CN107010945A - A kind of Zirconium oxide full-porcelain plants preparation - Google Patents

A kind of Zirconium oxide full-porcelain plants preparation Download PDF

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CN107010945A
CN107010945A CN201710335785.1A CN201710335785A CN107010945A CN 107010945 A CN107010945 A CN 107010945A CN 201710335785 A CN201710335785 A CN 201710335785A CN 107010945 A CN107010945 A CN 107010945A
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microwave
zirconium oxide
sintering
porcelain
slurry
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陈利祥
许申鸿
姜学军
陈欣言
马军艳
葛晓辉
武青
周旭波
徐韶鸿
石星军
孙光辉
刘华堂
李显辉
杜晓红
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Qingdao University
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Qingdao University
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    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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    • C04B35/632—Organic additives
    • C04B35/634—Polymers
    • C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63444—Nitrogen-containing polymers, e.g. polyacrylamides, polyacrylonitriles, polyvinylpyrrolidone [PVP], polyethylenimine [PEI]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2430/00—Materials or treatment for tissue regeneration
    • A61L2430/12—Materials or treatment for tissue regeneration for dental implants or prostheses
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Abstract

The invention belongs to new material tooth implant preparing technical field, it is related to a kind of Zirconium oxide full-porcelain plantation preparation, technical process is prepared including slurry, blank forming and microwave sintering totally three steps, CAD/CAM is utilized by zirconium oxide transformation toughening using nanoscale zirconia, cold conditions isostatic pressing method and microwave sintering process processing and fabricating tooth implant, sintering only needs surface polishing to can be used after finishing, improve the biocompatibility of tooth implant and dummy, rupture strength, fracture toughness, translucency, marginal and aesthetic effect, shorten clinical repair treatment time, reduce medical expense, reach the top standard of international similar technique, at home, outer popularization and application, bring benefit to the mankind；Its scientific in principle rationally, strong operability, energy consumption is low, small investment, high yield rate, cost are low, and life cycle is long, it is up to standard after can apply for that production is permitted, batch production, clinical application prospect is good.

Description

A kind of Zirconium oxide full-porcelain plants preparation
Technical field：
The invention belongs to new material tooth implant preparing technical field, it is related to a kind of Zirconium oxide full-porcelain planting body preparation side Method, prepares the Zirconium oxide full-porcelain planting body with high reliability, intensity and toughness and low cost, with alternative metals material The planting body of tooth-implanting.
Background technology：
Defect of dentition, missing are department of stomatology common disease frequently-occurring diseases, and restorative procedure mainly has removable denture, fixed denture and tooth Plantation；The development of Dental implantion had both indicated the progress of dentistry, also reflects the hair of the subjects such as biology, chemistry and materialogy Exhibition, is the crystallization that related discipline is interpenetrated, merged；The generation and development of Dental implantion represent people to stomatological aesthetics and function The pursuit of recovery；From 1960s so far, various implant systems used in modern Dental implantion are that Titanium is made, by Aesthetic effect is influenceed in the opaqueness of metal base station；It is a kind of hydrophily disclosed in Chinese patent 201610993456.1, anti- Bacterium dental implant system and preparation method thereof, by carrying out plasma oxidation surface modification treatment to implant system, is prepared Go out the surface with hydrophily, antibacterial characteristics, with the hydrophily of solution storage or the method holding surface of plasma clean or Person recovers the hydrophily on surface；The tooth implant of a kind of individuation bionic disclosed in Chinese patent 201610705564.4 and Its preparation method includes the planting body body of the original root of the tooth institutional framework of imitative patient's missing tooth, is combined with planting body body outer surface The biomimetic prosthetic alveolar bone structural outside layers for the imitative patient's alveolar bone tissue structure being integrated, and in outer layer with bioprotein point Son -- bone morphogenic protein BMP-2, due to integrally printing planting body body and biomimetic prosthetic alveolar bone structural outside layers using 3D, with The original root of the tooth of patient's missing tooth and alveolar bone tissue structure are close, and with the addition of the biology for promoting the BMP of quick bon e formation to modify Protein molecule；A kind of preparation side of tooth implant available for diabetic disclosed in Chinese patent 201510300710.0 Method comprises the following steps：Amino catechol compound, organic cation antiseptic and cushioning liquid are mixed, impregnated Solution, tooth implant body is put into dipping solution, and 12-36h, the tooth implant impregnated, with nothing are impregnated at 18-37 DEG C Water-ethanol and deionized water carry out supersound washing to the tooth implant of dipping, and drying at room temperature is obtained available for diabetic's Tooth implant；A kind of preparation method of dentistry implant and its composite surface disclosed in Chinese patent 201610346507.1, with Medical titanium or titanium alloy are base material, prepare porous pattern on its surface and deposit poly-dopamine and hydroxyapatite, are had Have the dentistry implant composite surface of excellent bioactivity, titanium substrate surface quickly formed the poroid oxide-film of uniform multilayer with Nanoporous pattern is obtained, and in surface tight adhesion albumen analog (poly-dopamine) one layer thin, final spatial induction sinks Product hydroxyapatite obtains three layers of composite surface；A kind of dental implant materials disclosed in Chinese patent 201610504547.4 and its Preparation method comprises the following steps：(1) by zirconium powder, zirconium dioxide, boron powder, aluminium powder, titanium sponge, potassium titanate, tin oxide and the third three Alcohol is mixed, and is ground 2-3 hour with grinder, and (2) are washed with deionized water only, filter, and (3) are put into baking oven in 80-100 DEG C of temperature Lower drying, (4) cross 200 mesh sieves, remove bulky grain, and (5) add nano titanium oxide, polyurethanes, polydimethylsiloxanes Alkane, polyethylene glycol and polyvinyl alcohol, high-speed stirred 5-10 minutes, (6) are put into stove, are vacuumized, and carry out melting, (7) remelting is again Refine 3-5 times and produce；Recently, research is found, the metal material in tooth implant, which can gradually permeate and stimulate body to produce, to be immunized instead Should, show as blood lymphocyte and increase, the metal positioned at oral cavity (outside jawbone) can also produce influence (puppet to magnetic resonance, CT examination Shadow).Therefore, a kind of Zirconium oxide full-porcelain plantation preparation of R ＆ D design, Dental implantion is prepared using zirconium oxide alternative metals Body, can not only avoid metal material to the harmful effect of body but also can improve the aesthetic orthopaedics effect of Dental implantion, the full porcelain of zirconium oxide Material will not also cause allergy and abnormal metabolism, also without hindrance to x-ray to penetrate, and be adapted to the tooth structure of compatriots.
The content of the invention：
It is an object of the invention to overcome the shortcoming that prior art is present, seek to design a kind of Zirconium oxide full-porcelain planting body Preparation method, tooth implant is prepared using zirconium oxide alternative metals, before avoiding metal material dysgenic to body generation Put, reduce production cost, improve the aesthetic orthopaedics effect of Dental implantion.
To achieve these goals, the technical process of Zirconium oxide full-porcelain plantation preparation of the present invention includes Prepared by slurry, blank forming and microwave sintering totally three steps：
(1), prepared by slurry：By acrylamide monomer and N, N ' methylene-bisacrylamides are according to 17:1 mass ratio is mixed Conjunction prepares mixture, then by mixture and water according to 18：85 mass ratio, which is mixed with, obtains pre-mixing liquor, in pre-mixing liquor Add the dispersant of 0.5% mass fraction, purity and be more than 99% and powdery 3Y-TZP of the granularity less than 20nm, being configured to pH value is 9.5th, solid volume fraction is more than 60% suspended substance, and suspended substance obtains viscosity after being mixed 10 hours through ball mill and is less than 200mPa.S aqueous systems ceramic slurry, mass percent of the mixture in aqueous systems ceramic slurry is 3%, completes slurry Prepare；
(2), blank forming：Slurry is carried out after application of vacuum using Gelcasting Technique, added in the slurry 1% mass percent initiator and 0.5% percent by volume catalyst formation mixture, by mixture at the uniform velocity be poured into mould Middle carry out gelation, is then stripped and is dried, and completes the shaping of base substrate；(3), microwave sintering：Base substrate is put into microwave to burn In the microwave sintering chamber for tying device, according to the heating curve of setting, base substrate is sintered.
Dispersant of the present invention is the ammonium polymethacrylate solution that mass percent concentration is 5%；Initiator is Mass percent concentration is 5% ammonium persulfate aqueous solution；Catalyst is the tetramethylethylenediamine that mass percent concentration is 5% The aqueous solution.
Yttria levels in Zirconium oxide full-porcelain planting body of the present invention are 3%mol, zirconium oxide tooth-implanting base station Density be 6.05 gram per centimeters3, hardness is 12.22GPa, and bending strength is 936.32MPa, and fracture toughness is 12.56Mpam1 /2。
The agent structure of microwave sintering device of the present invention include magnetron, microwave power supply, circulator, water load, Four tuners, heating chamber, load, antenna array, swinging mounting and pallet；It is provided with the microwave power supply and circulator of magnetron Left end duct type is connected, and the lower end of circulator is provided with the left end duct type of water load, the right-hand member of circulator and four tuners Connection, the right-hand member of four tuners is connected with the heating chamber duct type right angle of hollow type rectangular configuration, is provided with load heating chamber Top be provided with antenna array, the bottom of heating chamber is provided with swinging mounting, and the top of swinging mounting is provided with circular plate-like shape knot The pallet of structure；The microwave frequency of magnetron is 2.45GHZ；The peak power output of microwave power supply is 5KW；Circulator is used for The back wave of load is sent into water load, it is returned to magnetron, to protect magnetron；Water load is used to absorb circulator The back wave of feeding；The back wave that four tuners are used to control heating chamber to make load is minimum；The material of heating chamber is stainless steel； Antenna array is used for converging microwave and microwave is smoothly entered heating chamber；Swinging mounting is used to rotate and support pallet, pallet is existed Moved in a circle under the drive of swinging mounting；Pallet is used to carry the article being sintered.
Gelcasting Technique of the present invention, is suitable for large-scale production, it is possible to increase yield rate and finished product can By property, manufacturing cost is significantly reduced, the aggregate of ceramic powder particle is eliminated, the change of complicated form part in sintering process is reduced Shape and cracking, reduce the amount of machining of final products, obtain the ceramic material and part of high reliability；The green density of preparation and Intensity is high, uniformity is good, and appearance and size is not fixed；Microwave sintering device is by microwave energy by converging day line traffic control in certain space In the range of, increase heated perimeter and energy will be uniformly distributed, realize ceramic material serialization microwave sintering, and can be burnt with conventional Tie equipment to be used in combination, microwave sintering combination normal sintering can make up the warming temperature gradient that normal sintering leans on heat transfer to heat Greatly, material is heated uneven, heat time length and the big shortcoming of power consumption, while avoid ceramic material absorbs microwave in low temperature Can be poor the problem of.
The present invention compared with prior art, uses nanoscale zirconia to make Zirconium oxide full-porcelain planting body for raw material, The rupture strength of base station is set to reach 1200Mpa by zirconium oxide transformation toughening, fracture toughness reaches 10Mpa*m1/2More than, use CAD/CAM, cold conditions isostatic pressing method and microwave sintering process processing and fabricating precision highest and the minimum tooth implant of work difference And dummy, meet tooth biological requirement and close to natural teeth mechanical strength, sintering only needs surface to polish after finishing Use, it is to avoid the attrition process process after sintering, with intensity is high, wearability is good, preferably, coefficient of friction is small, chi for polishability Very little stability is good and the characteristics of good self-lubricating property, meanwhile, biocompatibility, the anti-folding for improving tooth implant and dummy are strong Degree, fracture toughness, translucency, marginal and aesthetic effect, shorten clinical repair treatment time, reduce medical expense, reach To the top standard of international similar technique, at home, outer popularization and application, bring benefit to the mankind；Its scientific in principle is rationally, operational By force, energy consumption is low, small investment, high yield rate, cost are low, and life cycle is long, it is up to standard after can apply for that production is permitted, batch is raw Production, clinical application prospect is good.
Brief description of the drawings：
Fig. 1 is process flow diagram of the invention.
Fig. 2 is the agent structure principle schematic of microwave sintering device of the present invention.
Fig. 3 is the agent structure schematic diagram of Zirconium oxide full-porcelain planting body of the present invention.
Fig. 4 is the cross-sectional view of Zirconium oxide full-porcelain planting body of the present invention.
Embodiment：
Below by embodiment and the invention will be further described with reference to accompanying drawing.
Embodiment 1：
The technical process of Zirconium oxide full-porcelain manufactured in the present embodiment plantation preparation include slurry prepare, base substrate into Type and microwave sintering totally three steps：
(1), prepared by slurry：By acrylamide monomer and N, N ' methylene-bisacrylamides are according to 17:1 mass ratio is mixed Conjunction prepares mixture, then by mixture and water according to 18：85 mass ratio, which is mixed with, obtains pre-mixing liquor, in pre-mixing liquor Add the dispersant of 0.5% mass fraction, purity and be more than 99% and powdery 3Y-TZP of the granularity less than 20nm, being configured to pH value is 9.5th, solid volume fraction is more than 60% suspended substance, and suspended substance obtains viscosity after being crushed 10 hours through ball mill and is less than 200mPa.S aqueous systems ceramic slurry, mass percent of the mixture in aqueous systems ceramic slurry is 3%, completes slurry Prepare；
(2), blank forming：Slurry is carried out after application of vacuum using Gelcasting Technique, added in the slurry 1% mass percent initiator and 0.5% percent by volume catalyst formation mixture, by mixture at the uniform velocity be poured into mould Middle carry out gelation, is then stripped and is dried, and completes the shaping of base substrate；(3), microwave sintering：Base substrate is put into microwave to burn In the microwave sintering chamber for tying device, according to the heating curve of setting, base substrate is sintered.
The dispersant that the present embodiment is related to is the ammonium polymethacrylate solution (PMAA- that mass percent concentration is 5% NH4)；Initiator is the ammonium persulfate aqueous solution that mass percent concentration is 5%；Catalyst is that mass percent concentration is 5% The tetramethylethylenediamine aqueous solution.
Yttria levels in Zirconium oxide full-porcelain planting body manufactured in the present embodiment are 3%mol, zirconium oxide tooth-implanting base The density of platform is 6.05 gram per centimeters3, hardness is 12.22GPa, and bending strength is 936.32MPa, and fracture toughness is 12.56Mpam1/2。
The agent structure for the microwave sintering device that the present embodiment is related to includes magnetron 1, microwave power supply 2, circulator 3, water Load 4, four tuners 5, heating chamber 6, load 7, antenna array 8, swinging mounting 9 and pallet 10；It is provided with the microwave of magnetron 1 Power supply 2 is connected with the left end duct type of circulator 3, and the lower end of circulator 3 is provided with water load 4, the right-hand member of circulator 3 and four The left end duct type connection of tuner 5, the right-hand member of four tuners 5 and the duct type right angle of heating chamber 6 of hollow type rectangular configuration Connection, the top for being provided with 7 heating chambers 6 of load is provided with antenna array 8, and the bottom of heating chamber 6 is provided with swinging mounting 9, rotates The top of support 9 is provided with the pallet 10 of circular plate-like shape structure；The microwave frequency that magnetron 1 is launched is 2.45GHZ；Microwave power supply 2 peak power output is 5KW；Circulator 3 is used to the back wave for loading 7 sending into water load 4, it is returned to magnetron 1, to protect magnetron 1；Water load 4 is used for the back wave for absorbing the feeding of circulator 3；Four tuners 5 are used to control heating chamber 6 Make the back wave of load 7 minimum；The material of heating chamber 6 is stainless steel；Antenna array 8 is used for converging microwave and microwave is smoothly entered Heating chamber 6；Swinging mounting 9 is used to rotate and support pallet 10, pallet 10 is moved in a circle under the drive of swinging mounting 9； Pallet 10 is used to carry the article being sintered.
The Gelcasting Technique that the present embodiment is related to, is suitable for large-scale production, it is possible to increase yield rate and finished product Reliability, significantly reduces manufacturing cost, eliminates the aggregate of ceramic powder particle, reduces complicated form part in sintering process Deformation and cracking, reduce the amount of machining of final products, obtain the ceramic material and part of high reliability；The green density of preparation Good with intensity height, uniformity, appearance and size is not fixed；Microwave sintering device is by microwave energy by converging day line traffic control certain empty Between in the range of, increasing heated perimeter simultaneously will be uniformly distributed energy, realize ceramic material serialization microwave sintering, and can and it is conventional Agglomerating plant is used in combination, and microwave sintering combination normal sintering can make up the heating-up temperature ladder that normal sintering is heated by heat transfer Uneven, heat time length that degree is big, material is heated and the big shortcoming of power consumption, while avoid ceramic material absorbs micro- in low temperature The problem of wave energy is poor.

Claims (5)

1. a kind of Zirconium oxide full-porcelain plants preparation, it is characterised in that technical process includes slurry preparation, blank forming With microwave sintering totally three steps：
(1), prepared by slurry：By acrylamide monomer and N, N ' methylene-bisacrylamides are according to 17:1 mass ratio mixing system It is standby to obtain mixture, then by mixture and water according to 18：85 mass ratio, which is mixed with, obtains pre-mixing liquor, is added in pre-mixing liquor The dispersant of 0.5% mass fraction, purity be more than 99% and granularity be less than 20nm powdery 3Y-TZP, be configured to pH value for 9.5, Solid volume fraction is more than 60% suspended substance, and suspended substance obtains viscosity and is less than 200mPa.S's after being mixed 10 hours through ball mill Aqueous systems ceramic slurry, mass percent of the mixture in aqueous systems ceramic slurry is 3%, completes the preparation of slurry；
(2), blank forming：Slurry is carried out after application of vacuum using Gelcasting Technique, 1% matter is added in the slurry Measure percentage initiator and 0.5% percent by volume catalyst formation mixture, by mixture at the uniform velocity be poured into mould Row gelation, is then stripped and is dried, and completes the shaping of base substrate；
(3), microwave sintering：Base substrate is put into the microwave sintering chamber of microwave sintering device, it is right according to the heating curve of setting Base substrate is sintered.
2. Zirconium oxide full-porcelain according to claim 1 plants preparation, it is characterised in that the dispersant is matter Measure the ammonium polymethacrylate solution that percent concentration is 5%；Initiator is the ammonium persulfate water that mass percent concentration is 5% Solution；Catalyst is the tetramethylethylenediamine aqueous solution that mass percent concentration is 5%.
3. Zirconium oxide full-porcelain according to claim 1 plants preparation, it is characterised in that the full porcelain of zirconium oxide Yttria levels in tooth implant are 3%mol, and the density of zirconium oxide tooth-implanting base station is 6.05 gram per centimeters3, hardness is 12.22GPa, bending strength is 936.32MPa, and fracture toughness is 12.56Mpam1/2。
4. Zirconium oxide full-porcelain according to claim 1 plants preparation, it is characterised in that the microwave sintering dress The agent structure put include magnetron, microwave power supply, circulator, water load, four tuners, heating chamber, load, antenna array, Swinging mounting and pallet；The left end duct type of the microwave power supply and circulator that are provided with magnetron is connected, and the lower end of circulator is set Water load is equipped with, the right-hand member of circulator is connected with the left end duct type of four tuners, the right-hand member and hollow type of four tuners The heating chamber duct type right angle connection of rectangular configuration, the top for being provided with load heating chamber is provided with antenna array, the bottom of heating chamber End is provided with swinging mounting, and the top of swinging mounting is provided with the pallet of circular plate-like shape structure；The microwave frequency of magnetron For 2.45GHZ；The peak power output of microwave power supply is 5KW；Circulator is used to the back wave of load sending into water load, makes it Magnetron will not be returned to, to protect magnetron；Water load is used for the back wave for absorbing circulator feeding；Four tuners are used to control Heating chamber processed makes the back wave of load minimum；The material of heating chamber is stainless steel；Antenna array is used for converging microwave and makes microwave suitable Profit enters heating chamber；Swinging mounting is used to rotate and support pallet, pallet is moved in a circle under the drive of swinging mounting；Support Disk is used to carry the article being sintered.
5. Zirconium oxide full-porcelain according to claim 1 plants preparation, it is characterised in that the gel injection-moulding into Type technology, is suitable for large-scale production, it is possible to increase yield rate and finished product reliability, significantly reduces manufacturing cost, eliminates ceramics The aggregate of powder granule, reduces the deformation of complicated form part and cracking in sintering process, reduces the machining of final products Amount, obtains the ceramic material and part of high reliability；The green density and intensity of preparation are high, uniformity is good, and appearance and size is not solid It is fixed；Microwave energy by converging day line traffic control in the range of certain space, is increased heated perimeter and by uniformly by microwave sintering device Distribution energy, realizes ceramic material serialization microwave sintering, and can be used in combination with normal sintering equipment, and microwave sintering is combined Normal sintering can make up normal sintering by heat transfer heat warming temperature gradient is big, material is heated the uneven, heat time The long and big shortcoming that consumes energy, while avoiding ceramic material absorbs the problem of microwave energy is poor in low temperature.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107986777A (en) * 2017-11-08 2018-05-04 中南大学 One zirconia ceramic matrix composite and preparation method thereof
CN109095921A (en) * 2018-10-31 2018-12-28 北京安颂科技有限公司 A kind of zirconia ceramics bone implant prosthese and preparation method thereof
CN109336592A (en) * 2018-10-31 2019-02-15 北京安颂科技有限公司 A kind of zirconia ceramics bone implant prosthese and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10332802A1 (en) * 2002-07-19 2004-03-11 Mediceram Chirurgische Implantate Gmbh Production of an oxide ceramic structure used in the production of denture or bone replacement in humans and animals comprises virtually constructing the structure as three-dimensional computer model in computer-aided design arrangement
CN101347385A (en) * 2008-09-02 2009-01-21 沈阳爱尔创新材料有限公司 Zirconia ceramic dentistry repair body ceramic block without presintering and method for producing the same
CN105338948A (en) * 2013-06-27 2016-02-17 义获嘉伟瓦登特股份有限公司 Nanocrystalline zirconia and methods of processing thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10332802A1 (en) * 2002-07-19 2004-03-11 Mediceram Chirurgische Implantate Gmbh Production of an oxide ceramic structure used in the production of denture or bone replacement in humans and animals comprises virtually constructing the structure as three-dimensional computer model in computer-aided design arrangement
CN101347385A (en) * 2008-09-02 2009-01-21 沈阳爱尔创新材料有限公司 Zirconia ceramic dentistry repair body ceramic block without presintering and method for producing the same
CN105338948A (en) * 2013-06-27 2016-02-17 义获嘉伟瓦登特股份有限公司 Nanocrystalline zirconia and methods of processing thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
肖奇等: "《无机材料热工基础》", 31 January 2010, 冶金工业出版社 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107986777A (en) * 2017-11-08 2018-05-04 中南大学 One zirconia ceramic matrix composite and preparation method thereof
CN109095921A (en) * 2018-10-31 2018-12-28 北京安颂科技有限公司 A kind of zirconia ceramics bone implant prosthese and preparation method thereof
CN109336592A (en) * 2018-10-31 2019-02-15 北京安颂科技有限公司 A kind of zirconia ceramics bone implant prosthese and preparation method thereof
CN109336592B (en) * 2018-10-31 2021-05-25 北京安颂科技有限公司 Zirconia ceramic bone implantation prosthesis and preparation method thereof

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