CN105669191B - Black zirconia ceramic and preparation method thereof - Google Patents
Black zirconia ceramic and preparation method thereof Download PDFInfo
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- CN105669191B CN105669191B CN201610254718.2A CN201610254718A CN105669191B CN 105669191 B CN105669191 B CN 105669191B CN 201610254718 A CN201610254718 A CN 201610254718A CN 105669191 B CN105669191 B CN 105669191B
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- black zirconia
- oxide
- zirconia ceramics
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 220
- 239000000919 ceramic Substances 0.000 title claims abstract description 100
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 81
- 229910000449 hafnium oxide Inorganic materials 0.000 claims abstract description 29
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 claims abstract description 29
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 23
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 16
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims abstract description 16
- 238000002834 transmittance Methods 0.000 claims abstract description 9
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims abstract description 8
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(II) oxide Inorganic materials [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 8
- 239000011787 zinc oxide Substances 0.000 claims abstract description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910000480 nickel oxide Inorganic materials 0.000 claims abstract description 7
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims abstract description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 6
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 58
- 238000005245 sintering Methods 0.000 claims description 28
- 238000005266 casting Methods 0.000 claims description 27
- 239000000758 substrate Substances 0.000 claims description 27
- 238000000465 moulding Methods 0.000 claims description 25
- 238000003825 pressing Methods 0.000 claims description 25
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 21
- 239000011230 binding agent Substances 0.000 claims description 21
- 238000001746 injection moulding Methods 0.000 claims description 19
- 239000002270 dispersing agent Substances 0.000 claims description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 13
- 238000000498 ball milling Methods 0.000 claims description 10
- 239000007924 injection Substances 0.000 claims description 10
- 238000002347 injection Methods 0.000 claims description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- 238000007766 curtain coating Methods 0.000 claims description 9
- 238000005238 degreasing Methods 0.000 claims description 9
- 239000012467 final product Substances 0.000 claims description 9
- 235000019580 granularity Nutrition 0.000 claims description 9
- 230000003647 oxidation Effects 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- 229910052573 porcelain Inorganic materials 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 238000004080 punching Methods 0.000 claims description 8
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 7
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims description 7
- -1 polypropylene Polymers 0.000 claims description 7
- 229920002125 Sokalan® Polymers 0.000 claims description 6
- 239000004584 polyacrylic acid Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
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- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 4
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- 239000004698 Polyethylene Substances 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- 239000012188 paraffin wax Substances 0.000 claims description 3
- 238000005453 pelletization Methods 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 239000001993 wax Substances 0.000 claims description 3
- 241000208340 Araliaceae Species 0.000 claims 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 claims 1
- 235000003140 Panax quinquefolius Nutrition 0.000 claims 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims 1
- 235000008434 ginseng Nutrition 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 9
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 5
- IUYLTEAJCNAMJK-UHFFFAOYSA-N cobalt(2+);oxygen(2-) Chemical compound [O-2].[Co+2] IUYLTEAJCNAMJK-UHFFFAOYSA-N 0.000 abstract 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 abstract 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- 239000000047 product Substances 0.000 description 9
- 230000008859 change Effects 0.000 description 8
- 239000003086 colorant Substances 0.000 description 7
- 229910052845 zircon Inorganic materials 0.000 description 7
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 6
- 239000012298 atmosphere Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000010941 cobalt Substances 0.000 description 4
- 229910017052 cobalt Inorganic materials 0.000 description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- 229910052726 zirconium Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 206010008190 Cerebrovascular accident Diseases 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- 208000006011 Stroke Diseases 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 241001044369 Amphion Species 0.000 description 1
- 241001280173 Crassula muscosa Species 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical group [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 241000872198 Serjania polyphylla Species 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- 230000007815 allergy Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- KQHQLIAOAVMAOW-UHFFFAOYSA-N hafnium(4+) oxygen(2-) zirconium(4+) Chemical compound [O--].[O--].[O--].[O--].[Zr+4].[Hf+4] KQHQLIAOAVMAOW-UHFFFAOYSA-N 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 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
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses black zirconia ceramic material composition which comprises the following components in percentage by mass: 0-5% of ferric oxide, 0-5% of cobaltous oxide, 0-5% of chromic oxide, 0-5% of aluminum oxide, 0-5% of nickel oxide, 0-5% of manganese oxide, 0-5% of zinc oxide, 2-6% of yttrium oxide, 0-5% of titanium oxide, 0-5% of silicon dioxide, 0-5% of cerium oxide and the balance of zirconium oxide containing hafnium oxide. The black zirconia ceramic material composition disclosed by the invention is small in powder granularity and uniform in distribution, and black zirconia ceramic containing the black zirconia ceramic material composition is relatively good in covering power, high in blackness and relatively low in transmittance of light. Meanwhile the invention further discloses black zirconia ceramic prepared from the black zirconia ceramic material composition and a preparation method of the black zirconia ceramic.
Description
Technical field
The present invention relates to a kind of ceramic material and preparation method thereof, especially a kind of zirconia ceramics material and its preparation side
Method.
Background technology
Zirconium dioxide due to excellent mechanics, calorifics, electric property, in structural material, optical element, oxygen sensitive element
Have a wide range of applications with the aspect such as fuel cell.In recent years, the high speed development with people to ornament demand, black oxidation
Zircon ceramic becomes high-grade decoration with its excellent mechanical performance, chromatic colour, metallic luster and the features such as act on without allergy
New lover's material, has wide market prospect in high-grade watch chain, bangle, phone housing etc..
The preparation of black zirconia ceramics at present mainly adopts following two methods：1st, zirconia ceramicss are carried out very
Black in empty, reducing atmosphere or inert atmosphere, form Lacking oxygen, so as to form the point defect of colour center, produce the absorption to light and imitate
Should；2nd, the colorant oxide such as doping iron, cobalt, nickel in zirconium oxide, by adding absorption of the colorant raising to light, so as to improve oxygen
Change the covering power and blackness of zirconia material.Using vacuum drying oven, reducing atmosphere stove or inert atmosphere stove, need zirconium oxide in atmosphere
Sinter porcelain into, then black in above-mentioned sintering furnace, do so has been significantly greatly increased the cost of production technology, to special shape and thickness
The product for differing, easily because colour center inhomogeneities cause aberration occur, causes not enough grade of product blackness one to be during nigrescence
Row problem.And in zirconium oxide the colorant oxide such as doping iron, cobalt, nickel, due to each oxide it is inconsistent to the absorbing wavelength of light,
Easily cause black not black, product colour occur it is partially red, partially blue, partially green situations such as.And institute's oxygenates easily rise with yttrium, zirconium
Reaction, the stability of disruptive oxidation zirconium easily causes product Transformation Cracking.In preparation process to colorant addition and temperature
Require more strictly, once management and control is bad to be easy for the problems such as color differs between batch occur.
From the foregoing, existing black zirconia ceramics are present, Color uniformity is poor, and blackness is not enough, and light transmission is good, color
The bad shortcoming such as hiding lack.The requirement of the outward appearance elements such as high blackness mobile phone board cannot be met.
The content of the invention
It is an object of the invention to overcome above-mentioned the deficiencies in the prior art part and provide a kind of with higher covering power
Black zirconia ceramics material compositions relatively low with blackness, transmittance and the black zirconia ceramics containing the compositionss.
Meanwhile, present invention also offers the preparation method of the black zirconia ceramics.
For achieving the above object, the technical scheme taken of the present invention is：A kind of black zirconia ceramics material compositions, bag
Composition containing following weight/mass percentage composition：Ferrum oxide 0-5%, cobalt oxide 0-5%, chromium oxide 0-5%, aluminium oxide 0-5%, oxidation
Nickel 0-5%, manganese oxide 0-5%, Zinc Oxide 0-5%, yittrium oxide 2-6%, titanium oxide 0-5%, silicon dioxide 0-5%, cerium oxide
0-5%, the balance of zirconium oxide containing hafnium oxide.
The present invention black zirconia ceramics material compositions in, with the addition of the coloring agent of black, can significantly improve by
The covering power of its black zirconia ceramics for preparing and black, reduce transmittance.
It is described containing hafnium oxide as the preferred implementation of black zirconia ceramics material compositions of the present invention
In zirconium oxide, the weight/mass percentage composition of the hafnium oxide is less than 50%.
As the preferred implementation of black zirconia ceramics material compositions of the present invention, the black zirconia pottery
Composition of the ceramic material compositionss comprising following weight/mass percentage composition：Ferrum oxide 2-4%, cobalt oxide 1.5-3.5%, chromium oxide 1.5-
3.5%th, aluminium oxide 2-4%, nickel oxide 2-4%, manganese oxide 1.5-3.5%, Zinc Oxide 1.5-3.5%, yittrium oxide 2-4%, oxygen
Change titanium 1.5-3.5%, silica 1 .5-3.5%, cerium oxide 1.5-3.5%, the balance of zirconium oxide containing hafnium oxide.
As the preferred implementation of black zirconia ceramics material compositions of the present invention, the black zirconia pottery
Ceramic material compositionss are powder body, and powder body D50 granularities are 0.1-3 μm, and specific surface area is 5-25m2/g。
In addition, another object of the present invention is to providing a kind of black with high blackness, high light-proofness and low light transmission
Zirconia ceramicss, in order to achieve this, the technical scheme that the present invention takes is：A kind of black zirconia ceramics, the black oxygen
Change zircon ceramic and include black zirconia ceramics material compositions as above.
The black zirconia ceramics of the present invention contain black zirconia ceramics material compositions as above, with higher
Covering power and blackness, be provided simultaneously with relatively low transmittance.The black zirconia ceramics of the present invention are by black oxidation described above
After zircon ceramic material compositions are prepared from, formed to the oxygen containing hafnium oxide by atoms such as ferrum, cobalt, chromium, aluminum, nickel, manganese, zinc
Change the Surface coating of zirconium crystal grain, one layer of oxide skin(coating) is formed on the zirconia grains surface containing hafnium oxide, by different colorants
Absorption to visible wavelength, so as to reduce reflection of the light on zirconia ceramicss surface, and can have under less than 1mm thickness
The covering power that high blackness is become reconciled.And due to being doped using surface coating technology, neither affect yttria-zirconia
Stable system solid solution, while inhibited oxidation zirconium crystal grain is grown up, can effectively improve the ageing resistace of zirconia ceramicss and thermally-stabilised
Property.
Used as the preferred implementation of black zirconia ceramics of the present invention, the black zirconia ceramics are thick for polishing
Transmittance ＜ 0.5, OD values ＞ 3.0, the potsherd of chromatic value L≤45 under degree 0.1-1.0mm, 550nm wavelength.
Finally, it is still another object of the present invention to provide a kind of process is simple, the black oxidation described above for facilitating implementation
The preparation method of zircon ceramic, in order to achieve this, the technical scheme that the present invention takes is：A kind of black zirconia pottery as described above
The preparation method of porcelain, comprises the following steps：
(1) each composition contained by black zirconia ceramics material compositions is mixed, obtains black zirconia ceramics material
Compositionss；
(2) the black zirconia ceramics material compositions that step (1) is obtained are carried out into molding, roasting obtains black zirconia
Ceramics；
Flow casting molding, dry-pressing formed, injection moulding, hot-forming or gel casting are shaped in the step (2).
The preparation method of black zirconia ceramics of the present invention, the Zirconium powder granularity of preparation is little, is uniformly dispersed, and mixes
Miscellaneous oxide is evenly coated at Zirconium powder surface, can effectively improve powder active, and processability is excellent, can meet dry
The different ceramic demands using technique such as pressure, curtain coating, injection, the ceramic section for being sintered is fine and close, the defect such as pore-free, crackle.
It is easy to operate and the technique is prepared simply, do not increase production process and workload, volume production is capable of achieving, with preferably stable
Property, homogenizing for product can be realized.
The black zirconia ceramics prepared using the method for the invention, into porcelain density >=5.8g/cm3, 3 points resist
Folding intensity >=1200Mpa, Vickers hardness >=1200.
As the preferred implementation of the preparation method of black zirconia ceramics of the present invention, in the step (2)
It is shaped to flow casting molding, dry-pressing formed or injection moulding；
The flow casting molding is comprised the following steps：
(1a) ball milling：The black zirconia ceramics material compositions are mixed with dispersant and binding agent in ball mill
Uniformly；
(2a) flow casting molding：Slurry after ball milling is uniformly dispersed carries out flow casting molding in casting machine, adjusts curtain coating work
Skill parameter, is obtained curtain coating base substrate of the thickness for 0.2-1.1mm；
(3a) punch forming：Obtained curtain coating base substrate is put in the mould for designing carries out punch forming, and punching press is obtained
Base；
(4a) dumping sintering：Punching press base substrate is carried out into dumping sintering, the wherein dumping time is 60-100h, and sintering time is
40-60h, obtains final product the black zirconia ceramics；
It is described dry-pressing formed to comprise the following steps：
(1b) ball milling pelletize：By the black zirconia ceramics material compositions and dispersant, binding agent in ball mill
Mix homogeneously, and drying-granulating is carried out on sponging granulator；
(2b) dry-pressing：The good powder body of pelletize is laid in the dry pressing die set for designing carries out dry-pressing formed, prepared dry-pressing
Base；
(3b) dumping sintering：Punching press base substrate is carried out into dumping sintering, the wherein dumping time is 60-100h, and sintering time is
40-60h, obtains final product the black zirconia ceramics；
The injection moulding is comprised the following steps：
(1c) internally mix：The black zirconia ceramics material compositions and binding agent are carried out in internal mixer to mix
It is even, make injection molding raw material；
(2c) pelletize：The pockets of raw material of internally mix is carried out extruding pelletization in comminutor, granule of uniform size is produced
Material, particle length is in 2-3mm；
(3c) injection moulding：The good particulate material of pelletize is carried out molding using injection (mo(u)lding) machine, base substrate, injection temperature is produced
Degree is 160-175 DEG C, and injection pressure is 30-60Mpa；
(4c) defat：First the good base substrate of injection moulding is put in solvent carries out extraction dewaxing, then the base substrate of de- good wax
Put into and carry out in draft glue discharging furnace thermal debinding, solvent degreasing temperature is 45-55 DEG C, and degreasing time is 15-20h, and thermal debinding temperature is
400-500 DEG C, degreasing time is 45-55h；
(5c) sinter：The base substrate for having taken off fat is put in sintering furnace and is sintered, make base substrate into porcelain, sintering temperature 1300-
1600 DEG C, sintering time is 25-35h, obtains final product the black zirconia ceramics.
As the preferred implementation of the preparation method of black zirconia ceramics of the present invention, in the flow casting molding,
Dispersant in step (1a) is at least one in polyacrylic acid, Polyethylene Glycol and glycerol, the bonding in the step (1a)
Agent is at least one in PVB, DOP, BBP, DBP；It is described it is dry-pressing formed in, the dispersant in step (1b) be PEG, DBS and
At least one of polyacrylic acid apoplexy due to endogenous wind, the binding agent in step (1b) is at least one in PVA, PMMA；The injection moulding
In, the binding agent in step (1c) is the mixture of polypropylene, polyethylene and paraffin.
In the flow casting molding, dispersing uniformity of the powder in casting slurry directly affects the quality of base film, so as to shadow
Ring the series of characteristics such as compactness, the porosity and the mechanical property of material.In tape-casting commonly use dispersant have nonionic,
Anion, cation and the type of amphion 4.Dispersant prioritizing selection polyacrylic acid；During flow casting molding, in order to base
Panel material is separated and taking and placing are convenient, and casting films must possess certain intensity, toughness and ductility.For this purpose, needing to add in the slurry
Enter binding agent.Binding agent is divided into nonionic, anion and the class of cation 3, binding agent preferred PVB, DOP, BBP, DBP by functional group
One or more.It is described it is dry-pressing formed in, the dispersibility of powder body directly affects the mobility and apparent density of powder body in dry-pressing,
Further affect compactness, the porosity and the mechanical property of material.Conventional dispersant is one kind of PEG, DBS and polyacrylic
Or it is several.And binding agent then affects the intensity of dry-pressing base, it is generally preferable to PVA, PMMA etc. one or more.
Black zirconia ceramics material compositions of the present invention, powder granularity is little, is uniformly dispersed, the black oxygen containing it
Change zircon ceramic and there is higher covering power and blackness, with relatively low transmittance.Black zirconia ceramics of the present invention, ferrum,
The atoms such as cobalt, chromium, aluminum, nickel, manganese form the Surface coating to the zirconia grains containing hafnium oxide, in the oxidation containing hafnium oxide
Zirconium grain surface forms one layer of oxide skin(coating), by absorption of the different colorants to visible wavelength, so as to reduce light in oxidation
The reflection on zircon ceramic surface, and less than the covering power that can have under 1mm thickness high blackness to become reconciled.Black oxygen of the present invention
Change the preparation method of zircon ceramic material, technique is prepared simply, easy to operate, does not increase production process and workload, be capable of achieving volume production,
With preferable stability, homogenizing for product can be realized.
Specific embodiment
To better illustrate the object, technical solutions and advantages of the present invention, below in conjunction with specific embodiment to the present invention
It is described further.
Embodiment 1
A kind of embodiment of black zirconia ceramics material compositions of the present invention, black zirconia ceramics described in the present embodiment
Material compositions contain the component of following weight/mass percentage composition：Yittrium oxide 6%, the balance of zirconium oxide containing hafnium oxide；It is described
In zirconium oxide containing hafnium oxide, weight/mass percentage composition of the hafnium oxide in the zirconium oxide containing hafnium oxide is 30%.
The black zirconia ceramics material compositions of the present embodiment are powder body, and the powder body D50 granularities are 3 μm, specific surface
Product is 5m2/g。
Embodiment 2
A kind of embodiment of black zirconia ceramics material compositions of the present invention, black zirconia ceramics described in the present embodiment
Material compositions contain the component of following weight/mass percentage composition：Ferrum oxide 2%, cobalt oxide 1.5%, chromium oxide 1.5%, aluminium oxide
4%th, nickel oxide 2%, manganese oxide 3.5%, Zinc Oxide 1.5%, yittrium oxide 4%, titanium oxide 3.5%, silicon dioxide 3.5%, oxygen
Change cerium 3.5%, the balance of zirconium oxide containing hafnium oxide；In the zirconium oxide containing hafnium oxide, hafnium oxide contains described
Weight/mass percentage composition in the zirconium oxide of hafnium oxide is 15%.
The black zirconia ceramics material compositions of the present embodiment are powder body, and the powder body D50 granularities are 1 μm, specific surface
Product is 20m2/g。
Embodiment 3
A kind of embodiment of black zirconia ceramics material compositions of the present invention, black zirconia ceramics described in the present embodiment
Material compositions contain the component of following weight/mass percentage composition：Ferrum oxide 3%, cobalt oxide 2%, chromium oxide 3.5%, aluminium oxide
3%th, nickel oxide 2.5%, manganese oxide 3%, Zinc Oxide 3%, yittrium oxide 3%, titanium oxide 3%, silicon dioxide 3%, cerium oxide
3%, the balance of zirconium oxide containing hafnium oxide；In the zirconium oxide containing hafnium oxide, hafnium oxide contains hafnium oxide described
Zirconium oxide in weight/mass percentage composition be 10%.
The black zirconia ceramics material compositions of the present embodiment are powder body, and the powder body D50 granularities are 2 μm, specific surface
Product is 15m2/g。
Embodiment 4
A kind of embodiment of black zirconia ceramics material compositions of the present invention, black zirconia ceramics described in the present embodiment
Material compositions contain the component of following weight/mass percentage composition：Ferrum oxide 4%, cobalt oxide 3.5%, chromium oxide 4%, aluminium oxide
2%th, nickel oxide 4%, manganese oxide 1.5%, Zinc Oxide 3.5%, yittrium oxide 2%, titanium oxide 1.5%, silica 1 .5%, oxygen
Change cerium 1.5%, the balance of zirconium oxide containing hafnium oxide；In the zirconium oxide containing hafnium oxide, hafnium oxide contains described
Weight/mass percentage composition in the zirconium oxide of hafnium oxide is 20%.
The black zirconia ceramics material compositions of the present embodiment are powder body, and the powder body D50 granularities are 0.1 μm, compare table
Area is 25m2/g。
Embodiment 5
A kind of embodiment of black zirconia ceramics material compositions of the present invention, black zirconia ceramics described in the present embodiment
Material compositions contain the component of following weight/mass percentage composition：Ferrum oxide 5%, cobalt oxide 5%, chromium oxide 5%, aluminium oxide 5%,
Nickel oxide 5%, manganese oxide 5%, Zinc Oxide 5%, yittrium oxide 5%, titanium oxide 5%, silicon dioxide 5%, cerium oxide 5%, surplus
It is the zirconium oxide containing hafnium oxide；In the zirconium oxide containing hafnium oxide, hafnium oxide is in the zirconium oxide containing hafnium oxide
In weight/mass percentage composition be 5%.
The black zirconia ceramics material compositions of the present embodiment are powder body, and the powder body D50 granularities are 2.5 μm, compare table
Area is 10m2/g。
Embodiment 6
The performance test of black zirconia ceramics
The present embodiment arranges test group 1～5, and the black zirconia ceramics material of the test group 1～5 is respectively adopted enforcement
The black zirconia ceramics material compositions of example 1～5 are prepared from, and the black zirconia of test group 1～5 adopts same preparation
Method is prepared from, and the preparation method is comprised the following steps：
(1) by each material mixing contained by black zirconia ceramics material compositions, black zirconia ceramics material is obtained
Compositionss；
(2) the black zirconia ceramics material compositions that step (1) is obtained are carried out into molding, roasting obtains black zirconia
Ceramics；
Flow casting molding, dry-pressing formed, injection moulding, hot-forming or gel casting are shaped in the step (2).
Wherein, the flow casting molding is comprised the following steps：
(1a) ball milling：By the black zirconia ceramics material compositions, (dispersant is excellent with dispersant and binding agent
Select at least one in polyacrylic acid, Polyethylene Glycol and glycerol, at least in the binding agent preferred PVB, DOP, BBP, DBP
Kind) mix homogeneously in ball mill；
(2a) flow casting molding：Slurry after ball milling is uniformly dispersed carries out flow casting molding in casting machine, adjusts curtain coating work
Skill parameter, is obtained curtain coating base substrate of the thickness for 0.2-1.1mm；
(3a) punch forming：Obtained curtain coating base substrate is put in the mould for designing carries out punch forming, and punching press is obtained
Base；
(4a) dumping sintering：Punching press base substrate is carried out into dumping sintering, the wherein dumping time is 60-100h, and sintering time is
40-60h, obtains final product the black zirconia ceramics；
It is described dry-pressing formed to comprise the following steps：
(1b) ball milling pelletize：By the black zirconia ceramics material compositions and dispersant, the binding agent (dispersant
It is preferred that at least one of PEG, DBS and polyacrylic acid apoplexy due to endogenous wind, at least one in the binding agent preferred PVA, PMMA) in ball milling
Mix homogeneously in machine, and drying-granulating is carried out on sponging granulator；
(2b) dry-pressing：The good powder body of pelletize is laid in the dry pressing die set for designing carries out dry-pressing formed, prepared dry-pressing
Base；
(3b) dumping sintering：Punching press base substrate is carried out into dumping sintering, the wherein dumping time is 60-100h, and sintering time is
40-60h, obtains final product the black zirconia ceramics；
The injection moulding is comprised the following steps：
(1c) internally mix：By the black zirconia ceramics material compositions and binding agent (the preferred polypropylene of the binding agent,
The mixture of polyethylene and paraffin) mix homogeneously is carried out in internal mixer, make injection molding raw material；
(2c) pelletize：The pockets of raw material of internally mix is carried out extruding pelletization in comminutor, granule of uniform size is produced
Material, particle length is in 2-3mm；
(3c) injection moulding：The good particulate material of pelletize is carried out molding using injection (mo(u)lding) machine, base substrate, injection temperature is produced
Degree is 160-175 DEG C, and injection pressure is 30-60Mpa；
(4c) defat：First the good base substrate of injection moulding is put in solvent carries out extraction dewaxing, then the base substrate of de- good wax
Put into and carry out in draft glue discharging furnace thermal debinding, solvent degreasing temperature is 45-55 DEG C, and degreasing time is 15-20h, and thermal debinding temperature is
400-500 DEG C, degreasing time is 45-55h；
(5c) sinter：The base substrate for having taken off fat is put in sintering furnace and is sintered, make base substrate into porcelain, sintering temperature 1300-
1600 DEG C, sintering time is 25-35h, obtains final product the black zirconia ceramics.
The molding mode that test group 1～5 is adopted is identical, and the polishing thickness of the black zirconia ceramics of test group 1～5 is also equal
Identical (being 0.5mm).Transmittance, OD values, colourity under the 550nm wavelength of the black zirconia ceramics for surveying test group 1～5 respectively
Value, into porcelain density, 3 rupture strengths and Vickers hardness, test result is as shown in table 1.
The performance test results of the black zirconia ceramics of table 1
| Project | Test group 1 | Test group 2 | Test group 3 | Test group 4 | Test group 5 |
| Transmittance under 550nm wavelength | 0.45 | 0.40 | 0.10 | 0.35 | 0.40 |
| OD values | 3.5 | 3.8 | 6.0 | 3.5 | 4.0 |
| Chromatic value | 45 | 42 | 20 | 40 | 44 |
| Into porcelain density (g/cm3) | 5.8 | 6.0 | 6.1 | 5.9 | 6.1 |
| 3 rupture strengths (Mpa) | 1200 | 1250 | 1240 | 1220 | 1210 |
| Vickers hardness | 1200 | 1234 | 1225 | 1205 | 1225 |
As seen from the results in Table 1, black zirconia ceramics of the invention have higher covering power and black, relatively low printing opacity
Degree, the especially black zirconia ceramics of test group 3, effect is more preferable.
It is last to should be noted that above example only to illustrate technical scheme rather than protect to the present invention
The restriction of shield scope, although being explained in detail to the present invention with reference to preferred embodiment, one of ordinary skill in the art should
Understand, technical scheme can be modified or equivalent, without deviating from the essence of technical solution of the present invention
And scope.
Claims (7)
1. a kind of black zirconia ceramics material compositions, it is characterised in that the composition comprising following weight/mass percentage composition：Oxidation
Ferrum 2-4%, cobalt oxide 1.5-3.5%, chromium oxide 1.5-3.5%, aluminium oxide 2-4%, nickel oxide 2-4%, manganese oxide 1.5-
3.5%th, Zinc Oxide 1.5-3.5%, yittrium oxide 2-4%, titanium oxide 1.5-3.5%, silica 1 .5-3.5%, cerium oxide
1.5-3.5%, the balance of zirconium oxide containing hafnium oxide.
2. black zirconia ceramics material compositions as claimed in claim 1, it is characterised in that the black zirconia ceramics
Material compositions are powder body, and powder body D50 granularities are 0.1-3 μm, and specific surface area is 5-25m2/g。
3. a kind of black zirconia ceramics, it is characterised in that the black zirconia ceramics comprising as claim 1～2 it is arbitrary
Black zirconia ceramics material compositions described in.
4. black zirconia ceramics as claimed in claim 3, it is characterised in that the black zirconia ceramics are polishing thickness
Transmittance ＜ 0.5, OD values ＞ 3.0, the potsherd of chromatic value L≤45 under 0.1-1.0mm, 550nm wavelength.
5. a kind of preparation method of the black zirconia ceramics as described in claim 3 or 4, it is characterised in that comprise the following steps：
(1) each composition contained by black zirconia ceramics material compositions is mixed, obtains black zirconia ceramics combination of materials
Thing；
(2) the black zirconia ceramics material compositions that step (1) is obtained are carried out into molding, roasting obtains black zirconia pottery
Porcelain；
Flow casting molding, dry-pressing formed, injection moulding, hot-forming or gel casting are shaped in the step (2).
6. the preparation method of black zirconia ceramics as claimed in claim 5, it is characterised in that in the step (2) into
Type is flow casting molding, dry-pressing formed or injection moulding；
The flow casting molding is comprised the following steps：
(1a) ball milling：The black zirconia ceramics material compositions are mixed with dispersant and binding agent in ball mill
It is even；
(2a) flow casting molding：Slurry after ball milling is uniformly dispersed carries out flow casting molding in casting machine, adjusts casting technique ginseng
Number, is obtained curtain coating base substrate of the thickness for 0.2-1.1mm；
(3a) punch forming：Obtained curtain coating base substrate is put in the mould for designing carries out punch forming, and blank is obtained；
(4a) dumping sintering：Punching press base substrate is carried out into dumping sintering, the wherein dumping time is 60-100h, and sintering time is 40-
60h, obtains final product the black zirconia ceramics；
It is described dry-pressing formed to comprise the following steps：
(1b) ball milling pelletize：The black zirconia ceramics material compositions are mixed with dispersant, binding agent in ball mill
Uniformly, and on sponging granulator drying-granulating is carried out；
(2b) dry-pressing：The good powder body of pelletize is laid in the dry pressing die set for designing carries out dry-pressing formed, prepared dry-pressing base；
(3b) dumping sintering：Punching press base substrate is carried out into dumping sintering, the wherein dumping time is 60-100h, and sintering time is 40-
60h, obtains final product the black zirconia ceramics；
The injection moulding is comprised the following steps：
(1c) internally mix：The black zirconia ceramics material compositions are mixed homogeneously with binding agent in internal mixer, is made
Make injection molding raw material；
(2c) pelletize：The pockets of raw material of internally mix is carried out extruding pelletization in comminutor, particulate material of uniform size is produced,
Grain length is in 2-3mm；
(3c) injection moulding：The good particulate material of pelletize is carried out molding using injection (mo(u)lding) machine, base substrate is produced, injection temperature is
160-175 DEG C, injection pressure is 30-60Mpa；
(4c) defat：First the good base substrate of injection moulding is put in solvent carries out extraction dewaxing, then the base substrate for taking off good wax is put into
Thermal debinding is carried out in draft glue discharging furnace, solvent degreasing temperature is 45-55 DEG C, degreasing time is 15-20h, thermal debinding temperature is 400-500
DEG C, degreasing time is 45-55h；
(5c) sinter：The base substrate for having taken off fat is put in sintering furnace and is sintered, make base substrate into porcelain, sintering temperature 1300-1600
DEG C, sintering time is 25-35h, obtains final product the black zirconia ceramics.
7. the preparation method of black zirconia ceramics as claimed in claim 6, it is characterised in that in the flow casting molding, step
Suddenly the dispersant in (1a) is at least one in polyacrylic acid, Polyethylene Glycol and glycerol, the binding agent in the step (1a)
For at least one in PVB, DOP, BBP, DBP；It is described it is dry-pressing formed in, the dispersant in step (1b) is PEG, DBS and poly-
At least one in acrylic compounds, the binding agent in step (1b) is at least one in PVA, PMMA；In the injection moulding,
Binding agent in step (1c) is the mixture of polypropylene, polyethylene and paraffin.
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