CN109456041B - Zirconium oxide/aluminum oxide composite photosensitive paste homogenizing preparation technology based on SLA-3D printing - Google Patents
Zirconium oxide/aluminum oxide composite photosensitive paste homogenizing preparation technology based on SLA-3D printing Download PDFInfo
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Abstract
The invention belongs to the technical field of photosensitive ceramic paste preparation, and particularly relates to a zirconium oxide/aluminum oxide composite photosensitive paste homogenizing preparation technology based on SLA-3D printing, which comprises the following steps: 1) adding composite ceramic powder consisting of alumina and zirconia into an ethanol solution containing a dispersant for ball milling dispersion, drying and sieving to obtain zirconia/alumina composite ceramic powder; 2) mixing an active diluent, a prepolymer and a photoinitiator to prepare a photosensitive premixed solution; mixing the photosensitive premixed solution and a plasticizer to prepare an organic solution; 3) uniformly mixing the composite ceramic powder prepared in the step 1) with the organic solution in the step 2), and slowly evaporating the solution to obtain the final homogenized composite ceramic photosensitive paste. The solid content of the photosensitive paste prepared by the invention is more than 75 wt%, and the dispersion uniformity of the composite ceramic powder in the organic resin is effectively ensured.
Description
Technical Field
The invention relates to the technical field of photosensitive ceramic paste preparation, in particular to a zirconium oxide/aluminum oxide composite photosensitive paste homogenizing preparation technology based on SLA-3D printing.
Background
The ceramic SLA (stereo Lithography application) 3D printing technology based on the stereolithography principle has the advantages of high forming quality, large size range of prepared parts, density close to a theoretical value and the like, and is one of important trends of the development of the future ceramic 3D printing technology. In the SLA-3D printing ceramic technology, the ceramic raw material is generally a mixed paste of powder solid particles and liquid photosensitive resin, diluent monomer and other additives. The properties of the ceramic powder in the paste, such as components, dispersion uniformity and the like, directly influence the performance of the final ceramic part, and play an important role in the whole 3D printing technical process. Therefore, the homogenization suitable for the SLA-3D printing technology and the research and development of the composite photosensitive ceramic raw material are always hot research hotspots at home and abroad.
Alumina and zirconia ceramics are widely applied to the fields of mechanical engineering, aerospace, medical treatment and the like by virtue of the characteristics of excellent mechanical properties and excellent chemical stability. The SLA-3D printing technology can realize the preparation of parts with complex shapes of alumina and zirconia ceramics, and greatly promotes the wider and deep application of the parts in various fields. At present, French 3D ceramics company has realized the research and development of single-phase ceramic paste materials such as alumina, hydroxyapatite and the like, and the developed photosensitive paste materials have high solid content (>75 wt.%), a shear rate of 30s-1Moderate viscosity (C)>10000 mPa.s), and the like, and is better applied to SLA-3D printing equipment, thereby successfully completing a plurality of aerospace engineering and biomedical cases.
Patent document 201711478974.0 discloses a ceramic paste for 3D printing and a preparation method thereof, and relates to the field of ceramic pastes. The ceramic paste is prepared by the following method: weighing raw materials according to a formula, wherein the formula comprises, by mass, 60-85% of ceramic powder, 5-15% of a binder, 1-10% of a defoaming agent, and the balance of a solvent; the ceramic paste for 3D printing is prepared by the steps of putting weighed ceramic powder, a binder, a defoaming agent and a solvent into a ball milling tank, putting grinding balls into the ball milling tank, putting the ball milling tank on a planetary ball mill, carrying out ball milling on the planetary ball mill at a low speed, and uniformly mixing the raw materials by ball milling to obtain the ceramic paste for 3D printing. The preparation method is convenient and feasible, and the equipment is simple. Meanwhile, the ceramic paste for 3D printing, which has the advantages of high solid content, simple formula, short production period and low cost, can be prepared by the method. Studies have shown that the particle size of ceramic powders is closely linked to mechanical properties such as flexural strength and compactness, and generally, the smaller the particle size of the powder, the higher the surface active energy of the powder, and the lower the sintering temperature required, and the better the properties such as flexural strength and hardness. The ceramic particles used in this patent document have a diameter controlled in the range of 5 to 50um, and a large particle size makes sintering densification difficult, and very high sintering temperatures are required to achieve densification of 3D printed ceramic parts.
In conclusion, the composite photosensitive ceramic paste based on the SLA-3D printing technology still has the following problems: the ceramic solid content in the paste is low, so that the paste is not beneficial to precise forming on SLA 3D printing equipment; however, when the solid content is increased, the ceramic fine powder is difficult to be uniformly dispersed in the organic resin, and the final quality of the part is affected.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a zirconium oxide/aluminum oxide composite photosensitive paste homogenizing preparation technology based on SLA-3D printing. The invention can prepare the solid content of the ceramic>75 wt% of photosensitive paste, wherein the zirconia content is 1-50 wt%, when the shear rate is 30s-1The viscosity of the paste is in the range of 10000-30000 mPa.s, and the leveling requirement of SLA-3D printing equipment on the paste is met. In addition, the method can effectively ensure the dispersion uniformity of the composite ceramic powder in the organic resin.
One of the purposes of the invention is to provide a zirconium oxide/aluminum oxide composite photosensitive paste homogenizing preparation technology based on SLA-3D printing.
The invention also aims to provide application of the zirconium oxide/aluminum oxide composite photosensitive paste homogenizing preparation technology based on SLA-3D printing.
In order to realize the purpose, the invention discloses the following technical scheme:
the invention discloses a zirconium oxide/aluminum oxide composite photosensitive paste homogenizing preparation technology based on SLA-3D printing, which comprises the following steps:
s1, adding composite ceramic powder consisting of alumina and zirconia into an ethanol solution containing a dispersing agent for ball milling dispersion, drying and sieving to obtain zirconia/alumina composite ceramic powder for later use;
s2, mixing an active diluent, a prepolymer and a photoinitiator to prepare a photosensitive premixed solution; mixing an organic solvent, a photosensitive premixed solution and a plasticizer to prepare an organic solution;
s3, uniformly mixing the composite ceramic powder prepared in the step S1 with the organic solution obtained in the step S2, and evaporating the solvent to obtain the final homogenized composite ceramic photosensitive paste.
Specifically, the homogenized preparation technology of the zirconium oxide/aluminum oxide composite photosensitive paste based on SLA-3D printing comprises the following steps:
(1) adding alumina and zirconia into an ethanol solution containing a dispersing agent, carrying out ball milling for 10-30 h, then carrying out vacuum drying and sieving to obtain composite ceramic powder for later use;
(2) mixing an active diluent, a prepolymer and a photoinitiator, and ultrasonically dispersing for 0.5-2 h at the temperature of 30-50 ℃ to prepare a photosensitive premixed solution; then adding an organic solvent, a plasticizer and a defoaming agent into the photosensitive premixed solution, and uniformly stirring to obtain an organic solution containing photosensitive resin for later use;
(3) mixing the composite ceramic powder in the step (1) with the organic solution containing photosensitive resin in the step (2), and stirring for 4-20 h; and then heating to 60-150 ℃, removing the redundant solvent, and cooling to room temperature to obtain the homogeneous zirconia/alumina composite photosensitive paste.
In the step (1), the average grain diameter of the alumina and the average grain diameter of the zirconia are both less than or equal to 5 mu m, and the purity is more than or equal to 99.5 percent.
In the step (1), the ZrO2The content accounts for 1-50% of the total mass of the alumina and the zirconia; the powder can contain one or more of trace magnesium oxide, calcium oxide, cerium oxide and yttrium oxide.
In the step (1), the dispersant comprises one or more of organic oligomer and unsaturated organic acid.
In the step (1), the dosage of the dispersant is 0.3-3% of the total mass of the alumina and the zirconia.
Further, the organic oligomer dispersant includes, but is not limited to, one or more of polyester polyol, polyether polyol, polyethylene glycol or acrylic resin.
Further, the unsaturated organic acid includes but is not limited to one or more of oleic acid, linoleic acid, stearic acid or adipic acid.
In the step (2), the photoinitiator comprises: one or more of alpha-hydroxyalkyl benzophenone, 1-hydroxycyclohexyl phenyl ketone or benzoin dimethyl ether and the like.
In the step (2), the reactive diluent comprises: one or more of tripropylene glycol diacrylate, 1, 6-hexanediol diacrylate, dipropylene glycol diacrylate or propoxylated neopentyl glycol diacrylate.
In the step (2), the prepolymer includes: one or more of trimethylolpropane triacrylate, ethoxylated pentaerythritol tetraacrylate or di-trimethylolpropane tetraacrylate.
In the step (2), the organic solvent includes: one or more of methanol, ethanol and glycerol.
In the step (2), the plasticizer includes: phthalic esters or di (2-ethylhexyl) phthalate.
In the step (2), the defoaming agent comprises: silicone antifoam, polyoxyethylene polyoxypropylene amine ether or polydimethylsiloxane.
Further, in the step (2), the mass ratio of the reactive diluent to the prepolymer is 0.25-4, and the dosage of the photoinitiator is 2-5% of the total mass of the reactive diluent and the prepolymer.
Further, in the step (2), the addition amount of the plasticizer is 0.1-2% of the mass of the composite ceramic powder in the step (1); the addition amount of the defoaming agent is 0.1-1% of the total mass of the alumina and the zirconia.
In the step (3), the volume ratio of the ceramic powder to the organic solution containing photosensitive resin is 0.1-1;
the SLA-3D printing of the ceramic is a process of solidifying, stacking and accumulating ceramic paste layer by layer, and the laying quality of each layer of the ceramic blank determines the mechanical property of the final ceramic part, so that the dispersion uniformity of ceramic powder in a photosensitive paste system has very important influence on the performance of the final 3D ceramic part. Researches show that the surfaces of alumina and zirconia ceramics contain certain-OH groups and present certain hydrophilicity, so that the alumina and zirconia ceramics have certain difficulty in dispersing in oily organic photosensitive premixed solution; in addition, the smaller the ceramic powder particle size, the greater the surface activity, the easier the particle agglomeration is caused, and the powder agglomeration phenomenon in the ceramic paste with high solid content is particularly serious. The patent provides an effective solution, and a dispersing agent is added in the step 1), so that the compatibility of the powder and an organic system solution is improved, and the dispersibility of the powder is improved; the viscosity of the photosensitive premix is reduced in step 2) by adding an organic solvent, a plasticizer, and the like. The treatment of the step 1-2) greatly reduces the difficulty of dispersing the alumina and zirconia fine powder in the step 3). And (3) partially evaporating the organic solvent in the paste system to obtain a paste with high solid content (>75 wt%) and good dispersibility.
Finally, the invention discloses an application of the zirconium oxide/aluminum oxide composite photosensitive paste homogenizing preparation technology based on SLA-3D printing in the fields of mechanical engineering, aerospace, medical treatment and the like.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention provides a preparation method of a high-solid-content zirconia/alumina composite photosensitive paste material suitable for SLA 3D printing. The nano-phase zirconia is added into a photosensitive paste system, so that toughening and reinforcement of a superfine alumina (less than 5um) matrix are realized, the mechanical property of a 3D printing alumina part is improved, the application range of ceramic 3D printing is expanded, and the application effect of the ceramic 3D printing is improved.
(2) The invention provides a technology capable of realizing the homogenization and dispersion of a zirconia/alumina composite photosensitive paste, which solves the contradiction between high powder content and difficult powder dispersion in an organic photosensitive paste; the invention can prepare the solid content of the ceramic>75 wt% of photosensitive paste, wherein the zirconia content is 1-50 wt%, when the shear rate is 30s-1The viscosity of the paste is 10000-30000mAnd the requirement of SLA-3D printing equipment on the leveling property of the paste is met within the range of Pa & s. In addition, the method can effectively ensure the dispersion uniformity of the composite ceramic powder in the organic resin, and is beneficial to the sintering compactness, the shape precision and the size precision of the 3D printing ceramic blank in the post-treatment.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the application and, together with the description, serve to explain the application and are not intended to limit the application.
FIG. 1 is a schematic diagram of a process for preparing an alumina/zirconia composite photosensitive paste according to the present invention;
FIG. 2 microscopic Structure of ceramic paste prepared in example 1.
FIG. 3 is a drawing of a ceramic part prepared in example 1.
FIG. 4 partial microscopic structure of the ceramic part prepared in example 1.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
As described in the background art, the conventional composite photosensitive ceramic paste based on the SLA-3D printing technology still has the problem of low solid content of ceramic in the paste, so that the paste is not beneficial to precise forming on SLA-3D printing equipment; however, when the solid content is increased, the ceramic powder is difficult to be uniformly dispersed in the organic resin, and the final quality of the part is affected. Therefore, the invention provides a zirconium oxide/aluminum oxide composite photosensitive paste homogenizing preparation technology based on SLA-3D printing, and the invention is further described by combining the accompanying drawings and the specific implementation mode.
Example 1
As shown in fig. 1, a zirconium oxide/aluminum oxide composite photosensitive paste homogenizing preparation technology based on SLA-3D printing comprises the following steps:
(1) preparing composite ceramic powder: mixing 800g of Al2O3、200g ZrO2(the grain diameter is 0.02-5 mu m, the purity is 99.9%), 30g of stearic acid (SA, chemical purity) and 1500g of ethanol (the purity is 99.5%) are mixed and ball-milled for 10 hours, and the alumina/zirconia composite ceramic powder is prepared after vacuum drying and sieving for later use.
(2) Preparation of organic solution containing photosensitive resin: taking 35.2g of prepolymer (ditrimethylolpropane acrylate), 140.8g of reactive diluent (propoxylated neopentyl glycol diacrylate) and 5% of photoinitiator (1-hydroxycyclohexyl phenyl ketone) of the total mass of the reactive diluent and the prepolymer; placing the photoinitiator, the reactive diluent and the prepolymer in a beaker, and performing ultrasonic dispersion for 2 hours at 40 ℃ to obtain photosensitive resin; then 20g of plasticizer (di (2-ethylhexyl) phthalate), 10g of organic silicon defoamer and 900g of ethanol are mixed with photosensitive resin to obtain organic solution containing the photosensitive resin for later use.
(3) Preparing a composite photosensitive paste material: respectively taking the composite ceramic powder in the step (1) and the organic solution containing photosensitive resin in the step (2) according to the volume ratio of 1, and stirring for 20 hours; and then heating to 150 ℃, removing part of the solvent, and cooling to room temperature to obtain the homogeneous zirconia/alumina composite photosensitive paste.
The composite photosensitive paste prepared in this example had a solid content of 85.4 wt% and a shear rate of 30s-1The viscosity of the paste is 30000mPa & s, and the paste completely meets the application requirements of SLA 3D printing equipment; the microstructure of the obtained composite photosensitive paste is shown in figure 2, and fine particles can be seen<5um) are uniformly dispersed, and no obvious agglomeration occurs. The ceramic gear obtained by SLA-3D printing of the composite photosensitive paste of this example is shown in FIGS. 3 and 4,as can be seen, the ceramic gear has smooth surface and basically no deformation, the density is more than 99 percent, and the content of residual carbon is less than 0.2 percent, thus reflecting the good applicability of the paste prepared by the invention.
Example 2
A zirconium oxide/aluminum oxide composite photosensitive paste homogenizing preparation technology based on SLA-3D printing comprises the following steps: (1) preparing composite ceramic powder: 500g of Al2O3、500g ZrO2Mixing (particle size of 0.02-5 μm, purity of 99.9%), 10g of oleic acid (OA, chemical purity) and 2000g of ethanol (purity of 99.5%), ball-milling for 30h, vacuum drying, and sieving to obtain the alumina/zirconia composite ceramic powder for later use.
(2) Preparation of organic solution containing photosensitive resin: 266.6g of prepolymer (ethoxylated pentaerythritol tetraacrylate), 66.6g of reactive diluent (1, 6-hexanediol diacrylate) and 2 percent of photoinitiator (alpha-hydroxyalkyl benzophenone) by mass of the total mass of the reactive diluent and the prepolymer are taken; placing the photoinitiator, the reactive diluent and the prepolymer in a beaker, and performing ultrasonic dispersion for 0.5h at the temperature of 30 ℃ to obtain photosensitive resin; then 1g of plasticizer (phthalate), 5g of polyoxyethylene polyoxypropylene ether and 700g of methanol are mixed with the photosensitive resin to obtain an organic solution containing the photosensitive resin for later use.
(3) Preparing a composite photosensitive paste material: respectively taking the composite ceramic powder in the step (1) and the organic solution containing photosensitive resin in the step (2), and stirring for 10 hours; then heating to 60 ℃, removing part of the solvent, and cooling to room temperature to obtain the homogeneous zirconia/alumina composite photosensitive paste.
The composite photosensitive paste prepared in this example had a solid content of 75.8 wt% and a shear rate of 30s-1The viscosity of the paste is about 10000mPa & s, which completely meets the application requirement of SLA 3D printing equipment.
Example 3
A zirconium oxide/aluminum oxide composite photosensitive paste homogenizing preparation technology based on SLA-3D printing comprises the following steps:
(1) preparing composite ceramic powder: 990g of Al2O3、100g ZrO2(particle diameter of 0.02-5 μm, purity of 99.9%) 3Mixing polyester polyol (chemical purity) and 2000g ethanol (purity 99.5%), ball-milling for 30h, vacuum drying, and sieving to obtain the alumina/zirconia composite ceramic powder for later use.
(2) Preparation of organic solution containing photosensitive resin: taking 50.3g of prepolymer (ethoxylated trimethylolpropane triacrylate), 75.6g of reactive diluent (dipropylene glycol diacrylate) and 3% of photoinitiator (benzoin dimethyl ether) in the total mass of the reactive diluent and the prepolymer; placing the photoinitiator, the reactive diluent and the prepolymer in a beaker, and performing ultrasonic dispersion for 1.5 hours at 50 ℃ to obtain photosensitive resin; then 1g of plasticizer (phthalate), 1g of polydimethylsiloxane and 600g of glycerol are mixed with the photosensitive resin to obtain an organic solution containing the photosensitive resin for later use.
(3) Preparing a composite photosensitive paste material: respectively taking the composite ceramic powder in the step (1) and the organic solution containing photosensitive resin in the step (2) according to the volume ratio of 0.4, and stirring for 4 hours; then heating to 100 ℃, removing part of the solvent, and cooling to room temperature to obtain the homogeneous zirconia/alumina composite photosensitive paste.
The composite photosensitive paste prepared in this example had a solid content of 83.4 wt% and a shear rate of 30s-1The viscosity of the paste is 26000mPa & s, which completely meets the application requirements of SLA 3D printing equipment.
Example 4
A zirconium oxide/aluminum oxide composite photosensitive paste homogenizing preparation technology based on SLA-3D printing comprises the following steps:
(1) preparing composite ceramic powder: 700g of Al2O3、100g ZrO2(the grain diameter is 0.02-5 mu m, the purity is 99.9%), 3g of polyether polyol (chemical purity) and 1800g of ethanol (the purity is 99.5%) are mixed and ball-milled for 25h, and the alumina/zirconia composite ceramic powder is prepared after vacuum drying and sieving for later use.
(2) Preparation of organic solution containing photosensitive resin: taking 100g of prepolymer (trimethylolpropane triacrylate), 200g of reactive diluent (tripropylene glycol diacrylate) and 4% of photoinitiator (1-hydroxycyclohexyl phenyl ketone) in terms of the total mass of the reactive diluent and the prepolymer; placing the photoinitiator, the reactive diluent and the prepolymer in a beaker, and performing ultrasonic dispersion for 1.0h at 35 ℃ to obtain photosensitive resin; then 1g of plasticizer (di (2-ethylhexyl) phthalate), 3g of defoaming agent (polydimethylsiloxane) and 700g of methanol are mixed with photosensitive resin to obtain an organic solution containing the photosensitive resin for later use.
(3) Preparing a composite photosensitive paste material: respectively taking the composite ceramic powder in the step (1) and the organic solution containing photosensitive resin in the step (2) according to the volume ratio of 0.8, and stirring for 15 hours; and then heating to 80 ℃, removing part of the solvent, and cooling to room temperature to obtain the homogeneous zirconia/alumina composite photosensitive paste.
The composite photosensitive paste prepared in this example had a solid content of 81.6 wt% and a shear rate of 30s-1The viscosity of the paste is about 18000 mPa.s, which completely meets the application requirements of SLA 3D printing equipment.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (17)
1. A zirconium oxide/aluminum oxide composite photosensitive paste homogenizing preparation technology based on SLA-3D printing is characterized by comprising the following steps:
s1, adding the composite ceramic powder consisting of alumina and zirconia into an ethanol solution containing a dispersant for ball milling and dispersion, drying and sieving to obtain zirconia/alumina composite ceramic powder for later use;
s2, mixing the reactive diluent, the prepolymer and the photoinitiator to prepare a photosensitive premix; mixing an organic solvent, a photosensitive premixed solution and a plasticizer to prepare an organic solution;
s3, uniformly mixing the composite ceramic powder prepared in the step S1 with the organic solution in the step S2, and evaporating the solution to obtain a final homogenized composite ceramic photosensitive paste;
the grain diameter of the zirconium oxide is 0.02-5 mu m;
in step S2, the organic solvent includes: one or more of methanol, ethanol and glycerol.
2. The technology for preparing the zirconium oxide/aluminum oxide composite photosensitive paste material based on SLA-3D printing through homogenization according to claim 1 is characterized by comprising the following specific steps:
(1) adding alumina and zirconia into an ethanol solution containing a dispersing agent, carrying out ball milling for 10-30 h, then carrying out vacuum drying and sieving to obtain composite ceramic powder for later use;
(2) mixing an active diluent, a prepolymer and a photoinitiator, and ultrasonically dispersing for 0.5-2 h at the temperature of 30-50 ℃ to prepare a photosensitive premixed solution; then adding an organic solvent, a plasticizer and a defoaming agent into the photosensitive premixed solution, and uniformly stirring to obtain an organic solution containing photosensitive resin for later use;
(3) mixing the composite ceramic powder obtained in the step S1 with the organic solution containing photosensitive resin obtained in the step S2, and stirring for 4-20 h; and slowly heating to 60-150 ℃, removing the redundant solvent, and cooling to room temperature to obtain the homogeneous zirconia/alumina composite photosensitive paste.
3. The technology for preparing the zirconium oxide/aluminum oxide composite photosensitive paste material through homogenization based on SLA-3D printing according to claim 1, wherein in the step S1, the average grain diameter of the aluminum oxide is less than or equal to 5 μm, and the purity is more than or equal to 99.5%.
4. The technology for preparing the zirconium oxide/aluminum oxide composite photosensitive paste material through homogenization based on SLA-3D printing according to claim 1, wherein in the step S1, the content of zirconium oxide accounts for 1-50% of the total mass of aluminum oxide and zirconium oxide.
5. The technology for preparing the zirconium oxide/aluminum oxide composite photosensitive paste material based on SLA-3D printing through homogenization according to claim 1, wherein in the step S1, the dispersing agent comprises one or more of organic oligomer and unsaturated organic acid.
6. The technology for preparing the zirconium oxide/aluminum oxide composite photosensitive paste material through homogenization based on SLA-3D printing according to claim 1, wherein in the step S1, the amount of the dispersant is 0.3-3% of the total mass of the aluminum oxide and the zirconium oxide.
7. The technology for preparing the zirconium oxide/aluminum oxide composite photosensitive paste material based on SLA-3D printing through homogenization according to claim 5, wherein the organic oligomer dispersant includes but is not limited to one or more of polyester polyol, polyether polyol, polyethylene glycol or acrylic resin.
8. The technology for preparing the zirconium oxide/aluminum oxide composite photosensitive paste material through homogenization based on SLA-3D printing according to claim 5, wherein the unsaturated organic acid comprises one or more of oleic acid, linoleic acid, stearic acid or adipic acid.
9. The technology for preparing homogenized zirconia/alumina composite photosensitive paste based on SLA-3D printing according to claim 1, wherein in step S2, the photoinitiator comprises: one or more of alpha-hydroxyalkyl benzophenone, 1-hydroxycyclohexyl phenyl ketone or benzoin dimethyl ether and the like.
10. The SLA-3D printing-based zirconia/alumina composite photosensitive paste homogenization preparation technology according to claim 1, wherein in step S2, the reactive diluent comprises: one or more of tripropylene glycol diacrylate, 1, 6-hexanediol diacrylate, dipropylene glycol diacrylate or propoxylated neopentyl glycol diacrylate.
11. The SLA-3D printing based zirconia/alumina composite photosensitive paste homogenization preparation technique according to claim 1, wherein in step S2, the prepolymer comprises: one or more of trimethylolpropane triacrylate, ethoxylated pentaerythritol tetraacrylate or di-trimethylolpropane tetraacrylate.
12. The SLA-3D printing based zirconia/alumina composite photosensitive paste homogenization preparation technique according to claim 1, wherein in step S2, the plasticizer comprises: phthalic esters or di (2-ethylhexyl) phthalate.
13. The technology for preparing the homogenized zirconia/alumina composite photosensitive paste based on SLA-3D printing according to claim 2, wherein in the step (2), the defoaming agent comprises: silicone antifoam, polyoxyethylene polyoxypropylene amine ether or polydimethylsiloxane.
14. The technology for preparing the zirconium oxide/aluminum oxide composite photosensitive paste material through homogenization based on SLA-3D printing according to claim 1, wherein in the step S2, the mass ratio of the reactive diluent to the prepolymer is 2: 3-9: 1, and the amount of the photoinitiator is 2-5% of the total mass of the reactive diluent and the prepolymer.
15. The technology for preparing the zirconium oxide/aluminum oxide composite photosensitive paste material through homogenization based on SLA-3D printing according to claim 2, wherein in the step S2, the adding amount of the plasticizer is 0.1-2% of the mass of the composite ceramic powder material in the step S1; the addition amount of the defoaming agent is 0.1-1% of the total mass of the alumina and the zirconia.
16. The technology for preparing the zirconium oxide/aluminum oxide composite photosensitive paste through homogenization based on SLA-3D printing according to claim 1, wherein in the step S3, the volume ratio of the ceramic powder and the organic solution containing photosensitive resin is 0.1-1.
17. Use of the SLA-3D printing based zirconia/alumina composite photosensitive paste homogenization preparation technology according to any of claims 1 to 16 in the fields of mechanical engineering, aerospace and medical treatment.
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| CN113929500B (en) * | 2021-10-08 | 2022-08-16 | 西安交通大学 | Method for preparing aluminum oxide ceramic surface composite coating for vacuum arc-extinguishing chamber through 3D printing |
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