CN113929501B - Flashover-resistant gradient composite coating on surface of aluminum oxide ceramic and preparation method thereof - Google Patents
Flashover-resistant gradient composite coating on surface of aluminum oxide ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an alumina ceramic surface flashover-resistant gradient composite coating and a preparation method thereof, belonging to the field of alumina ceramic surface composite coatings. Selecting chromium oxide body with low secondary electron emission coefficient, low relative dielectric constant and low surface resistivityAs the flashover resistant coating, the substrate is alumina ceramic, and the outermost coating is a chromium oxide coating, so that Cr is used 2 O 3 The content increases layer by layer, while Al 2 O 3 The content is reduced layer by layer to make its composition and electric properties continuously change, and the Cr content in the coating can be changed 2 O 3 To achieve control of the relative dielectric constant/surface resistivity of the coating. The main component content of each coating is changed in a gradient manner, the coating has good binding force with a substrate, and meanwhile, the deformation caused by thermal stress is reduced.
Description
Technical Field
The invention belongs to the field of composite coatings on the surfaces of aluminum oxide ceramics, and relates to a flashover-resistant gradient composite coating on the surfaces of the aluminum oxide ceramics and a preparation method thereof.
Background
The vacuum arc-extinguishing chamber is one of the core components in the vacuum electrical equipment, plays roles of rapidly extinguishing arc and inhibiting current in the power-on and power-off processes of a high-voltage circuit, and requires that a shell material of the vacuum arc-extinguishing chamber has the characteristics of high voltage resistance, vacuum insulation, small leakage current and the like. Ceramic materials as insulating media, e.g. Al 2 O 3 The ceramic has a compressive strength of 300-400 kV/cm and Al 2 O 3 The ceramic can be used as a structural member to support the vacuum structure of the arc extinguish chamber. Vacuum is used as a special insulating medium, the breakdown strength of the vacuum can reach 350kV/cm, but electric lines at the three joint points of the insulating medium, the vacuum and the electrodes are easy to gather to cause a discharge phenomenon, the penetration breakdown occurs between the electrodes under the action of high voltage, the vacuum can fail under the electric field strength of 16-25 kV/cm,this failure mode is called surface-creeping flashover. Generally, the condition of the surface flashover phenomenon is often far lower than the breakdown condition of vacuum or the insulating medium, and the service life and stability of the vacuum electrical equipment are severely limited by the surface flashover phenomenon.
In summary, the aluminum oxide materials used in the present vacuum arc-extinguishing chamber still have the problems of too high secondary electron emission coefficient, insufficient flashover voltage resistance, etc., so the insulating material of the vacuum arc-extinguishing chamber needs to be improved to improve the flashover performance of the vacuum arc-extinguishing chamber along the surface.
Disclosure of Invention
The invention aims to overcome the defects of overhigh secondary electron emission coefficient and insufficient flashover resistant voltage of an aluminum oxide material used for a vacuum arc-extinguishing chamber in the prior art, and provides an aluminum oxide ceramic surface flashover resistant gradient composite coating and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the flashover-resistant gradient composite coating on the surface of the alumina ceramic comprises Cr which is upwards arranged along the surface of a substrate 2 O 3 And Al 2 O 3 Four-layer coating with gradient content and Cr 2 O 3 And Al 2 O 3 The gradient change direction of the content is opposite; the thickness of each coating is 5-10 μm.
Preferably, the first coating comprises 20-40% of Cr by mass 2 O 3 50-70% of Al 2 O 3 And 5-10% of a sintering aid; the second coating comprises 40-60% of Cr 2 O 3 30 to 50% of Al 2 O 3 And 5-10% of a sintering aid; the third coating comprises 60-80% of Cr 2 O 3 10 to 30% of Al 2 O 3 5-10% of sintering aid; the fourth coating comprises 90-95% of Cr 2 O 3 And 5-10% of a sintering aid.
Preferably, the sintering aid is TiO 2 、MnO 2 Or one or more of MgO;
in each coating, the total content of the sintering aid is 5-10% by mass, wherein TiO 2 1-5% of MnO 2 The content is 0-5%, and the MgO content is 0-5%.
A preparation method of the flashover-resistant gradient composite coating on the surface of the alumina ceramic comprises the following steps:
step 1) adding Cr 2 O 3 、Al 2 O 3 Mixing the sintering aid and the solvent to obtain Cr 2 O 3 And Al 2 O 3 Four slurries with gradient content and a volume solid content of 10-60 vol.%;
step 2) sequentially and uniformly coating the four slurries on the surface of an insulator matrix along gradient change, standing and drying to obtain an alumina insulator with four coatings on the surface;
and 3) sintering the alumina insulator with the four layers of coatings on the surface to obtain the flashover resistant gradient composite coating on the surface of the alumina ceramic substrate.
Preferably, a dispersing agent is added into the four slurries in the step 1), and the mass percentage of the dispersing agent in each slurry is 0.4-2%.
Preferably, the dispersant is one of polyvinylpyrrolidone, sodium polyacrylate or polyvinyl alcohol.
Preferably, the solvent is one of absolute ethanol, silica sol or aluminum sol.
Preferably, the conditions of the sintering process are:
vacuum pressure 3.6X 10 -3 Pa, the sintering temperature is 1300-1500 ℃, the sintering time is 1-4 h, and nitrogen or argon is filled during sintering.
Preferably, the standing and drying conditions of step 2) are as follows: standing and drying for 8h at room temperature.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a flashover-resistant gradient composite coating on the surface of alumina ceramic, which selects a chromium oxide system with low secondary electron emission coefficient, low relative dielectric constant and low surface resistivity as a flashover-resistant coating, a plurality of layers of transition coatings are added between a substrate and the flashover-resistant layer, the contents of main components of the coatings are in gradient change, and the coatings have good binding force with the substrate and simultaneously reduce the deformation caused by thermal stress.
The invention also discloses a preparation method of the flashover-resistant gradient composite coating on the surface of the alumina ceramic, and the substrate is the alumina ceramic, and the outermost coating is the chromium oxide coating, so that Cr is contained in the chromium oxide coating 2 O 3 The content increases layer by layer, while Al 2 O 3 The content is reduced layer by layer, the components and the electrical property of the coating are continuously changed, the thermal stress between the coating and the substrate is reduced, and simultaneously, the Cr in the coating is changed 2 O 3 To achieve control of the relative dielectric constant/surface resistivity of the coating. The coating prepared by the method effectively improves the surface flashover resistance of the insulating medium on the basis of ensuring the original good structural strength and pressure resistance of the insulating medium matrix.
Drawings
FIG. 1 is a SEM image of the cross section of a flashover resistant gradient composite coating on the surface of the alumina ceramic obtained in example 2;
FIG. 2 is a SEM image of the cross section of the flashover resistant gradient composite coating on the surface of the alumina ceramic obtained in example 2;
FIG. 3 is a SEM image of the cross section of the flashover resistant gradient composite coating on the surface of the alumina ceramic obtained in example 6;
FIG. 4 is a sectional EDS diagram of the flashover resistant gradient composite coating on the surface of the alumina ceramic obtained in example 6;
FIG. 5 is a SEM image of the cross section of the flashover resistant gradient composite coating on the surface of the alumina ceramic obtained by the comparative example;
FIG. 6 is a sectional EDS diagram of the flashover resistant gradient composite coating on the surface of the alumina ceramic obtained by the comparative example;
FIG. 7 is a side macro photograph of the flashover gradient resistant composite coatings on the surfaces of the alumina ceramics obtained in examples 1, 2 and 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 obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, shall fall within the protection scope of the present invention.
It should be noted that the terms "comprises" and "comprising," and any variations thereof, are intended to cover a non-exclusive inclusion, 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:
step 1) adding Cr 2 O 3 、Al 2 O 3 Mixing the sintering aid and the solvent to obtain Cr 2 O 3 And Al 2 O 3 The content of the four slurries changes in a gradient manner, and the volume solid content of the four slurries is 10-60%;
step 2) sequentially and uniformly coating the four slurries on the surface of an insulator matrix along gradient change, standing and drying to obtain an alumina insulator with four coatings on the surface;
and 3) sintering the alumina insulator with the four layers of coatings on the surface to obtain the flashover resistant gradient composite coating on the surface of the alumina ceramic substrate.
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 composition of the raw materials of the chromium oxide coating systems selected in the examples
TABLE 2 slurry proportioning and sintering process of chromium oxide coating system selected in the invention
According to the proportion shown in the table 2, the dispersant is polyvinylpyrrolidone, the solid content of the system is adjusted to the numerical value in the table through solvent absolute ethyl alcohol, the mixture is uniformly mixed and ball-milled for 24 hours, then the mixture is uniformly sprayed on the surface of the insulator matrix by using an electric spray gun, the single-layer spraying thickness is 5-10 mu m, and the mixture is stood for 8 hours at room temperature. All coatings are applied to the surface of the insulator step by step in the coating sequence from inside to outside (i.e., the first layer adjacent to the surface of the substrate).
Putting the obtained insulator into a vacuum sintering furnace, and vacuumizing to be lower than 3.6 multiplied by 10 -3 And Pa, according to the sintering process shown in the table 2, introducing high-purity argon, 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 2 are, in mass percent, Cr in the first coating slurry 2 O 3 50% of Al 2 O 3 40% of TiO 2 MnO content of 5% 2 The content is 2 percent, and the content of MgO is3 percent; cr in the second layer coating slurry 2 O 3 90% of Al 2 O 3 0% of TiO 2 MnO content of 5% 2 The content is 5%, and the MgO content is 0%. Coating all the coatings on the surface of the insulator in the order of inside and outside, placing the obtained insulator into a vacuum sintering furnace, and vacuumizing to less than 3.6 multiplied by 10 -3 Pa, filling high-purity argon, 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 3.5, and the surface resistivity is reduced to 1.1 multiplied by 10 10 Omega/sq, the flashover resistance of the surface is greatly improved.
The microstructure of the cross section of the flashover resistant gradient composite coating on the surface of the alumina ceramic obtained in example 2 is shown in fig. 1, the overall thickness of the coating is 10-20 μm, and the corresponding EDS result is shown in fig. 2, which shows that the distribution of Cr element is difficult to distinguish in the interior except for a layer with concentrated surface, the distribution of Cr element is not flat enough, but becomes a curve, the average thickness is 7 μm, the surface roughness of the coating is large, and a plurality of concave-convex structures exist.
In percentage by mass, the coating raw materials of example 6 are the first layer of coating slurry containing Cr 2 O 3 35% of Al 2 O 3 60% of TiO 2 Content of 1% MnO 2 The content is 1 percent, and the MgO content is 3 percent; cr in the second layer coating slurry 2 O 3 55% of Al 2 O 3 40% of TiO 2 Content of 2%, MnO 2 The content is 1 percent, and the MgO content is 2 percent; cr in third layer coating slurry 2 O 3 75% of Al 2 O 3 20% of TiO 2 Content of 3% MnO 2 The content is 1 percent, and the MgO content is 1 percent; cr in the fourth layer coating slurry 2 O 3 95% of TiO 2 Content of 4% MnO 2 The content is 1%. The dispersant content was 1.2% and the volume solids content was 30 vol%. Coating all the coatings on the surface of the insulator in the order of inside and outside, and coating the obtained insulatorPutting the flange into a vacuum sintering furnace, and vacuumizing to be less than 3.6 multiplied by 10 -3 Pa, filling high-purity argon, 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 3.4, and the surface resistivity is reduced to 8.2 multiplied by 10 9 Omega/sq, the flashover resistance of the surface is greatly improved.
The section microstructure of the flashover resistant gradient composite coating on the surface of the alumina ceramic obtained in example 6 is shown in fig. 3, the overall thickness of the coating is 10-20 μm, and the corresponding EDS result is shown in fig. 4, which shows that the Cr element distribution is in a gradient transition structure, and the Cr element distribution is in a gradient transition structure 2 O 3 Has been partially infiltrated with Al 2 O 3 In the matrix, due to the introduction of the transition coating, a fixed boundary line does not exist between the coating and the matrix, the fact that the coating is basically compact and has strong binding force can be seen, and in combination with performance data of each embodiment in table 3, the alumina ceramic surface flashover-resistant gradient composite coating prepared by the method can effectively reduce the relative dielectric constant and the surface resistivity of the insulator and improve the flashover-resistant capability of the surface.
The microstructure of the cross section of the alumina ceramic of the comparative example is shown in FIG. 5, and the corresponding EDS diagram is shown in FIG. 6, it can be seen that the microstructure of the alumina matrix with a flat and dense cross section and the Al element uniformly distributed are observed, since the alumina ceramic has a high relative dielectric constant (11.7) and a high surface resistivity (2.3X 10) 13 ) The flashover resistance of the surface is poor.
Fig. 7 is a side photomicrograph of the gradient coated samples of example 1, example 2, and example 6, respectively. The coated wafer samples sintered at 1400 ℃ were observed from the side and the entire side was red, indicating Cr 2 O 3 The diffusion depth of the coating at high temperature is very large. The single layer sample of example 1 was subjected to a large deformation, the diameter of the sample was 90mm, and the displacement of the center point in the axial direction was 2mm, which was due to the macroscopic deformation of Cr 2 O 3 Diffusion of the coating to Al 2 O 3 The lattice distortion generated in the matrix induces stress, and the stress is very large. The two-layer sample example 2 was relatively free of much distortion, but had a slightly textured surfaceThe bulge is 1mm, which indicates that large stress exists in the sample to cause macroscopic deformation. The four-layer sample of example 6 was also sintered at 1400 ℃ without significant stress-induced deformation, indicating that the gradient structure coating had Cr in its depth direction 2 O 3 With Al 2 O 3 The content gradually-changed area can effectively inhibit the generation of stress in the high-temperature sintering process, and ensures that the coating sample cannot generate macroscopic deformation.
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)
1. The flashover-resistant gradient composite coating on the surface of the alumina ceramic is characterized by comprising Cr which is upwards arranged along the surface of a substrate 2 O 3 And Al 2 O 3 Four layers of coating with gradient content and Cr 2 O 3 And Al 2 O 3 The gradient change direction of the content is opposite; the thickness of each coating is 5-10 μm; wherein the first coating comprises 20-40% of Cr by mass 2 O 3 50-70% of Al 2 O 3 And 5-10% of a sintering aid; the second coating comprises 40-60% of Cr 2 O 3 30 to 50% of Al 2 O 3 And 5-10% of a sintering aid; the third coating comprises 60-80% of Cr 2 O 3 10 to 30% of Al 2 O 3 5-10% of sintering aid; the fourth coating comprises 90-95% of Cr 2 O 3 And 5-10% of a sintering aid.
2. The alumina ceramic surface flashover-resistant gradient composite coating of claim 1, wherein the sintering aid is TiO 2 、MnO 2 Or one or more of MgO;
in each coating layer, the mass percentage of the sintering aidThe total content is 5-10%, wherein TiO 2 1-5% of MnO 2 The content is 0-5%, and the MgO content is 0-5%.
3. A method for preparing the flashover-resistant gradient composite coating on the surface of the alumina ceramic according to claim 1 or 2, which is characterized by comprising the following steps:
step 1) adding Cr 2 O 3 、Al 2 O 3 Mixing the sintering aid and the solvent to obtain Cr 2 O 3 And Al 2 O 3 Four slurries with gradient content and a volume solid content of 10-60 vol.%;
step 2) sequentially and uniformly coating the four slurries on the surface of an insulator matrix along gradient change, standing and drying to obtain an alumina insulator with four coatings on the surface;
and 3) sintering the alumina insulator with the four layers of coatings on the surface to obtain the flashover resistant gradient composite coating on the surface of the alumina ceramic substrate.
4. The method for preparing the flashover-resistant gradient composite coating on the surface of the alumina ceramic according to claim 3, wherein a dispersing agent is added into the four kinds of slurry in the step 1), and the mass percent of the dispersing agent in each kind of slurry is 0.4-2%.
5. The method for preparing the flashover resistant gradient composite coating on the surface of the alumina ceramic according to claim 4, wherein the dispersing agent is one of polyvinylpyrrolidone, sodium polyacrylate or polyvinyl alcohol.
6. The method for preparing the flashover resistant gradient composite coating on the surface of the alumina ceramic according to claim 3, wherein the solvent is one of absolute ethyl alcohol, silica sol or aluminum sol.
7. The method for preparing the flashover-resistant gradient composite coating on the surface of the alumina ceramic according to claim 3, wherein the conditions of the sintering process are as follows:
vacuum pressure 3.6X 10 -3 Pa, the sintering temperature is 1300-1500 ℃, the sintering time is 1-4 h, and nitrogen or argon is filled during sintering.
8. The method for preparing the flashover-resistant gradient composite coating on the surface of the alumina ceramic according to claim 3, wherein the standing and drying conditions of the step 2) are as follows: standing and drying for 8h at room temperature.
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