CN113929500B - Method for preparing aluminum oxide ceramic surface composite coating for vacuum arc-extinguishing chamber through 3D printing - Google Patents
Method for preparing aluminum oxide ceramic surface composite coating for vacuum arc-extinguishing chamber through 3D printing Download PDFInfo
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Abstract
The invention discloses a method for preparing an aluminum oxide ceramic surface composite coating for a vacuum arc-extinguishing chamber by 3D printing, and belongs to the technical field of preparation of aluminum oxide ceramic surface composite coatings. The method selects extremely low secondary electron emission coefficient and can reduce A1 2 O 3 Cr of ceramic secondary electron emission coefficient and surface resistivity 2 O 3 As a raw material of the coating, A1 2 O 3 The good performances of the ceramic and the coating are combined, and the overall advantages of the two materials are highlighted. Meanwhile, the 3D printing technology is adopted, the efficiency is improved, the coating can be uniformly coated on the surface of the complex component, the good body insulation performance of the insulating medium substrate is ensured, and the surface flashover resistance of the insulating medium is effectively improved.
Description
Technical Field
The invention belongs to the technical field of preparation of an aluminum oxide ceramic surface composite coating, and relates to a method for preparing an aluminum oxide ceramic surface composite coating for a vacuum arc-extinguishing chamber by 3D printing.
Background
Vacuum is a common high-voltage insulating medium, and has excellent dielectric properties, so that it is widely used in electrical equipment and vacuum devices. In order to meet the requirement of equipment support, solid insulators with the same gap length are inserted between different potential conductors in a vacuum environment, but surface flashover is caused after the insulators are introduced. The insulator vacuum surface flashover refers to a penetrating discharge phenomenon generated in a desorption gas layer on the surface of the insulator, and the voltage loaded during flashover is generally far lower than the bulk breakdown voltage and the vacuum gap breakdown voltage of an insulating material. The alumina ceramic has good electric insulation performance, heat conductivity and high temperature resistance, and is widely applied to the fields of electric vacuum insulation and high voltage. However, due to the excessively high secondary electron emission coefficient and surface resistivity, a large amount of charges are easily accumulated on the surface of the silicon carbide under high electric fields and complex environments, and the creeping flashover voltage is reduced, so that creeping discharge accidents are caused.
Therefore, in order to improve the lifetime and stability of vacuum electrical equipment, it is necessary to find a method for suppressing the accumulation of surface charges of dielectrics to improve the flashover performance along the surface thereof.
Disclosure of Invention
The invention aims to overcome the defects that charges are easy to accumulate on the surface of the aluminum oxide ceramic and the surface flashover voltage is reduced in the prior art, and provides a method for preparing an aluminum oxide ceramic surface composite coating for a vacuum arc extinguish chamber through 3D printing.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the method for preparing the aluminum oxide ceramic surface composite coating for the vacuum arc-extinguishing chamber by 3D printing comprises the following steps:
step 1) adding Cr 2 O 3 、Al 2 O 3 Cr prepared from sintering assistant and photosensitive resin 2 O 3 And Al 2 O 3 The three paste materials with gradient content are used as 3D printing raw materials and are sequentially printed on the surface of an alumina porcelain shell according to gradient change to obtain a three-layer coating from bottom to top on the surface of the alumina porcelain shell, and the alumina porcelain shell with a transition layer on the surface is obtained after standing until a solvent is volatilized;
and 2) sintering the alumina porcelain shell with the transition layer on the surface at high temperature to obtain the gradient coating on the surface of the insulator.
Preferably, in the step 1), the mass ratio of the photosensitive resin to the powder is 3: 7;
for the powder, the first coating contains Cr in percentage by mass 2 O 3 30-50% of Al 2 O 3 The content is 40-60%, and the total content of the sintering aids is 5-10%; in the second coating layer, Cr 2 O 3 50-70% of Al 2 O 3 The content is 20-40%, and the total content of the sintering aids is 5-10%; in the third coating, Cr 2 O 3 The content is 90-95%, and the total content of the sintering aids is 5-10%; the thickness of each layer of coating is 10-15 μm.
Preferably, a modifier is added into all the three pastes;
the modifier is silane coupling agent or phthalate ester.
Preferably, the mass of the modifier added in each paste is 0.5-5% of the total mass of each paste.
Preferably, the photosensitive resin includes a prepolymer, a monomer, a photoinitiator, a dispersant, a defoaming agent, and a viscosity modifier;
the prepolymer is formed by mixing one or more of epoxy acrylate, polyurethane acrylate, methacrylate, polyester acrylate and cationic photosensitive resin;
the monomer is formed by mixing one or more of butyl acrylate, HDDA and TPG-DA;
the photoinitiator is formed by mixing one or more of TPO, benzoin dimethyl ether, benzophenone and diaryl iodonium salt;
the dispersant is prepared by mixing one or more of KH550, KH570, hyperdispersant 9076 and Triton X-100;
viscosity modifiers include PEG and/or glycerol;
the defoaming agent is formed by mixing one or more of fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene and fatty acid polyoxyethylene.
Preferably, the photosensitive resin comprises, by mass, 55-65% of a prepolymer, 25-35% of a monomer, 1-5% of a photoinitiator, 1-5% of a dispersant, 1-8% of a viscosity regulator, and 1-3% of an antifoaming agent.
Preferably, the sintering aid is TiO 2 And MnCO 3 One or two of them;
in each paste material, the total content of the sintering aid is 5-10% by mass, and the TiO content is 2 1-7% of MnCO 3 The content is 0-5%.
Preferably, in the step 2), the sintering conditions are as follows: vacuum pressure 3.6X 10 -3 Pa, sintering at 1200-1500 ℃ for 2-4 h.
Preferably, in step 2), nitrogen or argon is filled during sintering.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a preparation method of an aluminum oxide ceramic surface composite coating for a vacuum arc-extinguishing chamber by 3D printing, which selects an extremely low secondary electron emission coefficient and can reduce A1 2 O 3 Cr of ceramic secondary electron emission coefficient and surface resistivity 2 O 3 As a raw material of the coating, A1 2 O 3 The good performances of the ceramic and the coating are combined, and the overall advantages of the two materials are highlighted. Meanwhile, the 3D printing technology is adopted, the efficiency is improved, the coating can be uniformly coated on the surface of the complex component, the good body insulation performance of the insulating medium substrate is ensured, and the surface flashover resistance of the insulating medium is effectively improved.
Drawings
FIG. 1 is a SEM image of the cross section of the flashover resistant composite coating on the surface of the alumina ceramic obtained in example 6;
FIG. 2 is a sectional EDS diagram of the flashover resistant composite coating on the surface of the alumina ceramic obtained in example 6;
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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 invention.
It should be noted that the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover non-exclusive inclusions, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
the method for preparing the aluminum oxide ceramic surface composite coating for the vacuum arc extinguish chamber through 3D printing is characterized by comprising the following steps of:
step 1) adding Cr 2 O 3 、Al 2 O 3 Cr prepared from sintering assistant, photosensitive resin and solvent 2 O 3 And Al 2 O 3 The three pastes with gradient change in content are used as 3D printing raw materials and are sequentially printed on the surface of the insulator substrate according to the gradient change to obtain a three-layer coating from bottom to top on the surface of the insulator substrate, and the insulator with a transition layer coated on the surface is obtained after standing until a solvent is volatilized;
and 2) sintering the insulator with the transition layer on the surface at a high temperature to obtain the aluminum oxide ceramic surface composite coating for the vacuum arc-extinguishing chamber on the surface of the insulator.
The compositional content of each layer in each example is shown in Table 1, and the production conditions for each example are shown in Table 2.
TABLE 1 raw material composition of chromium oxide coating system selected for use in the present invention
TABLE 2 slurry proportioning and sintering process of chromium oxide coating system selected in the invention
| Examples | Amount of dispersant used | Solid content of paste | Sintering temperature | Time of heat preservation |
| 1 | 1.2wt.％ | 70vol.％ | 1400℃ | 2h |
| 2 | 2wt.％ | 60vol.％ | 1300℃ | 4h |
| 3 | 1.5wt.％ | 40vol.％ | 1500℃ | 2h |
| 4 | 0.4wt.％ | 80vol.％ | 1200℃ | 3h |
| 5 | 1.8wt.％ | 50vol.％ | 1400℃ | 2h |
| 6 | 1.2wt.％ | 30vol.％ | 1400℃ | 4h |
And (2) additionally adding polyvinylpyrrolidone accounting for 0.4-2% of the powder as a dispersing agent according to the proportion in the table 2, adjusting the solid content of the system to the value in the table by absolute ethyl alcohol, sequentially printing the three layers of coatings on the surface of the 95 ceramic alumina substrate by adopting 3D printing, standing for 8 hours at room temperature, and obtaining the substrate with the surface coated with the transition layer after the solvent is volatilized.
Putting the obtained insulator into a vacuum sintering furnace, and vacuumizing to be lower than 3.6 multiplied by 10 -3 And Pa, filling high-purity nitrogen according to the sintering process shown in the table 2, heating to a specified temperature, and keeping the temperature, wherein the heating rate is 5 ℃/min, so as to obtain the flashover resistant gradient composite coating on the surface of the alumina ceramic. The alumina insulator with the gradient coating on the surface obtained by the method is measured by a broadband dielectric spectrum testing system; measuring the surface resistivity by using a resistance tester; the microstructure was observed on the cross section of the specimen with a scanning electron microscope. These electrical property results are shown in table 3, using alumina ceramics without a chromium oxide coating as comparative examples.
TABLE 3 Performance of the flashover gradient resistant composite coating on the surface of the alumina ceramic of the present invention
As can be seen from Table 3, the coating materials of example 6 were prepared in the proportion of Cr in the first coating paste 2 O 3 50% of Al 2 O 3 40% of TiO 2 Content of MnCO 5% 3 The content is 5 percent; cr in the second coating paste 2 O 3 70% of Al 2 O 3 20% of TiO 2 6% of MnCO 3 The content is 4%; cr in the third layer coating paste 2 O 3 90% of Al 2 O 3 0% of TiO 2 The content of MnCO is 7 percent 3 The content is 3 percent, and the MgO content is 1 percent; the volume solids content was 30 vol.%. And sequentially printing the three layers of coatings on the surface of the 95 ceramic alumina substrate by adopting 3D printing, standing for 8 hours at room temperature, and volatilizing a solvent to obtain the substrate with the surface covered with the transition layer. Putting the obtained insulator into a vacuum sintering furnace, and vacuumizing to be lower than 3.6 multiplied by 10 -3 Pa, filling high-purity nitrogen, heating to 1400 ℃, and keeping the temperature for 4h, wherein the heating rate is 5 ℃/min, the relative dielectric constant of the obtained alumina insulator with the surface coated with the gradient coating is as low as 3.3, and the surface resistivity is reduced to 8.1 multiplied by 10 9 Omega/sq, the flashover resistance of the surface is greatly improved.
FIG. 1 is a cross-sectional microstructure photograph of the composite coating on the surface of the alumina ceramic obtained in example 6, wherein the overall thickness of the coating is 5-15 μm, and the coating can be seen to be dense and uniformly distributed on the surface of the substrate. As can be seen from the EDS chart (as shown in FIG. 2), Cr 2 O 3 With Al 2 O 3 There is a clear boundary between the substrates, and part of the Cr element has penetrated deeply into Al 2 O 3 The depth of penetration in the substrate was about 30 μm, further illustrating the uniform distribution of the coating on the substrate surface and also the good bonding between the coating and the substrate. By combining the performance data of each embodiment in table 3, the flashover resistant composite coating on the surface of the alumina ceramic prepared by the invention can effectively reduce the relative dielectric constant and the surface resistivity of the insulator and improve the flashover resistant capability of the surface.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (8)
- The method for preparing the aluminum oxide ceramic surface composite coating for the vacuum arc-extinguishing chamber through 3D printing is characterized by comprising the following steps of:step 1) adding Cr 2 O 3 、Al 2 O 3 Cr prepared from sintering assistant and photosensitive resin 2 O 3 And Al 2 O 3 The three paste materials with gradient content are used as 3D printing raw materials and are sequentially printed on the surface of an alumina porcelain shell according to gradient change to obtain a three-layer coating from bottom to top on the surface of the alumina porcelain shell, and the alumina porcelain shell with a transition layer on the surface is obtained after standing until a solvent is volatilized; the mass ratio of the photosensitive resin to the powder is 3: 7;for the powder, the first coating contains Cr in percentage by mass 2 O 3 30-50% of Al 2 O 3 The content is 40-60%, and the total content of the sintering aids is 5-10%; in the second coating layer, Cr 2 O 3 50-70% of Al 2 O 3 The content is 20-40%, and the total content of the sintering aids is 5-10%; in the third coating, Cr 2 O 3 The content is 90-95%, and the total content of the sintering aids is 5-10%; the thickness of each layer of coating is 10-15 mu m; and 2) sintering the alumina porcelain shell with the transition layer on the surface at high temperature to obtain the gradient coating on the surface of the insulator.
- 2. The 3D printing method for preparing the aluminum oxide ceramic surface composite coating for the vacuum arc-extinguishing chamber according to claim 1, wherein a modifier is added into each of the three pastes;the modifier is silane coupling agent or phthalate ester.
- 3. The method for preparing the aluminum oxide ceramic surface composite coating for the vacuum arc extinguish chamber through 3D printing according to claim 2, wherein the mass of the modifier added in each paste is 0.5-5% of the total mass of each paste.
- 4. The 3D printing method for preparing the aluminum oxide ceramic surface composite coating for the vacuum arc-extinguishing chamber according to claim 1, wherein the photosensitive resin comprises a prepolymer, a monomer, a photoinitiator, a dispersant, a defoaming agent and a viscosity regulator;the prepolymer is formed by mixing one or more of epoxy acrylate, polyurethane acrylate, methacrylate, polyester acrylate and cationic photosensitive resin;the monomer is formed by mixing one or more of butyl acrylate, HDDA and TPG-DA;the photoinitiator is formed by mixing one or more of TPO, benzoin dimethyl ether, benzophenone and diaryl iodonium salt;the dispersant is prepared by mixing one or more of KH550, KH570, hyper-dispersant 9076 and Triton X-100;viscosity modifiers include PEG and/or glycerol;the defoaming agent comprises one or more of fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether and fatty acid polyoxyethylene ester.
- 5. The method for preparing the aluminum oxide ceramic surface composite coating for the vacuum arc-extinguishing chamber by 3D printing according to claim 1, wherein the photosensitive resin comprises, by mass, 55-65% of prepolymer, 25-35% of monomer, 1-5% of photoinitiator, 1-5% of dispersant, 1-8% of viscosity regulator and 1-3% of defoaming agent.
- 6. The method for preparing the aluminum oxide ceramic surface composite coating for the vacuum arc-extinguishing chamber by 3D printing according to claim 1, wherein the sintering aid is TiO 2 And MnCO 3 One or two of them;in each paste material, the total content of the sintering aid is 5-10% by mass, and the TiO content is 2 1-7% of MnCO 3 The content is 0-5%.
- 7. The 3D printing method for preparing the aluminum oxide ceramic surface composite coating for the vacuum arc-extinguishing chamber according to claim 1, wherein in the step 2), the sintering conditions are as follows: vacuum pressure 3.6X 10 -3 Pa, sintering at 1200-1500 ℃ for 2-4 h.
- 8. The 3D printing method for preparing the aluminum oxide ceramic surface composite coating for the vacuum arc-extinguishing chamber according to claim 1, wherein in the step 2), nitrogen or argon is filled during sintering.
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