CN110963824B - Yttrium oxide doped calcined mullite-zirconium silicate environmental barrier coating and preparation method thereof - Google Patents

Yttrium oxide doped calcined mullite-zirconium silicate environmental barrier coating and preparation method thereof Download PDF

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CN110963824B
CN110963824B CN201911376317.4A CN201911376317A CN110963824B CN 110963824 B CN110963824 B CN 110963824B CN 201911376317 A CN201911376317 A CN 201911376317A CN 110963824 B CN110963824 B CN 110963824B
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mullite
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曾毅
熊翔
钱天笑
伦惠林
叶子名
胡锦润
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Central South University
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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Abstract

The invention discloses an yttrium oxide doped calcined mullite-zirconium silicate environmental barrier coating and a preparation method thereof, comprising a SiC bonding layer and a composite layer, wherein the composite layer is made of ZrSiO4Powder, Y2O3Powder and mullite powder as raw materials, Y2O3Powder, mullite powder and ZrSiO4The molar ratio of the powder is (0.1-1.0): (0.2-1.0): 0.3-1.0). The invention is based on the discovery that2O3The powder and the mullite are blended and sintered, so that a large amount of amorphous silicon dioxide in the mullite is converted, and the porous layer is prevented from being formed under the action of high-temperature water vapor, and the aim of improving the stability of the mullite is fulfilled. The invention adopts a brush coating-sintering method, has low process cost, short preparation time and simple process, and the prepared composite coating has compact structure. The environment barrier coating prepared by the invention has uniform components and good steam corrosion resistance.

Description

Yttrium oxide doped calcined mullite-zirconium silicate environmental barrier coating and preparation method thereof
Technical Field
The invention belongs to the technical field of high-temperature coatings, and particularly relates to an yttrium oxide doped calcined mullite-zirconium silicate environmental barrier coating and a preparation method thereof.
Background
The silicon carbide ceramic matrix composite is a novel high-temperature structural material and functional material which can meet the requirement of high-temperature use. The material has great potential as a high-temperature structural material, particularly as a structural material for special parts of aerospace aircrafts which need to bear extremely high temperature. The silicon carbide ceramic matrix composite has high density, high specific strength, high temperature resistance and ablation resistanceThe composite material is a novel composite material which integrates thermal protection, structural bearing and oxidation resistance, and is widely applied to the fields of aviation, aerospace and the like, such as heat-proof structural members of aerospace vehicles, long-term oxidation-resistant parts of engine materials, aircraft brake pads and the like. However, in the aeroengine gas environment, a certain amount of water vapor (10%) is inevitably generated in the gas due to the combustion of hydrocarbon fuel, the water vapor increases the oxidation rate of SiC by several orders of magnitude, and SiO is generated2Reaction with steam produces predominantly volatile Si (OH)4The oxidation of the carbon fiber/silicon carbide fiber and matrix material is accelerated, resulting in a rapid degradation of the performance of the composite.
Accordingly, environmental barrier coatings have been extensively studied in recent years to improve the corrosion resistance of silicon carbide composites in high temperature water vapor environments. Mullite is considered a promising material for environmental barrier coatings due to its chemical compatibility, high stability in oxidizing environments, and a well-matched coefficient of thermal expansion to SiC. The sol-gel method is the most widely used method for preparing mullite having high purity and crystallinity. However, the precursors used in this process are generally expensive, thus limiting the large-scale production of mullite. Moreover, this method is extremely time consuming. In contrast, the calcination process is much cheaper and simpler, and mullite powder can be produced by a simple process at low cost, for example by solid phase sintering of silica and alumina. However, mullite produced by calcination generally contains a large amount of impurities such as amorphous silica, which causes its phase structure to be extremely unstable in a high-temperature water vapor environment-amorphous silica is converted into volatile Si (OH) in hot water vapor4Form porous Al2O3Layers and significant damage to the coating.
It is also reported that high temperature moisture causes deterioration of the mullite material. To improve the resistance of mullite coatings to water vapor corrosion, rare earth silicates (RE-silicates), especially yttrium silicate materials, are often added thereto. The yttrium silicate doped mullite coatings exhibit excellent stability in hot steam. In addition, yttrium silicate matches the SiC layer due to its Coefficient of Thermal Expansion (CTE)The low volatility in water vapor is considered as the best additive for mullite coating, but at present, many coatings are prepared by mixing mullite and Y2Si2O7After mixing, the coating was prepared, but this method had little improvement in mullite stability. Thus, patent CN105384467A reports a method for preparing a mullite and yttrium silicate multilayer composite coating by a plasma spraying method, wherein a single mullite layer is adopted at a part which is combined with SiC, and then step concentration is prepared; amount of mullite and Y2Si2O7A mixed layer, a single Y is prepared on the outermost surface2Si2O7Although the composite coating structure can effectively improve the high-temperature oxidation resistance of the coating (the composite coating still has a stable structure after static oxidation for 300 hours), the composite coating comprises a plurality of layers (at least 6 layers), and the formula of each layer of material is changed, so that the thickness of the finally prepared coating is large, and the process is complicated.
Disclosure of Invention
The invention aims to provide an yttrium oxide doped calcined mullite-zirconium silicate environmental barrier coating which is resistant to high temperature and oxygen water corrosion and low in cost and a preparation method thereof.
The yttrium oxide doped calcined mullite-zirconium silicate environmental barrier coating comprises a SiC bonding layer and a composite layer, wherein the composite layer is formed by ZrSiO4Powder, Y2O3Powder and mullite powder, Y2O3Powder, mullite powder and ZrSiO4The molar ratio of the powder is (0.1-1.0): (0.2-1.0): 0.3-1.0).
Preferably, said Y is2O3Powder, mullite powder and ZrSiO4The molar ratio of the powder is (0.1-0.3): (0.2-0.5): 0.3-0.6).
Preferably, said Y is2O3Powder, mullite powder and ZrSiO4The molar ratio of the powders was 0.15:0.3: 0.55.
The ZrSiO4The purity of the powder is more than or equal to 99 percent, and the granularity of the powder is micron; said Y is2O3The purity of the powder is more than or equal to 99 percent, and the particles areThe degree is micron level; the purity of the mullite powder is more than or equal to 98 percent, and the granularity of the mullite powder is micron-sized.
The preparation method of the yttrium oxide doped calcined mullite-zirconium silicate environmental barrier coating comprises the following steps:
1) preparing a bonding layer: depositing a SiC coating on the surface of the C/C-SiC composite material matrix by using a chemical vapor deposition technology to serve as a bonding layer;
2) preparing mixed powder: ZrSiO4Powder, Y2O3Mixing the powder and mullite in proportion, performing ball milling, uniformly mixing and drying to obtain mixed powder;
3) preparing a composite coating: and 2) mixing the mixed powder polyvinyl alcohol solution obtained in the step 2), stirring and uniformly mixing to obtain slurry, uniformly coating the slurry on the SiC bonding layer, drying the SiC bonding layer, sintering the dried sample, and cooling to room temperature after sintering to obtain the yttrium oxide doped calcined mullite-zirconium silicate environmental barrier coating.
In the step 1), the thickness of the SiC bonding layer is 30-40 um.
In the step 2), ball milling time is 4-6 h, ball milling medium is ethanol or water, ball milling rotation speed is 200-400 rmp, and ball-to-material ratio is (5-10): 1; the drying temperature is 40-60 ℃.
In the step 3), the ratio of mixed powder to mixed slurry of polyvinyl alcohol solution is (1-2) to 1, and the concentration of the polyvinyl alcohol solution is (1-3)/100 g/mL; the coating thickness is 100-200 um; the drying temperature is 100-140 ℃, and the drying time is 18-30 h; sintering is carried out under inert atmosphere or vacuum condition; the sintering temperature is 1300-1600 ℃, the heating rate is 5-10 ℃/min, and the heat preservation time is 1-2 h.
The inert atmosphere is argon or helium, and the vacuum degree is less than 5 Pa.
The principle of the invention is as follows: y is2O3The doping can remove residual silicon dioxide in calcined mullite powder and cristobalite phase generated in the high-temperature sintering process to generate Y2Si2O7-a mullite eutectic composition. ZrSiO4Is a heat expansionThe coefficient of expansion is close to that of SiC and is compared with Y2Si2O7And materials in which mullite is more stable under high temperature water corrosion conditions. Stabilized mullite-Y is formed by brushing an yttria-doped calcined mullite-zirconium silicate coating2Si2O7-ZrSiO4And (4) coating.
The invention has the beneficial effects that: 1) the invention is based on the discovery that2O3The powder and the mullite are blended and sintered, so that a large amount of amorphous silicon dioxide in the mullite is converted, and the porous layer is prevented from being formed under the action of high-temperature water vapor, and the aim of improving the stability of the mullite is fulfilled. 2) The invention adopts a brush coating-sintering method, has low process cost, short preparation time and simple process, and the prepared composite coating has compact structure. (3) The environment barrier coating prepared by the invention has uniform components and good steam corrosion resistance.
Drawings
FIG. 1 is an XRD pattern of the composite coatings prepared in examples 1 and 2;
FIG. 2 is a cross-sectional SEM image of a sample prepared according to example 2 and containing a coating;
FIG. 3 is a cross-sectional SEM image of a sample containing a coating prepared in example 3;
FIG. 4 shows the weight loss of the coatings of examples 1 and 2 due to high-temperature water corrosion: (a) example 2 corrosion of a coating sample under pure water vapor or air conditions was prepared; (b) examples 1 and 2 preparation of coated samples and uncoated samples for changes in mass loss rate under high temperature conditions; (c) examples 1 and 2 coated samples were prepared and uncoated samples were prepared with a change in the rate of mass loss.
Detailed Description
Example 1
1. Preparation of the bonding layer: and depositing a layer of SiC coating of about 33um on the surface of the C/C-SiC composite material matrix by using a chemical vapor deposition technology as a bonding layer.
2. Preparing a composite coating: will Y2O3Powder, mullite powder, ZrSiO4Powder (wherein the granularity of the mullite powder is-5000 meshes, Y2O3、ZrSiO4Powder is-2000 mesh, purity more than or equal to 99%) in a planetary ball mill at a rotation speed of 300rpm for 5h (the ball milling medium is ethanol, the ball-material ratio is 5:1) according to a molar ratio of 0.2:0.4:0.4, and after the ball milling is finished, drying the mixture at 40 ℃ and sieving the dried mixture to obtain mixed powder.
And (3) mixing the mixed powder with a polyvinyl alcohol solution with the concentration of 2g/100ml (the slurry ratio is 2:1), stirring for 5 hours by using a magnetic stirrer, uniformly coating the obtained slurry on the surface of the C/C-SiC matrix SiC bonding layer, and brushing the slurry to the thickness of 200 mu m. After the brush coating is finished, the paint is dried in a forced air drying oven at 120 ℃ for 24 hours. Carrying out high-temperature sintering on the sample which is brushed and dried, wherein the sintering process is carried out under the argon atmosphere, and the conditions of the sintering process are as follows: and heating to 1300 ℃, preserving the heat for 60min, cooling to room temperature at the heating rate of 10 ℃/min, and taking out to obtain the sample with the environmental barrier coating.
XRD analysis of the composite coating of the sample showed that the composite coating was formed from ZrSiO as shown in FIG. 14Mullite, Y2Si2O7The composition and the distribution of each phase are relatively uniform.
Samples with environmental barrier coatings were tested at 1300 ℃ and 95% H2O-5％O2，9.4×10-1After 10 hours of corrosion under the condition of m/s flow velocity, the mass loss of the C/C-SiC coated with the coating is 3.43%, as shown in FIG. 4b, compared with the uncoated C/C-SiC material, the loss rate is 1/4, which shows that the coating of the embodiment has good high-temperature water oxygen resistance. In the corrosion process, the recession rate of the coating is shown in fig. 4C, the coating of example 1 is stably recession, and the recession of the C/C-SiC material without the coating is very obvious.
Example 2
1. Preparation of the bonding layer: and depositing a SiC coating layer of about 40um on the surface of the C/C-SiC composite material matrix by using a chemical vapor deposition technology as a bonding layer.
2. Preparing a composite coating: will Y2O3Powder, mullite powder, ZrSiO4Powder (wherein the granularity of the mullite powder is-5000 meshes, Y2O3、ZrSiO4Powder of-2000 meshes and purity of more than or equal to 99%) according to the molar ratio of 0.15:0.3:0.55 in a planetary ball mill at the rotation speed of 300rpmAnd (3) carrying out rapid ball milling for 5h (the ball milling medium is ethanol, the ball-to-material ratio is 5:1), drying the mixture at 40 ℃ after the ball milling is finished, and sieving the dried mixture to obtain mixed powder.
And (3) mixing the mixed powder with a polyvinyl alcohol solution with the concentration of 2g/100ml (the slurry ratio is 2:1), stirring for 5 hours by using a magnetic stirrer, uniformly coating the obtained slurry on the surface of the C/C-SiC matrix SiC bonding layer, and brushing the slurry to the thickness of 200 mu m. After the brush coating is finished, the paint is dried in a forced air drying oven at 120 ℃ for 24 hours. Carrying out high-temperature sintering on the sample which is brushed and dried, wherein the sintering process is carried out under the argon atmosphere, and the conditions of the sintering process are as follows: and heating to 1300 ℃, preserving the heat for 60min, cooling to room temperature at the heating rate of 10 ℃/min, and taking out to obtain the sample with the environmental barrier coating.
XRD analysis of the composite coating of the sample showed that the composite coating was formed from ZrSiO as shown in FIG. 14Mullite, Y2Si2O7The composition and the distribution of each phase are relatively uniform.
The sample with the environmental barrier coating was subjected to SEM analysis, and as a result, as shown in fig. 2, from the sample of fig. 2, there were 3 layers, a C/C — SiC composite base layer (Substrate), a SiC bonding layer (SiC) and a composite coating layer (EBC), wherein the thickness of the bonding layer was about 40 μm and the thickness of the EBC was about 82 μm.
After the sample with the environmental barrier coating is corroded for 10 hours at 1300 ℃ under the action of pure oxygen and pure water vapor, the mass loss rate is shown in fig. 4a, and it can be known that the corrosion effect of high-temperature water vapor on the coating is obvious in a relatively pure oxygen environment.
Samples with environmental barrier coatings were tested at 1300 ℃ and 95% H2O-5％O2，9.4×10-1After 10 hours of corrosion at m/s flow rate, the mass loss of C/C-SiC coated with the coating was 1.62%. As shown in FIG. 4b, the loss rate is 1/8, which indicates that the coating of this example has a good resistance to high temperature water oxygen, compared with the uncoated C/C-SiC material. The deterioration rate of the coating during the corrosion process is shown in fig. 4c, and the stable deterioration rate of the coating of example 2 is continuously decreased, so that it is presumed that it has a long-term corrosion resistance effect.
Example 3
1. Preparation of the bonding layer: and depositing a SiC coating layer of about 30um on the surface of the C/C-SiC composite material matrix by using a chemical vapor deposition technology as a bonding layer.
2. Preparing a composite coating: will Y2O3Powder, mullite powder, ZrSiO4Powder (wherein the granularity of the mullite powder is-5000 meshes, Y2O3、ZrSiO4The powder is-2000 meshes, the purity is more than or equal to 99 percent) is milled for 5 hours (the milling medium is ethanol, the ball-material ratio is 5:1) in a planetary ball mill at the rotating speed of 300rpm according to the molar ratio of 0.15:0.3:0.55, and after the ball milling is finished, the powder is dried at 40 ℃ and sieved to obtain mixed powder.
And (3) mixing the mixed powder with a polyvinyl alcohol solution with the concentration of 2g/100ml (the slurry ratio is 2:1), stirring for 5 hours by using a magnetic stirrer, uniformly coating the obtained slurry on the surface of the C/C-SiC matrix SiC bonding layer, and brushing the slurry to the thickness of 200 mu m. After the brush coating is finished, the paint is dried in a forced air drying oven at 120 ℃ for 24 hours. Carrying out high-temperature sintering on the sample which is brushed and dried, wherein the sintering process is carried out under the argon atmosphere, and the conditions of the sintering process are as follows: and heating to 1500 ℃, keeping the temperature for 60min, cooling to room temperature at a heating rate of 10 ℃/min, and taking out to obtain a sample with the environmental barrier coating.
XRD analysis of the composite coating of the sample showed that the composite coating was formed from ZrSiO as shown in FIG. 14Mullite, Y2Si2O7The composition and the distribution of each phase are relatively uniform.
SEM analysis of the sample having the environmental barrier coating showed that the sample had a cross section having 3 layers, a C/C-SiC composite base layer (Substrate), a SiC bond layer (SiC) and a composite coating layer (EBC), wherein the thickness of the bond layer was about 50 μm and the thickness of the EBC was about 100 μm, as shown in FIG. 3. EBC coating is very dense, Y2Si2O7Coinciding with mullite, ZrSiO4The phase is largely dispersed in the outer EBC coating.
Samples with environmental barrier coatings were tested at 1300 deg.C, 95% H2O-5％O2，9.4×10-1After 10 hours of corrosion under the condition of m/s flow velocity, the coating is coatedThe mass loss of C/C-SiC was 2.47%.
Example 4
1. Preparation of the bonding layer: and depositing a SiC coating layer of about 36um on the surface of the C/C-SiC composite material matrix by using a chemical vapor deposition technology as a bonding layer.
2. Preparing a composite coating: will Y2O3Powder, mullite powder, ZrSiO4Powder (wherein the granularity of the mullite powder is-5000 meshes, Y2O3、ZrSiO4The powder is-2000 meshes, the purity is more than or equal to 99 percent) is milled for 4 hours (the milling medium is ethanol, the ball-material ratio is 7:1) in a planetary ball mill at the rotating speed of 400rpm according to the molar ratio of 0.1:1.0:0.6, and after the ball milling is finished, the powder is dried at the temperature of 50 ℃ and sieved to obtain mixed powder.
And (3) mixing the mixed powder with a polyvinyl alcohol solution with the concentration of 3g/100ml (the slurry ratio is 1.5:1), stirring for 4 hours by using a magnetic stirrer, uniformly coating the obtained slurry on the surface of the C/C-SiC matrix SiC bonding layer, and brushing to the thickness of 150 microns. After the brush coating is finished, the paint is dried in a forced air drying oven at 140 ℃ for 18 hours. Carrying out high-temperature sintering on the sample which is brushed and dried, wherein the sintering process is carried out under the argon atmosphere, and the conditions of the sintering process are as follows: and heating to 1600 ℃, preserving the heat for 80min, cooling to room temperature at a heating rate of 7 ℃/min, and taking out to obtain the sample with the environmental barrier coating.
Samples with environmental barrier coatings were tested at 1300 deg.C, 95% H2O-5％O2，9.4×10-1After 10 hours of corrosion under the condition of m/s flow velocity, the mass loss of the C/C-SiC coated with the coating is 1.87%.
Example 5
1. Preparation of the bonding layer: and depositing a SiC coating layer of about 36um on the surface of the C/C-SiC composite material matrix by using a chemical vapor deposition technology as a bonding layer.
2. Preparing a composite coating: will Y2O3Powder, mullite powder, ZrSiO4Powder (wherein the granularity of the mullite powder is-5000 meshes, Y2O3、ZrSiO4Powder of-2000 meshes and purity of more than or equal to 99 percent) is milled for 6 hours (the milling medium is ethanol and the ball-material ratio is 10:1) in a planetary ball mill at the rotating speed of 200rpm according to the mol ratio of 1.0:0.8:0.9After finishing, drying the powder at 60 ℃ and sieving the powder to obtain mixed powder.
And (3) mixing the mixed powder with a polyvinyl alcohol solution with the concentration of 1g/100ml (the slurry ratio is 2:1), stirring for 4 hours by using a magnetic stirrer, uniformly coating the obtained slurry on the surface of the C/C-SiC matrix SiC bonding layer, and brushing to the thickness of 100 mu m. After the brush coating is finished, the paint is dried in a forced air drying oven for 30 hours at the temperature of 100 ℃. Carrying out high-temperature sintering on the sample which is brushed and dried, wherein the sintering process is carried out under the argon atmosphere, and the conditions of the sintering process are as follows: and heating to 1400 ℃, keeping the temperature for 90min, cooling to room temperature at the heating rate of 5 ℃/min, and taking out to obtain the sample with the environmental barrier coating.
Samples with environmental barrier coatings were tested at 1300 deg.C, 95% H2O-5％O2，9.4×10-1After 10 hours of corrosion at m/s flow rate, the mass loss of C/C-SiC coated with the coating was 2.34%.

Claims (8)

1. An yttria-doped calcined mullite-zirconium silicate environmental barrier coating is characterized by comprising a SiC bonding layer and a composite layer, wherein the composite layer is formed by ZrSiO4Powder, Y2O3Powder and mullite powder as raw materials, Y2O3Powder, mullite powder and ZrSiO4The mol ratio of the powder is (0.1-1.0): (0.2-1.0): 0.3-1.0);
the preparation method of the yttrium oxide doped calcined mullite-zirconium silicate environmental barrier coating comprises the following steps:
1) preparing a bonding layer: depositing a SiC coating on the surface of the C/C-SiC composite material matrix by using a chemical vapor deposition technology to serve as a bonding layer;
2) preparing mixed powder: ZrSiO4Powder, Y2O3Mixing the powder and mullite in proportion, performing ball milling, uniformly mixing and drying to obtain mixed powder;
3) preparing a composite coating: mixing the mixed powder polyvinyl alcohol solution obtained in the step 2), stirring and uniformly mixing to obtain slurry, uniformly coating the slurry on a SiC bonding layer, drying the SiC bonding layer, sintering the dried sample, and cooling to room temperature after sintering to obtain the yttrium oxide doped calcined mullite-zirconium silicate environmental barrier coating;
in the step 3), sintering is carried out under inert atmosphere or vacuum condition; the sintering temperature is 1300-1600 ℃, the heating rate is 5-10 ℃/min, and the heat preservation time is 1-2 h.
2. The yttria-doped calcined mullite-zirconium silicate environmental barrier coating of claim 1 wherein Y is2O3Powder, mullite powder and ZrSiO4The molar ratio of the powder is (0.1-0.3): (0.2-0.5): 0.3-0.6).
3. The yttria-doped calcined mullite-zirconium silicate environmental barrier coating of claim 1 wherein Y is2O3Powder, mullite powder and ZrSiO4The molar ratio of the powders was 0.15:0.3: 0.55.
4. The yttria-doped calcined mullite-zirconium silicate environmental barrier coating of claim 1, wherein the ZrSiO is4The purity of the powder is more than or equal to 99 percent, and the granularity of the powder is micron; said Y is2O3The purity of the powder is more than or equal to 99 percent, and the granularity of the powder is micron; the purity of the mullite powder is more than or equal to 98 percent, and the granularity of the mullite powder is micron-sized.
5. The yttria-doped calcined mullite-zirconium silicate environmental barrier coating of claim 1, wherein in step 1), the SiC bonding layer has a thickness of 30 to 40 μm.
6. The yttria-doped calcined mullite-zirconium silicate environmental barrier coating of claim 1, wherein in the step 2), the ball milling time is 4-6 h, the ball milling medium is ethanol or water, the ball milling rotation speed is 200-400 rmp, and the ball-to-material ratio is (5-10): 1; the drying temperature is 40-60 ℃.
7. The yttria-doped calcined mullite-zirconium silicate environmental barrier coating of claim 1, wherein in the step 3), the slurry ratio of the mixed powder to the polyvinyl alcohol solution is (1-2): 1, and the concentration of the polyvinyl alcohol solution is (1-3)/100 g/mL; the coating thickness is 100-200 um; the drying temperature is 100-140 ℃, and the drying time is 18-30 h.
8. The yttria-doped calcined mullite-zirconium silicate environmental barrier coating of claim 1, wherein in step 3), the inert atmosphere is an argon or helium atmosphere and the vacuum is less than 5 Pa.
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