CN111153701A - ZrB2-SiC composite coating and preparation method thereof - Google Patents
ZrB2-SiC composite coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a ZrB2-SiC composite coating and preparation method thereof, the ZrB2the-SiC composite coating comprises 50-80% of ZrB21-30% of SiC and 10-30% of adhesive by weight, wherein the adhesive is contained in the formula system, the compactness of the adhesive can be effectively improved, and ZrB2Controllable composition of-SiC composite coating matrix, ZrB2The content is high (50-80%), the ablation resistance and the oxidation resistance of the material are obviously improved, the preparation process is simple, the use is convenient, a coating can be directly prepared on the surface of a component by adopting a brush coating method,and the thickness of the coating can be adjusted by a method of brushing for multiple times according to requirements. The viscosity of the slurry can be adjusted, and the thickness of the single-layer coating can be adjusted through adjusting the viscosity. The coating is applied to various shapes of base materials by a brush coating method.
Description
Technical Field
The invention relates to the technical field of materials, in particular to ZrB2-SiC composite coating and preparation method thereof.
Background
Graphite materials and other carbon-based materials, such as C/C composites and the like, have a variety of excellent properties, but are easily oxidized under high-temperature oxygen-containing conditions, greatly limiting the range of applications. In order for graphite materials to meet the requirements for use in high temperature oxidation environments, their oxidation resistance must be improved.
At present, two main approaches are used for improving the oxidation resistance of graphite materials. One is matrix modification, namely adding an antioxidant into a graphite matrix to reduce the oxidation rate of the material; the other method is a surface coating method, namely, a layer of oxidation resistant coating is coated on the surface of the graphite material, so that the graphite material is isolated from oxidizing gas, and the gas is prevented from entering, thereby improving the oxidation resistance.
For ZrB2-SiC-based ceramic materials having excellent high temperature oxidation resistance. The material consists of ZrB2And SiC, the ceramic material has good oxidation resistance in the temperature range from room temperature to 1600 ℃. Thus, ZrB2The composition of-SiC is suitable for being used as a composition material of a high-temperature resistant oxidation-resistant coating. However, ZrB2the-SiC ceramic is difficult to sinter, and a compact structure is difficult to obtain in the process of preparing the coating, so that the application of the-SiC ceramic as an anti-oxidation coating is limited.
Disclosure of Invention
In order to solve the problems, the invention provides ZrB2-SiC composite coating and preparation method thereof, the ZrB2the-SiC composite coating has good high-temperature oxidation resistance, good sintering performance and easy forming, and the invention has the following specific contents:
the invention aims to provide ZrB2-SiC composite coating, which consists in: said ZrB2the-SiC composite coating comprises the following components in percentage by weight: is the ZrB2ZrB with the weight of 50-80% of that of-SiC composite coating2Said ZrB2SiC accounting for 1-30% of the weight of the-SiC composite coating and ZrB2Adhesive accounting for 10-30% of the weight of the-SiC composite coating, and ZrB2The median particle size of the SiC is 0.1-10 mu m, and the median particle size of the SiC is 0.5-10 mu m.
In some embodiments of the invention, said ZrB2The median particle size of the SiC is 0.5-5 mu m, and the median particle size of the SiC is 1-5 mu m.
In some embodiments of the invention, said ZrB2The median particle size of the SiC is 1-3 mu m, and the median particle size of the SiC is 2-5 mu m.
In some embodiments of the present invention, the adhesive is at least one of ethyl cellulose, hydroxyethyl cellulose and hydroxypropyl cellulose.
In some embodiments of the invention, said ZrB2Occupies the ZrB260-70% of the weight of the-SiC composite coating.
In one embodiment of the present invention, the SiC occupies the ZrB210-25% of the weight of the-SiC composite coating.
In some embodiments of the invention, said ZrB2Has a purity of not less than 90 percent and ZrB2The median particle size of the SiC is 0.1-10 mu, and the purity of the SiC is more than or equal to 95%.
Another object of the present invention is to provide a ZrB2The preparation method of the-SiC composite coating is characterized by comprising the following steps: weighing ZrB2Dispersing SiC and an adhesive for 60-120 min at a rotating speed of 100-200 rpm by using a dispersion machine, and then grinding for several times by using a three-roll grinder until the granularity of aluminum paste is less than 10 mu m to obtain ZrB2-SiC composite coating.
Compared with the prior art, the invention has the beneficial effects that:
1. ZrB of the invention2The preparation process of the-SiC composite coating is simple, the use is convenient, the coating can be prepared on the surface of the component by directly adopting a brush coating method, and the thickness of the coating can be adjusted by a method of brushing for multiple times according to the requirement. The viscosity of the slurry can be adjusted, and the thickness of the single-layer coating can be adjusted through adjusting the viscosity. The coating is applied to various shapes of base materials by a brush coating method.
2. ZrB of the invention2The formula system of the-SiC composite coating contains an adhesive, the density of the adhesive can be effectively improved, and ZrB2controllable-SiC composite coating matrix composition，ZrB2The content is high (50-80%), and the ablation resistance and the oxidation resistance of the material are obviously improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below so that those skilled in the art can better understand the advantages and features of the present invention, and thus the scope of the present invention will be more clearly defined. The embodiments described herein are only a few embodiments of the present invention, rather than all embodiments, and all other embodiments that can be derived by one of ordinary skill in the art without inventive faculty based on the embodiments described herein are intended to fall within the scope of the present invention.
Example 1
ZrB2the-SiC composite coating comprises the following components in percentage by weight: is the ZrB2ZrB with the weight of 65% of-SiC composite coating2Said ZrB215% SiC and ZrB of SiC composite coating220% of adhesive based on the weight of the SiC composite coating, ZrB2The median particle diameter of the SiC is 5 μm, and the median particle diameter of the SiC is 5 μm.
Wherein the adhesive is ethyl cellulose.
In some embodiments of the invention, said ZrB2The purity of the SiC is more than or equal to 90 percent, and the purity of the SiC is more than or equal to 95 percent.
ZrB prepared according to the formula2The method for preparing the-SiC composite coating comprises the following steps: weighing ZrB2Dispersing the SiC and the adhesive for 90min at the rotating speed of 150rpm by using a dispersion machine, and then grinding the mixture for several times by using a three-roll grinder until the granularity of the aluminum paste is less than 10 mu m to obtain the ZrB2-SiC composite coating.
The fiber reinforcement with deposited interface was placed in ZrB prepared in this example2And (3) soaking the-SiC composite coating for 30min under the condition of vacuum degree of-0.08 MPa. And drying the impregnated fiber cloth at 60 ℃ to obtain the carbon fiber preform. The slurry is cast into a film and dried at room temperature, and ZrB2-SiC casting biscuit with the thickness of about 100 mu m is obtained. The obtained carbon fiber preform and the obtained tape castingThe blank comprises 1 layer of carbon fiber preform (as a carbon fiber preform layer)/1 layer of ZrB2-SiC cast greens (as cast greens layers) are cut after being alternately laminated (10 times of alternate lamination). And under the vacuum environment, heating the obtained material to 800 ℃ at the speed of 10 ℃/min, and preserving heat for 2h to discharge the glue. And then heating to 2000 ℃ at a speed of 10 ℃/min (pressurizing to 30MPa perpendicular to the lamination direction when the temperature reaches 2000 ℃), and sintering for 2h to finish the material preparation. The prepared laminated structure Cf/ZrB2The porosity of the-SiC ultrahigh-temperature ceramic matrix composite material is 2.5 percent, and the air plasma ablation is 3MW/m2The rate of line ablation after 2min of ablation was only 1.5 μm/s.
Example 2
ZrB2the-SiC composite coating comprises the following components in percentage by weight: is the ZrB2ZrB accounting for 80 percent of weight of-SiC composite coating2Said ZrB2SiC accounting for 10 percent of the weight of the-SiC composite coating and ZrB accounting for the weight of the-SiC composite coating2Adhesive accounting for 10 percent of the weight of the SiC composite coating, ZrB2The median particle size of the SiC is 0.1 μm, and the median particle size of the SiC is 0.5 μm.
Wherein the adhesive is hydroxyethyl cellulose.
In some embodiments of the invention, said ZrB2The purity of the SiC is more than or equal to 90 percent, and the purity of the SiC is more than or equal to 95 percent.
ZrB prepared according to the formula2The method for preparing the-SiC composite coating comprises the following steps: weighing ZrB2Dispersing the SiC and the adhesive for 120min at the rotating speed of 100rpm by using a dispersion machine, and then grinding for several times by using a three-roll grinder until the granularity of the aluminum paste is less than 10 mu m to obtain the ZrB2-SiC composite coating.
The fiber reinforcement with deposited interface was placed in ZrB prepared in this example2And (3) soaking the-SiC composite coating for 30min under the condition of vacuum degree of-0.08 MPa. And drying the impregnated fiber cloth at 60 ℃ to obtain the carbon fiber preform. The slurry is cast into a film and dried at room temperature, and ZrB2-SiC casting biscuit with the thickness of about 100 mu m is obtained. The obtained carbon fiber preform and the obtained casting biscuit are divided into 1 layer of carbon fiber preform (as a carbon fiber preform layer)/1 layer of ZrB2-alternate lamination of SiC cast greenbodies (as cast greenbody layers)And (alternate lamination 10 times) post-trimming. And under the vacuum environment, heating the obtained material to 800 ℃ at the speed of 10 ℃/min, and preserving heat for 2h to discharge the glue. And then heating to 2000 ℃ at a speed of 10 ℃/min (pressurizing to 30MPa perpendicular to the lamination direction when the temperature reaches 2000 ℃), and sintering for 2h to finish the material preparation. The prepared laminated structure Cf/ZrB2The porosity of the-SiC ultrahigh-temperature ceramic matrix composite material is 2.4%, and the air plasma ablation is 3MW/m2The rate of line ablation after 2min of ablation was only 1.3 μm/s.
Example 3
ZrB2the-SiC composite coating comprises the following components in percentage by weight: is the ZrB2ZrB with the weight of 50 percent of-SiC composite coating2Said ZrB2-SiC accounting for 0% of the weight of the SiC composite coating and ZrB accounting for the weight of the SiC composite coating220% of adhesive based on the weight of the SiC composite coating, ZrB2The median particle diameter of the SiC is 0.5 mu m, and the median particle diameter of the SiC is 8 mu m.
Wherein the adhesive is hydroxypropyl cellulose.
In some embodiments of the invention, said ZrB2The purity of the SiC is more than or equal to 90 percent, and the purity of the SiC is more than or equal to 95 percent.
ZrB prepared according to the formula2The method for preparing the-SiC composite coating comprises the following steps: weighing ZrB2Dispersing SiC and adhesive for 60min at the rotating speed of 200rpm by using a dispersion machine, and then grinding for several times by using a three-roll grinder until the granularity of the aluminum paste is less than 10 mu m to obtain ZrB2-SiC composite coating.
The fiber reinforcement with deposited interface was placed in ZrB prepared in this example2And (3) soaking the-SiC composite coating for 30min under the condition of vacuum degree of-0.08 MPa. And drying the impregnated fiber cloth at 60 ℃ to obtain the carbon fiber preform. The slurry is cast into a film and dried at room temperature, and ZrB2-SiC casting biscuit with the thickness of about 100 mu m is obtained. The obtained carbon fiber preform and the obtained casting biscuit are divided into 1 layer of carbon fiber preform (as a carbon fiber preform layer)/1 layer of ZrB2-SiC cast greens (as cast greens layers) are cut after being alternately laminated (10 times of alternate lamination). And under the vacuum environment, heating the obtained material to 800 ℃ at the speed of 10 ℃/min, and preserving heat for 2h to discharge the glue. Then, at 10 ℃And (3) heating to 2000 ℃ in min (pressurizing to 30MPa perpendicular to the lamination direction when the temperature reaches 2000 ℃) and preserving heat for 2h for sintering to finish the material preparation. The prepared laminated structure Cf/ZrB2The porosity of the-SiC ultrahigh-temperature ceramic matrix composite material is 2.8 percent, and the air plasma ablation is 3MW/m2The rate of line ablation after 2min of ablation was only 1.7 μm/s.
Example 4
ZrB2the-SiC composite coating comprises the following components in percentage by weight: is the ZrB2ZrB with the weight of 60 percent of-SiC composite coating2Said ZrB230% of SiC and ZrB in weight percent of-SiC composite coating220% of adhesive based on the weight of the SiC composite coating, ZrB2The median particle diameter of the SiC is 1 μm, and the median particle diameter of the SiC is 7 μm.
Wherein the adhesive is a mixture of ethyl cellulose and hydroxyethyl cellulose.
In some embodiments of the invention, said ZrB2The purity of the SiC is more than or equal to 90 percent, and the purity of the SiC is more than or equal to 95 percent.
ZrB prepared according to the formula2The method for preparing the-SiC composite coating comprises the following steps: weighing ZrB2Dispersing the SiC and the adhesive for 100min at the rotating speed of 140rpm by using a dispersion machine, and then grinding the mixture for several times by using a three-roll grinder until the granularity of the aluminum paste is less than 10 mu m to obtain the ZrB2-SiC composite coating.
The fiber reinforcement with deposited interface was placed in ZrB prepared in this example2And (3) soaking the-SiC composite coating for 30min under the condition of vacuum degree of-0.08 MPa. And drying the impregnated fiber cloth at 60 ℃ to obtain the carbon fiber preform. The slurry is cast into a film and dried at room temperature, and ZrB2-SiC casting biscuit with the thickness of about 100 mu m is obtained. The obtained carbon fiber preform and the obtained casting biscuit are divided into 1 layer of carbon fiber preform (as a carbon fiber preform layer)/1 layer of ZrB2-SiC cast greens (as cast greens layers) are cut after being alternately laminated (10 times of alternate lamination). And under the vacuum environment, heating the obtained material to 800 ℃ at the speed of 10 ℃/min, and preserving heat for 2h to discharge the glue. Then heating to 2000 deg.C at a rate of 10 deg.C/min (pressurizing to 30MPa perpendicular to the lamination direction when the temperature reaches 2000 deg.C), and sintering for 2h to obtain the final productAnd (4) preparing the material. The prepared laminated structure Cf/ZrB2The porosity of the-SiC ultrahigh-temperature ceramic matrix composite material is 3.5 percent, and the air plasma ablation is 3MW/m2The rate of line ablation after 2min of ablation was only 1.8 μm/s.
Example 5
ZrB2the-SiC composite coating comprises the following components in percentage by weight: is the ZrB2ZrB with the weight of 70 percent of-SiC composite coating2Said ZrB2SiC accounting for 5 percent of the weight of the-SiC composite coating and ZrB accounting for the weight of the-SiC composite coating225% of adhesive based on the weight of the-SiC composite coating, ZrB2The median particle diameter of the SiC is 3 mu m, and the median particle diameter of the SiC is 7 mu m.
Wherein the adhesive is a mixture of ethyl cellulose and hydroxypropyl cellulose.
In some embodiments of the invention, said ZrB2The purity of the SiC is more than or equal to 90 percent, and the purity of the SiC is more than or equal to 95 percent.
ZrB prepared according to the formula2The method for preparing the-SiC composite coating comprises the following steps: weighing ZrB2Dispersing SiC and adhesive for 80min at the rotating speed of 180rpm by using a dispersion machine, and then grinding for several times by using a three-roll grinder until the granularity of the aluminum paste is less than 10 mu m to obtain ZrB2-SiC composite coating.
The fiber reinforcement with deposited interface was placed in ZrB prepared in this example2And (3) soaking the-SiC composite coating for 30min under the condition of vacuum degree of-0.08 MPa. And drying the impregnated fiber cloth at 60 ℃ to obtain the carbon fiber preform. The slurry is cast into a film and dried at room temperature, and ZrB2-SiC casting biscuit with the thickness of about 100 mu m is obtained. The obtained carbon fiber preform and the obtained casting biscuit are divided into 1 layer of carbon fiber preform (as a carbon fiber preform layer)/1 layer of ZrB2-SiC cast greens (as cast greens layers) are cut after being alternately laminated (10 times of alternate lamination). And under the vacuum environment, heating the obtained material to 800 ℃ at the speed of 10 ℃/min, and preserving heat for 2h to discharge the glue. And then heating to 2000 ℃ at a speed of 10 ℃/min (pressurizing to 30MPa perpendicular to the lamination direction when the temperature reaches 2000 ℃), and sintering for 2h to finish the material preparation. The prepared laminated structure Cf/ZrB2The porosity of the-SiC ultrahigh-temperature ceramic matrix composite material is 2.0% air plasma ablation 3MW/m2The rate of line ablation after 2min of ablation was only 1.1 μm/s.
Example 6
ZrB2the-SiC composite coating comprises the following components in percentage by weight: is the ZrB2ZrB with the weight of 70 percent of-SiC composite coating2Said ZrB2SiC accounting for 10 percent of the weight of the-SiC composite coating and ZrB accounting for the weight of the-SiC composite coating220% of adhesive based on the weight of the SiC composite coating, ZrB2The median particle diameter of the SiC is 8 mu m, and the median particle diameter of the SiC is 2 mu m.
The adhesive is a mixture of ethyl cellulose, hydroxyethyl cellulose and hydroxypropyl cellulose.
In some embodiments of the invention, said ZrB2The purity of the SiC is more than or equal to 90 percent, and the purity of the SiC is more than or equal to 95 percent.
ZrB prepared according to the formula2The method for preparing the-SiC composite coating comprises the following steps: weighing ZrB2Dispersing the SiC and the adhesive for 75min at the rotating speed of 140rpm by using a dispersion machine, and then grinding the mixture for several times by using a three-roll grinder until the granularity of the aluminum paste is less than 10 mu m to obtain the ZrB2-SiC composite coating.
The fiber reinforcement with deposited interface was placed in ZrB prepared in this example2And (3) soaking the-SiC composite coating for 30min under the condition of vacuum degree of-0.08 MPa. And drying the impregnated fiber cloth at 60 ℃ to obtain the carbon fiber preform. The slurry is cast into a film and dried at room temperature, and ZrB2-SiC casting biscuit with the thickness of about 100 mu m is obtained. The obtained carbon fiber preform and the obtained casting biscuit are divided into 1 layer of carbon fiber preform (as a carbon fiber preform layer)/1 layer of ZrB2-SiC cast greens (as cast greens layers) are cut after being alternately laminated (10 times of alternate lamination). And under the vacuum environment, heating the obtained material to 800 ℃ at the speed of 10 ℃/min, and preserving heat for 2h to discharge the glue. And then heating to 2000 ℃ at a speed of 10 ℃/min (pressurizing to 30MPa perpendicular to the lamination direction when the temperature reaches 2000 ℃), and sintering for 2h to finish the material preparation. The prepared laminated structure Cf/ZrB2The porosity of the-SiC ultrahigh-temperature ceramic matrix composite material is 3.3 percent, and the air plasma ablation is 3MW/m2The rate of line ablation after 2min of ablation was only 1.6 μm/s.
The invention only provides ZrB2The present invention relates to a method for preparing SiC composite coating, a method for preparing the same, and a method for implementing the same, and a method for preparing the same, which are only preferred embodiments of the present invention, and it should be noted that, for those skilled in the art, a plurality of modifications and refinements can be made without departing from the principle of the present invention, and these modifications and refinements should be regarded as the protection scope of the present invention, and each component not specified in the present embodiment can be implemented by using the existing technology.
Claims (8)
1. ZrB2-SiC composite coating, characterized in that: said ZrB2the-SiC composite coating comprises the following components in percentage by weight: is the ZrB2ZrB with the weight of 50-80% of that of-SiC composite coating2Said ZrB2SiC accounting for 1-30% of the weight of the-SiC composite coating and ZrB2Adhesive accounting for 10-30% of the weight of the-SiC composite coating, and ZrB2The median particle size of the SiC is 0.1-10 mu m, and the median particle size of the SiC is 0.5-10 mu m.
2. A ZrB according to claim 12-SiC composite coating, characterized in that: said ZrB2The median particle size of the SiC is 0.5-5 mu m, and the median particle size of the SiC is 1-5 mu m.
3. ZrB according to claim 12-SiC composite coating, characterized in that: said ZrB2The median particle size of the SiC is 1-3 mu m, and the median particle size of the SiC is 2-5 mu m.
4. A ZrB according to any one of claims 1-32-SiC composite coating, characterized in that: the adhesive is at least one of ethyl cellulose, hydroxyethyl cellulose and hydroxypropyl cellulose.
5. A ZrB according to claim 42-SiC composite coating, characterized in that: said ZrB2Occupies the ZrB260-70% of the weight of the-SiC composite coating.
6. ZrB according to claim 52-SiC composite coating, characterized in that: the SiC occupies the ZrB210-25% of the weight of the-SiC composite coating.
7. ZrB according to claim 62-SiC composite coating, characterized in that: said ZrB2Has a purity of not less than 90 percent and ZrB2The median particle size of the SiC is 0.1-10 mu, and the purity of the SiC is more than or equal to 95%.
8. ZrB2The preparation method of the-SiC composite coating is characterized by comprising the following steps: weighing ZrB according to the formula of claims 1 to 72Dispersing SiC and an adhesive for 60-120 min at a rotating speed of 100-200 rpm by using a dispersion machine, and then grinding for several times by using a three-roll grinder until the granularity of aluminum paste is less than 10 mu m to obtain ZrB2-SiC composite coating.
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