CN113213922A - Colored ceramic and preparation method thereof - Google Patents
Colored ceramic and preparation method thereof Download PDFInfo
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- CN113213922A CN113213922A CN202110706328.5A CN202110706328A CN113213922A CN 113213922 A CN113213922 A CN 113213922A CN 202110706328 A CN202110706328 A CN 202110706328A CN 113213922 A CN113213922 A CN 113213922A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 133
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000003086 colorant Substances 0.000 claims abstract description 46
- 239000002002 slurry Substances 0.000 claims abstract description 33
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000000465 moulding Methods 0.000 claims abstract description 22
- 238000000016 photochemical curing Methods 0.000 claims abstract description 16
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 11
- 238000005238 degreasing Methods 0.000 claims abstract description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 72
- 239000000843 powder Substances 0.000 claims description 46
- 239000011224 oxide ceramic Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 8
- 229910052723 transition metal Inorganic materials 0.000 claims description 8
- 150000003624 transition metals Chemical class 0.000 claims description 8
- 230000001590 oxidative effect Effects 0.000 claims description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052574 oxide ceramic Inorganic materials 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052575 non-oxide ceramic Inorganic materials 0.000 claims description 3
- 239000011225 non-oxide ceramic Substances 0.000 claims description 3
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000001723 curing Methods 0.000 abstract description 29
- 238000002835 absorbance Methods 0.000 abstract description 10
- 239000011347 resin Substances 0.000 abstract description 9
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- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 abstract description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract description 6
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- 239000011651 chromium Substances 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 3
- 239000002356 single layer Substances 0.000 description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 description 3
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 description 2
- -1 CoO and Cr Chemical class 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 description 2
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- LYCAIKOWRPUZTN-NMQOAUCRSA-N 1,2-dideuteriooxyethane Chemical group [2H]OCCO[2H] LYCAIKOWRPUZTN-NMQOAUCRSA-N 0.000 description 1
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- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 1
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- GUCYFKSBFREPBC-UHFFFAOYSA-N [phenyl-(2,4,6-trimethylbenzoyl)phosphoryl]-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C(=O)C1=C(C)C=C(C)C=C1C GUCYFKSBFREPBC-UHFFFAOYSA-N 0.000 description 1
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 1
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- 125000001931 aliphatic group Chemical group 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- VFHVQBAGLAREND-UHFFFAOYSA-N diphenylphosphoryl-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C1=CC=CC=C1 VFHVQBAGLAREND-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- YBYGDBANBWOYIF-UHFFFAOYSA-N erbium(3+);trinitrate Chemical compound [Er+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YBYGDBANBWOYIF-UHFFFAOYSA-N 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 description 1
- 235000012736 patent blue V Nutrition 0.000 description 1
- 229920003366 poly(p-phenylene terephthalamide) Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical group [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- 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
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- C04B2235/9661—Colour
Abstract
The invention relates to the technical field of photocuring molding, in particular to a colored ceramic and a preparation method thereof. The preparation method of the color ceramic comprises the steps of carrying out photocuring molding on ceramic slurry containing white and/or light-colored colorants to obtain a ceramic blank, and then sequentially carrying out degreasing and sintering on the ceramic blank to obtain the color ceramic; wherein, the compound and the compound contain CoO and Cr2O3、Fe2O3Compared with the light curing molding of the color ceramic slurry of rare earth metal or transition metal oxide, the ceramic slurry containing white and/or light-colored colorant has low absorbance, high energy for light curing resin, slows down the shallow curing depth in the curing molding process of the ceramic slurry, improves the deformation of a ceramic blank body caused by the shallow curing depth compared with the preset three-dimensional ceramic blank body shape by a computer, and improves the light curing molding of the ceramic slurryEfficiency and precision of the embryo body. The color ceramic and the preparation method thereof can solve the technical problems of low efficiency and low precision of photocuring and forming of the color ceramic.
Description
Technical Field
The invention relates to the technical field of photocuring molding, in particular to a colored ceramic and a preparation method thereof.
Background
In recent years, with the use of a large amount of structural ceramics, such as zirconia ceramics, on the outer surface, a single color has restricted the application of the ceramics and can not meet the requirements of most people on the appearance of structural devices, so that the application field of ceramic materials can be greatly widened by developing rich and colorful colors, and the ceramic materials have wide development prospects.
In order to make the prepared ceramic show color, oxide or other compounds of colored transition metal or rare earth metal, such as CoO and Cr, are added into the light-cured ceramic slurry2O3、Fe2O3And the like. However, the light source wavelength of the light curing device is generally 405nm, and the color ceramic slurry formed after adding the oxide of the transition metal or the rare earth metal or other compounds is dark in color, so that the absorbance of the slurry is increased, the energy of the resin in the light curing color ceramic slurry is reduced, the curing depth is reduced, even the resin cannot be cured, and the efficiency and the precision of the light curing color ceramic are reduced.
Disclosure of Invention
In view of this, the present application provides a color ceramic and a method for preparing the same, which can solve the technical problem of low efficiency and accuracy of forming a color ceramic by photocuring.
The first aspect of the application provides a preparation method of a colored ceramic, which comprises the following steps:
step 2, degreasing and sintering the ceramic blank to obtain color ceramic;
the colorant comprises a white colorant and/or a light-colored colorant that can form a crystalline coloration and/or a colloidal particle coloration.
In addition, CoO and Cr are added2O3、Fe2O3Compared with the color ceramic slurry of rare earth metal or transition metal oxide, the addition of white and/or light-colored colorant which can form molecular coloring and crystal coloring and/or colloidal particle coloring slows down the increase of absorbance caused by the darkening of the color of the ceramic slurry, thereby improving the printing efficiency and precision of the color ceramic.
Preferably, the light-colored colorant comprises a light violet colorant.
It should be noted that the light source of the light curing device is generally a light purple laser with a wavelength of 405nm, and therefore, the selection of the colorant presenting light purple can reduce the absorbance of the ceramic slurry, thereby improving the light curing forming efficiency and precision of the colored ceramic.
Preferably, the photocuring molding comprises SLA molding and/or DLP molding.
Preferably, the photocuring molding is DLP molding;
the DLP forming parameters comprise XY resolution, base layer number, base layer curing time and single-layer curing time;
the XY resolution is 20 μm and 50 μm;
the number of the base layer layers is 3-10;
the curing time of the base layer is 10-40 s;
the single layer curing time is 3-10 s.
Preferably, the degreasing comprises vacuum degreasing and air degreasing.
It should be noted that, the hydrogen element in the photosensitive resin is removed by vacuum degreasing, and then the carbon element in the photosensitive resin is removed by air degreasing, so that the deformation of the ceramic blank body in the degreasing process can be slowed down.
Preferably, the vacuum gel discharging comprises heating to 500 ℃ at a heating rate of 3-10 ℃/min, heating to 650-750 ℃ at a heating rate of 1-5 ℃/min, and then keeping the temperature for 2-5 h.
Preferably, the air gel discharging comprises heating to 500 ℃ at a heating rate of 5-10 ℃/min, heating to 650-750 ℃ at a heating rate of 1-5 ℃/min, and then keeping the temperature for 2-5 h.
Preferably, the sintering comprises heating to 800 ℃ at a heating rate of 5-10 ℃/min, then heating to 1650 ℃ at a heating rate of 1-10 ℃/min, and then keeping the temperature for 1.5-3 h.
Preferably, the preparation method of the ceramic slurry comprises the following steps:
step 101, ball-milling a coloring agent and ceramic powder to obtain composite ceramic powder;
102, ball-milling and mixing the composite ceramic powder, the photosensitive resin, the photoinitiator and the organic solvent to obtain ceramic slurry.
Preferably, the colorant is added in an amount of 5 to 50 wt% in the ceramic slurry.
Preferably, the solid content of the ceramic slurry is 60 to 80 wt%.
Preferably, the colorant has a particle size of less than 20 microns and an absorbance of less than 2.
Preferably, the colorant has a particle size of less than 1 micron and an absorbance of less than 1.
Preferably, the ball milling time in the step 101 and the step 102 is 1-5h, the rotation speed is 150- & lt 350 & gt rad/min, and the ball material mass ratio is 1: 1.5-2.
Preferably, the mass percentage of the photoinitiator is 0.1-3 wt% of the mass of the photosensitive resin.
Preferably, the photosensitive resin comprises one or more of ethoxylated pentaerythritol tetraacrylate, aliphatic urethane acrylate, 1, 6-ethylene glycol diacrylate.
Preferably, the photoinitiator comprises one or more of 2-hydroxy-2-methyl-1-phenyl-1-propanone, phenylbis (2,4, 6-trimethylbenzoyl) phosphine oxide, (2,4, 6-trimethylbenzoyl) diphenylphosphine oxide, and 2-isopropylthioxanthone.
Preferably, the organic solvent comprises one or more of PPTA, cyclohexane, UDPA, ethyl acetate, n-octanol, isopropanol, PEG-300, methyl acetate and the like.
Preferably, the colorant comprises a transition metal and/or a rare earth metal.
It should be noted that the colorant including transition metal and/or rare earth metal may exhibit colors such as red, green, blue, etc. after sintering, since unpaired electrons are present on the outermost layer s and the second outermost layer f of the transition metal and/or rare earth metal ions, and these electrons are very unstable, and are liable to undergo transition between the layers, from the ground state to the excited state, so that, as long as the energy difference between the ground state and the excited state is within the visible light wave energy range, the corresponding monochromatic light is absorbed to exhibit complementary colors.
Preferably, the sintering comprises reducing atmosphere sintering and/or oxidizing atmosphere sintering.
It should be noted that, the transition metal and/or the rare earth metal is sintered in a reducing atmosphere and/or in an oxidizing atmosphere, and a series of chemical reactions can occur to generate color ions of the transition metal and/or the rare earth metal in the form of crystals or colloidal particles, such as red, green, blue, and the like, thereby achieving the effects of crystal coloring and/or colloidal particle coloring.
Preferably, the oxidizing atmosphere sintering comprises air atmosphere sintering.
Preferably, the ceramic powder comprises oxide ceramic powder and/or non-oxide ceramic powder.
Preferably, the oxide ceramic powder comprises one or more of zirconia ceramic powder, alumina ceramic powder, silica ceramic powder, magnesia ceramic powder and titanium oxide ceramic powder.
Preferably, the zirconia ceramic powder comprises yttria-stabilized zirconia ceramic powder.
The second aspect of the present application provides a colored ceramic prepared by the above colored ceramic preparation method.
In summary, the present application provides a colored ceramic and a method for preparing the same; the preparation method of the colored ceramic comprises the steps of firstly carrying out ball milling on white and/or light-colored colorant and ceramic powder to obtain composite ceramic powder, then carrying out photocuring molding on ceramic slurry containing the composite ceramic powder to obtain a ceramic blank, and then sequentially carrying out degreasing and sintering on the ceramic blank to obtain the colored ceramic; wherein, the compound and the compound contain CoO and Cr2O3、Fe2O3Compared with color ceramic slurry such as rare earth metal or transition metal oxide, the ceramic slurry containing the white and/or light-colored colorant has low absorbance, reduces the loss of light curing energy, slows down the lightening of curing depth in the curing and forming process of the ceramic slurry, even can not be cured, improves the deformation of a ceramic blank body caused by the lightening of curing depth compared with the shape of a three-dimensional ceramic blank body preset by a computer, and improves the effect of forming the ceramic blank body by light curingRate and precision; and containing CoO and Cr2O3、Fe2O3When the color of the ceramic blank containing the white and/or light-colored colorant is not changed in the sintering process, the coloring matter in the white or light-colored colorant is subjected to oxidation and/or reduction and other complex chemical reactions in the sintering process to generate coloring ions in the form of crystals or colloid particles, and the coloring ions are like the coloring ions in the form of abundant and colorful glaze after the porcelain is sintered in a kiln, so that the ceramic blank containing the white and/or light-colored colorant is subjected to a process from no/light to obvious color in the sintering process to obtain the colored ceramic.
Description of the drawings:
in order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
FIG. 1 is an absorption spectrum of a zirconia ceramic slurry and an absorption spectrum of a colored zirconia ceramic thereof provided in example 1 of the present application;
fig. 2 shows a zirconia ceramic green body and a colored zirconia ceramic thereof provided in embodiments 1 to 3 of the present application.
The specific implementation mode is as follows:
the application provides a colored ceramic and a preparation method thereof, which can solve the technical problems of low efficiency and low precision of photocuring forming of the colored ceramic.
The technical solutions in the embodiments of the present application will be described clearly and completely below, and it should be understood that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The reagents or raw materials used in the following examples are commercially available or self-made.
Example 1
The embodiment 1 of the present application provides a first method for preparing a color ceramic, which comprises the following steps:
1. preparing ceramic slurry containing zirconia ceramic powder.
1.1, respectively weighing 1 part by mass of colorant powder, 19 parts by mass of 3 mol% yttria stabilized zirconia ceramic powder, taking absolute ethyl alcohol as a dispersing agent, taking zirconia balls as a grinding medium, ball-milling for 2 hours at a rotating speed of 150-350rad/min, drying, and removing ethyl alcohol to obtain zirconia composite powder;
1.2, weighing 10 parts by mass of 1, 6-ethylene glycol diacrylate and 2 parts by mass of organic solvent n-octanol, and uniformly mixing to obtain a premixed solution;
1.3, taking zirconia balls as grinding media, ball-milling and mixing 90 parts by mass of zirconia composite powder, 30 parts by mass of premixed liquid and 0.5 part by mass of photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-acetone for 2 hours, and drying to obtain ceramic slurry containing zirconia ceramic powder;
it should be noted that, the preparation of the ceramic slurry containing zirconia ceramic powder is only a preferred implementation method, and other preparation methods can be adopted in the present application, for example, the sequence of steps 1.1 and 1.2 is changed, and the ceramic slurry is prepared by mixing to obtain a premixed solution, then preparing to obtain zirconia composite powder, and finally preparing to obtain zirconia ceramic slurry;
the colorant powder selected in the present application is selected from colorant powders produced from Jiangxisai porcelain, and the colorant powder contains zirconium oxychloride, erbium nitrate, yttrium nitrate, magnesium carbonate, and aluminum ammonium sulfate, and can form pink colored crystals after sintering.
2. And (5) carrying out photocuring to form the zirconia ceramic blank.
2.1, importing the CAD three-dimensional model of the zirconia ceramic blank into printing software to generate an STL printing file, and setting printing parameters as follows: the XY resolution is 20 mu m, the number of base layers is 7, the base layer curing time is 35s, and the single-layer curing time is 7 s; and slicing and layering the CAD three-dimensional model of the zirconia ceramic blank to form section data and a printing track.
And 2.2, paving the ceramic slurry containing the zirconia ceramic powder on a printing workbench, adopting a high-precision DLP technology of bottom-to-top projection, curing and molding layer by layer, and stacking to form a zirconia ceramic blank body, wherein the color of the zirconia ceramic blank body is white.
3. And preparing the colored zirconia ceramics.
3.1, placing the zirconia ceramic blank in a vacuum glue discharging furnace, heating to 500 ℃ at the heating rate of 3-10 ℃/min, heating to 750 ℃ at the heating rate of 1-5 ℃/min, and then preserving heat for 2-5 h; and then placing the ceramic blank in an air gel removal furnace, heating to 800 ℃ at the heating rate of 5-10 ℃/min, heating to 1650 ℃ at the heating rate of 1-10 ℃/min, and then preserving heat for 1.5-3h to obtain the zirconium oxide ceramic blank after gel removal.
3.2, placing the zirconium oxide ceramic blank after the binder removal in a high-temperature sintering furnace, introducing air, heating to 800 ℃ at the heating rate of 5-10 ℃/min, then heating to 1650 ℃ at the heating rate of 1-10 ℃/min, and then preserving heat for 1.5-3h, and sintering to obtain the pink zirconium oxide ceramic.
FIG. 1-a shows the absorption spectrum of the zirconia ceramic slurry prepared in this example, and FIG. 1-b shows the absorption spectrum of the pink zirconia ceramic prepared in this example, from FIG. 1-a, it can be seen that the absorbance of the zirconia ceramic slurry is low, and the absorbance of the pink zirconia ceramic prepared by sequentially photocuring and sintering the zirconia ceramic slurry is high; based on this, the present application uses the commercial white and/or light-colored ceramic colorant in the field of photocuring molding, and uses CoO and Cr in the prior art2O3、Fe2O3Compared with the rare earth metal or transition metal oxide as the coloring agent for light curing molding, the white and/or light-colored ceramic coloring agent has low absorbance, increases the energy for light curing resin, slows down the lightening of the curing depth in the curing molding process of the ceramic slurry, even can not be cured, improves the deformation of a ceramic blank body caused by the lightening of the curing depth compared with the preset three-dimensional ceramic blank body shape by a computer, and improves the efficiency and the precision of light curing molding of colored ceramic.
Example 2
Example 2 of the present application provides a second method for preparing a colored ceramic, which is different from example 1 in that a second coloring agent is selected, the zirconia ceramic green body obtained by photocuring is light yellow, and the zirconia ceramic obtained by sintering is red.
The colorant powder selected in the present application is selected from colorant powders produced from Jiangxisai porcelain, and the colorant contains chromium nitrate, yttrium nitrate and aluminum nitrate, and can form dark red colored crystals after sintering.
Example 3
Example 3 of the present application provides a third method for preparing a colored ceramic, which is different from example 1 in that a third colorant is selected, and the prepared zirconia ceramic green body is light gray and the zirconia ceramic is blue.
The colorant powder selected in the present application is selected from colorant powders produced from Jiangxisai porcelain, and the colorant powder contains alumina, zinc oxide and nickel oxide, and can form sky-blue colored crystals after sintering.
Example 4
Example 4 of the present application provides a fourth method for preparing a color ceramic, which is different from example 1 in that the forming method of the photocuring-formed zirconia ceramic green body is SLA forming.
Example 5
Example 5 of the present application provides a fifth method for preparing a color ceramic, which is different from example 1 in that the ceramic powder is a silicon carbide ceramic powder in a non-oxide ceramic.
The foregoing is only a preferred embodiment of the present application and it should be noted that modifications can be made by those skilled in the art without departing from the principle of the present application and these modifications should also be considered as the protection scope of the present application.
Claims (10)
1. The preparation method of the colored ceramic is characterized by comprising the following steps of:
step 1, carrying out photocuring molding on ceramic slurry containing a colorant to obtain a ceramic blank;
step 2, degreasing and sintering the ceramic blank to obtain color ceramic;
the colorant comprises a white colorant and/or a light-colored colorant that can form a crystalline coloration and/or a colloidal particle coloration.
2. The method of claim 1, wherein the light-colored colorant comprises a purplish colorant.
3. The method for preparing a colored ceramic according to claim 1, wherein the photocuring molding comprises SLA molding and/or DLP molding.
4. The method of claim 1, wherein the colorant comprises a transition metal and/or a rare earth metal.
5. The method of claim 4, wherein the sintering comprises reducing atmosphere sintering and/or oxidizing atmosphere sintering.
6. The method of claim 5, wherein the oxidizing atmosphere sintering comprises air atmosphere sintering.
7. The method of claim 1, wherein the ceramic slurry comprises an oxide ceramic powder and/or a non-oxide ceramic powder.
8. The method according to claim 7, wherein the oxide ceramic powder comprises one or more of zirconia ceramic powder, alumina ceramic powder, silica ceramic powder, magnesia ceramic powder, and titania ceramic powder.
9. The method according to claim 8, wherein the zirconia ceramic powder comprises yttria-stabilized zirconia ceramic powder.
10. A colored ceramic, characterized by being obtained by the production method according to any one of claims 1 to 9.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107673758A (en) * | 2017-10-30 | 2018-02-09 | 广东工业大学 | A kind of preparation method of ceramic slurry and zirconium oxide base composite ceramic |
| CN111320480A (en) * | 2020-03-02 | 2020-06-23 | 广东省新材料研究所 | 3D printing photocuring ceramic particle and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107673758A (en) * | 2017-10-30 | 2018-02-09 | 广东工业大学 | A kind of preparation method of ceramic slurry and zirconium oxide base composite ceramic |
| CN111320480A (en) * | 2020-03-02 | 2020-06-23 | 广东省新材料研究所 | 3D printing photocuring ceramic particle and preparation method thereof |
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| CN117285349A (en) * | 2023-09-05 | 2023-12-26 | 中国地质大学（武汉） | 3D printing color zirconia ceramic slurry and preparation method and application thereof |
| CN117285349B (en) * | 2023-09-05 | 2024-03-08 | 中国地质大学（武汉） | 3D printing color zirconia ceramic slurry and preparation method and application thereof |
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