CN110204333A - A kind of processing technology for the multilayer zirconium oxide porcelain block that can quickly prepare even transition - Google Patents
A kind of processing technology for the multilayer zirconium oxide porcelain block that can quickly prepare even transition Download PDFInfo
- Publication number
- CN110204333A CN110204333A CN201910613981.XA CN201910613981A CN110204333A CN 110204333 A CN110204333 A CN 110204333A CN 201910613981 A CN201910613981 A CN 201910613981A CN 110204333 A CN110204333 A CN 110204333A
- Authority
- CN
- China
- Prior art keywords
- zirconium oxide
- porcelain block
- rate
- oxide porcelain
- risen
- 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
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 229910001928 zirconium oxide Inorganic materials 0.000 title claims abstract description 104
- 229910052573 porcelain Inorganic materials 0.000 title claims abstract description 89
- 230000007704 transition Effects 0.000 title claims abstract description 33
- 238000012545 processing Methods 0.000 title description 6
- 238000005516 engineering process Methods 0.000 title description 4
- 238000005245 sintering Methods 0.000 claims abstract description 66
- 239000000843 powder Substances 0.000 claims abstract description 23
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 238000004040 coloring Methods 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 17
- 238000009826 distribution Methods 0.000 claims description 16
- 238000003754 machining Methods 0.000 claims description 11
- 238000000462 isostatic pressing Methods 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 33
- 230000008569 process Effects 0.000 abstract description 21
- 238000009738 saturating Methods 0.000 abstract description 8
- 239000011797 cavity material Substances 0.000 abstract description 3
- 210000000214 mouth Anatomy 0.000 abstract description 3
- 235000013350 formula milk Nutrition 0.000 description 49
- 239000010410 layer Substances 0.000 description 38
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 14
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 13
- 229910010271 silicon carbide Inorganic materials 0.000 description 12
- 239000000047 product Substances 0.000 description 8
- 239000000919 ceramic Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 230000009467 reduction Effects 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 230000035699 permeability Effects 0.000 description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 4
- 235000013339 cereals Nutrition 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 230000000704 physical effect Effects 0.000 description 4
- 235000020610 powder formula Nutrition 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 4
- 229910052845 zircon Inorganic materials 0.000 description 4
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- HDGGAKOVUDZYES-UHFFFAOYSA-K erbium(iii) chloride Chemical compound Cl[Er](Cl)Cl HDGGAKOVUDZYES-UHFFFAOYSA-K 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 2
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 208000002193 Pain Diseases 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 239000004098 Tetracycline Substances 0.000 description 1
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- CFYGEIAZMVFFDE-UHFFFAOYSA-N neodymium(3+);trinitrate Chemical compound [Nd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CFYGEIAZMVFFDE-UHFFFAOYSA-N 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- YWECOPREQNXXBZ-UHFFFAOYSA-N praseodymium(3+);trinitrate Chemical compound [Pr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YWECOPREQNXXBZ-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229960002180 tetracycline Drugs 0.000 description 1
- 229930101283 tetracycline Natural products 0.000 description 1
- 235000019364 tetracycline Nutrition 0.000 description 1
- 150000003522 tetracyclines Chemical class 0.000 description 1
- 238000003325 tomography Methods 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
- A61C13/00—Dental prostheses; Making same
- A61C13/08—Artificial teeth; Making same
- A61C13/083—Porcelain or ceramic teeth
-
- 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
- C04B35/01—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
- C04B35/481—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 containing silicon, e.g. zircon
-
- 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
-
- 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
- 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
-
- 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
- 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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5276—Whiskers, spindles, needles or pins
-
- 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
- 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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
-
- 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
- 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
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6565—Cooling rate
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/661—Multi-step sintering
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/75—Products with a concentration gradient
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9646—Optical properties
- C04B2235/9661—Colour
Abstract
The invention belongs to oral cavity material fields, and in particular to one kind can quickly prepare the sintering process of the uniform zirconium oxide porcelain block of intensity, color transition.More particularly to a kind of high tenacity zirconium oxide porcelain block, by mass fraction, the powder composition of the zirconium oxide porcelain block are as follows: 1.5~12% yttrium oxide, 0~2.5% SiC Nanometer Whiskers, 0~1.5% coloring object and the zirconium oxide of surplus.And a kind of comprehensive mechanical property and color are provided based on the porcelain block, spends thoroughly and crosses uniform multilayer zirconium oxide porcelain block.A kind of technique that efficiently high-quality can complete above-mentioned zirconium oxide porcelain block sintering is provided simultaneously.Using technical solution provided by the invention, it is excellent that comprehensive mechanical property can be obtained within the time short as far as possible, and color, saturating spend cross uniform zirconium oxide porcelain block.
Description
Technical field
The invention belongs to oral cavity material fields, and in particular to one kind can quickly prepare intensity, color transition uniformly aoxidizes
The processing technology of zircon porcelain block.
Background technique
With the diversification that social progress and development, oral cavity material are used, zirconium oxide porcelain block is outer because its gentle such as jade
See, good mechanical property and it is increasingly heavier in dental industry accounting.And as the improvement of people's living standards, to zirconium oxide porcelain
The artificial tooth of block production requires also higher and higher, and it is excellent not require nothing more than comprehensive mechanical property, it is also desirable to have good appearance attribute.
And dental zirconium oxide porcelain block, translucency, moistnes, bending strength, fracture toughness etc. are matched by zirconium oxide porcelain block simultaneously
It is influenced while side and high-sintering process, and the influence of these factors is largely nonlinear.Therefore, do not have at present
Any prior art provides a kind of zirconium oxide porcelain that can have both excellent comprehensive mechanical property and good appearance attribute simultaneously
Block preparation process, however be exactly cannot achieve color nature transition, otherwise be exactly machining or high temperature sintering in occur chipping,
Scrappage is excessively high, otherwise is exactly that the zirconium oxide porcelain block comprehensive mechanical property finally obtained is unable to satisfy demand, numerous.
Summary of the invention
The object of the present invention is to provide the sintering process that one kind can quickly prepare the multilayer zirconium oxide porcelain block of even transition.
For achieving the above object, the technical scheme adopted by the invention is that: a kind of high tenacity zirconium oxide porcelain block, by matter
Measure score, the powder composition of the zirconium oxide porcelain block are as follows: 1.5~12% yttrium oxide, 0~2.5% SiC Nanometer Whiskers,
0~1.5% coloring object and the zirconium oxide of surplus.
Preferably, the multilayer zirconium oxide porcelain block includes at least most bleached bed and most dark layer；The multilayer zirconium oxide porcelain
The preparation method of block includes the following steps:
(1) SiC Nanometer Whiskers and yttrium oxide determined in each layer powder composition respectively are spent according to required toughness and thoroughly
Content；
(2) component and content that object is coloured in each layer powder composition are determined respectively according to required color；
(3) according to the content of yttrium oxide and SiC Nanometer Whiskers in each formula, most bleached bed and most dark is adjusted respectively
The particle diameter distribution of powder in layer powder composition, is adjusted to the most bleached bed and the sintered shrinking percentage diversity factor < of most dark layer
3‰；
(4) most bleached bed, most dark layer are successively placed by shade sequence, isostatic pressing, pre-sintering, mechanical added
Work, high temperature sintering complete preparation.
Preferably, the multilayer zirconium oxide porcelain block further includes transition zone.
Preferably, the transition zone is arranged 2~5 layers.
Preferably, the transition zone is arranged 5 layers, and in mass ratio, the formula of each transition zone is respectively most bleached bed: most deep
Chromatograph=2:1,3:2,1:1,2:3,1:2.
Preferably, it includes at least: isostatic pressing, pre-sintering, machining, high temperature sintering；
The high temperature sintering includes the following steps:
(1) with the rate of 3~6 DEG C/min, 200 DEG C is risen to from room temperature, keeps the temperature 8~12min；
(2) again with the rate of 8~25 DEG C/min, 1000 DEG C are risen to from 200 DEG C；
(3) 1530 DEG C are risen to from 1000 DEG C with the rate of 3~6 DEG C/min again, keep the temperature 60~180min；
(4) again with the rate of 3~10 DEG C/min, 1200 DEG C are down to by 1530 DEG C, or be down to 800 DEG C；
(5) finally with furnace cooled to room temperature.
Preferably, when the preparation long bridge of 1~3 unit, the high temperature sintering includes the following steps:
(1) with the rate of 3~6 DEG C/min, 200 DEG C is risen to from room temperature, keeps the temperature 8~12min；
(2) again with the rate of 16~25 DEG C/min, 1000 DEG C are risen to from 200 DEG C；
(3) 1530 DEG C are risen to from 1000 DEG C with the rate of 3~6 DEG C/min again, keep the temperature 60~180min；
(4) again with the rate of 6~10 DEG C/min, 1200 DEG C are down to by 1530 DEG C；
(5) finally with furnace cooled to room temperature.
Preferably, when the preparation long bridge of 4~7 units, the high temperature sintering includes the following steps:
(1) with the rate of 3~6 DEG C/min, 200 DEG C is risen to from room temperature, keeps the temperature 8~12min；
(2) again with the rate of 8~12 DEG C/min, 1000 DEG C are risen to from 200 DEG C；
(3) 1530 DEG C are risen to from 1000 DEG C with the rate of 3~6 DEG C/min again, keep the temperature 60~180min；
(4) again with the rate of 6~10 DEG C/min, 1200 DEG C are down to by 1530 DEG C；
(5) finally with furnace cooled to room temperature.
Preferably, when the preparation long bridge of 8~14 units, the high temperature sintering includes the following steps:
(1) with the rate of 3~6 DEG C/min, 200 DEG C is risen to from room temperature, keeps the temperature 8~12min；
(2) again with the rate of 8~12 DEG C/min, 1000 DEG C are risen to from 200 DEG C；
(3) 1530 DEG C are risen to from 1000 DEG C with the rate of 3~6 DEG C/min again, keep the temperature 60~180min；
(4) again with the rate of 3~6 DEG C/min, 800 DEG C are down to by 1530 DEG C；
(5) finally with furnace cooled to room temperature.
The invention has the following advantages:
1, the natural transition for having color because of the tooth of people and spending thoroughly, so also being needed when zirconium oxide porcelain block is processed as artificial tooth
It carries out certain color and saturating spend is crossed；One monolith same color is installed, the artificial tooth spent thoroughly can seem very lofty.Therefore,
Demand to artificial tooth carries out color, degree is handled thoroughly is very urgent.General processing mode is extrinsic staining, and the present invention is around
And it is gone, using endogenous dyeing/screening color method, make the zirconium oxide porcelain block obtained after sintering that naturally there is the natural color of transition
With saturating degree, and color keep is consistent inside and outside zirconium oxide, will not dye as external source/hide color, zirconium oxide porcelain block can be can increase
Thickness, so as to cause artificial tooth size with it is expected that the skimble-scamble situation of size；Effect is substantially better than general external source brushing, impregnates
Equal colouring methods.There is the natural color of transition in order to reach zirconium oxide porcelain block naturally and spend this effect thoroughly, the present invention uses
Different zirconium oxide powder multilayers are co-pressed, sintering method.And provide light end, the respective adaptability zirconium oxide in dark end
Powder composition mainly adjusts the saturating degree of zirconium oxide porcelain block by adjusting the difference of yttria levels, by adjusting coloring object
Type and proportion adjust the color of zirconium oxide porcelain block.Inventor also found that the content of control coloring object is 1.5% hereinafter, a side
Face can guarantee the color needs of zirconium oxide porcelain block, on the other hand can also ignore not on the influence of the shrinking percentage of zirconium oxide porcelain block
Meter.
Inventor also found, by the adjusting to each component in formula, can obtain the different oxidation of comprehensive mechanical property
Zircon porcelain block.Co-pressed, co-sintering is carried out using the different Zirconium powder formula of each comprehensive mechanical property, can be obtained resultant force
Learn the uniform zirconium oxide porcelain block of performance transition.Difficult point is how i.e. to guarantee that color and saturating degree in formula are met the requirements, and protects
Card mechanical property is met the requirements.Inventor has been obtained formula provided by the present invention, has been matched using this after many experiments early period
Side simultaneously combines specific preparation method in invention, can meet above-mentioned requirements simultaneously.
2 but the zirconium oxide powders of different formulations crystallization process is different when sintering at high temperature, shrinking percentage can also change correspondingly,
Shrinking percentage difference value is once more than a certain range, and bridge will bend, deform, and gently then influences beauty, it is heavy then scrap, can not
It uses.
For this problem, how inventor reduces shrinking percentage if not being conceived to, but creatively proposes a kind of complete
New thinking: how each layer shrinking percentage to be adjusted to unanimously.By a large amount of early-stage study, inventors have found that true in inventor
Recognize Zirconium powder formula in, the shrinking percentage of zirconia ceramics be mainly formulated in yttrium oxide content and zirconium oxide, oxidation
The particle diameter distribution of yttrium powder body controls.Therefore, it after inventor carries out a large number of experiments, finds out under specific yttria levels, aoxidizes
Relationship between zirconium, yttrium oxide particle diameter distribution and shrinking percentage, and completely new technical solution is proposed accordingly: it is (pre- according to actual needs
Precalculated artificial tooth size etc.) the suitable shrinking percentage of selection, zirconium oxide and oxidation in each formula are reversely adjusted further according to shrinking percentage
The particle diameter distribution of yttrium is consistent with controlling zirconia ceramics overall shrinkage.Finally obtaining naturally has color, spends thoroughly, is comprehensive
Mechanical property transition is closed naturally, the layering zirconium oxide porcelain block that shrinking percentage is almost consistent.
3, in order to further ensure the final performance of the zirconium oxide porcelain block, inventor also sets about from sintering process, provides
A kind of new, specific high-sintering process.In sintering process, three heating rate, soaking time and rate of temperature fall factors
Finished product is influenced maximum.Heating rate is too fast, is easy to cause ceramics to have little time whole while shrinking, be easy to appear deformation, prepares
Finished product it is integrally impermeable, matt, various aspects physical property is poor.Heating rate is too slow, and it is too long to will lead to the sintering period, unfavorable
In the preparation of processing factory's workpiece.Soaking time is short, and not exclusively, whole permeability is poor, and various aspects physical property is poor for finished product sintering.It protects
The phenomenon that warm time is too long, and the zirconia grains growth of sintering is too much, also will appear burning, finished product permeability increases, is physical
It can be declined；Soaking time is inadequate, and sintering process does not carry out completely, and sample defects are more, and permeability is poor, physical property fluctuates
Greatly.Rate of temperature fall is too fast, is easy to cause the non-overall shrinkage of finished product, generates internal stress and concentrates, and serious person causes the fracture of porcelain block broken
It is broken.Rate of temperature fall is excessively slow, also results in the square in product object phase to rectangle phase transition, physical property is caused to decline.Invention
People is based ultimately upon formula of the invention and provides three kinds of sintering process for being suitble to the long bridge of every unit by largely groping.
Specific embodiment
The oxygen that the present invention provides a kind of ductile strengths greatly, color and hardness transition are uniform, overall shrinkage is consistent
Change the high efficiency sintering process of zircon porcelain block.
One, the formula of zirconium oxide porcelain block
By mass fraction, total formula of the zirconium oxide porcelain block includes: 1.5~12% yttrium oxide, 0~2.5% carbon
SiClx nano whisker, 0~1.5% coloring object and the zirconium oxide of surplus.It is described in the case where sintering process is identical
In formula, the factor influenced on each core capabilities of zirconium oxide porcelain block is mainly as follows:
1, about sintering shrinkage.In the formula, coloring object content is lower than 1.5%, by experimental verification, to zirconium oxide
The sintering shrinkage of porcelain block influences negligible.In the formula, influence zirconium oxide porcelain block shrinking percentage principal element be with
The content of yttrium oxide in side, the content and zirconium oxide of SiC Nanometer Whiskers, the partial size of yttrium oxide and SiC Nanometer Whiskers divide
Cloth.
2, it spends thoroughly about zirconium oxide porcelain block and color (with the displaying of semi-transparent rate).
The major influence factors spent thoroughly include: the content and particle diameter distribution of SiC Nanometer Whiskers: because of nanometer silicon carbide
The addition of whisker can help to form zirconium oxide fine grain in crystallization inside zirconium oxide porcelain block, reduce the crystal grain of crystal of zirconium oxide
Diameter；And the semi permeability of crystal grain diameter and zirconia ceramics is in non-linear relation.The content of yttrium oxide: in this formula range, no
When adding SiC Nanometer Whiskers, yttria levels and semi permeability correlation.
In the range of above-mentioned total formula, light layer formula and dark layer formula can be gone out with appropriate adjustment.In addition, to understand
Several layers of degree, color transition layers thoroughly are arranged in the problem of certainly saturating degree, color tomography again between most bleached bed and most dark layer.It is described
Transition zone is generally arranged 2~5 layers.
3, the comprehensive mechanical property about zirconium oxide porcelain block.Zirconium oxide porcelain block is in machining molding and high-temperature sintering process
In, often due to fracture toughness is inadequate, situations such as being easy to appear chipping, lead to scrap of the product.And zirconium oxide porcelain block is prepared as
After artificial tooth, the comprehensive mechanical property that the different location of artificial tooth needs is also different.The occlusal end of artificial tooth connects with other teeth
Touching, the hardness needed is more relatively low, in order to avoid wear remaining tooth.But comprehensive mechanical property can also be carried out according to demands of individuals
Can different settings, such as require occlusal end close to endface mechanical property more by force, be more convenient for being engaged, occlusal end is to bottom end
Transition, comprehensive mechanical property first weakens to be gradually increased again, to guarantee to realize machining at long bridge.
Major influence factors to comprehensive mechanical property include: the content of yttrium oxide: yttrium oxide, can be with one as stabilizer
Determine that zirconium oxide crystal phase is inhibited to be changed by cubic opposite monoclinic phase in degree, to help to improve fracture toughness；But it is non-to promote effect
Often limited, in this formula range, compared with not adding yttrium oxide, fracture toughness is can be improved in the yttrium oxide for adding 1.5%；But
In the case where adding yttrium oxide, the fracture toughness negative correlation of yttria levels and zirconium oxide porcelain block.Nanometer silicon carbide
The content of whisker: on the one hand SiC Nanometer Whiskers can also inhibit zirconium oxide crystal phase to cubic phase transition, on the other hand, carbonization
Silicon nanocrystal itself must have the synthesis reinforcing effect to mechanical property, can further promote the synthesis mechanical property of zirconium oxide porcelain block
Energy.
Two, the sintering process of zirconium oxide porcelain block
It experienced zirconium oxide porcelain block raw material weighing, mixing, pre-molding, isostatic pressing, pre-sintering, machining
After (carving milling), it is also necessary to which final high temperature sintering link could obtain finished product zirconium oxide porcelain block.Formula composition itself is to influence oxygen
Change the deciding factor of the core capabilities such as comprehensive mechanical property, the saturating degree of zircon porcelain block.But in above-mentioned total formula range, use certain
When the completely specified formula of one numerical value, the concrete technology in high temperature sintering influences the performance of zirconium oxide porcelain block huge.Agglomerant
In skill, the influence of three heating rate, soaking time and rate of temperature fall factors to zirconium oxide porcelain block final product is maximum.The present invention mentions
Supply one kind can be in the case where guaranteeing comprehensive mechanical property and degree thoroughly, the technique of as much as possible high efficiency completion sintering.Separately
Outside, the artificial tooth of the long bridge of commensurate does not require difference to comprehensive mechanical property, is also required to different sintering process accordingly.The present invention mentions
The sintering process of confession specifically comprises the following steps:
1, preparing the long bridge of 1~3 unit, (the long bridge of unit refers to the quantity of artificial tooth on long bridge, and quantity is more, to comprehensive mechanics
The requirement of performance is higher):
(1) with the rate of 3~6 DEG C/min, 200 DEG C is risen to from room temperature, keeps the temperature 8~12min；
(2) again with the rate of 16~25 DEG C/min, 1000 DEG C are risen to from 200 DEG C；
(3) 1530 DEG C are risen to from 1000 DEG C with the rate of 3~6 DEG C/min again, keep the temperature 60~180min；
(4) it controls furnace temperature reduction of speed and is down to 1200 DEG C by 1530 DEG C with the rate of 6~10 DEG C/min；
(5) finally with furnace cooled to room temperature.
A length of 288~378min when control always sintering.
Preferred technique are as follows:
(1) with the rate of 5 DEG C/min, 200 DEG C are risen to from 50 DEG C, keep the temperature 10min；
(2) again with the rate of 20 DEG C/min, 1000 DEG C are risen to from 200 DEG C；
(3) 1530 DEG C are risen to from 1000 DEG C with the rate of 5 DEG C/min again, keep the temperature 60~180min；
(4) it controls furnace temperature reduction of speed and is down to 1200 DEG C by 1530 DEG C with the rate of 8 DEG C/min；
(5) finally with furnace cooled to room temperature.
2, the long bridge of 4~7 units is prepared:
(1) with the rate of 3~6 DEG C/min, 200 DEG C are risen to from 50 DEG C, keep the temperature 8~12min；
(2) again with the rate of 8~12 DEG C/min, 1000 DEG C are risen to from 200 DEG C；
(3) 1530 DEG C are risen to from 1000 DEG C with the rate of 3~6 DEG C/min again, keep the temperature 60~180min；
(4) it controls furnace temperature reduction of speed and is down to 1200 DEG C by 1530 DEG C with the rate of 6~10 DEG C/min；
(5) finally with furnace cooled to room temperature.
A length of 328~418min when control always sintering.
Preferred technique are as follows:
(1) with the rate of 5 DEG C/min, 200 DEG C are risen to from 50 DEG C, keep the temperature 10min；
(2) again with the rate of 10 DEG C/min, 1000 DEG C are risen to from 200 DEG C；
(3) 1530 DEG C are risen to from 1000 DEG C with the rate of 5 DEG C/min again, keep the temperature 60~180min；
(4) it controls furnace temperature reduction of speed and is down to 1200 DEG C by 1530 DEG C with the rate of 8 DEG C/min；
(5) finally with furnace cooled to room temperature.
3, the long bridge of 8~14 units is prepared:
(1) with the rate of 3~6 DEG C/min, 200 DEG C are risen to from 50 DEG C, keep the temperature 8~12min；
(2) again with the rate of 8~12 DEG C/min, 1000 DEG C are risen to from 200 DEG C；
(3) 1530 DEG C are risen to from 1000 DEG C with the rate of 3~6 DEG C/min again, keep the temperature 60~180min；
(4) it controls furnace temperature reduction of speed and is down to 800 DEG C by 1530 DEG C with the rate of 3~6 DEG C/min；
(5) finally with furnace cooled to room temperature.
A length of 432~522min when control always sintering.
Preferred technique are as follows:
(1) with the rate of 5 DEG C/min, 200 DEG C are risen to from 50 DEG C, keep the temperature 10min；
(2) again with the rate of 10 DEG C/min, 1000 DEG C are risen to from 200 DEG C；
(3) 1530 DEG C are risen to from 1000 DEG C with the rate of 5 DEG C/min again, keep the temperature 60~180min；
(4) it controls furnace temperature reduction of speed and is down to 800 DEG C by 1530 DEG C with the rate of 5 DEG C/min；
(5) finally with furnace cooled to room temperature.
Below with reference to specific embodiment, technical solution of the present invention is further explained.
Embodiment one: the comprehensive mechanical property of zirconium oxide porcelain block and the thoroughly displaying of degree effect
1, by the zirconium oxide porcelain block of 35 groups of monoliths of above-mentioned total formula preparation, every group sets 20 repetitions.Each group zirconium oxide porcelain block
Specific formula it is as shown in table 1, numerical value is mass fraction in table, and surplus is Zirconium oxide powder；In each group zirconium oxide porcelain block,
The coloring equal content of object is to use 0.4%.The coloring object can for erbium chloride, iron chloride, neodymium nitrate, manganese nitrate, ammonium metavanadate,
The mixture of any one or more in cerous nitrate, praseodymium nitrate, cobalt nitrate and nickel nitrate.For convenience of operation, institute of the invention
Have in embodiment is the coloring object obtained after 6:1:2 mixing using erbium chloride, iron chloride, manganese nitrate in mass ratio, and color is
Tetracycline ash.It should be noted that applicant has not only carried out the test of table 1, but because length limits, it only has chosen most
Representative several groups of data are shown.
Each group zirconia ceramics specific is the preparation method comprises the following steps: weigh each component, after mixing well, the pressure maintaining at 150MPa
10min carries out isostatic pressing；2h is kept the temperature at 1050 DEG C again, is pre-sintered；Take out 10 repetitions respectively from each group,
It is machined the shape and size of most artificial tooth；Every group of another 10 repetitions are without machining processes.It then will be each
Group respectively repeats high temperature sintering, completion prepare (each duplicate zirconia ceramics of each group, no matter the chipping in mechanical processing process
Whether, continue high temperature sintering).The high temperature sintering specifically comprises the processes of: with the rate of 5 DEG C/min, risen to from 50 DEG C
200 DEG C, keep the temperature 10min；Again with the rate of 10 DEG C/min, 1000 DEG C are risen to from 200 DEG C；Again with the rate of 5 DEG C/min, from 1000
1530 DEG C DEG C are risen to, 120min is kept the temperature；Again with the rate of 5 DEG C/min, 800 DEG C are down to by 1530 DEG C with furnace；Last natural cooling
To room temperature.
The formula of 1 each group zirconium oxide porcelain block of table shows table
2, each duplicate chipping rate of above-mentioned each group is measured using indentation method；Wherein, the chipping occurred in machining is not
It is included in high temperature sintering, the chipping rate in high temperature sintering only calculates the zirconium oxide pottery that chipping occurs again in high-temperature sintering process
The quantity of porcelain and the percentage in whole group.Simultaneously calculate each group three-point bending resistance intensity (referring to GB30356-2013 into
Row), fracture toughness and light transmittance；Wherein, light transmittance takes every group of 20 duplicate average values, the bending strength and fracture of final product
Toughness takes the average value of every group of not machined zirconia ceramics.The results are shown in Table 2.
The performance of 2 each group zirconium oxide porcelain block of table shows table
Embodiment two: the shrinking percentage of most bleached bed and most dark layer zirconium oxide porcelain block is determined
1, according to patient's actual conditions, or the powder composition of each layer zirconium oxide porcelain block is selected according to primary demand.This implementation
Primary demand is pressed in example, the formula that one group 31 of selection example as occlusal end formula, make by the formula that one group 23 of selection example
For long bridge end formula.And coloring object is accordingly added, adjust the color of each group of formula.Because occlusal end requires color more shallow, stinging
The coloring object of addition 0.3% in the formula of end is closed, and accordingly reduces by 0.3% Zirconium oxide powder content, as most light layer formula；
0.5% coloring object is added in the formula of long bridge end, and accordingly reduces by 0.5% Zirconium oxide powder content, as most dark layer
Formula.
2, with the formula of above-mentioned determination, the corresponding monolith zirconium oxide porcelain block of most light layer formula and most dark layer are carried out respectively
It is formulated the production of corresponding monolith zirconium oxide porcelain block, measures under same recipe, different zirconium oxides, yttrium oxide and nano silicon carbide silicon wafer
When palpus particle diameter distribution, the shrinking percentage of zirconium oxide porcelain block.Under above-mentioned same recipe, adjusts zirconium oxide, yttrium oxide in formula and receive
The particle diameter distribution of rice silicon carbide whisker measures each grain after the isostatic pressing of the same terms, pre-sintering, high temperature sintering
Shrinking percentage under diameter distribution.The isostatic pressing condition, pre-sintering condition are and high-sintering process is the same as embodiment one.It should
Understand, what the adjustment of the particle diameter distribution was really carried out for entire formula.For example, 10~50 μm of particle diameter distribution accountings
70%, for the partial size of all components in 10~50 μ ms, accounting 70% is not necessarily referring to the grain of a certain specific components in assignment side
Diameter accounting 70% in 10~50 μ ms；Such as the nanometer silicon carbide whiskers, practical particle size range is 50 μm~250 μm, and
There is no 10~50 μm of particle size ranges, but have no effect on the powder material that 70% mass fraction is distributed in 10~50 μ ms
Material.Under different particle size distribution, the shrinking percentage of the zirconium oxide porcelain block of most light layer formula preparation is as shown in table 3；Most dark layer formula
The shrinking percentage of the zirconium oxide porcelain block of preparation is as shown in table 4.
The shrinking percentage of the most light layer formula of table 3 shows table
The shrinking percentage of the most dark layer formula of table 4 shows table
3, most light layer formula and the shrinking percentage of most dark layer formula to consistent (shrinking percentage maximum difference degree < 3 ‰ are adjusted
It can be considered consistent).Selection shrinking percentage is similarly 17.45%, 17.82%, 19.01%, 20.55% particle diameter distribution, setting 4
The powder composition of group zirconium oxide porcelain block, respectively organizes 1,2,3,4, every group sets 3 repetitions.Being similarly 17.45% with shrinking percentage is
Example, that is, in most light layer formula, diameter of particle distribution are as follows: 10~50 μm, accounting 50%；50~150 μm, accounting 40%；150
~300 μm, accounting 10%.In most dark layer formula, the particle diameter distribution of zirconium oxide and yttrium oxide are as follows: 10~50 μm, accounting 70%；
50~150 μm, accounting 20%；150~300 μm, accounting 10%.Remaining organizes other particle diameter distribution and so on, repeats no more.
4, according to the most light layer formula and most dark layer formula after adjusting, the formula of transition zone is determined.In mass ratio, respectively
Group transition zone mass ratio be respectively most bleached bed: most dark layer=2:1,3:2,1:1,2:3,1:2, will most light layer formula and
Most dark layer formula is mixed, and obtains backing powder formula 1,2,3,4,5 respectively.Because most bleached bed and most dark interlayer have defined
The shrinking percentage difference of the maximum difference degree of shrinking percentage, the sintering shrinkage of the transition zone of preparation and most bleached bed, most dark interlayer
Degree does not exceed the value, to guarantee that the layering zirconium oxide porcelain block shrinking percentage finally obtained is consistent.
5, by the sequence of most bleached bed, transition zone 1, transition zone 2, transition zone 3, transition zone 4, transition zone 5, most dark layer,
It is sequentially placed each layer powder, by method isostatic pressing, pre-sintering, machining, the high temperature sintering of step 2, i.e. acquisition each group
Zirconium oxide porcelain block.The zirconium oxide porcelain block shrinking percentage diversity factor is measured, and visual inspection is spent thoroughly and the transient condition of color.Knot
Fruit is as shown in table 5.
5 each group effect of table shows table
Embodiment three: high-sintering process effect is shown
1,21 component layers Zirconium powder formulas, 10 repetitions of every group of setting are arranged in the group 1 of selection example two；By reality
Apply example two mode sequentially placed each layer powder, isostatic pressing, pre-sintering, machining after, then respectively press table 6 side
Method carries out high temperature sintering.
6 each group high-sintering process parameter list of table
2, the bending strength of the zirconium oxide porcelain block of measurement each group preparation, and each group zirconium oxide porcelain block is observed in high temperature sintering
Chipping rate, observation each group zirconium oxide porcelain block it is saturating spend, color transition situation, the results are shown in Table 7.
The performance of 7 each group zirconium oxide porcelain block of table is shown
Claims (9)
1. a kind of high tenacity zirconium oxide porcelain block, it is characterised in that: press mass fraction, the powder composition of the zirconium oxide porcelain block are as follows:
1.5~12% yttrium oxide, 0~2.5% SiC Nanometer Whiskers, 0~1.5% coloring object and the zirconium oxide of surplus.
2. utilizing the multilayer zirconium oxide porcelain block of the preparation of powder composition described in claim 1, it is characterised in that: the multilayer zirconium oxide
Porcelain block includes at least most bleached bed and most dark layer；The preparation method of the multilayer zirconium oxide porcelain block includes the following steps:
(1) containing for the SiC Nanometer Whiskers and yttrium oxide determined in each layer powder composition respectively is spent according to required toughness and thoroughly
Amount；
(2) component and content that object is coloured in each layer powder composition are determined respectively according to required color；
(3) according to the content of yttrium oxide and SiC Nanometer Whiskers in each formula, most bleached bed and most dark layer powder are adjusted respectively
The particle diameter distribution of powder in body formula, is adjusted to the most bleached bed and the sintered shrinking percentage diversity factor < 3 ‰ of most dark layer；
(4) will most bleached bed, most dark layer successively place by shade sequence, isostatic pressing, pre-sintering, machining,
High temperature sintering completes preparation.
3. multilayer zirconium oxide porcelain block according to claim 2, it is characterised in that: the multilayer zirconium oxide porcelain block further included
Cross layer.
4. multilayer zirconium oxide porcelain block according to claim 3, it is characterised in that: the transition zone is arranged 2~5 layers.
5. multilayer zirconium oxide porcelain block according to claim 4, it is characterised in that: the transition zone is arranged 5 layers, by quality
Than the formula of each transition zone is respectively most bleached bed: most dark layer=2:1,3:2,1:1,2:3,1:2.
6. the preparation method of zirconium oxide porcelain block as claimed in claim 1 or 2, it is characterised in that: include at least: isostatic pressing, pre-
Sintering, machining, high temperature sintering；
The high temperature sintering includes the following steps:
(1) with the rate of 3~6 DEG C/min, 200 DEG C is risen to from room temperature, keeps the temperature 8~12min；
(2) again with the rate of 8~25 DEG C/min, 1000 DEG C are risen to from 200 DEG C；
(3) 1530 DEG C are risen to from 1000 DEG C with the rate of 3~6 DEG C/min again, keep the temperature 60~180min；
(4) again with the rate of 3~10 DEG C/min, 1200 DEG C are down to by 1530 DEG C, or be down to 800 DEG C；
(5) finally with furnace cooled to room temperature.
7. the preparation method of zirconium oxide porcelain block according to claim 6, it is characterised in that: when the preparation long bridge of 1~3 unit,
The high temperature sintering includes the following steps:
(1) with the rate of 3~6 DEG C/min, 200 DEG C is risen to from room temperature, keeps the temperature 8~12min；
(2) again with the rate of 16~25 DEG C/min, 1000 DEG C are risen to from 200 DEG C；
(3) 1530 DEG C are risen to from 1000 DEG C with the rate of 3~6 DEG C/min again, keep the temperature 60~180min；
(4) again with the rate of 6~10 DEG C/min, 1200 DEG C are down to by 1530 DEG C；
(5) finally with furnace cooled to room temperature.
8. the preparation method of zirconium oxide porcelain block according to claim 6, it is characterised in that: when the preparation long bridge of 4~7 units,
The high temperature sintering includes the following steps:
(1) with the rate of 3~6 DEG C/min, 200 DEG C is risen to from room temperature, keeps the temperature 8~12min；
(2) again with the rate of 8~12 DEG C/min, 1000 DEG C are risen to from 200 DEG C；
(3) 1530 DEG C are risen to from 1000 DEG C with the rate of 3~6 DEG C/min again, keep the temperature 60~180min；
(4) again with the rate of 6~10 DEG C/min, 1200 DEG C are down to by 1530 DEG C；
(5) finally with furnace cooled to room temperature.
9. the preparation method of zirconium oxide porcelain block according to claim 6, it is characterised in that: when the preparation long bridge of 8~14 units,
The high temperature sintering includes the following steps:
(1) with the rate of 3~6 DEG C/min, 200 DEG C is risen to from room temperature, keeps the temperature 8~12min；
(2) again with the rate of 8~12 DEG C/min, 1000 DEG C are risen to from 200 DEG C；
(3) 1530 DEG C are risen to from 1000 DEG C with the rate of 3~6 DEG C/min again, keep the temperature 60~180min；
(4) again with the rate of 3~6 DEG C/min, 800 DEG C are down to by 1530 DEG C；
(5) finally with furnace cooled to room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910613981.XA CN110204333B (en) | 2019-07-09 | 2019-07-09 | Processing technology capable of rapidly preparing multi-layer zirconium oxide ceramic blocks with uniform transition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910613981.XA CN110204333B (en) | 2019-07-09 | 2019-07-09 | Processing technology capable of rapidly preparing multi-layer zirconium oxide ceramic blocks with uniform transition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110204333A true CN110204333A (en) | 2019-09-06 |
| CN110204333B CN110204333B (en) | 2021-10-12 |
Family
ID=67796835
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910613981.XA Active CN110204333B (en) | 2019-07-09 | 2019-07-09 | Processing technology capable of rapidly preparing multi-layer zirconium oxide ceramic blocks with uniform transition |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110204333B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111803386A (en) * | 2020-06-17 | 2020-10-23 | 深圳市美鸣齿科技术有限公司 | False tooth outer crown and preparation method thereof |
| CN112516381A (en) * | 2020-12-28 | 2021-03-19 | 杭州而然科技有限公司 | Whisker reinforced zirconia implant |
| CN112656990A (en) * | 2020-12-28 | 2021-04-16 | 杭州而然科技有限公司 | Whisker reinforced zirconia planting integrated crown |
| CN112691232A (en) * | 2020-12-28 | 2021-04-23 | 杭州而然科技有限公司 | Whisker reinforced zirconia base |
| CN113402282A (en) * | 2021-07-30 | 2021-09-17 | 广东工业大学 | Bionic human bone based on 3D printing and manufacturing method thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1083155A1 (en) * | 1999-09-08 | 2001-03-14 | Ferro Enamels (Japan) Limited | Method of manufacturing frit for ceramic glaze |
| EP1845073A1 (en) * | 2006-04-10 | 2007-10-17 | Consorzio Interuniversitario per lo Sviluppo dei Sistemi a Grande Interfase, C.S.G.I | Compositions comprising nanoparticles of zirconium hydroxide and/or glass frits for coating ceramic products |
| CN101638317A (en) * | 2008-08-02 | 2010-02-03 | 比亚迪股份有限公司 | Fully stabilized zirconia ceramic material and preparation method thereof |
| CN101880163A (en) * | 2009-05-07 | 2010-11-10 | 宁波大学 | Method for preparing silicon carbide whisker in-situ reinforced aluminum oxide ceramic |
| CN103693988A (en) * | 2013-12-23 | 2014-04-02 | 秦皇岛爱迪特高技术陶瓷有限公司 | Internal dyeing method of dental zirconium oxide restoration body |
| CN105565807A (en) * | 2015-12-08 | 2016-05-11 | 河北工业大学 | Zirconia ceramic slurry for manufacturing false tooth as well as preparation method and application thereof |
| CN106336216A (en) * | 2015-07-07 | 2017-01-18 | 北京欧纳材料科技有限公司 | Zirconia dental ceramic with gradient change color and preparation method thereof |
| CN106631012A (en) * | 2016-12-21 | 2017-05-10 | 汕头大学 | Tetragonal zirconia based composite ceramic ultrathin cover plate and preparation process thereof |
-
2019
- 2019-07-09 CN CN201910613981.XA patent/CN110204333B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1083155A1 (en) * | 1999-09-08 | 2001-03-14 | Ferro Enamels (Japan) Limited | Method of manufacturing frit for ceramic glaze |
| EP1845073A1 (en) * | 2006-04-10 | 2007-10-17 | Consorzio Interuniversitario per lo Sviluppo dei Sistemi a Grande Interfase, C.S.G.I | Compositions comprising nanoparticles of zirconium hydroxide and/or glass frits for coating ceramic products |
| CN101638317A (en) * | 2008-08-02 | 2010-02-03 | 比亚迪股份有限公司 | Fully stabilized zirconia ceramic material and preparation method thereof |
| CN101880163A (en) * | 2009-05-07 | 2010-11-10 | 宁波大学 | Method for preparing silicon carbide whisker in-situ reinforced aluminum oxide ceramic |
| CN103693988A (en) * | 2013-12-23 | 2014-04-02 | 秦皇岛爱迪特高技术陶瓷有限公司 | Internal dyeing method of dental zirconium oxide restoration body |
| CN106336216A (en) * | 2015-07-07 | 2017-01-18 | 北京欧纳材料科技有限公司 | Zirconia dental ceramic with gradient change color and preparation method thereof |
| CN105565807A (en) * | 2015-12-08 | 2016-05-11 | 河北工业大学 | Zirconia ceramic slurry for manufacturing false tooth as well as preparation method and application thereof |
| CN106631012A (en) * | 2016-12-21 | 2017-05-10 | 汕头大学 | Tetragonal zirconia based composite ceramic ultrathin cover plate and preparation process thereof |
Non-Patent Citations (2)
| Title |
|---|
| 穆柏春等著: "《陶瓷材料的强韧化》", 31 July 2002 * |
| 陆小荣等编: "《陶瓷工艺学》", 31 January 2005 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111803386A (en) * | 2020-06-17 | 2020-10-23 | 深圳市美鸣齿科技术有限公司 | False tooth outer crown and preparation method thereof |
| CN112516381A (en) * | 2020-12-28 | 2021-03-19 | 杭州而然科技有限公司 | Whisker reinforced zirconia implant |
| CN112656990A (en) * | 2020-12-28 | 2021-04-16 | 杭州而然科技有限公司 | Whisker reinforced zirconia planting integrated crown |
| CN112691232A (en) * | 2020-12-28 | 2021-04-23 | 杭州而然科技有限公司 | Whisker reinforced zirconia base |
| CN112691232B (en) * | 2020-12-28 | 2022-05-17 | 杭州而然科技有限公司 | Whisker reinforced zirconia base |
| CN113402282A (en) * | 2021-07-30 | 2021-09-17 | 广东工业大学 | Bionic human bone based on 3D printing and manufacturing method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110204333B (en) | 2021-10-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110204333A (en) | A kind of processing technology for the multilayer zirconium oxide porcelain block that can quickly prepare even transition | |
| US11413122B2 (en) | Controlling of sintering kinetics of oxide ceramics | |
| US11801668B2 (en) | Multilayer oxide ceramic body with aligned sintering behaviour | |
| CN110317059A (en) | A kind of each uniform layering zirconium oxide porcelain block technology of layer contraction | |
| KR101276616B1 (en) | Manufacturing method of dental zirconia block with shade gradient | |
| CN100398489C (en) | Cuttable colored zirconium oxide ceramics and its use | |
| CN108455983B (en) | Darkened zirconia ceramic material and machinable sintered ceramic body made therefrom | |
| CN107175747A (en) | Intensity, dental zirconium oxide repair materials of color even transition and preparation method thereof | |
| JP5943537B2 (en) | Method for producing colored ceramic sintered body especially for dentistry applications | |
| EP4219425A1 (en) | Method for producing zirconia sintered compact | |
| EP4079702A1 (en) | Method for producing zirconia sintered compact | |
| JP2020109069A (en) | Dental ceramic material | |
| Grech et al. | Optimization of two-step sintering conditions of zirconia blanks for dental restorations | |
| US20210363068A1 (en) | Multilayer zirconia ceramic block with uniform transition and method for preparing the same | |
| EP3712121A1 (en) | High permeable zirconia blank capable of sintering at high speed | |
| CN110342926A (en) | The adjusting method of zirconium oxide muffin, Preparation method and use and its shrinkage | |
| CN112341195A (en) | Sintering method of colored zirconia false tooth | |
| JP2022184793A (en) | Method for sintering dental zirconia sintered body | |
| CN115403373A (en) | Zirconia blank and dental restoration | |
| WO2023234399A1 (en) | Zirconia composite sintered body and method for producing same | |
| JP2022066182A (en) | ZIRCONIA CUT BODY FOR DENTAL CUTTING CONTAINING In AND Y | |
| JP2020075862A (en) | Zirconia sintered body and dental product | |
| EP3892461A1 (en) | Zirconia mill blank having layers with different contents of yttria and alumina | |
| JPH0566335B2 (en) |
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 | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A Processing Technology for Quickly Preparing Multilayer Zirconia Ceramic Blocks with Uniform Transition Effective date of registration: 20231220 Granted publication date: 20211012 Pledgee: Chengdu Branch of China CITIC Bank Co.,Ltd. Pledgor: CHENGDU BESMILE BIOTECHNOLOGY Co.,Ltd. Registration number: Y2023980072829 |