1330 ℃ for 0.5 hour;
(6) Annealing: taking out the die, putting the die 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;
fourth step, preparation of glass ceramic material
And (3) heat treatment: and (3) carrying out primary heat treatment on the matrix glass material at 550 ℃ for 10 minutes, then carrying out secondary heat treatment on the heat-treated matrix glass material at 790 ℃ for 5 minutes, and cooling along with a 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 of
First, a framework material formula:
the formula of the framework material comprises: siO (SiO) 2 :80，LiO 2 :8，CaO:2，CeO 2 :2，B 2 O 3 4, dispersing agent: 4, a polyurethane sponge having ppi 25;
(2) The formula of the melt 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, preparing skeleton material
(1) And (3) batching: weighing all components except the polyurethane sponge according to prescription;
(2) Ball milling: adding a proper amount of sodium tripolyphosphate 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 60 minutes;
(3) Sieving: the slurry after ball milling is passed through a 300-400 mesh screen to obtain a filtered suspension;
(3) Coating: filling the suspension into polyurethane sponge, and removing bubbles in the suspension through vibration to obtain polyurethane sponge filled with the suspension;
(4) And (3) drying: placing polyurethane sponge filled with the suspension into an oven, drying at 80 ℃, and evaporating and discharging water in the suspension to obtain a skeleton blank;
(5) And (3) glue discharging: placing the skeleton blank into a glue discharging furnace, preserving heat for 1.5 hours at 500 ℃, and decomposing and volatilizing polyurethane sponge organic materials in the blank to obtain a skeleton biscuit firing blank;
third step, preparing the matrix glass material
(1) Weighing: weighing all raw materials according to a melt formula;
(2) Mixing: the weighed raw materials are put into a mixer, and mixed for 3 hours to obtain evenly mixed powder;
(3) Firing: placing the skeleton biscuit firing blank into a mould, placing the mould into a kiln, and preserving the temperature for 30 minutes at 1470 ℃;
(4) Melting: pouring the mixed powder into a crucible, putting the crucible into a kiln, melting the powder at 1420 ℃, and preserving the heat for 3 hours to obtain a melt with good fluidity;
(5) Casting: taking out the framework biscuit which is being fired from the kiln, casting the melt into the framework biscuit, putting the framework biscuit into the kiln again after casting is finished, and preserving heat for 1 hour at 1380 ℃;
(6) Annealing: taking out the die, putting the die into an annealing furnace to anneal the material, wherein the annealing temperature is 450 ℃, the annealing time is 80 minutes, and cooling along with the furnace to obtain a matrix glass material;
fourth step, preparation of glass ceramic material
And (3) heat treatment: and (3) performing primary heat treatment on the matrix glass material at 600 ℃ for 25 minutes, performing secondary heat treatment on the heat-treated matrix glass material at 830 ℃ for 45 minutes, and cooling along with a 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 of
First, a framework material formula:
the formula of the framework material comprises: siO2:82, liO2:5, caO:1, ceO2:2, B2O3:2, dispersant: 8, a polyurethane sponge with ppi of 40;
(2) The formula of the melt is as follows:
SiO2:7，LiO2:61，P2O5:10，K2O:12，Al2O3:7，ZrO2:2；
second step, preparing skeleton material
(1) And (3) batching: weighing all components except the polyurethane sponge according to prescription;
(2) Ball milling: adding a proper amount of sodium stearate 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 120 minutes;
(3) Sieving: the slurry after ball milling is passed through a 300-400 mesh screen to obtain a filtered suspension;
(3) Coating: filling the suspension into polyurethane sponge, and removing bubbles in the suspension through vibration to obtain polyurethane sponge filled with the suspension;
(4) And (3) drying: placing polyurethane sponge filled with the suspension into an oven, drying at 120 ℃, and evaporating and discharging water in the suspension to obtain a skeleton blank;
(5) And (3) glue discharging: placing the skeleton blank into a glue discharging furnace, preserving heat for 1 hour at 600 ℃, and decomposing and volatilizing polyurethane sponge organic materials in the blank to obtain a skeleton biscuit firing blank;
third step, preparing the matrix glass material
(1) Weighing: weighing all raw materials according to a melt formula;
(2) Mixing: the weighed raw materials are put into a mixer, and mixed for 4.5 hours to obtain evenly mixed powder;
(3) Firing: placing the skeleton biscuit firing blank into a mould, placing the mould 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 the heat for 4.5 hours to obtain a melt with better fluidity;
(5) Casting: taking out the framework biscuit which is being fired from the kiln, casting the melt into the framework biscuit, putting the framework biscuit into the kiln again after casting is finished, and preserving heat for 2 hours at 1450 ℃;
(6) Annealing: taking out the die, putting the die into an annealing furnace to anneal the material, wherein the annealing temperature is 500 ℃, the annealing time is 120 minutes, and cooling along with the furnace to obtain a matrix glass material;
fourth step, preparation of glass ceramic material
And (3) heat treatment: and (3) performing primary heat treatment on the matrix glass material at 680 ℃ for 55 minutes, performing secondary heat treatment on the heat-treated matrix glass material at 930 ℃ for 110 minutes, and cooling along with a 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 of
First, 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 parts of dispersing agent: 0-8, ppi:15-40 parts of polyurethane sponge;
(2) The formula of the melt 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, preparing skeleton material
(1) And (3) batching: weighing all components except the polyurethane sponge according to 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 percent, and performing ball milling for 30 to 150 minutes;
(3) Sieving: the slurry after ball milling is passed through a 300-400 mesh screen to obtain a filtered suspension;
(3) Coating: filling the suspension into polyurethane sponge, and removing bubbles in the suspension through vibration to obtain polyurethane sponge filled with the suspension;
(4) And (3) drying: placing polyurethane sponge filled with the suspension into an oven, drying at 80-120 ℃, and evaporating and discharging water in the suspension to obtain a skeleton blank;
(5) And (3) glue discharging: placing the skeleton blank into a glue discharging furnace, preserving heat for 1-3 hours at 400-600 ℃, and decomposing and volatilizing polyurethane sponge organic materials in the blank to obtain a skeleton biscuit firing blank;
third step, preparing the matrix glass material
(1) Weighing: weighing all raw materials according to a melt formula;
(2) Mixing: the weighed raw materials are put into a mixer, and mixed for 2 to 5 hours to obtain evenly mixed powder;
(3) Firing: placing the skeleton biscuit firing blank into a mould, placing the mould 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 the temperature for 1-5 hours to obtain a melt with better fluidity;
(5) Casting: taking out the framework biscuit which is being fired from the kiln, casting the melt into the framework biscuit, putting the framework biscuit into the kiln again after casting, and preserving the temperature for 0.5-2 hours at 1300-1450 ℃;
(6) Annealing: taking out the die, putting the die into an annealing furnace to anneal the material, wherein the annealing temperature is 350-500 ℃, the annealing time is 30-120 minutes, and cooling along with the furnace to obtain a matrix glass material;
fourth step, preparation of glass ceramic material
(1) And (3) heat treatment: and (3) performing primary heat treatment on the matrix glass material at 500-700 ℃ for 5-60 minutes, performing secondary 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 the lithium disilicate glass ceramic material according to claim 1, wherein the dispersing agent is hydrochloric acid, ammonia water, inorganic acid and alkali, sodium silicate, sodium tripolyphosphate or sodium stearate lower organic matters.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210675438.4A CN114920459B (en) | 2022-06-15 | 2022-06-15 | Preparation method of lithium disilicate glass ceramic material |
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| CN202210675438.4A CN114920459B (en) | 2022-06-15 | 2022-06-15 | Preparation method of lithium disilicate glass ceramic material |
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| EP1505041A1 (en) * | 2003-08-07 | 2005-02-09 | Ivoclar Vivadent AG | Lithium silicate materials |
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| US8241395B2 (en) * | 2007-06-11 | 2012-08-14 | Schott Corporation | Glass-ceramic membranes |
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| EP0294176A2 (en) * | 1987-06-02 | 1988-12-07 | Corning Glass Works | Lightweight laminated or composite structures |
| CA2351154A1 (en) * | 2000-06-28 | 2001-12-28 | Marcel Schweiger | Low-temperature-sintering potassium-zinc-silicate glass |
| EP1505041A1 (en) * | 2003-08-07 | 2005-02-09 | Ivoclar Vivadent AG | Lithium silicate materials |
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| DE102014018464A1 (en) * | 2014-12-12 | 2016-06-16 | Schott Ag | THERMOCHROMIC PIGMENTS, THERMOCHROME COATING, METHOD FOR THE PRODUCTION THEREOF AND THEIR USE |
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