CN114075071A - Preparation method of zirconia ceramic and ceramic scalpel - Google Patents
Preparation method of zirconia ceramic and ceramic scalpel Download PDFInfo
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- CN114075071A CN114075071A CN202010833921.1A CN202010833921A CN114075071A CN 114075071 A CN114075071 A CN 114075071A CN 202010833921 A CN202010833921 A CN 202010833921A CN 114075071 A CN114075071 A CN 114075071A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 112
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 24
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims abstract description 20
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000498 ball milling Methods 0.000 claims abstract description 17
- 239000002245 particle Substances 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 15
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 14
- 238000005238 degreasing Methods 0.000 claims abstract description 14
- 238000000462 isostatic pressing Methods 0.000 claims abstract description 14
- 238000010030 laminating Methods 0.000 claims abstract description 14
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 14
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 12
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000000853 adhesive Substances 0.000 claims abstract description 8
- 230000001070 adhesive effect Effects 0.000 claims abstract description 8
- 238000010345 tape casting Methods 0.000 claims abstract description 6
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 46
- 239000011268 mixed slurry Substances 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 7
- 238000005498 polishing Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 229920000058 polyacrylate Polymers 0.000 claims description 5
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 14
- 230000032683 aging Effects 0.000 abstract description 9
- 229910001404 rare earth metal oxide Inorganic materials 0.000 abstract description 7
- 239000003381 stabilizer Substances 0.000 abstract description 6
- 230000003993 interaction Effects 0.000 abstract description 4
- 238000005266 casting Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 6
- 238000010304 firing Methods 0.000 description 5
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 5
- 229910052727 yttrium Inorganic materials 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000003712 anti-aging effect Effects 0.000 description 3
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- 231100000241 scar Toxicity 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000001356 surgical procedure Methods 0.000 description 3
- 208000032544 Cicatrix Diseases 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- 229910000734 martensite Inorganic materials 0.000 description 2
- 239000011224 oxide ceramic Substances 0.000 description 2
- 230000037387 scars Effects 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003462 bioceramic Substances 0.000 description 1
- 238000013130 cardiovascular surgery Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000002316 cosmetic surgery Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000002682 general surgery Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
- 230000000399 orthopedic effect Effects 0.000 description 1
- 230000019612 pigmentation Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B17/00—Surgical instruments, devices or methods, e.g. tourniquets
- A61B17/32—Surgical cutting instruments
- A61B17/3209—Incision instruments
- A61B17/3211—Surgical scalpels, knives; Accessories therefor
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- 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
- C04B35/63—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 using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/638—Removal thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3229—Cerium oxides or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6025—Tape casting, e.g. with a doctor blade
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- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
The application discloses a zirconia ceramic, which comprises zirconia, ceria and yttria, wherein the mass percent of zirconia is 90-92 mol.%, the mass percent of ceria is 5-6.5 mol.%, and the mass percent of yttria is 2-4 mol.%. The application also discloses a preparation method of the ceramic scalpel, which comprises the steps of ball milling, mixing and stirring with an adhesive, defoaming, tape casting, laminating, isostatic pressing, degreasing and sintering through the mixed particles of zirconium oxide, cerium oxide and yttrium oxide. The zirconia ceramic and ceramic scalpel takes zirconia as a base material, and rare earth oxide yttrium oxide and cerium oxide are added, so that the zirconia base material can obtain higher toughness and hardness, has excellent mechanical properties, and optimizes the properties of the material in other aspects such as ageing resistance, phase stability and the like through the interaction of a multi-element stabilizer.
Description
Technical Field
The application relates to the technical field of ceramic composite materials and preparation thereof, in particular to a preparation method of zirconia ceramics and a ceramic scalpel.
Background
The existing scalpels or scissors are made of stainless steel materials, and doctors and patients are familiar with the materials, but the doctors and the patients are not aware of the defects of the existing scalpels or scissors. The metal knife is the main culprit of scars, the incision of the metal knife is sawtooth-shaped, although the incision is difficult to distinguish by naked eyes, the wound is slow to heal and easy to scar, and metal diffusion substances exist to pollute the wound and generate pigmentation. Even the disposable steel knife can be used for dozens of times by the current cosmetologist, and the sharpness of the knife can be thought. Therefore, existing steel scalpels and scissors have not been adequate for the needs of the surgery.
Because the metal knife has metal diffusion, the wound is easily polluted, and the limited sharpness of the cutting edge of the metal knife has jagged incision, although the metal knife cannot be seen by human eyes, the wound is slow to recover and easily scars are left in reality.
Since bioceramics have good biocompatibility and osteoconductivity, they can exhibit good affinity with biological tissues such as cells, and have been used in many fields such as orthopedics, plastic surgery, dentistry, oral surgery, cardiovascular surgery, ophthalmic surgery, otolaryngology, and general surgery.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a zirconia ceramic.
In order to achieve the purpose, the invention adopts the following technical scheme:
a zirconia ceramic comprising zirconia, ceria, and yttria, wherein the zirconia is present in an amount of 90 to 92 mol.%, the ceria is present in an amount of 5 to 6.5 mol.%, and the yttria is present in an amount of 2 to 4 mol.%.
Preferably, the mass percent of zirconia is 91 mol.%, the mass percent of yttria is 3 mol.%, and the mass percent of ceria is 5.5 mol.%.
Preferably, the composite material also comprises lanthanum oxide, and the mass percentage of the lanthanum oxide is 0-2 mol.%.
Preferably, the mass percent of lanthanum oxide is 0.5 mol.%.
The zirconia ceramic of the invention takes zirconia as a basic material, and rare earth oxide yttrium oxide and cerium oxide are added, so that the zirconia-based material can obtain higher toughness and hardness, has excellent mechanical properties, and optimizes the properties of the material in other aspects such as ageing resistance, phase stability and the like through the interaction of a multi-element stabilizer. In addition, a small amount of lanthanum oxide is introduced to serve as a preferred component, so that the toughening effect and a certain anti-aging effect are further enhanced.
The invention also aims to provide a preparation method of the ceramic scalpel.
A preparation method of a ceramic scalpel comprises the following steps:
step a, performing ball milling treatment on the zirconia ceramic particles in any one of the schemes;
b, mixing and stirring the mixed particles subjected to ball milling in the step a and an adhesive, and removing bubbles to obtain mixed slurry;
step c, carrying out tape casting treatment on the mixed slurry obtained in the step b to obtain a green sheet of the ceramic scalpel;
d, laminating and isostatic pressing the ceramic scalpel green sheet obtained in the step c to obtain a ceramic scalpel green sheet;
and e, degreasing and sintering the ceramic scalpel green body obtained in the step d to obtain the ceramic scalpel.
Preferably, the sintering in the step e is to move the ceramic scalpel green body into a kiln, fire the ceramic scalpel green body for 20-40 min at 450-550 ℃, then raise the temperature in the kiln to 1450-1500 ℃, and sinter the ceramic scalpel green body again at high temperature.
Preferably, the method further comprises the step f: and e, performing fine grinding and surface polishing treatment on the blade of the ceramic scalpel obtained in the step e.
Preferably, the binder in step b is one or more of polyacrylate, polyvinyl alcohol and carboxymethyl cellulose.
According to the preparation method of the ceramic scalpel, the ceramic scalpel with excellent mechanical property, ageing resistance and high stability is obtained by performing ball milling on the mixed particles of the rare earth oxide, mixing and stirring with the adhesive, defoaming, tape casting, laminating, isostatic pressing, degreasing and sintering.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is 2 mol.% Y of the present invention2O3-x CeO2Vickers hardness and fracture toughness maps of (a);
FIG. 2 is 2 mol.% Y of the present invention2O3-x CeO2Vickers hardness and fracture toughness maps of (a);
FIG. 3 is 3 mol.% Y of the present invention2O3-x CeO2Vickers hardness and fracture toughness maps of (a);
FIG. 4 is 4 mol.% Y of the present invention2O3-x CeO2Vickers hardness and fracture toughness maps of (a);
FIG. 5 is 2 mol.% Y of the present invention2O3-5.5mol.%CeO2XRD patterns after roasting treatment at different temperatures;
FIG. 6 is a photograph of a green ceramic scalpel according to a first embodiment of the present invention;
fig. 7 is a photograph of a sintered sample of a ceramic scalpel according to a first embodiment of the present invention.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to fig. 1 to 7, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The zirconia ceramic comprises zirconia, ceria, yttria and lanthana, wherein the mass percent of zirconia is 90-92 mol.%, the mass percent of ceria is 5-6.5 mol.%, the mass percent of yttria is 2-4 mol.%, and the mass percent of lanthana is 0-2 mol.%.
Preferably, the mass percent of zirconia is 91 mol.%, the mass percent of ceria is 5.5 mol.%, the mass percent of yttria is 3 mol.%, and the mass percent of lanthana is 0.5 mol.%.
As shown in FIGS. 1 to 5, the rare earth oxide cerium oxide (CeO) was determined based on the comprehensive use conditions and target properties of the products of the comprehensive projects2) Yttrium oxide (Y)2O3) Lanthanum oxide (La)2O3) Is a basic ingredient scheme of a basic crystal form stabilizer. On one hand, the zirconia-based material can obtain higher toughness and hardness to meet the application requirements, and on the other hand, the material can also obtain the performance meeting the use requirements in other aspects such as ageing resistance, phase stability and the like through the interaction of the multi-element stabilizer. The multi-element rare earth oxide co-stabilization target material is prepared by regulating and controlling the combination and collocation of the rare earth stabilizers. On the basis of excellent mechanical and mechanical properties of yttria-stabilized zirconia, cerium oxide and trace lanthanum oxide are introduced to improve the hydrothermal aging resistance of zirconia ceramic and further improve the metastable t-phase stability. Determined in 2 mol.% Y2O35.5mol.%CeO2A small amount of lanthanum oxide is introduced into the basic cutter component in a proper amount.
Further, yttrium oxide (Y)2O3) Has obvious effect on stabilizing the performance of the zirconium oxide and can lead t-ZrO to be2To m-ZrO2The phase transition temperature of the zirconium oxide ceramic is reduced from 1170 ℃ to room temperature, so that the zirconium oxide ceramic is mainly tetragonal phase at room temperature, when the periphery of the crack is extruded by compressive stress, the tetragonal phase is induced to be transformed into monoclinic phase and accompanied with 5% volume expansion, and the effect of phase transition toughening is achieved. However, this phase change may also occur within the ceramic, leading to degradation of the ceramic, and another disadvantage of yttria-stabilized zirconia ceramics is their low density, which is typically maintained below 95%. In order to overcome the aging phenomenon of zirconia, cerium oxide is doped on the basis of yttria-stabilized zirconia. The results of the previous studies show that cerium oxide has no great influence on the sintering properties of yttria-stabilized zirconia-based ceramics, and that the stable tetragonal phase follows oxygenThe content of yttrium oxide and cerium oxide increases. The yttria dispersed in the ceria and zirconia can improve the hardness of the zirconia ceramic and increases with the amount of yttria. As shown in fig. 2, cerium oxide may maximize fracture toughness in a certain range and then show a decreasing tendency as the content increases, and when the content of yttrium oxide is more than 3 mol%, the toughening effect is not significant.
When the lanthanum oxide is matched with the yttrium oxide and added into the zirconium oxide, a certain toughening effect is achieved, and a certain anti-aging effect is achieved, but on the other hand, the compactness, the heat conductivity and the thermal cycle life are reduced. Secondly, numerous studies have found that La is present in trace amounts2O3When the zirconium oxide is added into the Y-TZP, the zirconium oxide can be completely dissolved in the zirconium oxide crystal lattice in a solid solution mode, on one hand, the solid solution strengthening effect is achieved, on the other hand, the crystal form can be stabilized, the tetragonal phase in the zirconium oxide can be kept stable, and the phase stability of the Y-TZP is improved. Further inhibiting the tetragonal phase from generating martensite transformation under low temperature and humid environment, namely promoting the material to have aging resistance and keeping high performance for a long time. After excessive addition, uphill diffusion occurs in the high-temperature heat treatment process, and La is formed at the crystal boundary2O3When the ratio of the La atomic substance to the Zr atomic substance in the local area is higher than 0.87 when the enrichment area is cooled to room temperature, lanthanum zirconate is generated, and the generation of the lanthanum zirconate promotes the volume expansion and promotes the martensite phase transformation of the nonequilibrium tetragonal phase, thereby reducing the La atomic substance content2O3Phase stability of YSZ system.
The zirconia ceramic of the invention takes zirconia as a basic material, and rare earth oxide yttrium oxide and cerium oxide are added, so that the zirconia-based material can obtain higher toughness and hardness, has excellent mechanical properties, and optimizes the properties of the material in other aspects such as ageing resistance, phase stability and the like through the interaction of a multi-element stabilizer. In addition, a small amount of lanthanum oxide is introduced to serve as a preferred component, so that the toughening effect and a certain anti-aging effect are further enhanced.
The preparation method of the ceramic scalpel comprises the following steps:
step a, performing ball milling treatment on mixed particles of zirconium oxide, cerium oxide, yttrium oxide and lanthanum oxide;
b, mixing and stirring the mixed particles subjected to ball milling in the step a and an adhesive, and removing bubbles to obtain mixed slurry;
the adhesive used in the step is one or more of polyacrylate, polyvinyl alcohol and carboxymethyl cellulose.
Step c, carrying out tape casting treatment on the mixed slurry obtained in the step b to obtain a green sheet of the ceramic scalpel;
d, laminating and isostatic pressing the ceramic scalpel green sheet obtained in the step c to obtain a ceramic scalpel green sheet;
and e, degreasing and sintering the ceramic scalpel green body obtained in the step d to obtain the ceramic scalpel.
In the step, the sintering treatment specifically comprises the steps of moving the ceramic scalpel green body into a kiln, firing for 20-40 min at 450-550 ℃, then raising the temperature in the kiln to 1450-1500 ℃, and sintering again at high temperature.
Step f: and e, performing fine grinding and surface polishing treatment on the blade of the ceramic scalpel obtained in the step e.
According to the preparation method of the ceramic scalpel, the ceramic scalpel with excellent mechanical property, ageing resistance and high stability is obtained by performing ball milling on the mixed particles of the rare earth oxide, mixing and stirring with the adhesive, defoaming, tape casting, laminating, isostatic pressing, degreasing and sintering. In addition, the blade point of the ceramic scalpel is finely ground, the sharpness of the ceramic scalpel is improved, the surface of the ceramic scalpel is polished, and the surface smoothness of the ceramic scalpel is improved.
The method for producing the zirconia ceramic or ceramic scalpel according to the present invention will be described in more detail below with reference to examples one to four.
Example one
The preparation method of the ceramic scalpel in the embodiment comprises the following steps:
firstly, mixed particles of zirconia, ceria, yttria and lanthana are put into a planetary ball mill for ball milling treatment. Wherein the mass percent of zirconia is 90 mol.%, the mass percent of ceria is 5 mol.%, the mass percent of yttria is 4 mol.%, and the mass percent of lanthana is 1 mol.%.
And then, mixing and stirring the mixed particles subjected to ball milling and polyvinyl alcohol, and then placing the mixture into a defoaming machine for defoaming to obtain mixed slurry.
And then, placing the mixed slurry obtained in the step into a casting machine for casting treatment to obtain the green sheet of the ceramic scalpel.
And then, putting the ceramic scalpel green sheet obtained through the steps into a laminating machine for laminating, and then putting the laminated ceramic scalpel green sheet into a warm isostatic pressing machine for isostatic pressing treatment to obtain the ceramic scalpel green sheet.
And then, putting the ceramic scalpel green body obtained through the steps into a degreasing machine for degreasing, moving the ceramic scalpel green body into a kiln, firing for 40min at 450 ℃ in advance, raising the temperature in the kiln to 1480 ℃, and sintering for 2 hours at high temperature again to obtain the ceramic scalpel.
And finally, carrying out fine grinding and surface polishing treatment on the blade of the ceramic scalpel obtained through the steps.
The ceramic scalpel prepared by the implementation has the Vickers hardness of 1001.425GPa and the fracture toughness of 7.119573 MPa-m1/2。
Example two
The preparation method of the ceramic scalpel in the embodiment comprises the following steps:
firstly, mixed particles of zirconia, ceria and yttria are put into a planetary ball mill for ball milling treatment. Wherein the mass percent of zirconia is 92 mol.%, the mass percent of ceria is 5.5 mol.%, the mass percent of yttria is 2.5 mol.%, and the mass percent of lanthana is 0 mol.%.
And then, mixing and stirring the mixed particles subjected to ball milling and polyacrylate, and then putting the mixture into a defoaming machine for defoaming to obtain mixed slurry.
And then, placing the mixed slurry obtained in the step into a casting machine for casting treatment to obtain the green sheet of the ceramic scalpel.
And then, putting the ceramic scalpel green sheet obtained through the steps into a laminating machine for laminating, and then putting the laminated ceramic scalpel green sheet into a warm isostatic pressing machine for isostatic pressing treatment to obtain the ceramic scalpel green sheet.
And then, putting the ceramic scalpel green body obtained through the steps into a degreasing machine for degreasing, moving the ceramic scalpel green body into a kiln, firing for 40min at 450 ℃ in advance, raising the temperature in the kiln to 1500 ℃, and sintering for 2 hours at high temperature again to obtain the ceramic scalpel.
And finally, carrying out fine grinding and surface polishing treatment on the blade of the ceramic scalpel obtained through the steps.
The ceramic scalpel prepared by the implementation has the Vickers hardness of 1045.35GPa and the fracture toughness of 6.726347 MPa-m1/2。
EXAMPLE III
The preparation method of the ceramic scalpel in the embodiment comprises the following steps:
firstly, mixed particles of zirconia, ceria, yttria and lanthana are put into a planetary ball mill for ball milling treatment. Wherein the mass percent of zirconia is 91 mol.%, the mass percent of ceria is 6.5 mol.%, the mass percent of yttria is 2 mol.%, and the mass percent of lanthana is 0.5 mol.%.
And then, mixing and stirring the mixed particles subjected to ball milling and carboxymethyl cellulose, and then putting the mixture into a defoaming machine for defoaming to obtain mixed slurry.
And then, placing the mixed slurry obtained in the step into a casting machine for casting treatment to obtain the green sheet of the ceramic scalpel.
And then, putting the ceramic scalpel green sheet obtained through the steps into a laminating machine for laminating, and then putting the laminated ceramic scalpel green sheet into a warm isostatic pressing machine for isostatic pressing treatment to obtain the ceramic scalpel green sheet.
And then, putting the ceramic scalpel green body obtained through the steps into a degreasing machine for degreasing, moving the ceramic scalpel green body into a kiln, firing for 30min at 500 ℃, raising the temperature in the kiln to 1460 ℃, and sintering for 3 hours at high temperature to obtain the ceramic scalpel.
And finally, carrying out fine grinding and surface polishing treatment on the blade of the ceramic scalpel obtained through the steps.
The ceramic scalpel prepared by the implementation has the Vickers hardness of 1090.225GPa and the fracture toughness of 7.584863 MPa-m1/2。
Example four
The preparation method of the ceramic scalpel in the embodiment comprises the following steps:
firstly, mixed particles of zirconia, ceria, yttria and lanthana are put into a planetary ball mill for ball milling treatment. Wherein the mass percent of zirconia is 90 mol.%, the mass percent of ceria is 5 mol.%, the mass percent of yttria is 3 mol.%, and the mass percent of lanthana is 2 mol.%.
And then, mixing and stirring the mixed particles subjected to ball milling and polyacrylate, and then putting the mixture into a defoaming machine for defoaming to obtain mixed slurry.
And then, placing the mixed slurry obtained in the step into a casting machine for casting treatment to obtain the green sheet of the ceramic scalpel.
And then, putting the ceramic scalpel green sheet obtained through the steps into a laminating machine for laminating, and then putting the laminated ceramic scalpel green sheet into a warm isostatic pressing machine for isostatic pressing treatment to obtain the ceramic scalpel green sheet.
And then, putting the ceramic scalpel green body obtained through the steps into a degreasing machine for degreasing, moving the ceramic scalpel green body into a kiln, firing for 20min at 550 ℃, raising the temperature in the kiln to 1450 ℃, and sintering for 3 hours at high temperature again to obtain the ceramic scalpel.
And finally, carrying out fine grinding and surface polishing treatment on the blade of the ceramic scalpel obtained through the steps.
The ceramic scalpel prepared by the implementation has the Vickers hardness of 948.52GPa and the fracture toughness of 7.396666 MPa-m1 /2。
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A zirconia ceramic characterized by: comprises zirconium oxide, cerium oxide and yttrium oxide, wherein the mass percent of zirconium oxide is 90-92 mol.%, the mass percent of cerium oxide is 5-6.5 mol.%, and the mass percent of yttrium oxide is 2-4 mol.%.
2. The zirconia ceramic of claim 1, wherein: the mass percent of zirconia was 91 mol.%, the mass percent of yttria was 3 mol.%, and the mass percent of ceria was 5.5 mol.%.
3. The zirconia ceramic of claim 1, wherein: the lanthanum oxide is further included, and the mass percentage of the lanthanum oxide is 0-2 mol%.
4. The zirconia ceramic of claim 3, wherein: the mass percent of lanthanum oxide was 0.5 mol.%.
5. A preparation method of a ceramic scalpel is characterized by comprising the following steps: the method comprises the following steps:
step a, performing ball milling treatment on the zirconia ceramic particles according to any one of claims 1 to 4;
b, mixing and stirring the mixed particles subjected to ball milling in the step a and an adhesive, and removing bubbles to obtain mixed slurry;
step c, carrying out tape casting treatment on the mixed slurry obtained in the step b to obtain a green sheet of the ceramic scalpel;
d, laminating and isostatic pressing the ceramic scalpel green sheet obtained in the step c to obtain a ceramic scalpel green sheet;
and e, degreasing and sintering the ceramic scalpel green body obtained in the step d to obtain the ceramic scalpel.
6. The method for manufacturing a ceramic scalpel according to claim 5, wherein: and the sintering in the step e is to move the ceramic scalpel green body into a kiln, fire the ceramic scalpel green body for 20-40 min at 450-550 ℃, then raise the temperature in the kiln to 1450-1500 ℃, and sinter the ceramic scalpel green body at high temperature again.
7. The method for manufacturing a ceramic scalpel according to claim 5, wherein: further comprising step f, step f: and e, performing fine grinding and surface polishing treatment on the blade of the ceramic scalpel obtained in the step e.
8. The method for manufacturing a ceramic scalpel according to claim 5, wherein: the adhesive in the step b is one or more of polyacrylate, polyvinyl alcohol and carboxymethyl cellulose.
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CN116023164B (en) * | 2023-03-29 | 2023-06-06 | 湖南康纳新材料有限公司 | Porous zirconia ceramic block for dental restoration and preparation method and application thereof |
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