CN113860743A - Multilayer glass ceramic blank and preparation method and application thereof - Google Patents
Multilayer glass ceramic blank and preparation method and application thereof Download PDFInfo
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- CN113860743A CN113860743A CN202111098320.1A CN202111098320A CN113860743A CN 113860743 A CN113860743 A CN 113860743A CN 202111098320 A CN202111098320 A CN 202111098320A CN 113860743 A CN113860743 A CN 113860743A
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- 239000002241 glass-ceramic Substances 0.000 title claims abstract description 237
- 238000002360 preparation method Methods 0.000 title abstract description 26
- 239000000178 monomer Substances 0.000 claims abstract description 135
- 238000010438 heat treatment Methods 0.000 claims abstract description 62
- 239000002243 precursor Substances 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 19
- 238000012805 post-processing Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 47
- 239000002994 raw material Substances 0.000 claims description 32
- 238000002156 mixing Methods 0.000 claims description 20
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 20
- 239000003086 colorant Substances 0.000 claims description 16
- 239000011521 glass Substances 0.000 claims description 15
- 238000004321 preservation Methods 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 14
- 238000002834 transmittance Methods 0.000 claims description 13
- 238000005520 cutting process Methods 0.000 claims description 10
- 229910052697 platinum Inorganic materials 0.000 claims description 10
- 238000005498 polishing Methods 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000000919 ceramic Substances 0.000 claims description 8
- 238000005266 casting Methods 0.000 claims description 7
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 claims description 6
- 229910000531 Co alloy Inorganic materials 0.000 claims description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 5
- 229910000629 Rh alloy Inorganic materials 0.000 claims description 5
- 229910000929 Ru alloy Inorganic materials 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- CLBRCZAHAHECKY-UHFFFAOYSA-N [Co].[Pt] Chemical compound [Co].[Pt] CLBRCZAHAHECKY-UHFFFAOYSA-N 0.000 claims description 5
- 229910045601 alloy Inorganic materials 0.000 claims description 5
- 239000000956 alloy Substances 0.000 claims description 5
- 239000010431 corundum Substances 0.000 claims description 5
- 239000011574 phosphorus Substances 0.000 claims description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims description 5
- PXXKQOPKNFECSZ-UHFFFAOYSA-N platinum rhodium Chemical compound [Rh].[Pt] PXXKQOPKNFECSZ-UHFFFAOYSA-N 0.000 claims description 5
- CFQCIHVMOFOCGH-UHFFFAOYSA-N platinum ruthenium Chemical compound [Ru].[Pt] CFQCIHVMOFOCGH-UHFFFAOYSA-N 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 5
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 4
- 229910000820 Os alloy Inorganic materials 0.000 claims description 4
- 229910001252 Pd alloy Inorganic materials 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- 229910000946 Y alloy Inorganic materials 0.000 claims description 4
- 229910001093 Zr alloy Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- WBLJAACUUGHPMU-UHFFFAOYSA-N copper platinum Chemical compound [Cu].[Pt] WBLJAACUUGHPMU-UHFFFAOYSA-N 0.000 claims description 4
- IYZXTLXQZSXOOV-UHFFFAOYSA-N osmium platinum Chemical compound [Os].[Pt] IYZXTLXQZSXOOV-UHFFFAOYSA-N 0.000 claims description 4
- IMTFPWYLPOWRGG-UHFFFAOYSA-N platinum yttrium Chemical compound [Y].[Pt].[Pt].[Pt].[Pt].[Pt] IMTFPWYLPOWRGG-UHFFFAOYSA-N 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 3
- 229910052691 Erbium Inorganic materials 0.000 claims description 3
- 229910052693 Europium Inorganic materials 0.000 claims description 3
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 3
- 229910052689 Holmium Inorganic materials 0.000 claims description 3
- 229910052779 Neodymium Inorganic materials 0.000 claims description 3
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 3
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
- 229910052771 Terbium Inorganic materials 0.000 claims description 3
- 229910052775 Thulium Inorganic materials 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 claims description 3
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 claims description 3
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 3
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims description 3
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 3
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 3
- 238000010791 quenching Methods 0.000 claims description 3
- 230000000171 quenching effect Effects 0.000 claims description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 3
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- 239000011135 tin Substances 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 229910052684 Cerium Inorganic materials 0.000 claims 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims 1
- 238000012986 modification Methods 0.000 claims 1
- 230000004048 modification Effects 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims 1
- 230000001276 controlling effect Effects 0.000 abstract description 7
- 230000001105 regulatory effect Effects 0.000 abstract description 5
- 230000003287 optical effect Effects 0.000 abstract description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 16
- 229910052573 porcelain Inorganic materials 0.000 description 14
- 239000000203 mixture Substances 0.000 description 9
- 230000008569 process Effects 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 description 3
- 229910052912 lithium silicate Inorganic materials 0.000 description 3
- 230000000149 penetrating effect Effects 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 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
- 230000008859 change Effects 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 2
- 239000006112 glass ceramic composition Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000005368 silicate glass Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 239000005337 ground glass Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000005495 investment casting Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 239000006060 molten glass Substances 0.000 description 1
- 239000011664 nicotinic acid Substances 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 210000000332 tooth crown Anatomy 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Images
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
- C03C10/0009—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 silica as main constituent
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/15—Compositions characterised by their physical properties
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/831—Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
- A61K6/836—Glass
-
- 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
- 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
- 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
- C03C4/00—Compositions for glass with special properties
- C03C4/02—Compositions for glass with special properties for coloured glass
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Epidemiology (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Animal Behavior & Ethology (AREA)
- Veterinary Medicine (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Plastic & Reconstructive Surgery (AREA)
- Ceramic Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
The invention provides a multilayer glass ceramic blank and a preparation method and application thereof. The multilayer glass-ceramic blank comprises at least two glass-ceramic monomers. The preparation method comprises the following steps: (1) placing at least two glass ceramic monomers into a mold, and performing first heat treatment to obtain a multilayer glass ceramic blank precursor; (2) and (2) post-processing the colored glass ceramic blank precursor in the step (1) to obtain the multilayer glass ceramic blank. The multilayer glass ceramic provided by the invention can well simulate the optical and mechanical properties of natural tooth materials, the preparation method is simple and easy to operate, the flowing state of the glass ceramic monomer softening material is controlled by regulating and controlling the time and temperature of heat treatment in the preparation process, and a proper mold is matched for use to obtain the multilayer glass ceramic blank.
Description
Technical Field
The invention relates to the technical field of dental all-ceramic materials, relates to a glass ceramic blank, and particularly relates to a multilayer glass ceramic blank and a preparation method and application thereof.
Background
Aesthetic restoration of teeth is becoming more and more important, and higher demands are being made on materials that meet the various requirements for applications in the field of dental restoration.
At present, the manufacturing method of the facing can be mainly divided into a porcelain facing, a cast porcelain facing, a zirconia facing and a glass ceramic facing.
The porcelain facing is that porcelain powder is baked layer by adopting a fire-resistant porcelain baking technology, the appearance is good, the bionic effect is achieved, and the thinness can be 0.2mm-0.3 mm. However, the porcelain facing process is relatively complicated and requires a high number of technicians, which makes it expensive. Meanwhile, the prepared porcelain veneer has crisp texture, larger shrinkage and easy fracture when falling off.
The cast porcelain facing is formed by melting porcelain powder by a lost wax casting method and casting by a casting machine of vacuum casting and pressing, and compared with the baked porcelain facing, the cast porcelain facing has the advantages of simple process, relatively low price, higher facing strength and difficult fracture. However, the cast porcelain veneer has a thickness of 0.5mm to 0.8mm, and a part of teeth needs to be ground to avoid tooth crown, which affects the appearance of a wearer and causes great damage to teeth. Generally speaking, cast porcelain facing is the mainstream facing processing method at present. The traditional ceramic veneering process is improved by some methods, and the resin wax patterns are processed by combining computer design and digital resin wax spraying illumination curing printing, so that the ceramic veneering with the thickness of less than 0.5mm is manufactured, and tooth grinding is avoided. However, the method still needs the procedures of preparing wax patterns and the like of the traditional cast porcelain veneering, the embedding and casting process is complicated, a large amount of labor is needed, the processing precision is poor, the fitting degree with teeth of a wearer is low, and the lead cycle is long. In addition, the method has the problems of wax pattern volatilization pollution and harm to the health of operators, and casting production is forbidden in some areas.
In addition, the method of facing by cutting is also included, but this method is only for facing zirconia because zirconia has the characteristics of good toughness, high surface hardness, and difficulty in breaking. However, zirconia materials have poor transparency, general aesthetic properties, and unsatisfactory adhesion, and facing with zirconia materials has been of limited popularity. As a result, zirconia materials have gradually exited the mainstream market for veneering.
Compared with zirconia, the glass ceramic material has high transparency and good cohesiveness, and especially the glass ceramic is manufactured by digital processing in the whole process, so the glass ceramic material gradually becomes a favorite repairing mode in the market. However, most glass ceramic veneers are made by digitalizing chair bypasses in clinics. Therefore, outpatient doctors or technicians are required to go to the outpatient department to carry out dyeing and sintering treatment on the glass ceramic veneers, which undoubtedly brings great investment for preparing the veneering of the system beside the chair. Therefore, if the gradient glass ceramic is directly sintered after being cut, doctors can directly use the glass ceramic after simply polishing the glass ceramic, and the production cost beside the chair is greatly saved.
Secondly, the glass ceramic has higher permeability and single color, and can simulate the neck color, the cut end color and the like of teeth only by means of technically superior external dyeing in aesthetic property, so if one glass ceramic with gradually changed color can realize gradual change of the permeability and gradual change of the strength, natural teeth can be simulated in aesthetic property, and the strength and the permeability are more similar.
CN 112272544a discloses a multi-colored blank for dental purposes, comprising a first layer and a second layer, which are based on glass, glass-ceramic or ceramic independently of each other, wherein the first and second layers differ in color and form a boundary surface, wherein the boundary surface extends obliquely. The method has a complex structure, the first layer of blank and the second layer of blank need to be arranged on the basis of different substrates, namely, barriers exist between the different blanks, which is not beneficial to the continuity of the blanks, and the method needs to adopt equipment for controlling the viscosity of the molten glass and equipment for controlling the pressure in the preparation process, so that the operation is complex.
CN 111792847a discloses a method for preparing a multi-colored glass-ceramic blank, the method comprising the steps of: (1) introducing lithium silicate glass powders of different colors or a suspension of lithium silicate glass powders of different colors in a liquid medium into a mold to form a glass blank; (2) optionally compacting the glass blank from step (1) by pressing; (3) heat-treating the glass blank from step (1) or (2) to obtain a glass-ceramic blank having lithium silicate as the main crystalline phase; (4) compacting the glass ceramic blank from step (3) by hot pressing. The method requires pressurization while heating at 550-770 deg.c, which is very expensive and inefficient to produce.
In summary, it is one of the problems to be solved in the art to provide a multi-layer glass ceramic blank with simple structure, simple preparation method and high production efficiency.
Disclosure of Invention
The invention aims to provide a multilayer glass ceramic blank and a preparation method and application thereof. The multilayer glass ceramic blank can well simulate the optical and mechanical properties of natural tooth materials, the preparation method is simple, the flowing state of the glass ceramic monomer softening material is controlled by regulating and controlling the time and temperature of heat treatment, and the multilayer glass ceramic blank is obtained by matching with a proper mold.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a multilayer glass-ceramic blank comprising at least two glass-ceramic monomers;
the glass-ceramic monomers have any one or a combination of at least two of different colors, transmittances or intensities.
The glass ceramic monomer has amorphous characteristics, namely the glass ceramic monomer is gradually softened and becomes muddy in the process of heating instead of being converted from solid to liquid at a certain temperature in the melting process, and the higher the temperature is, the stronger the fluidity is.
Preferably, the glass-ceramic monomer comprises the following components in molar mass percentage: silicon-containing oxides of 30 to 70%, for example 30%, 40%, 50%, 60% or 70%, but not limited to the values recited, other values not recited in the numerical ranges are equally applicable; lithium-containing oxides of 20 to 50%, for example 20%, 30%, 40% or 50%, are possible, but are not limited to the values listed, and other values not listed in the numerical range are equally applicable; from 0.5 to 20% of potassium-containing oxides, for example 0.5%, 1%, 5%, 10%, 15% or 20%, but not limited to the values listed, and other values not listed within the numerical range are equally applicable; sodium oxide 0% to 20%, for example 0%, 5%, 10%, 15% or 20%, but not limited to the recited values, and other values not recited within the numerical range are equally applicable; 0.1% to 20% of an aluminium-containing oxide, which may be, for example, 0.1%, 1%, 5%, 10%, 15% or 20%, is not limited to the values recited, other values not recited in the numerical range being equally applicable; from 0% to 20% of phosphorus-containing oxides, for example 0%, 5%, 10%, 15% or 20%, but not limited to the values listed, other values not listed in the numerical range also being applicable; titanium-containing oxides of 0% to 20%, for example 0%, 5%, 10%, 15% or 20%, but not limited to the values recited, other values not recited in the numerical ranges are equally applicable; zirconium-containing oxides of 0% to 20%, for example 0%, 5%, 10%, 15% or 20%, but not limited to the values recited, other values not recited in the numerical ranges are equally applicable; from 0% to 20% of an oxide containing zinc, for example 0%, 5%, 10%, 15% or 20%, but not limited to the values recited, other values not recited in the range of values being equally applicable; from 0% to 20% of boron-containing oxide, for example 0%, 5%, 10%, 15% or 20%, but not limited to the recited values, and other values within the range of values not recited are equally applicable; cerium oxide in the range of 0% to 20%, for example 0%, 5%, 10%, 15% or 20%, but not limited to the recited values, and other values not recited within the range of values are equally applicable; colorants 0 to 10%, for example 0%, 2%, 4%, 6%, 8% or 10%, are possible, but not limited to the values listed, and other values not listed in the numerical range are likewise suitable.
Preferably, the colorant comprises any one or a combination of at least two of manganese, cobalt, vanadium, erbium, iron, copper, nickel, tin, lanthanum, praseodymium, neodymium, europium, gadolinium, terbium, dysprosium, holmium, thulium, or ytterbium, with typical but non-limiting combinations including combinations of manganese, cobalt, and vanadium, erbium, iron, and copper, nickel, tin, lanthanum, and praseodymium, neodymium, europium, and gadolinium, or terbium, dysprosium, holmium, thulium, and ytterbium.
The glass ceramic monomer comprises multiple elements, wherein the content of silicon element, lithium element, phosphorus element and titanium element can adjust the strength of the glass ceramic monomer, the strength of the glass ceramic monomer shows a trend of increasing first and then decreasing along with the increase of the total content of the silicon element, the lithium element, the phosphorus element and the titanium element, and the total content of the silicon element, the lithium element, the phosphorus element and the titanium element is too high, so that the strength of the glass ceramic monomer is reduced, and the waste of resources is also caused;
the content of potassium element, aluminium element and zirconium element can adjust glass ceramic monomer's degree of penetrating, and increase potassium element and zirconium element can improve glass ceramic monomer's degree of penetrating, but increase aluminium element's content can reduce its degree of penetrating, in the preparation process, needs adjust the content ratio between the three to satisfy the demand of product.
The content and type of elements in the colorant can affect the color of the glass-ceramic monomer.
In a second aspect, the present invention provides a method for producing a multilayer glass-ceramic blank according to the first aspect, comprising the steps of:
(1) placing at least two glass ceramic monomers into a mold, and performing first heat treatment to obtain a multilayer glass ceramic blank precursor;
(2) and (2) post-processing the colored glass ceramic blank precursor in the step (1) to obtain the multilayer glass ceramic blank.
The glass ceramic monomer in the step (1) has any one or combination of at least two of different colors, transmittances or strengths.
According to the invention, the flow state of the softened glass ceramic monomers is controlled by regulating and controlling the temperature and the heat preservation time of the first heat treatment, and a plurality of glass ceramic monomers are heated to the extent that the contact surfaces of the glass ceramic monomers can be mutually adhered, but different glass ceramic monomers cannot mutually flow and influence, and a proper mold is matched for use, so that the multilayer glass ceramic blank is formed.
Before the glass ceramic monomer is put into the die in the step (1), the processing process of the glass ceramic monomer is also included, the processing process comprises grinding, compacting, crushing and the like, and the glass ceramic monomer can also be made into various special shapes, such as wave shape, sawtooth shape and the like, so as to ensure the strength, transparency and simulation of the multilayer glass ceramic.
Preferably, the preparation method of the glass ceramic monomer comprises the following steps:
mixing the raw materials according to the formula amount, and sequentially carrying out second heat treatment and post-treatment to obtain the glass ceramic monomer.
Preferably, the post-treatment comprises casting and/or water quenching.
In the preparation process, the raw materials are melted and water-quenched to obtain the glass powder, and the obtained glass powder has uneven particle size, so the method also comprises a grinding step after water quenching, and the average particle size of the ground glass powder is 0.1-100 mu m.
Preferably, the temperature of the second heat treatment is 1000-1700 ℃, for example 1000 ℃, 1100 ℃, 1200 ℃, 1300 ℃, 1400 ℃, 1500 ℃, 1600 ℃ or 1700 ℃, but not limited to the recited values, and other values not recited in the range of values are equally applicable.
Preferably, the holding time of the second heat treatment is 1-600min, for example, 1min, 10min, 50min, 100min, 200min, 300min, 400min, 500min or 600min, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the temperature of the first heat treatment in step (1) is 1000-; preferably 1150-.
Preferably, the first heat treatment in step (1) has a holding time of 1-600min, such as 1min, 10min, 50min, 100min, 200min, 300min, 400min, 500min or 600min, but not limited to the values listed, and other values not listed in the range of values are also applicable.
The temperature and time of the first heat treatment of the present invention are such that the interfaces of the glass-ceramic monomers having different colors in contact are fused together, but the color distribution is substantially unchanged. If the temperature is too high or the heat preservation time is too long, different glass ceramic monomers are thoroughly integrated, so that the product is changed into a single-color glass ceramic monomer with multiple colors, transmittances or strengths; if the temperature is too low or the heat preservation time is too short, interfaces of different glass ceramic monomers in contact cannot be integrated, so that the product is layered, and an integral multilayer glass ceramic blank cannot be formed.
It is worth noting that: in the first heat treatment process, the temperature is inversely proportional to the heat preservation time, and a higher temperature needs to be selected, so that a shorter heat preservation time needs to be selected; conversely, when the temperature is lower, the holding time needs to be selected longer.
Preferably, the material of the mold in step (1) includes any one of platinum, platinum-containing alloy, quartz, corundum, zirconium ceramic, zirconium alloy, silicon carbide and silicon nitride or a combination of at least two of them, and typical but non-limiting combinations include a combination of platinum, corundum and zirconium alloy, a combination of corundum, silicon carbide and silicon nitride or a combination of platinum, zirconium alloy and platinum-containing alloy.
Preferably, the platinum-containing alloy includes any one of platinum-palladium alloy, platinum-rhodium alloy, platinum-yttrium alloy, platinum-ruthenium alloy, platinum-cobalt alloy, platinum-osmium alloy, or platinum-copper alloy, or a combination of at least two thereof, and typical but non-limiting combinations include a combination of platinum-palladium alloy, platinum-rhodium alloy, and platinum-ruthenium alloy, a combination of platinum-cobalt alloy, platinum-osmium alloy, and platinum-copper alloy, or a combination of platinum-yttrium alloy, platinum-ruthenium alloy, platinum-cobalt alloy, and platinum-osmium alloy.
The die has the characteristic of high temperature resistance, the materials of some dies can be adhered to glass liquid, and all surfaces of the die can be designed into a detachable state so as to be convenient for extracting the multilayer glass blank in the die.
Preferably, the post-processing of step (2) further comprises a heat treatment of the multilayer glass ceramic blank.
Preferably, the temperature of the heat treatment is 450 ℃ to 900 ℃, for example, 450 ℃, 500 ℃, 550 ℃, 600 ℃, 700 ℃, 800 ℃ or 900 ℃, but not limited to the recited values, and other values not recited in the numerical range are also applicable.
As a preferred embodiment of the present invention, the method for producing a multilayer glass ceramic blank according to the second aspect comprises the steps of:
(1) placing at least two glass ceramic monomers into a mold, performing heat treatment at the temperature of 1000-1700 ℃, and performing heat preservation for 1-600min to obtain the multilayer glass ceramic blank;
(2) sequentially carrying out cutting, polishing, surface correction and heating treatment at the temperature of 450-900 ℃ on the multilayer glass ceramic blank obtained in the step (1);
the glass ceramic monomer has any one or the combination of at least two of different colors, transmittances or intensities;
the glass ceramic monomer in the step (1) is prepared by adopting the following method:
mixing the raw materials according to the formula amount, sequentially carrying out 1100-1700 ℃ heat treatment, preserving the heat for 1-600min, and pouring and/or frying glass powder to obtain the glass ceramic monomer.
In a third aspect, the present invention provides a use of a multilayer glass-ceramic blank according to the first aspect for dental restoration techniques.
The recitation of numerical ranges herein includes not only the above-recited numerical values, but also any numerical values between non-recited numerical ranges, and is not intended to be exhaustive or to limit the invention to the precise numerical values encompassed within the range for brevity and clarity.
Compared with the prior art, the invention has the following beneficial effects:
(1) the multilayer glass ceramic blank provided by the invention can well simulate the optical and mechanical properties of natural tooth materials;
(2) the multilayer glass ceramic blank provided by the invention has a simple structure, only comprises a plurality of glass ceramic monomers, and does not need to adopt any matrix as a support;
(3) the preparation method of the multilayer glass ceramic blank provided by the invention is simple, and the flow state of the glass ceramic monomer softening compound is controlled by regulating and controlling the time and temperature of heat treatment in the preparation process, and the multilayer glass ceramic blank is obtained by matching with a proper mould.
Drawings
FIG. 1 is a schematic view showing a state in which a glass ceramic monolith is placed in a mold in a manufacturing process provided in example 1 of the present invention.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a multilayer glass ceramic blank, which comprises three glass ceramic monomers, namely a first glass ceramic monomer, a second glass ceramic monomer and a third glass ceramic monomer.
The components of the first glass-ceramic monomer, the second glass-ceramic monomer and the third glass-ceramic monomer are shown in the table 1 in terms of molar mass fractions.
TABLE 1
The preparation method of the multilayer glass ceramic blank comprises the following steps:
(1) putting the three glass ceramic monomers into a mould, performing heat treatment at 1500 ℃ as shown in figure 1, and performing heat preservation for 3min to obtain a multilayer glass ceramic blank precursor; the material of the mould is platinum;
(2) sequentially cutting, polishing, surface correction and 600 ℃ heating treatment on the multilayer glass ceramic blank precursor obtained in the step (1) to obtain the multilayer glass ceramic blank;
the glass-ceramic monomers have different transmittances, wherein the transmittance of the third glass-ceramic monomer is the highest, and the transmittance of the second glass-ceramic monomer is the next lowest, and the transmittance of the first glass-ceramic monomer is the lowest.
The first glass ceramic monomer is prepared by the following method: mixing the raw materials according to the formula amount shown in Table 1, sequentially carrying out 1550 ℃ heat treatment, carrying out heat preservation for 90min, and pouring the raw materials into blocks to obtain a first glass ceramic monomer;
the second glass ceramic monomer is prepared by the following method: mixing the raw materials according to the formula amount shown in the table 1, sequentially carrying out heat treatment at 1350 ℃, preserving heat for 100min, and pouring into blocks to obtain a second glass ceramic monomer;
the third glass ceramic monomer is prepared by the following method: mixing the raw materials according to the formula amount shown in the table 1, sequentially carrying out heat treatment at 1700 ℃, preserving heat for 50min, and then frying the raw materials into glass powder to obtain a third glass ceramic monomer.
Example 2
The embodiment provides a multilayer glass ceramic blank, which comprises two glass ceramic monomers, namely a first glass ceramic monomer and a second glass ceramic monomer.
The components of the first glass-ceramic monomer, the second glass-ceramic monomer and the third glass-ceramic monomer are shown in the table 2 in terms of molar mass fractions.
TABLE 2
| First glass ceramic monomer | Second glass-ceramic monomer | |
| SiO2 | 60.89％ | 57.89％ |
| Li2O | 25％ | 25％ |
| K2O | 5％ | 5％ |
| Al2O3 | 1％ | 1％ |
| ZrO2 | 1％ | 1％ |
| P2O5 | 2％ | 5％ |
| CeO2 | 5％ | 5％ |
| Er2O3 | 0.1％ | 0.1％ |
| MnO2 | 0.01％ | 0.01％ |
The preparation method of the multilayer glass ceramic blank comprises the following steps:
(1) putting the two glass ceramic monomers into a mold, performing heat treatment at 1150 ℃, and performing heat preservation for 420min to obtain a multilayer glass ceramic blank precursor; the material of the die is platinum-rhodium alloy;
(2) sequentially cutting, polishing and correcting the surface of the multilayer glass ceramic blank precursor obtained in the step (1) to obtain the multilayer glass ceramic blank;
the glass-ceramic monomers have different strengths, wherein the second glass-ceramic monomer has the highest strength and the first glass-ceramic monomer has the lowest strength.
The first glass ceramic monomer is prepared by the following method: mixing the raw materials according to the formula amount shown in Table 2, sequentially carrying out heat treatment at 1600 ℃, carrying out heat preservation for 60min, and pouring the raw materials into blocks to obtain a first glass ceramic monomer;
the second glass ceramic monomer is prepared by the following method: mixing the raw materials according to the formula amount shown in Table 2, sequentially carrying out heat treatment at 1400 ℃, carrying out heat preservation for 100min, and pouring the mixture into blocks to obtain a second glass ceramic monomer.
Example 3
The embodiment provides a multilayer glass ceramic blank, which comprises three glass ceramic monomers, namely a first glass ceramic monomer, a second glass ceramic monomer and a third glass ceramic monomer.
The compositions of the first, second and third glass-ceramic monomers are shown in table 3 in terms of molar mass fractions.
TABLE 3
| First glass ceramic monomer | Second glass-ceramic monomer | Third glass ceramic monomer | |
| SiO2 | 58.89％ | 57.76％ | 56.45％ |
| Li2O | 25％ | 25％ | 25％ |
| K2O | 5％ | 5％ | 5％ |
| Al2O3 | 1％ | 1％ | 1％ |
| P2O5 | 5％ | 5％ | 5％ |
| CeO2 | 5％ | 6％ | 7％ |
| Er2O3 | 0.1％ | 0.3％ | 0.5％ |
| MnO2 | 0.01％ | 0.03％ | 0.05％ |
The preparation method of the multilayer glass ceramic blank comprises the following steps:
(1) putting the three glass ceramic monomers into a die, carrying out heat treatment at 1500 ℃, and carrying out heat preservation for 3min to obtain a multilayer glass ceramic blank precursor; the material of the mould is corundum;
(2) sequentially cutting, polishing, surface correction and 600 ℃ heating treatment on the multilayer glass ceramic blank precursor obtained in the step (1) to obtain the multilayer glass ceramic blank;
the glass ceramic monomers have different colors, wherein the third glass ceramic monomer has the darkest color, and the second glass ceramic monomer has the lightest color.
The first glass ceramic monomer is prepared by the following method: mixing the raw materials according to the formula amount shown in Table 3, sequentially carrying out 1450 ℃ heat treatment, preserving heat for 180min, and pouring the raw materials into blocks to obtain a first glass ceramic monomer;
the second glass ceramic monomer is prepared by the following method: mixing the raw materials according to the formula amount shown in Table 3, sequentially carrying out heat treatment at 1300 ℃, preserving heat for 600min, and pouring the mixture into blocks to obtain a second glass ceramic monomer;
the third glass ceramic monomer is prepared by the following method: mixing the raw materials according to the formula amount shown in the table 3, sequentially carrying out heat treatment at 1700 ℃, preserving heat for 50min, and then frying the raw materials into glass powder to obtain a third glass ceramic monomer.
Example 4
The embodiment provides a multilayer glass ceramic blank, which comprises three glass ceramic monomers, namely a first glass ceramic monomer, a second glass ceramic monomer and a third glass ceramic monomer.
The compositions of the first, second and third glass-ceramic monomers are shown in table 4 in terms of molar mass fractions.
TABLE 4
The preparation method of the multilayer glass ceramic blank comprises the following steps:
(1) putting the three glass ceramic monomers into a mold, performing heat treatment at 1150 ℃, and preserving heat for 450min to obtain a precursor of a multilayer glass ceramic blank; the material of the mould is silicon carbide;
(2) sequentially cutting, polishing, surface correction and 600 ℃ heating treatment on the multilayer glass ceramic blank precursor obtained in the step (1) to obtain the multilayer glass ceramic blank;
the glass-ceramic monomers have different colors, transmittances and strengths.
The first glass ceramic monomer is prepared by the following method: mixing the raw materials according to the formula amount shown in Table 4, sequentially carrying out 1450 ℃ heat treatment, preserving heat for 180min, and pouring the raw materials into blocks to obtain a first glass ceramic monomer;
the second glass ceramic monomer is prepared by the following method: mixing the raw materials according to the formula amount shown in Table 4, sequentially carrying out heat treatment at 1300 ℃, preserving heat for 600min, and pouring the mixture into blocks to obtain a second glass ceramic monomer;
the third glass ceramic monomer is prepared by the following method: mixing the raw materials according to the formula amount shown in Table 4, sequentially carrying out heat treatment at 1700 ℃, keeping the temperature for 50min, and then frying the raw materials into glass powder to obtain a third glass ceramic monomer.
Example 5
The embodiment provides a multilayer glass-ceramic body, which comprises four glass-ceramic monomers, namely a first glass-ceramic monomer, a second glass-ceramic monomer, a third glass-ceramic monomer and a fourth glass-ceramic monomer.
The components of the first glass ceramic monomer, the second glass ceramic monomer, the third glass ceramic monomer and the fourth glass ceramic monomer are shown in the table 5 in terms of molar mass fraction.
TABLE 5
The preparation method of the multilayer glass ceramic blank comprises the following steps:
(1) putting the three glass ceramic monomers into a mold, performing heat treatment at 1150 ℃, and preserving heat for 450min to obtain a precursor of a multilayer glass ceramic blank; the material of the mould is silicon carbide;
(2) sequentially cutting, polishing, surface correction and 600 ℃ heating treatment on the multilayer glass ceramic blank precursor obtained in the step (1) to obtain the multilayer glass ceramic blank;
the glass-ceramic monomers have different colors, transmittances and strengths.
The first glass ceramic monomer is prepared by the following method: mixing the raw materials according to the formula amount shown in Table 5, sequentially carrying out 1450 ℃ heat treatment, preserving heat for 180min, and pouring the raw materials into blocks to obtain a first glass ceramic monomer;
the second glass ceramic monomer is prepared by the following method: mixing the raw materials according to the formula amount shown in Table 5, sequentially carrying out heat treatment at 1100 ℃, preserving heat for 600min, and pouring the raw materials into blocks to obtain a second glass ceramic monomer;
the third glass ceramic monomer is prepared by the following method: mixing the raw materials according to the formula amount shown in Table 5, sequentially carrying out heat treatment at 1700 ℃, preserving heat for 50min, and then frying the raw materials into glass powder to obtain a third glass ceramic monomer;
the fourth glass ceramic monomer is prepared by adopting the following method: mixing the raw materials according to the formula amount shown in Table 5, sequentially carrying out 1600 ℃ heat treatment, keeping the temperature for 60min, and then frying the raw materials into glass powder to obtain a fourth glass ceramic monomer.
Example 6
This example provides a multilayer glass ceramic blank having the same composition as in example 4.
The multilayer ceramic green sheet was prepared in the same manner as in example 4, except that the heat treatment temperature in step (1) was changed to 1800 ℃.
In this embodiment, because the temperature of the heat treatment in step (1) is too high and the holding time is long, the first glass-ceramic monomer, the second glass-ceramic monomer and the third glass-ceramic monomer become liquid at high temperature and flow and fuse with each other, so that a whole glass-ceramic blank with consistent strength, transmittance and color is formed.
Example 7
This example provides a multilayer glass ceramic blank having the same composition as in example 4.
The preparation method of the multilayer ceramic blank is the same as that of the embodiment 4 except that the heat preservation time of the heat treatment in the step (1) is changed to 550 min.
Example 8
This example provides a multilayer glass ceramic blank having the same composition as in example 4.
The preparation method of the multilayer ceramic blank is the same as that of the embodiment 4 except that the temperature of the heat treatment in the step (1) is changed to 1000 ℃, and the heat preservation time is changed to 600 min.
Comparative example 1
This comparative example provides a glass-ceramic blank comprising a glass-ceramic monolith, the first glass-ceramic monolith provided in example 4.
The preparation method of the glass ceramic blank comprises the following steps:
(a) mixing raw materials according to the formula amount of a first glass ceramic monomer shown in Table 4, sequentially carrying out 1450 ℃ heat treatment, preserving heat for 180min, and pouring the mixture into blocks to obtain a glass ceramic blank precursor;
(b) and (c) sequentially carrying out cutting, polishing, surface correction and 600 ℃ heating treatment on the glass ceramic blank precursor in the step (a) to obtain the glass ceramic blank.
Comparative example 2
This comparative example provides a multilayer glass-ceramic blank as provided in example 1 of the embodiment of patent CN 111792847 a.
The product properties, chemical stabilities and densities of the glass ceramic blanks provided in examples 1 to 8 and comparative examples 1 to 2 were examined as shown in Table 6; the transparency and toughness are shown in Table 7.
The chemical stability is shown in Table 6 as a weight loss of the multilayer glass ceramic blank under hydrofluoric acid etching, wherein the concentration of hydrofluoric acid is 5 wt%.
TABLE 6
TABLE 7
As can be seen from Table 6, the density of the multilayer glass ceramic blank provided by the present invention is increased without decreasing the chemical stability, so that the multilayer glass ceramic blank has better compactness. As can be seen from Table 7, the transmittance and fracture toughness of the multilayer glass-ceramics provided by the present invention have a wide variation range. The transparency and the strength of each part of the natural tooth are different, and the multilayer glass ceramic blank prepared by the method can better simulate the condition of the natural tooth and has stronger simulation.
In conclusion, the multilayer glass ceramic provided by the invention can well simulate the optical and mechanical properties of natural tooth materials, the preparation method is simple and easy to operate, the flowing state of the glass ceramic monomer softening material is controlled by regulating and controlling the time and temperature of heat treatment in the preparation process, and a proper mold is matched for use to obtain the multilayer glass ceramic blank.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. A multi-layer glass-ceramic blank, comprising at least two glass-ceramic monomers.
2. The multilayer glass-ceramic blank according to claim 1, wherein the glass-ceramic monomers have any one or a combination of at least two of different colors, transmittances, or strengths;
preferably, the glass-ceramic monomer comprises the following components in molar mass percentage: 30 to 70 percent of silicon-containing oxide, 20 to 50 percent of lithium-containing oxide, 0.5 to 20 percent of potassium-containing oxide, 0 to 20 percent of sodium-containing oxide, 0.1 to 20 percent of aluminum-containing oxide, 0 to 20 percent of phosphorus-containing oxide, 0 to 20 percent of titanium-containing oxide, 0 to 20 percent of zirconium-containing oxide, 0 to 20 percent of zinc-containing oxide, 0 to 20 percent of boron-containing oxide, 0 to 20 percent of cerium-containing oxide and 0 to 10 percent of colorant;
preferably, the colorant comprises any one or a combination of at least two of manganese, cobalt, vanadium, erbium, iron, copper, nickel, tin, lanthanum, praseodymium, neodymium, europium, gadolinium, terbium, dysprosium, holmium, thulium, or ytterbium.
3. A method for producing a multilayer glass-ceramic blank according to claim 1 or 2, characterized in that it comprises the steps of:
(1) placing at least two glass ceramic monomers into a mold, and performing first heat treatment to obtain a multilayer glass ceramic blank precursor;
(2) and (2) post-processing the precursor of the multilayer glass ceramic blank in the step (1) to obtain the multilayer glass ceramic blank.
4. The method according to claim 3, wherein the method for preparing the glass ceramic monomer according to the step (1) comprises the steps of:
mixing the raw materials according to the formula amount, and sequentially carrying out second heat treatment and post-treatment to obtain a glass ceramic monomer;
preferably, the post-treatment comprises casting and/or water quenching.
5. The method as claimed in claim 4, wherein the temperature of the second heat treatment is 1000-1700 ℃;
preferably, the holding time of the second heat treatment is 1-600 min.
6. The method according to claim 3, wherein the temperature of the first heat treatment in step (1) is 1000-1700 ℃, preferably 1150-1520 ℃;
preferably, the holding time of the first heat treatment in the step (1) is 1-600 min.
7. The method according to claim 3, wherein the material of the mold in step (1) comprises any one or a combination of at least two of platinum, platinum-containing alloy, quartz, corundum, zirconium ceramic, zirconium alloy, silicon carbide and silicon nitride;
preferably, the platinum-containing alloy comprises any one of platinum-palladium alloy, platinum-rhodium alloy, platinum-yttrium alloy, platinum-ruthenium alloy, platinum-cobalt alloy, platinum-osmium alloy or platinum-copper alloy or a combination of at least two of the platinum-palladium alloy, the platinum-rhodium alloy, the platinum-yttrium alloy, the platinum-ruthenium alloy, the platinum-cobalt alloy or the platinum-copper alloy.
8. The production method according to any one of claims 3 to 7, wherein the post-processing of step (2) further comprises cutting, polishing, surface modification and heat treatment of the multi-layer glass ceramic blank;
preferably, the temperature of the heating treatment is 450-.
9. The method according to any one of claims 3 to 8, characterized by comprising the steps of:
(1) placing at least two glass ceramic monomers into a mold, performing heat treatment at the temperature of 1000-1700 ℃, and performing heat preservation for 1-600min to obtain a multilayer glass ceramic blank precursor;
(2) sequentially cutting, polishing, surface correction and heating treatment at the temperature of 450-900 ℃ on the multilayer glass ceramic blank precursor obtained in the step (1) to obtain the multilayer glass ceramic blank;
the glass ceramic monomer in the step (1) is prepared by adopting the following method:
mixing the raw materials according to the formula amount, sequentially carrying out heat treatment at the temperature of 1000-1700 ℃, preserving heat for 1-600min, and pouring and/or frying glass powder to obtain the glass ceramic monomer.
10. Use of a multilayer glass-ceramic blank according to claim 1 or 2 for dental restoration techniques.
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| CN114716149A (en) * | 2022-05-06 | 2022-07-08 | 爱迪特（秦皇岛）科技股份有限公司 | Lithium disilicate glass ceramic with gradually changed color and transmittance for dentistry, and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114716149A (en) * | 2022-05-06 | 2022-07-08 | 爱迪特（秦皇岛）科技股份有限公司 | Lithium disilicate glass ceramic with gradually changed color and transmittance for dentistry, and preparation method and application thereof |
| CN114716149B (en) * | 2022-05-06 | 2023-06-27 | 爱迪特（秦皇岛）科技股份有限公司 | Lithium disilicate glass ceramic with gradually changed color and transmittance for dentistry as well as preparation method and application thereof |
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