Preparation method of photocuring bionic color zirconium oxide material
By doping alumina into zirconia materials and controlling the sintering process, a biomimetic zirconia material with high strength, high toughness, and a color close to that of teeth was prepared. This solved the problems of low strength and uneven color of zirconia materials in the prior art and enabled efficient photopolymerization 3D printing.
Patent Information
- Application Number
- CN202410625384.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-05-20
- Publication Date
- 2025-11-21
AI Technical Summary
Existing technologies make it difficult to directly prepare biomimetic zirconia materials that closely resemble the natural color of teeth and have high strength and toughness through photopolymerization 3D printing. Furthermore, the low strength and low bonding strength of veneers reduce the success rate of zirconia denture restorations.
A mixed slurry containing alumina, modifiers, and solvents is used to form elongated grains through pre-sintering. Combined with a color developer and a photocurable slurry, a photocurable biomimetic zirconia material is prepared. The transformation of tetragonal zirconia grains is controlled to improve the strength and toughness of the material, and the color of the material is controlled through a precise sintering process.
The preparation of biomimetic colored zirconia materials with high strength, high toughness, and near-tooth color has been achieved, avoiding the problems of uneven expansion of zirconia grains and dark color, thus improving the molding quality and aesthetic effect of the material.
Abstract
Description
TECHNICAL FIELD
[0001] The application relates to the field of light-cured preparation of zirconia materials, in particular to the field of a light-cured biomimetic color zirconia material preparation method. BACKGROUND
[0002] Zirconia has excellent mechanical properties and biocompatibility and is widely used in the field of oral cavity repair.
[0003] 3D printing is more suitable for forming complex dentures and veneers due to its additive manufacturing characteristics. However, the strength of zirconia material is low, and 3D printed zirconia material is mostly chalky. In order to achieve a more natural tooth color and an aesthetic repair effect, post-ceramic decoration is required. However, the low strength and low bonding force of the ceramic decoration greatly reduce the success rate of zirconia denture repair, and the preparation process is complex.
[0004] Therefore, how to directly prepare a biomimetic color zirconia material close to the natural tooth color through light-cured 3D printing forming, and how to make the material have high strength and good toughness have become a difficult problem to be solved in the field. SUMMARY
[0005] The purpose of the present application is to provide a light-cured biomimetic color zirconia material preparation method, which directly prepares a biomimetic color zirconia material close to the natural tooth color through light-cured 3D printing forming, and the material has high strength and good toughness.
[0006] The application provides a light-cured biomimetic color zirconia material preparation method, which prepares an alumina mixed slurry, wherein the alumina mixed slurry comprises alumina, a modifying additive and a solvent, and the modifying additive comprises a strontium source and a chromium source.
[0007] The alumina mixed slurry is dried to obtain modified alumina, and the modified alumina is alumina with strontium elements and chromium elements attached to the surface of the alumina.
[0008] A ceramic mixed material slurry is prepared, and the ceramic mixed material slurry comprises zirconia powder and modified alumina.
[0009] After the ceramic mixed material slurry is dried, pre-sintering is performed to obtain a primary mixed ceramic material, and the pre-sintering temperature is 1000-1250 DEG C. The primary mixed ceramic material comprises long strip-shaped crystal grains.
[0010] The primary mixed ceramic material is ground and sieved to obtain a mixed ceramic material.
[0011] A light-cured slurry is prepared from the mixed ceramic material, and the light-cured slurry comprises the mixed ceramic material and a color developing agent.
[0012] The light-cured slurry is used to prepare a light-cured biomimetic color zirconia material blank through 3D printing.
[0013] The light-cured biomimetic color zirconia material blank is degreased and sintered to obtain the light-cured biomimetic color zirconia material.
[0014] The present application has the beneficial effect over the prior art that by the ceramic mixed slurry comprising zirconia powder and modified alumina, the alumina is doped in the zirconia, thereby improving the strength of the finished material;
[0015] The alumina mixed slurry comprises alumina, modified additives and solvent, the modified additives comprise strontium source and chromium source, the ceramic mixed slurry is dried and then pre-sintered to obtain the primary mixed ceramic material, and the pre-sintering temperature is 1000-1250 DEG C; in the pre-sintering process, the alumina powder reacts with the strontium source and the chromium source to obtain long strip-shaped grains, and the long strip-shaped grains obtained at this temperature are more and not too long, thereby avoiding the transformation of the zirconia tetragonal grains into monoclinic grains during the cooling after pre-sintering and the subsequent cooling after sintering, that is, the volume of the zirconia tetragonal grains expands to the periphery during the transformation of the zirconia tetragonal grains into monoclinic grains, and the existence of the long strip-shaped grains around the tetragonal grains inhibits the expansion of the zirconia grains, thereby avoiding the transformation of the zirconia tetragonal grains into monoclinic grains during the cooling process, and the high-toughness zirconia toughened alumina ceramic material obtained has a high content of tetragonal grains, thereby significantly improving the toughness of the high-toughness zirconia toughened alumina ceramic material, and simultaneously being beneficial to avoiding the reduction of the strength caused by the non-uniform internal structure of the material due to the overgrowth or non-uniform size of the long strip-shaped grains;
[0016] The light-cured slurry comprises mixed ceramic material and color developing agent, which can avoid the poor forming during the light-curing process caused by the deep color in the light-cured slurry, and can realize the color development after the sintering of the ligand obtained by the light-curing, thereby realizing that the light-cured biomimetic color zirconia material prepared has a biomimetic color close to the actual color of teeth.
[0017] Further, the preparation process of the alumina mixed slurry comprises the following steps:
[0018] The alumina, modified additives and solvent are mixed in a mass ratio of (70-80):(16-21):(90-110) to obtain the alumina mixed slurry.
[0019] The mass ratio of the strontium source and the chromium source is (2-4.5):(0.5-2.5).
[0020] The strontium source and the chromium source are both salt compounds.
[0021] The beneficial effect of the above step is that the long strip grain is suitable, and the long strip grain is too small to control the zirconia crystal phase, which reduces the toughness of the zirconia toughened alumina ceramic material.
[0022] Further, the strontium source includes one or more of strontium carbonate, strontium acetate, strontium oxalate, and strontium chloride;
[0023] The chromium source includes one or more of chromium oxide, chromium acetate, and chromium chloride.
[0024] The beneficial effect of the above step is that the strontium source and the chromium source are salts, which improves the generation rate of long strip grains.
[0025] Further, the ceramic mixture slurry preparation process is to mix zirconia powder, modified alumina, sintering aid, iron yttrate, and water in a mass ratio of (15-25):(72.5-88):(1-2.5):(1-1.5):(100-120) to obtain the ceramic mixture slurry; preferably, the sintering aid includes magnesium oxide and / or calcium oxide.
[0026] and / or
[0027] The drying temperature of the alumina mixed slurry to obtain modified alumina is 90-200°C.
[0028] The beneficial effect of the above step is that the long strip grain around the zirconia tetragonal grain is inhibited during sintering, which avoids the transformation of the zirconia tetragonal grain into monoclinic grain, thereby obtaining a high content of zirconia tetragonal grain in the finished material, thereby significantly improving the light-cured biomimetic color zirconia material; at the same time, it is beneficial to reduce the addition of stabilizers, i.e. without the need to increase the amount of yttrium-containing compounds to inhibit the generation of monoclinic grain, thereby avoiding the generation of zirconia cubic phase during sintering due to the large amount of yttrium-containing compounds; at the same time, the iron yttrate is beneficial to obtain a light-cured biomimetic color zirconia material close to the actual color of teeth.
[0029] The sintering aid includes magnesium oxide and / or calcium oxide, which is beneficial to reduce the sintering temperature.
[0030] Further, the mixed ceramic material preparation process comprises the following steps: ball milling the primary mixed ceramic material for 9-11 h, drying and sieving the ball-milled material through a 120-mesh sieve, and obtaining the mixed ceramic material by retaining the material below the 120-mesh sieve.
[0031] Further, the light-cured slurry preparation process comprises mixing the mixed ceramic material, the color-developing agent, the dispersant, the photoinitiator, and the light-cured resin in a mass ratio of (89.5-116.5):(0.13-7.2):(1-5):(0.26-1.38):(26-46) to obtain the light-cured slurry.
[0032] Further, the color-developing agent comprises an iron source, an erbium source, and a praseodymium source.
[0033] The mass ratio of the iron source, the erbium source, and the praseodymium source is (0.02-0.2):(0.1-5):(0.01-2).
[0034] Further, the iron source, the erbium source, and the praseodymium source are all salt compounds.
[0035] The iron source comprises one or more of ferric nitrate, ferric acetate, and ferric oxalate.
[0036] The erbium source comprises erbium acetate and / or erbium nitrate.
[0037] The praseodymium source comprises praseodymium acetate and / or praseodymium nitrate.
[0038] The beneficial effects of the above step are that the light-cured slurry including the color-developing agent can be light-cured without deep color, and the color of the light-cured biomimetic color zirconia material blank after curing is light, but the color of the light-cured biomimetic color zirconia material after sintering is close to the actual color of teeth.
[0039] Further, the dispersant comprises one or more of organosilicon and polyacrylate complex dispersant, polyoxyethylene-8-octylphenyl ether, and alkanolammonium salt.
[0040] The photoinitiator comprises one or more of phenyl bis(2,4,6-trimethylbenzoyl) phosphine oxide, 2-methyl-1-(4-methylthiophenyl)-2-morpholinyl-1-propanone, 4-chlorobenzophenone, and 2,4,6-trimethylbenzoyl-diphenyl phosphine oxide.
[0041] The light-cured resin comprises one or more of propoxylated trimethylolpropane triacrylate, 2-phenoxyethyl acrylate, and triethylene glycol dimethacrylate.
[0042] Further, the light-cured biomimetic color zirconia material body is subjected to a degumming process, which is heating from room temperature to 90-110℃ at a rate of 9-10℃ / min, heating from 90-110℃ to 280-320℃ at a rate of 5-6℃ / min, and heating from 280-320℃ to 580-620℃ at a rate of 3-4℃ / min.
[0043] and / or
[0044] The sintering process is heating to 100-120℃ at a rate of 7-8℃ / min, heating from 100-120℃ to 600-620℃ at a rate of 3-4℃, holding at 600-620℃ for 1.8-2.2h, heating from 600-620℃ to 1100-1250℃ at a rate of 1.5-2.5℃ / min, holding at 1100-1250℃ for 1-2h, heating from 1100-1250℃ to 1400-1500℃ at a rate of 1-1.5℃ / min, holding at 1400-1500℃ for 3-7h, and heating from 1400-1500℃ to 1500-1600℃ at a rate of 8-10℃ / min, and heating at 1500-1600℃ for 20-40min.
[0045] The above beneficial effects are adopted, which are heating from room temperature to 90-110℃ at a rate of 9-10℃ / min, which is beneficial to the rapid volatilization of small molecules, the formation of channels in the light-cured biomimetic color zirconia material body, and the uniformity of subsequent heat conduction; heating from 100-120℃ to 280-320℃ at a rate of 5-6℃ / min, and heating from 280-320℃ to 580-620℃ at a rate of 3-4℃ / min, which is beneficial to the slow volatilization of volatile substances with large molecular weight on the basis of the channels formed by small molecules, and the avoidance of cracking or damage of the body.
[0046] By the sintering process, heating to 100-120℃, the heating rate is 7-8℃ / min, which is conducive to realizing the rapid volatilization of the residual small molecular volatiles in the green body to form small-pore diameter pores; from 100-120℃ to 600-620℃, the heating rate is 3-4℃, and the temperature is kept at 600-620℃ for 1.8-2.2h, which is conducive to the volatilization of the residual larger molecules and macromolecules on the basis of the pores, thereby avoiding the occurrence of cracks or damage; from 600-620℃ to 1100-1250℃, the heating rate is 1.5-2.5℃ / min, and the temperature is kept at 1100-1250℃ for 1-2h, which is conducive to the generation of zirconia tetragonal grains; from 1100-1250℃ to 1400-1500℃, the heating rate is 1-1.5℃ / min, and the temperature is kept at 1400-1500℃ for 3-7h, which is conducive to the synchronous growth of zirconia tetragonal grains and long strip grains; from 1400-1500℃ to 1500-1600℃, the heating rate is 8-10℃ / min, and the temperature is kept at 1500-1600℃ for 20-40min, the heating rate is fast and the heating time is short at this temperature, which realizes that the long strip grains in the interior of the zirconia ceramic material are not obviously heated and thus the long strip grains in the interior do not obviously increase, while the long strip grains on the surface of the zirconia ceramic material grow to be long and thick, thereby improving the strength of the surface layer of the zirconia ceramic material. DETAILED DESCRIPTION
[0047] In order to better understand the technical solutions of the present application, the present application will be further described below in conjunction with specific examples.
[0048] Example 1
[0049] The present embodiment provides a preparation method of a photocured biomimetic color zirconia material, and an alumina mixed slurry is prepared, which comprises alumina, a modifying agent, and a solvent, wherein the modifying agent comprises a strontium source and a chromium source; the preparation process of the alumina mixed slurry comprises the following steps: mixing alumina, a modifying agent, and a solvent in a mass ratio of 75:18:100 to obtain the alumina mixed slurry.
[0050] The mass ratio of the strontium source and the chromium source is 3.2:1.5; the strontium source and the chromium source are both salt compounds.
[0051] The alumina mixed slurry is dried to obtain modified alumina, and the drying temperature of the alumina mixed slurry to obtain the modified alumina is 145℃; the modified alumina is alumina with strontium elements and chromium elements attached to the surface of the alumina;
[0052] The strontium source comprises strontium acetate; and the chromium source comprises chromium oxide.
[0053] A ceramic mixture slurry is prepared, which comprises zirconia powder, modified alumina; the ceramic mixture slurry is prepared by mixing zirconia powder, modified alumina, sintering aid, iron yttrate, and water in a mass ratio of 20:80.2:1.8:1.25:110; the sintering aid comprises magnesium oxide;
[0054] After drying the ceramic mixture slurry, pre-sintering is performed to obtain a primary mixed ceramic material, and the pre-sintering temperature is 1125°C; the primary mixed ceramic material comprises long strip-shaped grains;
[0055] The primary mixed ceramic material is ground and sieved to obtain a mixed ceramic material; the preparation process of the mixed ceramic material comprises the following steps: ball milling the primary mixed ceramic material for 10 hours, drying, sieving through a 120-mesh sieve, and collecting the material under the 120-mesh sieve to obtain the mixed ceramic material.
[0056] A photocuring slurry is prepared from the mixed ceramic material, which comprises mixed ceramic material and color developing agent; the photocuring slurry is prepared by mixing mixed ceramic material, color developing agent, dispersant, photoinitiator, and photocuring resin in a mass ratio of 103:3.66:3:0.82:36;
[0057] The color developing agent comprises iron source, erbium source, and praseodymium source; the mass ratio of the iron source, erbium source, and praseodymium source is 0.11:2.5:1; the iron source, erbium source, and praseodymium source are all salt compounds; the iron source comprises iron nitrate; the erbium source comprises erbium acetate; and the praseodymium source comprises praseodymium nitrate;
[0058] The dispersant comprises an organic silicon and polyacrylate compound dispersant;
[0059] The photoinitiator comprises phenyl bis(2,4,6-trimethylbenzoyl) phosphine oxide;
[0060] The photocuring resin comprises propoxylated trimethylolpropane triacrylate.
[0061] The photocuring slurry is used to prepare a photocuring biomimetic color zirconia material blank by 3D printing.
[0062] The photocuring biomimetic color zirconia material blank is degreased and sintered to obtain a photocuring biomimetic color zirconia material;
[0063] The degreasing process of the photocuring biomimetic color zirconia material blank is as follows: heating from room temperature to 100°C at a rate of 9.5°C / min; heating from 100°C to 300°C at a rate of 5.5°C / min; and heating from 300°C to 600°C at a rate of 3.5°C / min.
[0064] The sintering process is, the temperature is raised to 110℃, the temperature rising rate is 7.5℃ / min;From 110℃ to 610℃, the temperature rising rate is 3.5℃, from 610℃, 2h;From 610℃ to 1180℃, the temperature rising rate is 2℃ / min, 1h at 1180℃;From 1180℃ to 1450℃, the temperature rising rate is 1.25℃ / min, 5h at 1450℃;From 1450℃ to 1550℃, the temperature rising rate is 9℃ / min, 30min at 1550℃.
[0065] Example 2:
[0066] The same content of this embodiment as example 1 will not be repeated;The scheme different from example 1 is as follows:
[0067] The embodiment provides a kind of photocuring bionic color zirconia material preparation method:
[0068] The modification aid includes strontium source and chromium source;Alumina mixed slurry preparation process includes the following steps: alumina, modification aid, solvent are mixed according to mass ratio 72:17:93, and the alumina mixed slurry is obtained;
[0069] The mass ratio of the strontium source and the chromium source is 2.5:1;The strontium source and the chromium source are both salt compounds.
[0070] The drying temperature of the alumina mixed slurry is 100℃ to obtain modified alumina;The modified alumina is alumina with strontium and chromium elements attached to the surface;
[0071] The strontium source includes strontium oxalate;The chromium source includes chromium trichloride;
[0072] The ceramic mixed slurry preparation process is, zirconia powder, modified alumina, sintering aid, iron yttrate, water are mixed according to mass ratio 18:75:1.2:1.2:102, and the ceramic mixed slurry is obtained;The sintering aid includes calcium oxide;
[0073] The pre-sintering temperature is 1050℃, and the primary mixed ceramic material includes long strip-shaped grains;
[0074] The photocuring slurry preparation process is, mixed ceramic material, color developing material, dispersant, photoinitiator, photocuring resin are mixed according to mass ratio 95:0.5:1.5:0.52:30, and the photocuring slurry is obtained;
[0075] The color developing agent comprises an iron source, an erbium source and a praseodymium source; the mass ratio of the iron source, the erbium source and the praseodymium source is 0.08:1:0.08; the iron source, the erbium source and the praseodymium source are all salt compounds; the iron source comprises iron oxalate; the erbium source comprises erbium nitrate; and the praseodymium source comprises praseodymium acetate.
[0076] The dispersing agent comprises polyoxyethylene-8-octylphenyl ether.
[0077] The photoinitiator comprises 2-methyl-1-(4-methylthiophenyl)-2-morpholino-1-propanone.
[0078] The photocuring resin comprises 2-phenoxyethyl acrylate.
[0079] The degumming process of the photocuring biomimetic color zirconia material blank is as follows: from room temperature to 95 DEG C, the temperature rising rate is 9.2 DEG C / min; from 95 DEG C to 285 DEG C, the temperature rising rate is 5.2 DEG C / min; from 285 DEG C to 585 DEG C, the temperature rising rate is 3.2 DEG C / min.
[0080] The sintering process is as follows: the temperature is raised to 102 DEG C, the temperature rising rate is 7.2 DEG C / min; from 102 DEG C to 605 DEG C, the temperature rising rate is 3.2 DEG C, and the temperature is kept at 605 DEG C for 1.9 h; from 605 DEG C to 1120 DEG C, the temperature rising rate is 1.8 DEG C / min, and the temperature is kept at 1120 DEG C for 1.2 h; from 1120 DEG C to 1420 DEG C, the temperature rising rate is 1.1 DEG C / min, and the temperature is kept at 1420 DEG C for 3.8 h; from 1420 DEG C to 1520 DEG C, the temperature rising rate is 8.2 DEG C / min, and the temperature is kept at 1520 DEG C for 25 min.
[0081] Example 3:
[0082] The same content of the present embodiment as that of example 1 will not be described herein again; the different scheme of the present embodiment from that of example 1 is as follows:
[0083] The present embodiment provides a photocuring biomimetic color zirconia material preparation method:
[0084] The modification aid comprises a strontium source and a chromium source; the preparation process of the mixed slurry of aluminum oxide comprises the following steps: mixing aluminum oxide, a modification aid and a solvent according to a mass ratio of 78:20:108 to obtain the mixed slurry of aluminum oxide.
[0085] The mass ratio of the strontium source and the chromium source is 4:2.2; the strontium source and the chromium source are both salt compounds.
[0086] The drying temperature of the mixed slurry of aluminum oxide to obtain the modified aluminum oxide is 180 DEG C; the modified aluminum oxide is aluminum oxide with strontium elements and chromium elements attached to the surface of the aluminum oxide.
[0087] The strontium source comprises strontium oxalate; and the chromium source comprises chromium trichloride.
[0088] The ceramic mixture slurry is prepared by mixing zirconia powder, modified alumina, sintering aid, iron yttrate, and water in a mass ratio of 23:86:2.2:1.3:118; and the sintering aid comprises magnesium oxide and calcium oxide.
[0089] The pre-sintering temperature is 1230℃, and the primary mixed ceramic material comprises long strip-shaped grains.
[0090] The photocuring slurry is prepared by mixing the mixed ceramic material, color developing agent, dispersant, photoinitiator, and photocuring resin in a mass ratio of 113:6.8:4.5:1.2:44.
[0091] The color developing agent comprises iron source, erbium source, and praseodymium source; the mass ratio of the iron source, the erbium source, and the praseodymium source is 1.8:4.8:1.8; the iron source, the erbium source, and the praseodymium source are all salt compounds; the iron source comprises iron oxalate; the erbium source comprises erbium nitrate; and the praseodymium source comprises praseodymium acetate.
[0092] The dispersant comprises alkylol ammonium salt; and the photoinitiator comprises 4-chlorobenzophenone.
[0093] The photocuring resin comprises triethylene glycol dimethacrylate.
[0094] The degumming process of the photocuring biomimetic color zirconia material blank is performed by increasing the temperature from room temperature to 108℃ at a rate of 9.8℃ / min, increasing the temperature from 108℃ to 315℃ at a rate of 5.8℃ / min, and increasing the temperature from 315℃ to 610℃ at a rate of 3.8℃ / min.
[0095] The sintering process is performed by increasing the temperature to 118℃ at a rate of 7.8℃ / min, increasing the temperature from 118℃ to 615℃ at a rate of 3.8℃ / min, maintaining the temperature at 615℃ for 2.1h, increasing the temperature from 615℃ to 1220℃ at a rate of 2.2℃ / min, maintaining the temperature at 1220℃ for 1.8h, increasing the temperature from 1220℃ to 1480℃ at a rate of 1.3℃ / min, maintaining the temperature at 1480℃ for 6.5h, increasing the temperature from 1480℃ to 1580℃ at a rate of 9.5℃ / min, and maintaining the temperature at 1580℃ for 22min.
[0096] The above description is only the preferred embodiment of the present application and the explanation of the technical principles. It should be understood by those skilled in the art that the scope of the application involved in the present application is not limited to the technical solutions formed by the specific combinations of the above technical features, and should also cover other technical solutions formed by the combinations of the above technical features or their equivalent features without departing from the inventive concept. For example, the above features are equivalent to the features disclosed in the present application (but not limited to) with similar functions.
Claims
1. A method for preparing a photocured biomimetic color zirconia material, characterized in that, Preparation of alumina mixed slurry, the alumina mixed slurry comprises alumina, modification aid, solvent, the modification aid comprises strontium source and chromium source; The alumina mixed slurry is dried to obtain modified alumina, and the modified alumina is attached with strontium elements and chromium elements on the surface of alumina; Preparation of ceramic mixed material slurry, the ceramic mixed material slurry comprises zirconia powder and modified alumina; After drying the ceramic mixed material slurry, pre-sintering is carried out to obtain primary mixed ceramic material, the pre-sintering temperature is 1000-1250℃, and the primary mixed ceramic material comprises long strip-shaped crystal grains; The primary mixed ceramic material is ground and sieved to obtain mixed ceramic material; Preparation of photocuring slurry by the mixed ceramic material, the photocuring slurry comprises mixed ceramic material and color developing agent; The photocuring slurry is prepared into photocuring bionic color zirconia material blank by 3D printing; The photocuring bionic color zirconia material blank is degreased and sintered to obtain photocuring bionic color zirconia material.
2. The method of claim 1, wherein the method further comprises: The preparation process of the alumina mixed slurry comprises the following steps: Alumina, modification aid and solvent are mixed in a mass ratio of (70-80):(16-21):(90-110) to obtain the alumina mixed slurry; The mass ratio of the strontium source and the chromium source is (2-4.5):(0.5-2.5); The strontium source and the chromium source are both salt compounds.
3. The method of claim 2, wherein the method further comprises: The strontium source comprises one or more of strontium carbonate, strontium acetate, strontium oxalate and strontium chloride; The chromium source comprises one or more of chromium oxide, chromium acetate and chromium trichloride.
4. The method of claim 1, wherein the method further comprises, The preparation process of the ceramic mixed material slurry is that zirconia powder, modified alumina, sintering aid, yttrium iron and water are mixed in a mass ratio of (15-25):(72.5-88):(1-2.5):(1-1.5):(100-120) to obtain the ceramic mixed material slurry. And / or The drying temperature of the alumina mixed slurry to obtain the modified alumina is 90-200℃.
5. The method of claim 1, wherein the light-cured biomimetic color zirconia material is prepared by the steps of: The preparation process of the mixed ceramic material comprises the following steps: The primary mixed ceramic material is ball milled for 9-11h, and then dried and sieved through a 120-mesh screen to obtain the mixed ceramic material.
6. The method of claim 1, wherein the method further comprises, The preparation process of the photocuring slurry is that mixed ceramic material, color developing agent, dispersant, photoinitiator and photocuring resin are mixed in a mass ratio of (89.5-116.5):(0.13-7.2):(1-5):(0.26-1.38):(26-46) to obtain the photocuring slurry.
7. The method of claim 6, wherein the method further comprises, The color developing agent comprises iron source, erbium source and praseodymium source; The mass ratio of the iron source, the erbium source and the praseodymium source is (0.02-0.2):(0.1-5):(0.01-2).
8. The method of claim 6, wherein the method further comprises, The iron source, the erbium source and the praseodymium source are all salt compounds; The iron source comprises one or more of iron nitrate, iron acetate and iron oxalate; The erbium source comprises erbium acetate and / or erbium nitrate; The praseodymium source comprises praseodymium acetate and / or praseodymium nitrate.
9. The method of claim 6, wherein the method further comprises, The dispersant comprises one or more of organic silicon and polyacrylate compound dispersant, polyoxyethylene-8-octylphenyl ether and alkanol ammonium salt. The photoinitiator includes one or more of phenyl bis(2,4,6-trimethylbenzoyl) phosphine oxide, 2-methyl-1-(4-methylthiophenyl)-2-morpholinyl-1-propanone, 4-chlorobenzophenone, 2,4,6-trimethylbenzoyl-diphenylphosphine oxide; The photocuring resin includes one or more of propoxylated trimethylolpropane triacrylate, 2-phenoxyethyl acrylate, triethylene glycol dimethacrylate.
10. The method of claim 1, wherein the method further comprises, The degumming process of the photocured biomimetic color zirconia material blank is to increase the temperature from room temperature to 90-110℃ at a rate of 9-10℃ / min, to increase the temperature from 90-110℃ to 280-320℃ at a rate of 5-6℃ / min, and to increase the temperature from 280-320℃ to 580-620℃ at a rate of 3-4℃ / min; And / or The sintering process is to increase the temperature to 100-120℃ at a rate of 7-8℃ / min, to increase the temperature from 100-120℃ to 600-620℃ at a rate of 3-4℃, to keep the temperature at 600-620℃ for 1.8-2.2h, to increase the temperature from 600-620℃ to 1100-1250℃ at a rate of 1.5-2.5℃ / min, to keep the temperature at 1100-1250℃ for 1-2h, to increase the temperature from 1100-1250℃ to 1400-1500℃ at a rate of 1-1.5℃ / min, to keep the temperature at 1400-1500℃ for 3-7h, and to increase the temperature from 1400-1500℃ to 1500-1600℃ at a rate of 8-10℃ / min, and to keep the temperature at 1500-1600℃ for 20-40min.