CN115417600A - Lithium disilicate glass ceramic bracket and preparation method thereof - Google Patents
Lithium disilicate glass ceramic bracket and preparation method thereof Download PDFInfo
- Publication number
- CN115417600A CN115417600A CN202210978005.6A CN202210978005A CN115417600A CN 115417600 A CN115417600 A CN 115417600A CN 202210978005 A CN202210978005 A CN 202210978005A CN 115417600 A CN115417600 A CN 115417600A
- Authority
- CN
- China
- Prior art keywords
- disilicate glass
- lithium disilicate
- lithium
- glass ceramic
- bracket
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000919 ceramic Substances 0.000 title claims abstract description 87
- 239000003103 lithium disilicate glass Substances 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 64
- 239000003292 glue Substances 0.000 claims abstract description 46
- 239000002002 slurry Substances 0.000 claims abstract description 38
- 238000007639 printing Methods 0.000 claims abstract description 25
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 20
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 20
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 239000011347 resin Substances 0.000 claims abstract description 18
- 229920005989 resin Polymers 0.000 claims abstract description 18
- 238000000016 photochemical curing Methods 0.000 claims abstract description 16
- 238000000465 moulding Methods 0.000 claims abstract description 15
- -1 acrylic ester Chemical class 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims description 92
- 239000002243 precursor Substances 0.000 claims description 36
- 239000000243 solution Substances 0.000 claims description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 28
- 229910052744 lithium Inorganic materials 0.000 claims description 25
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 22
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 22
- 229910052710 silicon Inorganic materials 0.000 claims description 22
- 239000010703 silicon Substances 0.000 claims description 22
- 238000001816 cooling Methods 0.000 claims description 21
- 239000003153 chemical reaction reagent Substances 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 16
- 239000003999 initiator Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- WVMPCBWWBLZKPD-UHFFFAOYSA-N dilithium oxido-[oxido(oxo)silyl]oxy-oxosilane Chemical compound [Li+].[Li+].[O-][Si](=O)O[Si]([O-])=O WVMPCBWWBLZKPD-UHFFFAOYSA-N 0.000 claims description 12
- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 claims description 12
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 9
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 7
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229940065472 octyl acrylate Drugs 0.000 claims description 6
- ANISOHQJBAQUQP-UHFFFAOYSA-N octyl prop-2-enoate Chemical compound CCCCCCCCOC(=O)C=C ANISOHQJBAQUQP-UHFFFAOYSA-N 0.000 claims description 6
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 4
- FIHBHSQYSYVZQE-UHFFFAOYSA-N 6-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCCOC(=O)C=C FIHBHSQYSYVZQE-UHFFFAOYSA-N 0.000 claims description 3
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 3
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- XTUSEBKMEQERQV-UHFFFAOYSA-N propan-2-ol;hydrate Chemical compound O.CC(C)O XTUSEBKMEQERQV-UHFFFAOYSA-N 0.000 claims description 3
- OVARTBFNCCXQKS-UHFFFAOYSA-N propan-2-one;hydrate Chemical compound O.CC(C)=O OVARTBFNCCXQKS-UHFFFAOYSA-N 0.000 claims description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 3
- 239000006136 disilicate glass ceramic Substances 0.000 claims 6
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 238000007599 discharging Methods 0.000 description 30
- 238000002156 mixing Methods 0.000 description 21
- 230000008569 process Effects 0.000 description 16
- 239000000047 product Substances 0.000 description 16
- 230000006872 improvement Effects 0.000 description 8
- 238000000498 ball milling Methods 0.000 description 7
- 239000011521 glass Substances 0.000 description 7
- AZVCGYPLLBEUNV-UHFFFAOYSA-N lithium;ethanolate Chemical compound [Li+].CC[O-] AZVCGYPLLBEUNV-UHFFFAOYSA-N 0.000 description 7
- 238000007873 sieving Methods 0.000 description 7
- 239000012071 phase Substances 0.000 description 6
- 239000002241 glass-ceramic Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 229940113115 polyethylene glycol 200 Drugs 0.000 description 4
- 238000004513 sizing Methods 0.000 description 4
- 238000010146 3D printing Methods 0.000 description 3
- 239000004925 Acrylic resin Substances 0.000 description 3
- 229920000178 Acrylic resin Polymers 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000001723 curing Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 229940023487 dental product Drugs 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 230000008439 repair process Effects 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical group [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- BLHLJVCOVBYQQS-UHFFFAOYSA-N ethyllithium Chemical compound [Li]CC BLHLJVCOVBYQQS-UHFFFAOYSA-N 0.000 description 2
- 239000000156 glass melt Substances 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 229920005692 JONCRYL® Polymers 0.000 description 1
- 229920002873 Polyethylenimine Polymers 0.000 description 1
- 101100371219 Pseudomonas putida (strain DOT-T1E) ttgE gene Proteins 0.000 description 1
- ZVLDJSZFKQJMKD-UHFFFAOYSA-N [Li].[Si] Chemical compound [Li].[Si] ZVLDJSZFKQJMKD-UHFFFAOYSA-N 0.000 description 1
- WXZIKFXSSPSWSR-UHFFFAOYSA-N [Li]CCCCC Chemical compound [Li]CCCCC WXZIKFXSSPSWSR-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 239000005548 dental material Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000007656 fracture toughness test Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- JILPJDVXYVTZDQ-UHFFFAOYSA-N lithium methoxide Chemical compound [Li+].[O-]C JILPJDVXYVTZDQ-UHFFFAOYSA-N 0.000 description 1
- UBJFKNSINUCEAL-UHFFFAOYSA-N lithium;2-methylpropane Chemical compound [Li+].C[C-](C)C UBJFKNSINUCEAL-UHFFFAOYSA-N 0.000 description 1
- HAUKUGBTJXWQMF-UHFFFAOYSA-N lithium;propan-2-olate Chemical compound [Li+].CC(C)[O-] HAUKUGBTJXWQMF-UHFFFAOYSA-N 0.000 description 1
- DVSDBMFJEQPWNO-UHFFFAOYSA-N methyllithium Chemical compound C[Li] DVSDBMFJEQPWNO-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229920003986 novolac Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229940113116 polyethylene glycol 1000 Drugs 0.000 description 1
- 229940068918 polyethylene glycol 400 Drugs 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 description 1
- 239000012070 reactive reagent Substances 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000009974 thixotropic effect 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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
- A61C7/00—Orthodontics, i.e. obtaining or maintaining the desired position of teeth, e.g. by straightening, evening, regulating, separating, or by correcting malocclusions
- A61C7/12—Brackets; Arch wires; Combinations thereof; Accessories therefor
- A61C7/14—Brackets; Fixing brackets to teeth
- A61C7/141—Brackets with reinforcing structure, e.g. inserts
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Dentistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Ceramic Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses a lithium disilicate glass ceramic bracket and a preparation method thereof, and relates to the technical field of artificial tooth materials. The preparation method comprises the following steps: (1) Lithium disilicate glass ceramic powder, acrylic ester, polyethylene glycol and light-cured resin are mixed according to the proportion of (4-8): (0.01-0.2): (0.05-0.8): (0.5-1.5) to obtain slurry; (2) Photocuring, printing and molding the slurry to obtain a dental bracket blank; (3) And (4) removing the glue from the bracket blank, and sintering to obtain a finished product of the lithium disilicate glass ceramic bracket. By implementing the invention, the lithium disilicate glass ceramic bracket with high form, position and size precision and excellent mechanical property can be obtained; and the preparation method has high production efficiency and low cost.
Description
Technical Field
The invention relates to the technical field of artificial tooth materials, in particular to a lithium disilicate glass ceramic bracket and a preparation method thereof.
Background
The lithium disilicate glass ceramic is a common dental repair material, has high transparency of glass and high strength of ceramic, can meet the requirements of dental materials on aesthetics and mechanical properties, and plays an important role in the field of dental repair. The lithium disilicate glass ceramic-based products currently used clinically are mainly of the family of the ipse. The main preparation process is melt injection molding, namely pouring the glass melt into a concave die for molding at a high temperature, and then performing crystallization treatment after molding. Other patents related to the preparation of lithium disilicate products, such as CN104108883A, disclose a high-strength lithium disilicate glass ceramic and a preparation method thereof, wherein the process flow comprises selecting an initial raw material formula, uniformly mixing, placing in a crucible, melting at 1300-1600 ℃ for 1-24 h, rapidly cooling to obtain matrix glass, and performing heat treatment on the matrix glass to crystallize the matrix glass to obtain the glass ceramic with a main crystal phase of lithium disilicate; for another example, patent CN108751721A discloses a lithium disilicate glass ceramic for dental zirconia surface decoration, and a preparation method and application thereof, wherein the process flow comprises mixing and melting raw materials to obtain a melt, then pouring the melt into a mold for annealing to obtain a glass body, and crystallizing the body again to obtain the lithium disilicate glass ceramic.
As can be seen from the above description, the traditionally used dental repair glass ceramics are obtained by high temperature melt injection molding and post crystallization treatment, and the crystallization treatment is to form a crystalline phase of lithium disilicate, thereby improving the mechanical properties and chemical stability of the glass ceramics, because the crystalline phase has better mechanical and chemical stability than amorphous glass. The process flow has two problems, namely, when the dental product with a complex shape, particularly a dental product with an internal structure and an internal and external communicating structure, such as a bracket for dental orthodontics, needs to be prepared, the dental product cannot be formed at one time through a mould, needs to be processed at a later stage, is time-consuming and labor-consuming, and has low precision and low yield; on the other hand, in the lithium disilicate glass ceramic prepared based on the glass melt post-crystallization process, the content of the glass phase is high, which results in low chemical stability and mechanical stability of the lithium disilicate product, and the content of the lithium disilicate ceramic crystalline phase in the lithium disilicate glass ceramic needs to be further improved.
Disclosure of Invention
The technical problem to be solved by the invention is to provide the preparation method of the lithium disilicate glass ceramic bracket, the dental bracket product prepared by the preparation method has the advantages of high shape and size precision and good mechanical property, and the preparation method has high production efficiency.
The invention also aims to solve the technical problem of providing a lithium disilicate glass ceramic bracket.
In order to solve the problems, the invention discloses a preparation method of a lithium disilicate glass ceramic dental bracket, which comprises the following steps:
(1) Lithium disilicate glass ceramic powder, acrylic ester, polyethylene glycol and light-cured resin are mixed according to the proportion of (4-8): (0.01-0.2): (0.05-0.8): (0.5-1.5) to obtain slurry;
(2) Photocuring, printing and molding the slurry to obtain a dental bracket blank;
(3) And (4) removing the glue from the bracket blank, and sintering to obtain a finished product of the lithium disilicate glass ceramic bracket.
As an improvement of the technical scheme, the preparation method of the lithium disilicate glass ceramic powder comprises the following steps:
1) Silicon source reagent and lithium source reagent are mixed according to the silicon-lithium molar ratio of (0.5-2): 1 in a dispersing agent to obtain a precursor solution;
2) Adding an initiator into the precursor liquid to convert the precursor liquid into a gel liquid;
3) Drying and grinding the gel liquid to obtain precursor powder;
4) And (3) carrying out heat treatment on the precursor powder at 600-1000 ℃ for 0.5-10 h, cooling and grinding to obtain the finished product of the lithium disilicate glass ceramic powder, wherein the granularity of the product is less than or equal to 200 meshes.
As an improvement of the technical scheme, the silicon source reagent is one or more of tetraethoxysilane, silicate, silica sol and hexamethyldisiloxane; the lithium source reagent is selected from alkyl lithium and/or alcohol-based lithium.
As an improvement of the technical scheme, the initiator is selected from one or more of water, polyvinyl alcohol, water-ethanol mixed solution, water-acetone mixed solution, water-isopropanol mixed solution and polyethylene glycol;
the dosage of the initiator is 0.1-10% of the volume of the precursor liquid.
As an improvement of the above technical solution, in the step 1), the silicon source reagent and the lithium source reagent are mixed according to a molar ratio of silicon to lithium of (0.5-2): 1 in the dispersing agent, and stirring for 12-36 h at a stirring speed of 100-1000 rpm to obtain a precursor solution;
wherein, the dispersant is water and/or ethanol.
As an improvement of the technical scheme, the acrylic ester is one or more of methyl acrylate, ethyl acrylate, octyl acrylate, lauryl acrylate and 1, 6-hexanediol diacrylate;
the molecular weight of the polyethylene glycol is 200-2000 g/mol.
As an improvement of the technical scheme, the acrylic ester is lauryl acrylate.
As an improvement of the technical scheme, the molecular weight of the polyethylene glycol is 1000-2000 g/mol.
As an improvement of the technical scheme, the step (3) comprises the following steps:
(3.1) removing the glue of the dental bracket blank; wherein, the temperature curve that the binder removal adopted does: heating to 400-800 ℃ at a heating rate of 0.1-10 ℃/min, and keeping the temperature at 400-800 ℃ for 0.5-10 h;
(3.2) sintering the dental bracket blank after the glue is removed; wherein, the temperature curve that the sintering adopted is: heating to 800-1250 ℃ at the heating rate of 0.5-20 ℃/min, and preserving the heat for 0.5-10 h at the temperature of 800-1250 ℃.
Correspondingly, the invention also discloses a lithium disilicate glass ceramic bracket which is prepared by adopting the preparation method of the lithium disilicate glass ceramic bracket.
The implementation of the invention has the following beneficial effects:
1. the preparation method of the dental orthodontic bracket adopts the photocuring printing 3D printing method for forming, can form the lithium disilicate glass ceramic bracket with a complex shape, and has the advantages of high dimensional precision, excellent aesthetic property, short preparation flow and high production efficiency.
2. According to the preparation method of the lithium disilicate glass ceramic bracket, the slurry is obtained by mixing the lithium disilicate glass ceramic powder, the acrylate, the polyethylene glycol and the light-curing resin according to a specific proportion, the performance requirement of the slurry for light-curing printing forming printing can be met, the solid phase rate is high (more than 80 wt%), and the strength of a dental bracket product is effectively improved.
3. According to the invention, the lithium disilicate glass ceramic powder is prepared by a sol-gel method, one finished product is more spherical, and the slurry absorption amount is small, so that the high solid fraction slurry is effectively ensured to keep relatively good fluidity and shear thinning performance. In addition, the process improves the content of a crystalline phase in the lithium disilicate glass ceramic, thereby improving the mechanical stability and the chemical resistance of the glass ceramic, and also improving the mechanical property and the chemical resistance of a dental bracket product.
Drawings
FIG. 1 is an electron micrograph of a lithium disilicate glass ceramic powder obtained in example 6 of the present invention;
FIG. 2 is a graph showing the viscosity of the slurry obtained in example 6 of the present invention;
FIG. 3 is a view showing the construction of a dental bracket according to examples 1 to 7 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below.
The invention provides a preparation method of a lithium disilicate glass ceramic bracket, which comprises the following steps:
s1: lithium disilicate glass ceramic powder, acrylic ester, polyethylene glycol and light-cured resin are mixed according to the proportion of (4-8): (0.01-0.2): (0.05-0.8): (0.5-1.5) to obtain slurry;
wherein, the lithium disilicate glass ceramic powder can be glass ceramic powder obtained by traditional melting, rapid cooling and heat treatment, and can also be lithium disilicate glass ceramic powder prepared by a sol-gel method. Preferably, in an embodiment of the present invention, the lithium disilicate glass ceramic powder is prepared by a sol-gel method, which specifically includes the following steps:
s100: dispersing a silicon source reagent and a lithium source reagent in a dispersing agent to obtain a precursor solution;
the silicon source reagent is a reactive reagent containing silicon element, such as one or more of ethyl orthosilicate, silicate, silica sol, hexamethyldisiloxane, but not limited thereto. Preferably, the silicon source reagent is tetraethoxysilane. The lithium source reagent is a lithium element-containing reagent such as alkyl lithium (methyl lithium, ethyl lithium, butyl lithium, amyl lithium, etc.), alcohol lithium (lithium ethoxide, lithium methoxide, lithium isopropoxide, etc.), but is not limited thereto. Lithium ethoxide is preferred. The dispersant may be water and/or ethanol, but is not limited thereto. Ethanol is preferred.
Wherein, the molar ratio of the silicon element in the silicon source reagent to the lithium element in the lithium source reagent is (0.5-2): 1, exemplary is 0.8:1. 1.7.
Specifically, stirring is carried out for 12 to 36 hours at a stirring speed of 100 to 1000rpm after dispersion, so as to obtain the precursor solution.
S200: adding an initiator into the precursor liquid to convert the precursor liquid into gel liquid;
specifically, the initiator may be one or more of water, polyvinyl alcohol, water-ethanol mixed solution, water-acetone mixed solution, water-isopropanol mixed solution, and polyethylene glycol. The dosage of the initiator is 0.1-10% of the volume of the precursor liquid.
S300: drying and grinding the gel liquid to obtain precursor powder;
specifically, the gel liquid is dried at 40-180 ℃, and ground to a state of no hardening after drying, so that the precursor powder is obtained.
S400: heat treating the precursor powder at 600-1000 deg.c for 0.5-10 hr, cooling and grinding to 200 mesh or less to obtain the lithium disilicate glass ceramic powder product.
Based on the preparation method, the prepared lithium disilicate is mainly spherical in microscopic morphology, has less slurry absorption, can be matched with acrylate, polyethylene glycol, light-cured resin and the like to form slurry with reasonable rheological properties and solid phase rate of more than 85%, and improves various properties of the dental bracket.
Specifically, in the slurry formulation, the acrylate may be one or more selected from methyl acrylate, ethyl acrylate, octyl acrylate, lauryl acrylate, and 1, 6-hexanediol diacrylate, but is not limited thereto. The acrylate can be matched with polyethylene glycol to form slurry with stable performance, the slurry has proper viscoelasticity and viscosity, the fluidity requirement of photocuring printing forming printing can be met, and a good foundation is provided for stable printing. Preferably, the acrylate is lauryl acrylate. The sizing agent formed by adopting the lauryl acrylate can keep a better pore structure in the placing process and prevent O entering the sizing agent in the mixing process 2 Difficult to escape, resulting in difficult curing and reduced printing accuracy.
Specifically, the molecular weight of the polyethylene glycol is 200 to 2000g/mol, and is exemplified by 200g/mol, 400g/mol, 600g/mol, 1000g/mol, 1500g/mol, or 1800g/mol, but is not limited thereto. Preferably, the polyethylene glycol has a molecular weight of 1000 to 2000g/mol. Based on the polyethylene glycol with the molecular weight range, the thixotropic property of the obtained sizing agent is better (namely, the sizing agent still has good property after being placed for a plurality of times), and further, the defects of cracking, collapsing, missing and the like during printing are effectively prevented.
The light-cured resin is an ultraviolet light-cured resin which is common in the field. Exemplary are as follows: the epoxy resin comprises a standard UV epoxy acrylic resin of a blue Koehu L-6114, a Victoria WDS-2255 bisphenol A modified epoxy acrylic resin, a Huakai HL-183C70 novolac epoxy acrylate and a Pasteur Joncryl 848 epoxy acrylic resin.
Wherein, the dosage proportions of the lithium disilicate glass ceramic powder, the cellulose ester, the polyethyleneimine, the light-cured resin and the water are (4-8): (0.01-0.2): (0.05-0.8): (0.5-1.5): (0.1-1.5), the slurry obtained based on the proportion has no agglomeration and no caking, has reasonable fluidity and high solid content (more than or equal to 80wt percent), and can well meet the requirements of photocuring printing and forming. Preferably, the using proportion of the lithium disilicate glass ceramic powder, the acrylate, the polyethylene glycol and the light-cured resin is (6-8): (0.01-0.1): (0.05-0.3): (0.5-1.5). The slurry obtained based on the proportion has higher solid content, and the obtained dental bracket has better mechanical property.
S2: photocuring, printing and molding the slurry to obtain a dental bracket blank;
wherein, can adopt common photocuring to print formula 3D printer and carry out the shaping. Preferably, in one embodiment of the present invention, the ceramic 3D printing device is formed by using a pull-down type ceramic 3D printing device. Preferably, an ADT-ZP-DLP series 3D printer produced by Shenzhen miraculous science and technology Limited is adopted for molding. The series of 3D printers adopt a double-cylinder-sinking-scraping structure, the requirement on the flowability of the slurry is greatly reduced, the printing precision can be improved, and the consumption of the slurry is reduced.
S3: carrying out glue removal and sintering on the bracket blank to obtain a finished product of the lithium disilicate glass ceramic bracket;
specifically, S3 includes:
s31: carrying out glue removal on the dental bracket blank;
wherein, the temperature curve that the binder removal adopted does: heating to 400-800 ℃ at the heating rate of 0.1-10 ℃/min, and keeping the temperature at 400-800 ℃ for 0.5-10 h;
illustratively, the rate of the gel discharge temperature rise is 0.2 deg.C/min, 0.5 deg.C/min, 1 deg.C/min, 2 deg.C/min, 4 deg.C/min, 5 deg.C/min, or 8 deg.C/min, but is not limited thereto. When the heating rate is more than 10 ℃/min, the glue discharging rate is too fast, the blank is easy to crack, and when the heating rate is less than 0.5 ℃, the glue discharging rate is too slow.
S32: sintering the tooth bracket blank after the glue is removed; wherein, the temperature curve that the sintering adopted is: heating to 800-1250 ℃ at the heating rate of 0.5-20 ℃/min, and preserving the heat for 0.5-10 h at the temperature of 800-1250 ℃.
The invention is further described in the following embodiments, and it should be noted that the printing apparatus used in the following embodiments is Adventure 3D-ZP Printer-192-50 (Shenzhen miracle science and technology Co., ltd.). The resulting dental bracket structure is shown in fig. 3.
Example 1
The embodiment provides a preparation method of a lithium disilicate glass ceramic bracket, which comprises the following steps:
(1) Lithium disilicate glass ceramic powder, octyl acrylate, polyethylene glycol 200 (molecular weight 200 g/mol) and light-cured resin are prepared according to the proportion of 4:0.01:0.05:0.5 to obtain slurry; specifically, the lithium disilicate glass ceramic powder is prepared by adopting a preparation method of CN108751721A, and is crushed after preparation and then sieved by a 2000-mesh sieve;
(2) Photocuring, printing and molding the slurry to obtain a dental bracket blank;
(3) Putting the dental bracket blank into a low-temperature ceramic furnace to carry out glue discharging treatment in the air, wherein the glue discharging mode is as follows: heating to 300 ℃ at the speed of 0.5 ℃/min, keeping the temperature for 1h, heating to 480 ℃ at the speed of 0.5 ℃/min, keeping the temperature for 2h, heating to 600 ℃ at the speed of 1 ℃/min, keeping the temperature for 1h, and cooling to finish the glue discharging process. And then, the bracket subjected to glue discharge is placed into a high-temperature furnace and sintered in the air, wherein the specific sintering mode is as follows: heating to 600 ℃ at the temperature of 5 ℃/min, preserving heat for 1h, heating to 1000 ℃ at the temperature of 2 ℃/min, preserving heat for 2h, and cooling to obtain the lithium disilicate glass ceramic dental bracket.
Example 2
(1) Respectively dissolving ethyl orthosilicate and lithium ethylate into ethanol to form uniform transparent solutions of 2mol/L and 0.82mol/L, wherein the molar ratio of silicon to lithium is 1:1 mixing the two solutions and stirring for 12 hours at the rotating speed of 500r/min to obtain a uniform solution.
(2) Adding an initiator (water: ethanol =1 (weight ratio), in an amount of 1vol% of the solution volume) to form a gel;
(3) The gel was transferred to an oven at 60 ℃ and incubated for 12 hours, and then completely dried in an oven at 90 ℃. Grinding the dried gel to obtain precursor powder;
(4) Carrying out heat treatment on the precursor powder, wherein the heat treatment mode is as follows: heating to 600 ℃ at the speed of 3 ℃/min, then preserving heat for 1h, heating to 800 ℃ at the speed of 2 ℃/min, and preserving heat for 2h. And ball-milling the powder after heat treatment in a planetary ball mill for 1h at the rotating speed of 400r/min, and sieving the powder by a 2000-mesh sieve to obtain the lithium disilicate glass ceramic powder.
(5) Mixing lithium disilicate glass ceramic powder, octyl acrylate, polyethylene glycol 400 (molecular weight 400 g/mol) and light-cured resin according to a ratio of 4:0.01:0.05:0.5 to obtain slurry;
(6) Photocuring, printing and molding the slurry to obtain a dental bracket blank;
(7) Putting the dental bracket blank into a low-temperature ceramic furnace to carry out glue discharging treatment in the air, wherein the glue discharging mode is as follows: heating to 300 ℃ at a speed of 0.5 ℃/min, keeping the temperature for 1h, heating to 480 ℃ at a speed of 0.5 ℃/min, keeping the temperature for 2h, heating to 600 ℃ at a speed of 1 ℃/min, keeping the temperature for 1h, and cooling to finish the glue discharging process. And then, the bracket subjected to glue discharge is placed into a high-temperature furnace and sintered in the air, wherein the specific sintering mode is as follows: heating to 600 ℃ at the temperature of 5 ℃/min, preserving heat for 1h, heating to 1000 ℃ at the temperature of 2 ℃/min, preserving heat for 2h, and cooling to obtain the lithium disilicate glass ceramic dental bracket.
Example 3
(1) Respectively dissolving ethyl orthosilicate and lithium ethylate into ethanol to form 2mol/L and 0.82mol/L uniform transparent solutions, wherein the molar ratio of silicon to lithium is 1:1 mixing the two solutions and stirring for 12 hours at the rotating speed of 500r/min to obtain a uniform solution.
(2) Initiator (water: ethanol =2 (weight ratio), added in an amount of 3vol% of the solution volume) was added to form a gel;
(3) The gel was transferred to an oven at 60 ℃ and incubated for 12 hours, and then completely dried in an oven at 90 ℃. Grinding the dried gel to obtain precursor powder;
(4) Carrying out heat treatment on the precursor powder, wherein the heat treatment mode is as follows: heating to 600 ℃ at the speed of 3 ℃/min, then preserving heat for 1h, heating to 800 ℃ at the speed of 2 ℃/min, and preserving heat for 2h. Ball-milling the heat-treated powder in a planetary ball mill at the rotating speed of 400r/min for 1h, and sieving with a 2000-mesh sieve to obtain the lithium disilicate glass ceramic powder.
(5) Mixing lithium disilicate glass ceramic powder, octyl acrylate, polyethylene glycol 200 (molecular weight 200 g/mol) and light-cured resin according to the weight ratio of 8:0.2:0.8:1.5 to obtain slurry;
(6) Photocuring, printing and molding the slurry to obtain a dental bracket blank;
(7) Putting the dental bracket blank into a low-temperature ceramic furnace to carry out glue discharging treatment in the air, wherein the glue discharging mode is as follows: heating to 300 ℃ at a speed of 0.5 ℃/min, keeping the temperature for 1h, heating to 480 ℃ at a speed of 0.5 ℃/min, keeping the temperature for 2h, heating to 600 ℃ at a speed of 1 ℃/min, keeping the temperature for 1h, and cooling to finish the glue discharging process. And then, the bracket subjected to glue discharge is placed into a high-temperature furnace and sintered in the air, wherein the specific sintering mode is as follows: heating to 600 deg.C at 5 deg.C/min, maintaining for 1h, heating to 1000 deg.C at 2 deg.C/min, maintaining for 2h, and cooling to obtain the final product.
Example 4
(1) Respectively dissolving ethyl orthosilicate and lithium ethylate into ethanol to form 2mol/L and 0.82mol/L uniform transparent solutions, wherein the molar ratio of silicon to lithium is 1:1 mixing the two solutions and stirring for 12 hours at the rotating speed of 500r/min to obtain a uniform solution.
(2) Initiator (water: ethanol =2 (weight ratio), added in an amount of 3vol% of the solution volume) was added to form a gel;
(3) The gel was transferred to an oven at 60 ℃ and incubated for 12 hours, and then completely dried in an oven at 90 ℃. Grinding the dried gel to obtain precursor powder;
(4) Carrying out heat treatment on the precursor powder, wherein the heat treatment mode is as follows: heating to 600 ℃ at the speed of 3 ℃/min, then preserving heat for 1h, heating to 800 ℃ at the speed of 2 ℃/min, and preserving heat for 2h. Ball-milling the powder after heat treatment in a planetary ball mill for 1h at the rotating speed of 400r/min, and sieving the powder by a 2000-mesh sieve to obtain lithium disilicate glass ceramic powder;
(5) Mixing lithium disilicate glass ceramic powder, lauryl acrylate, polyethylene glycol 200 (molecular weight is 200 g/mol) and light-cured resin according to the weight ratio of 8:0.08:0.4:1.2, uniformly mixing to obtain slurry;
(6) Photocuring, printing and molding the slurry to obtain a dental bracket blank;
(7) Putting the dental bracket blank into a low-temperature ceramic furnace to carry out glue discharging treatment in the air, wherein the glue discharging mode is as follows: heating to 300 ℃ at the speed of 0.5 ℃/min, keeping the temperature for 1h, heating to 480 ℃ at the speed of 0.5 ℃/min, keeping the temperature for 2h, heating to 600 ℃ at the speed of 1 ℃/min, keeping the temperature for 1h, and cooling to finish the glue discharging process. And then, the bracket subjected to glue discharge is placed into a high-temperature furnace and sintered in the air, wherein the specific sintering mode is as follows: heating to 600 ℃ at the temperature of 5 ℃/min, preserving heat for 1h, heating to 1000 ℃ at the temperature of 2 ℃/min, preserving heat for 2h, and cooling to obtain the lithium disilicate glass ceramic dental bracket.
Example 5
(1) Respectively dissolving ethyl orthosilicate and lithium ethylate into ethanol to form uniform transparent solutions of 2mol/L and 0.82mol/L, wherein the molar ratio of silicon to lithium is 1:1 mixing the two solutions and stirring for 12 hours at the rotating speed of 500r/min to obtain a uniform solution.
(2) Initiator (water: ethanol =1 (weight ratio), added in an amount of 3vol% of the solution volume) was added to form a gel;
(3) The gel was transferred to an oven at 60 ℃ and incubated for 12 hours, and then completely dried in an oven at 90 ℃. Grinding the dried gel to obtain precursor powder;
(4) Carrying out heat treatment on the precursor powder, wherein the heat treatment mode is as follows: heating to 600 ℃ at the speed of 3 ℃/min, then preserving heat for 1h, heating to 800 ℃ at the speed of 2 ℃/min, and preserving heat for 2h. Ball-milling the heat-treated powder in a planetary ball mill at the rotating speed of 400r/min for 1h, and sieving with a 2000-mesh sieve to obtain lithium disilicate glass ceramic powder;
(5) Mixing lithium disilicate glass ceramic powder, lauryl acrylate, polyethylene glycol 200 (molecular weight is 200 g/mol) and light-cured resin according to the weight ratio of 8:0.08:0.4:1.2, uniformly mixing to obtain slurry;
(6) Photocuring, printing and molding the slurry to obtain a dental bracket blank;
(7) Putting the dental bracket blank into a low-temperature ceramic furnace to carry out glue discharging treatment in the air, wherein the glue discharging mode is as follows: heating to 300 ℃ at a speed of 0.5 ℃/min, keeping the temperature for 1h, heating to 480 ℃ at a speed of 0.5 ℃/min, keeping the temperature for 2h, heating to 600 ℃ at a speed of 1 ℃/min, keeping the temperature for 1h, and cooling to finish the glue discharging process. And then, the bracket subjected to glue discharging is placed into a high-temperature furnace and sintered in the air, wherein the specific sintering mode is as follows: heating to 600 ℃ at the temperature of 5 ℃/min, preserving heat for 1h, heating to 1000 ℃ at the temperature of 2 ℃/min, preserving heat for 2h, and cooling to obtain the lithium disilicate glass ceramic dental bracket.
Example 6
(1) Respectively dissolving ethyl orthosilicate and lithium ethylate into ethanol to form uniform transparent solutions of 2mol/L and 0.82mol/L, wherein the molar ratio of silicon to lithium is 1:1 mixing the two solutions and stirring for 12 hours at the rotating speed of 500r/min to obtain a uniform solution.
(2) Initiator (water: ethanol =1 (weight ratio), added in an amount of 3vol% of the solution volume) was added to form a gel;
(3) The gel was transferred to an oven at 60 ℃ and incubated for 12 hours, and then completely dried in an oven at 90 ℃. Grinding the dried gel to obtain precursor powder;
(4) Carrying out heat treatment on the precursor powder, wherein the heat treatment mode is as follows: heating to 600 ℃ at the speed of 3 ℃/min, then preserving heat for 1h, heating to 800 ℃ at the speed of 2 ℃/min, and preserving heat for 2h. Ball-milling the heat-treated powder in a planetary ball mill at the rotating speed of 400r/min for 1h, and sieving with a 2000-mesh sieve to obtain the lithium disilicate glass ceramic powder.
(5) Mixing lithium disilicate glass ceramic powder, lauryl acrylate, polyethylene glycol 1000 (molecular weight is 1000 g/mol) and light-cured resin according to the weight ratio of 8:0.08:0.4:1.2 to obtain slurry;
(6) Photocuring, printing and molding the slurry to obtain a dental bracket blank;
(7) Putting the dental bracket blank into a low-temperature ceramic furnace to carry out glue discharging treatment in the air, wherein the glue discharging mode is as follows: heating to 300 ℃ at the speed of 0.5 ℃/min, keeping the temperature for 1h, heating to 480 ℃ at the speed of 0.5 ℃/min, keeping the temperature for 2h, heating to 600 ℃ at the speed of 1 ℃/min, keeping the temperature for 1h, and cooling to finish the glue discharging process. And then, the bracket subjected to glue discharging is placed into a high-temperature furnace and sintered in the air, wherein the specific sintering mode is as follows: heating to 600 ℃ at the temperature of 5 ℃/min, preserving heat for 1h, heating to 1000 ℃ at the temperature of 2 ℃/min, preserving heat for 2h, and cooling to obtain the lithium disilicate glass ceramic dental bracket.
Example 7
(1) Respectively dissolving ethyl orthosilicate and tert-butyl lithium into ethanol to form 1mol/L and 0.5mol/L uniform transparent solutions, wherein the molar ratio of silicon to lithium is 1.2:1 mixing the two solutions and stirring for 8 hours at the rotating speed of 500r/min to obtain a uniform solution.
(2) Add (water: acetone =1 (weight ratio), in an amount of 5vol% of the solution volume) to form a gel;
(3) Transferring the gel to a 70 ℃ oven, preserving the heat for 24 hours, then completely drying the gel in a 120 ℃ oven, and grinding the dried gel to obtain precursor powder;
(4) Carrying out heat treatment on the precursor powder, wherein the heat treatment mode is as follows: heating to 500 ℃ at the speed of 1 ℃/min, then preserving heat for 2h, heating to 750 ℃ at the speed of 1 ℃/min, preserving heat for 3h, ball-milling and crushing the powder after heat treatment in a planetary ball mill at the rotating speed of 500r/min for 2h, and sieving by a screen of 1000 meshes to obtain the lithium disilicate glass ceramic powder.
(5) Mixing lithium disilicate glass ceramic powder, lauryl acrylate, polyethylene glycol 2000 (molecular weight 2000 g/mol) and light-cured resin according to the weight ratio of 6:0.05:0.3:1.1, uniformly mixing to obtain slurry;
(6) Photocuring, printing and molding the slurry to obtain a dental bracket blank;
(7) Putting the dental bracket blank into a low-temperature ceramic furnace to carry out glue discharging treatment in the air, wherein the glue discharging mode is as follows: heating to 240 ℃ at the speed of 1 ℃/min, preserving heat for 1h, heating to 380 ℃ at the speed of 1 ℃/min, preserving heat for 1h, heating to 470 ℃ at the speed of 0.5 ℃/min, preserving heat for 2h, heating to 600 ℃ at the speed of 1 ℃/min, preserving heat for 1h, and cooling to finish the glue discharging process. And then, the bracket subjected to glue removal is placed into a high-temperature furnace and sintered in vacuum, wherein the specific sintering mode is as follows: heating to 600 ℃ at the speed of 2 ℃/min, preserving heat for 1h, then heating to 1200 ℃ at the speed of 1 ℃/min, preserving heat for 2h, and cooling to obtain the lithium disilicate glass ceramic bracket.
Example 8
(1) Hexamethyldisiloxane and ethyl lithium are respectively dissolved in ethanol to form 3mol/L and 1mol/L of uniform transparent solution, and the molar ratio of silicon to lithium is 1:1 mixing the two solutions and stirring the mixture for 24 hours at the rotating speed of 800r/min to obtain a uniform solution.
(2) Adding (water: isopropanol =1 (weight ratio), added in an amount of 8vol% of the solution volume) to form a gel;
(3) Transferring the gel to a 50 ℃ oven, preserving the heat for 18 hours, then completely drying the gel in a 150 ℃ oven, and grinding the dried gel to obtain precursor powder;
(4) Carrying out heat treatment on the precursor powder, wherein the heat treatment mode is as follows: heating to 400 ℃ at the speed of 1 ℃/min, then preserving heat for 2h, heating to 600 ℃ at the speed of 1 ℃/min, then preserving heat for 2h, heating to 800 ℃ at the speed of 0.5 ℃/min, and preserving heat for 2h. Ball-milling the heat-treated powder in a planetary ball mill at the rotating speed of 300r/min for 4h, and sieving with a 3000-mesh sieve to obtain the lithium disilicate glass ceramic powder.
(5) Mixing lithium disilicate glass ceramic powder, lauryl acrylate, polyethylene glycol 1600 (molecular weight is 1600 g/mol) and light-cured resin according to the weight ratio of 7:0.05:0.25:0.9 to obtain slurry;
(6) Photocuring, printing and molding the slurry to obtain a dental bracket blank;
(7) Putting the dental bracket blank into a low-temperature ceramic furnace to carry out glue discharging treatment in the air, wherein the glue discharging mode is as follows: heating to 260 ℃ at a speed of 1 ℃/min, preserving heat for 0.5h, heating to 360 ℃ at a speed of 1 ℃/min, preserving heat for 2h, heating to 470 ℃ at a speed of 1 ℃/min, preserving heat for 2h, heating to 600 ℃ at a speed of 1 ℃/min, preserving heat for 2h, and cooling to finish the glue discharging process. And then, the bracket subjected to glue discharging is placed into a high-temperature furnace and sintered in a nitrogen atmosphere, wherein the specific sintering mode is as follows: heating to 600 ℃ at the speed of 2 ℃/min, preserving heat for 1h, heating to 1200 ℃ at the speed of 1 ℃/min, preserving heat for 2h, and cooling to obtain the lithium disilicate glass ceramic bracket.
The lithium disilicate glass ceramic brackets of examples 1 to 7 were tested as follows:
(1) Fracture toughness: measuring according to a GB/T23806-2009 fine ceramic fracture toughness test method-a unilateral pre-crack beam (SEPB) method;
(2) Hardness: the hardness is measured according to GB/T16534-2009-Fine ceramics room temperature hardness test method;
(3) Light transmittance: the transmittance of the translucent fine ceramic is measured according to JC/T2020-2010;
(4) And (3) measuring the printing yield: each embodiment prints 100 pieces of paper, and if the defects such as collapse, missing and the like occur in the printing process, the paper is counted as unqualified; observing the printed finished product after the glue is discharged, and if the finished product has a lamination crack, determining that the finished product is unqualified;
(5) And (3) determination of firing yield: 50 samples without macroscopic defects after glue discharging are collected and arranged in each example, and sintering and yield counting are carried out. Specifically, if cracking, deformation, or crushing occurs, the product is not qualified.
Specific test data are as follows:
while the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (10)
1. A preparation method of a lithium disilicate glass ceramic dental bracket is characterized by comprising the following steps:
(1) Lithium disilicate glass ceramic powder, acrylic ester, polyethylene glycol and light-cured resin are mixed according to the proportion of (4-8): (0.01-0.2): (0.05-0.8): (0.5-1.5) to obtain slurry;
(2) Photocuring, printing and molding the slurry to obtain a dental bracket blank;
(3) And (4) removing the glue from the bracket blank, and sintering to obtain a finished product of the lithium disilicate glass ceramic bracket.
2. The method for preparing a lithium disilicate glass-ceramic bracket according to claim 1, wherein the method for preparing the lithium disilicate glass-ceramic powder comprises:
1) Silicon source reagent and lithium source reagent are mixed according to the mol ratio of silicon to lithium (0.5-2): 1 in a dispersing agent to obtain a precursor solution;
2) Adding an initiator into the precursor liquid to convert the precursor liquid into gel liquid;
3) Drying and grinding the gel liquid to obtain precursor powder;
4) And (3) carrying out heat treatment on the precursor powder at 600-1000 ℃ for 0.5-10 h, cooling and grinding to obtain the finished product of the lithium disilicate glass ceramic powder, wherein the granularity of the product is less than or equal to 200 meshes.
3. The method for preparing a lithium disilicate glass-ceramic bracket according to claim 2, wherein the silicon source reagent is one or more selected from the group consisting of tetraethoxysilane, silicate, silica sol, hexamethyldisiloxane; the lithium source reagent is selected from alkyl lithium and/or alcohol-based lithium.
4. The method for preparing a lithium disilicate glass ceramic bracket according to claim 2, wherein the initiator is selected from one or more of water, polyvinyl alcohol, water-ethanol mixed solution, water-acetone mixed solution, water-isopropanol mixed solution and polyethylene glycol;
the dosage of the initiator is 0.1-10% of the volume of the precursor liquid.
5. The method for preparing a lithium disilicate glass ceramic bracket according to claim 2, wherein in the step 1), the silicon source reagent and the lithium source reagent are mixed in a molar ratio of silicon to lithium of (0.5-2): 1 in proportion, and stirring for 12-36 h at a stirring speed of 100-1000 rpm to obtain a precursor solution;
wherein the dispersant is water and/or ethanol.
6. The method for preparing a lithium disilicate glass ceramic bracket according to claim 1, wherein the acrylate is one or more selected from the group consisting of methyl acrylate, ethyl acrylate, octyl acrylate, lauryl acrylate, and 1, 6-hexanediol diacrylate;
the molecular weight of the polyethylene glycol is 200-2000 g/mol.
7. The method for preparing a lithium disilicate glass ceramic bracket according to claim 1, wherein the acrylate is lauryl acrylate.
8. The method for preparing a lithium disilicate glass ceramic bracket according to claim 7, wherein the molecular weight of the polyethylene glycol is 1000 to 2000g/mol.
9. The method for preparing a lithium disilicate glass-ceramic bracket according to claim 1, wherein the step (3) comprises:
(3.1) removing the glue of the dental bracket blank; wherein, the temperature curve that the binder removal adopted does: heating to 400-800 ℃ at the heating rate of 0.1-10 ℃/min, and keeping the temperature at 400-800 ℃ for 0.5-10 h;
(3.2) sintering the dental bracket blank after the glue is removed; wherein, the temperature curve that the sintering adopted is: heating to 800-1250 ℃ at the heating rate of 0.5-20 ℃/min, and preserving the heat for 0.5-10 h at the temperature of 800-1250 ℃.
10. A lithium disilicate glass-ceramic bracket prepared by the method for preparing a lithium disilicate glass-ceramic bracket according to any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210978005.6A CN115417600B (en) | 2022-08-16 | 2022-08-16 | Lithium disilicate glass ceramic bracket and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210978005.6A CN115417600B (en) | 2022-08-16 | 2022-08-16 | Lithium disilicate glass ceramic bracket and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115417600A true CN115417600A (en) | 2022-12-02 |
| CN115417600B CN115417600B (en) | 2024-05-31 |
Family
ID=84197680
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210978005.6A Active CN115417600B (en) | 2022-08-16 | 2022-08-16 | Lithium disilicate glass ceramic bracket and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115417600B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116375500A (en) * | 2023-03-28 | 2023-07-04 | 中国人民解放军空军军医大学 | Gradient zirconia and preparation method thereof |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170128174A1 (en) * | 2014-06-23 | 2017-05-11 | 3M Innovative Properties Company | Process for producing a sintered lithium disilicate glass ceramic dental restoration and kit of parts |
| CN106810215A (en) * | 2017-01-18 | 2017-06-09 | 深圳摩方新材科技有限公司 | A kind of preparation of ceramic size and 3D printing Stereolithography method |
| CN107353016A (en) * | 2017-06-16 | 2017-11-17 | 浙江大学 | The preparation method of hydroxyapatite and its application in 3D printing shaping |
| DE102017205432A1 (en) * | 2016-06-30 | 2018-01-04 | Institut für Bioprozess- und Analysenmesstechnik e.V. | Production of ceramic structures by means of multi-photon polymerization |
| CN109534681A (en) * | 2019-01-09 | 2019-03-29 | 福州大学 | A kind of preparation method of lithium bisilicate compound bio glass ceramics |
| CN109574657A (en) * | 2018-11-14 | 2019-04-05 | 上海交通大学医学院附属第九人民医院 | A method of dental zirconium oxide prosthesis is prepared based on Stereo Lithography Apparatus Rapid Prototyping technology |
| CN110511017A (en) * | 2019-07-31 | 2019-11-29 | 映维(苏州)数字科技有限公司 | A kind of preparation method of rapid photocuring high solids content ceramic slurry |
| CN110981203A (en) * | 2019-11-26 | 2020-04-10 | 中国科学院上海硅酸盐研究所 | High-strength lithium disilicate glass ceramic and preparation method and application thereof |
| CN114028240A (en) * | 2021-12-24 | 2022-02-11 | 深圳爱尔创口腔技术有限公司 | Lithium disilicate glass ceramic restoration and preparation method thereof |
| KR20220094487A (en) * | 2020-12-29 | 2022-07-06 | 주식회사 올덴솔루션 | Manufacturing method of dental prosthesis comprising lithium disilicate glass composition |
| CN114774002A (en) * | 2022-03-09 | 2022-07-22 | 张家港康得新光电材料有限公司 | Coating liquid, antireflection film and preparation method thereof |
-
2022
- 2022-08-16 CN CN202210978005.6A patent/CN115417600B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170128174A1 (en) * | 2014-06-23 | 2017-05-11 | 3M Innovative Properties Company | Process for producing a sintered lithium disilicate glass ceramic dental restoration and kit of parts |
| DE102017205432A1 (en) * | 2016-06-30 | 2018-01-04 | Institut für Bioprozess- und Analysenmesstechnik e.V. | Production of ceramic structures by means of multi-photon polymerization |
| CN106810215A (en) * | 2017-01-18 | 2017-06-09 | 深圳摩方新材科技有限公司 | A kind of preparation of ceramic size and 3D printing Stereolithography method |
| CN107353016A (en) * | 2017-06-16 | 2017-11-17 | 浙江大学 | The preparation method of hydroxyapatite and its application in 3D printing shaping |
| CN109574657A (en) * | 2018-11-14 | 2019-04-05 | 上海交通大学医学院附属第九人民医院 | A method of dental zirconium oxide prosthesis is prepared based on Stereo Lithography Apparatus Rapid Prototyping technology |
| CN109534681A (en) * | 2019-01-09 | 2019-03-29 | 福州大学 | A kind of preparation method of lithium bisilicate compound bio glass ceramics |
| CN110511017A (en) * | 2019-07-31 | 2019-11-29 | 映维(苏州)数字科技有限公司 | A kind of preparation method of rapid photocuring high solids content ceramic slurry |
| CN110981203A (en) * | 2019-11-26 | 2020-04-10 | 中国科学院上海硅酸盐研究所 | High-strength lithium disilicate glass ceramic and preparation method and application thereof |
| KR20220094487A (en) * | 2020-12-29 | 2022-07-06 | 주식회사 올덴솔루션 | Manufacturing method of dental prosthesis comprising lithium disilicate glass composition |
| CN114028240A (en) * | 2021-12-24 | 2022-02-11 | 深圳爱尔创口腔技术有限公司 | Lithium disilicate glass ceramic restoration and preparation method thereof |
| CN114774002A (en) * | 2022-03-09 | 2022-07-22 | 张家港康得新光电材料有限公司 | Coating liquid, antireflection film and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| FENG WANG等: "Sintering properties of sol–gel derived lithium disilicate glass ceramics", JOURNAL OF SOL-GEL SCIENCE AND TECHNOLOGY, vol. 87, no. 2, pages 372 - 379, XP036569438, DOI: 10.1007/s10971-018-4738-3 * |
| 罗绍华等: "《功能材料》", 东北大学出版社, pages: 320 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116375500A (en) * | 2023-03-28 | 2023-07-04 | 中国人民解放军空军军医大学 | Gradient zirconia and preparation method thereof |
| CN116375500B (en) * | 2023-03-28 | 2024-07-12 | 中国人民解放军空军军医大学 | Gradient zirconia and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115417600B (en) | 2024-05-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110590387A (en) | Inorganic fiber composite silicon-based ceramic core and preparation method thereof | |
| CN107721424B (en) | Method for preparing YAG transparent ceramic by gel casting | |
| CN108516818A (en) | A method of YAG crystalline ceramics is prepared based on improved Isobam gel rubber systems | |
| CN110342824B (en) | Low-loss low-thermal-expansion magnesium-aluminum-silicon-based microcrystalline glass material and preparation method thereof | |
| CN103803974A (en) | Injection molding zirconium oxide and preparation method for same | |
| CN111908797B (en) | Low-thermal-expansion cordierite-based microcrystalline glass material and preparation method thereof | |
| CN111233443A (en) | High-solid-content 3D printing ceramic core slurry and preparation method thereof | |
| CN109020523B (en) | Preparation method of low-iron ultra-white fused quartz ceramic crucible | |
| CN103896601A (en) | Hot pressed sintering method of ceramic products with high density and complex shapes | |
| CN102825649A (en) | Method for preparing MgAlON transparent ceramic bisque by gel casting and molding | |
| CN115417600A (en) | Lithium disilicate glass ceramic bracket and preparation method thereof | |
| CN109467419A (en) | A kind of graphene enhancing alumina based ceramic core and preparation method thereof | |
| CN103553339B (en) | Lithium bisilicate microcrystal glass material prepared by hybrid reaction sintering process and method thereof | |
| CN111270347A (en) | Method for preparing transparent ceramic optical fiber by gel injection molding | |
| CN107226695B (en) | A kind of easy milling zirconia ceramics and preparation method thereof | |
| CN108947257A (en) | A kind of cordierite-base microcrystal glass material and preparation method thereof | |
| CN108996998A (en) | A kind of composition and the method for preparing crystalline ceramics | |
| CN101407375B (en) | Material for repairing lithium-based ceramic oral cavity and preparation thereof | |
| CN103253867B (en) | A kind of molten state yellow phosphorus furnace slag prepares the Technology of devitrified glass | |
| CN104829221A (en) | Method for preparing Re:YAG transparent ceramic through gel injection mold forming | |
| CN102924077A (en) | Method for preparing large-size zinc-oxide based target by casting through novel low-toxicity gel | |
| CN100584795C (en) | Mullite nano crystallite ceramic product and preparation method thereof | |
| CN113880563B (en) | High-temperature creep-resistant ceramic material and preparation method thereof | |
| CN1015443B (en) | Microcrystal glass made from goose cord rock | |
| CN114890678B (en) | Large-size low-expansion glass-based composite material and slip casting method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |