CN115180930A - Powder for transition layer, preparation method and high-temperature-resistant refractory metal matrix protective layer - Google Patents
Powder for transition layer, preparation method and high-temperature-resistant refractory metal matrix protective layer Download PDFInfo
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- C04B35/58085—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicides
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- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/134—Plasma spraying
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3227—Lanthanum oxide or oxide-forming salts thereof
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
- C04B2235/3873—Silicon nitrides, e.g. silicon carbonitride, silicon oxynitride
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Abstract
The invention discloses powder for a transition layer, a preparation method and a high-temperature-resistant refractory metal matrix protection layer, wherein the preparation method of the powder for the transition layer forms the transition layer between a refractory metal matrix and a coating by thermally spraying the powder, and mainly comprises the following steps: weighing 20-60% of MoSi according to mass percentage 2 Powder, 20-60% SiO 2 Powder, 5-20% of Si 3 N 4 Powder and 1% -5% of La 2 O 3 Mixing the powder evenly to obtain mixed powder; sintering the mixed powder in a vacuum furnace to obtain a blank; grinding and sieving the blank, and taking undersize; placing the sieved powder in a powder feeder of a plasma spraying device for waitingCarrying out ion spraying treatment; and collecting the powder after plasma spraying, screening, and taking undersize products to obtain the powder for the thermal spraying transition layer. The development of the transition layer spraying material can effectively relieve the difference of thermal expansion deformation between a refractory metal matrix and a ceramic coating material, avoid the problems of cracks, falling off and the like in the use process of the coating, and is beneficial to improving the high-temperature oxidation resistance of the coating.
Description
Technical Field
The invention relates to the field of tungsten, molybdenum and other refractory metal materials, in particular to powder for a transition layer, a preparation method and a high-temperature-resistant refractory metal matrix protective layer.
Background
The refractory alloy has excellent mechanical properties and physical properties such as high-temperature strength and high-temperature hardness, good heat conductivity and electric conductivity, low thermal expansion coefficient and the like, and is widely applied to the fields of metallurgy, machinery, energy, chemical industry, national defense, electronics and the like. However, under the atmospheric condition, the refractory metal material starts to be oxidized at the temperature of 300-475 ℃, and the oxidation speed is gradually increased along with the increase of the temperature, so that the oxidation speed of the refractory metal material such as molybdenum, tungsten and the like under the atmospheric environment is reduced. At present, tungsten and molybdenum material suppliers mostly adopt Si-based coatings, oxide coatings or rare earth oxide coatings to solve the problem of oxidation loss of the tungsten and molybdenum materials under high-temperature air, but the phenomena of coating falling or coating cracks and the like can occur after the coatings are used for a period of time under the high-temperature air due to overlarge difference between the thermal expansion coefficients of refractory metals such as tungsten, molybdenum and the like and the selected coating materials. Therefore, the preparation of the transition layer spraying material with the thermal expansion coefficient between the coating material and the base material is very important for solving the problem of high-temperature oxidation of the tungsten and molybdenum refractory metals.
The high-temperature metal coating transition material commonly used in the market is usually NiCrAlY or NiCrAl series material, but the use temperature of refractory metals such as tungsten, molybdenum and the like is generally above 1000 ℃, and the material cannot meet the use scene when the temperature is higher than 1000 ℃. Therefore, how to prepare a transition layer material with a thermal expansion coefficient between a base metal or an alloy and a coating material for refractory metals such as tungsten and molybdenum becomes a major problem that the application of the refractory metals in high-temperature and atmospheric environments is currently limited.
Disclosure of Invention
The invention provides powder for a transition layer, a preparation method and a high-temperature-resistant refractory metal matrix protective layer, aiming at overcoming the conditions that the difference of thermal expansion coefficients of the existing refractory metal and an alloy product thereof and a Si-based coating, an oxide coating or a rare earth oxide coating material is overlarge, the coating is easy to fall off and the like.
In order to achieve the purpose, the invention adopts the specific scheme that:
the preparation method of the powder for the transition layer forms the transition layer between the refractory metal matrix and the coating by thermal spraying of the powder, and mainly comprises the following steps:
(1) Weighing 20-60% of MoSi according to mass percentage 2 Powder, 20-60% SiO 2 Powder, 5-20% of Si 3 N 4 Powder and 1% -5% of La 2 O 3 Mixing the powder evenly to obtain mixed powder;
(2) Placing the mixed powder in a vacuum furnace for sintering and forming to obtain a blank;
(3) Grinding and sieving the blank, and taking undersize products;
(4) Placing the screened powder into a powder feeder of plasma spraying equipment for plasma spraying treatment;
(5) And collecting and sieving the powder after plasma spraying, and taking the undersize powder with the granularity interval of 25-75 um as the thermal spraying transition layer powder.
Further, in the step (1), the Fisher particle sizes of MoSi2, siO2, si3N4 and La2O3 powders are all 3.5-4.3 um, the purities are all more than or equal to 99.5 percent, and the powder particles are clear and have no obvious agglomeration phenomenon.
Further, in the step (1), the mass percentage of Si3N4 is determined by the difference R in thermal expansion coefficient between the refractory metal substrate and the coating: if R is less than or equal to 5.0X 10 -6 K -1 Then Si is 3 N 4 5-10% by mass; if R > 5.0X 10 -6 K -1 Then Si is 3 N 4 The mass percentage of the component (A) is 10-20%.
Further, in the step (2), the sintering temperature is 600 to 1000 ℃, and the vacuum degree is more than or equal to 5.2 multiplied by 10 < -1 > Pa.
Further, in the step (3), the ground powder is sieved by a 200-mesh sieve, and undersize products are taken out to obtain mixed powder with the particle size not greater than 80 um.
Further, in the step (4), in the plasma spraying, the flow rate of the powder feeder is as follows: 0.2m 3 /h~0.6m 3 The voltage is 35 to 40V, and the current is 520 to 600A.
Further, in the step (5), the obtained powder is spherical powder with an average particle size of 50um, and the alloying degree is 96%.
The powder for the transition layer is prepared by the preparation method of the powder for the thermal spraying transition layer.
The protective layer comprises a transition layer and a coating, wherein the transition layer is prepared by utilizing the powder for the thermal spraying transition layer by adopting a thermal spraying process, and the coating is a silicon-based coating, an oxide coating or a rare earth oxide coating.
Has the advantages that:
the invention adopts the method of powder direct vacuum sintering and plasma spraying alloying, and prepares the powder with good fluidity and high alloying degree through the processes of primary densification sintering, secondary alloying spraying and the like of the powder. Meanwhile, due to the selected proportion of the mixed powder, the thermal expansion coefficient of the selected mixed powder is between that of the refractory metal and that of the ceramic coating material, so that the thermal expansion deformation difference between the refractory metal matrix and the ceramic coating material is favorably relieved, the problems of cracks, falling and the like in the using process of the coating are avoided, and the high-temperature oxidation resistance of the coating is favorably improved.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to specific embodiments, and it should be understood 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 any inventive step based on the embodiments of the present invention, belong to the scope of the present invention.
The preparation method of the powder for the transition layer forms the transition layer between the refractory metal matrix and the coating by thermal spraying of the powder, and mainly comprises the following steps:
(1) Weighing 20-60% of MoSi according to mass percentage 2 Powder, 20-60% SiO 2 Powder, 5-20% of Si 3 N 4 Powder and 1% -5% of La 2 O 3 The Fisher-Tropsch particle size of MoSi2, siO2, si3N4 and La2O3 powder is 3.5-4.3um, the purity is more than or equal to 99.5 percent, and the powder particlesClear, without obvious agglomeration, and mixed evenly to obtain mixed powder;
(2) Placing the mixed powder in a vacuum furnace for sintering and forming, wherein the sintering temperature is 600 to 1000 ℃, and the vacuum degree is more than or equal to 5.2 multiplied by 10 < -1 > Pa, so as to obtain a blank;
(3) Grinding and sieving the blank, taking undersize, sieving the ground powder by using a 200-mesh sieve, and taking the undersize to obtain mixed powder with the granularity not greater than 80 um;
(4) Placing the screened powder into a powder feeder of plasma spraying equipment for plasma spraying treatment, wherein in the plasma spraying, the flow rate of the powder feeder is as follows: 0.2m3/h-0.6m3/h, voltage of 35-40V and current of 520-600A;
(5) And collecting the powder after plasma spraying, screening, and taking undersize to obtain the powder for the thermal spraying transition layer, wherein the obtained powder is spherical powder with the average particle size of 50 mu m, and the alloying degree of the powder is 96%.
In step (1), the mass percentage of Si3N4 is determined by the difference R in the thermal expansion coefficient between the refractory metal substrate and the coating: if R is less than or equal to 5.0X 10 -6 K -1 Then Si is 3 N 4 The mass percentage of the component (A) is 5-10%; if R > 5.0X 10 -6 K -1 Then Si is 3 N 4 The mass percentage of the component (A) is 10-20%.
The powder for the transition layer is prepared by the preparation method of the powder for the thermal spraying transition layer.
The protective layer comprises a transition layer and a coating, wherein the transition layer is prepared by utilizing the powder for the thermal spraying transition layer by adopting a thermal spraying process, and the coating is a silicon-based coating, an oxide coating (such as zirconium oxide, aluminum oxide and the like) or a rare earth oxide coating.
It should be noted that the refractory metals include, but are not limited to, mo, W — Mo alloys.
The thermal expansion coefficient of the refractory metal matrix at a temperature of 20-100 ℃: mo: mo: 5.2X 10 -6 K -1 ，W：4.4×10 -6 K -1 ；Ta:6.5×10 -6 K -1 ；Nb:7.3×10 -6 K -1 (ii) a Thermal expansion coefficient of the outer coating: (6.8-10.5). Times.10 -6 K -1 The thermal expansion coefficient of the material of the transition layer is as follows: (5.5-8.4). Times.10 --6 K -1 It can be seen that the thermal expansion coefficient of the transition layer material is between the refractory metal substrate and the outer coating.
Example 1
The preparation method of the powder for the transition layer comprises the following steps:
step one, taking MoSi with the purity of 99.5 percent 2 、SiO 2 、Si 3 N 4 And La 2 O 3 The powder comprises the following components in percentage by weight: 40 percent, 16 percent and 4 percent, the average grain size is 4.0um-4.2um, and the mixture is placed in a V-shaped mixer to be mixed evenly.
And step two, putting the uniformly mixed powder in the step one into a vacuum furnace for sintering, wherein the vacuum degree is 4.0 multiplied by 10 < -1 > pa, and the sintering temperature is 600 ℃.
Step three: grinding the sintered blank in a grinder, and sieving with a 200-mesh sieve to obtain densified mixed powder with particle size not greater than 80 um;
step four: placing the mixed powder obtained in the step three in a powder feeder of plasma spraying equipment, wherein the flow rate of the powder feeder is as follows: 0.2m3/h, voltage: 35V, current: 520A;
and step five, collecting and screening the powder after plasma spraying to obtain spherical powder with the average particle size of 50um, wherein the alloying degree of the powder is 96%.
The utility model provides a high temperature resistant refractory metal (Mo) base member protective layer, the protective layer includes transition layer and coating, the transition layer utilizes foretell powder for the thermal spraying transition layer to adopt hot spraying process preparation, the coating is the ZrO2 coating.
Example 2
The preparation method of the powder for the transition layer comprises the following steps:
taking MoSi2, siO2, si3N4 and La2O3 powder with the purity of 99.5 percent, wherein the weight percentage is as follows: 60 percent, 30 percent, 8 percent and 2 percent, the average grain size is 3.6um-3.8um, and the mixture is placed in a V-shaped mixer to be mixed evenly.
And step two, putting the uniformly mixed powder in the step one into a vacuum furnace for sintering, wherein the vacuum degree is 2.0 multiplied by 10 < -1 > pa, and the sintering temperature is 800 ℃.
Step three: grinding the sintered blank in a grinder, and sieving with a 200-mesh sieve to obtain a mixed powder with a densification treatment and a particle size of less than or equal to 70 um;
step four: placing the mixed powder obtained in the step three into a powder feeder of plasma spraying equipment, wherein the flow rate of the powder feeder is as follows: 0.3m3/h, voltage: 35V, current: 520A;
and step five, collecting and screening the powder after plasma spraying to obtain spherical powder with the average particle size of 35um, wherein the alloying degree of the powder is 96.7%.
The high-temperature-resistant refractory metal (W) substrate protective layer comprises a transition layer and a coating, wherein the transition layer is prepared by utilizing the powder for the thermal spraying transition layer through a thermal spraying process, and the coating is Al 2 O 3 And (4) coating.
Example 3
The preparation method of the powder for the transition layer comprises the following steps:
taking MoSi2, siO2, si3N4 and La2O3 powder with the purity of 99.5 percent, wherein the weight percentage is as follows: 20 percent, 70 percent, 9 percent and 1 percent, the average grain size is 3.4um-3.7um, and the mixture is placed in a V-shaped mixer to be mixed evenly.
And step two, putting the uniformly mixed powder in the step one into a vacuum furnace for sintering, wherein the vacuum degree is 2.0 multiplied by 10 < -2 > pa, and the sintering temperature is 1000 ℃.
Step three: grinding the sintered blank in a grinder, and sieving with a 200-mesh sieve to obtain densified mixed powder with particle size not greater than 75 um;
step four: placing the mixed powder obtained in the step three in a powder feeder of plasma spraying equipment, wherein the flow rate of the powder feeder is as follows: 0.4m3/h, voltage: 40V, current: 600A;
and step five, collecting the powder after plasma spraying, and screening to obtain spherical powder with the average particle size of 45m, wherein the alloying degree of the powder is 96.7%.
The protective layer comprises a transition layer and a coating, wherein the transition layer is prepared by utilizing the powder for the thermal spraying transition layer by adopting a thermal spraying process, and the coating is a silicon-based coating.
The powder for the transition layer prepared in the embodiments 1 to 3 is respectively subjected to plasma spraying, then the outer layer is coated with a corresponding coating, and tests in a high-temperature and aerobic environment show that the powder for the transition layer has good high-temperature oxidation resistance and thermal shock resistance, which indicates that the prepared powder for the transition layer well solves the problems of large thermal expansion difference between the matrix metal or alloy and the material of the outer layer high-temperature resistant coating, and the coating is easy to crack and fall off.
The foregoing is merely a preferred embodiment of the invention and is not to be construed as limiting the invention in any way. All equivalent changes or modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (9)
1. The preparation method of the powder for the transition layer is characterized in that the transition layer is formed between a refractory metal matrix and a coating by thermally spraying the powder, and mainly comprises the following steps:
(1) Weighing 20-60% of MoSi according to mass percentage 2 Powder, 20-60% SiO 2 Powder, 5-20% of Si 3 N 4 Powder and 1% -5% of La 2 O 3 Mixing the powder evenly to obtain mixed powder;
(2) Placing the mixed powder in a vacuum furnace for sintering and forming to obtain a blank;
(3) Grinding and sieving the blank, and taking undersize products;
(4) Placing the screened powder into a powder feeder of plasma spraying equipment for plasma spraying treatment;
(5) And collecting the powder after plasma spraying, screening, and taking undersize products to obtain the powder for the thermal spraying transition layer.
2. The method for producing a powder for a transition layer according to claim 1, characterized in that: in step (1), moSi 2 、SiO 2 、Si 3 N 4 And La 2 O 3 The Fisher size of the powder is 3.5 to 4.3um, the purity is more than or equal to 99.5 percent, and the powder particles are clear without obvious agglomeration.
3. The method for producing a powder for a transition layer according to claim 1, characterized in that: in step (1), si 3 N 4 Is determined by the difference R in the coefficient of thermal expansion between the refractory metal substrate and the coating: if R is less than or equal to 5.0X 10 -6 K -1 Then Si is 3 N 4 The mass percentage of the component (A) is 5-10%; if R > 5.0X 10 -6 K -1 Then Si is 3 N 4 The mass percentage of the component (A) is 10-20%.
4. The method for producing a powder for a transition layer according to claim 1, characterized in that: in the step (2), the sintering temperature is 600 to 1000 ℃, and the vacuum degree is more than or equal to 5.2 multiplied by 10 -1 Pa。
5. The method for producing a powder for a transition layer according to claim 1, characterized in that: in the step (3), the ground powder is sieved by a 200-mesh sieve, and undersize products are taken out to obtain mixed powder with the particle size not greater than 80 mu m.
6. The method for producing a powder for a transition layer according to claim 1, characterized in that: in the step (4), in the plasma spraying, the flow rate of the powder feeder is as follows: 0.2m 3 /h~0.6m 3 The voltage is 35 to 40V, and the current is 520 to 600A.
7. The method for producing a powder for a transition layer according to claim 1, comprising: in the step (5), the obtained powder is spherical powder with the average particle size of 50 mu m, and the alloying degree of the powder is 96%.
8. The powder for a transition layer, characterized by being produced by the method for producing a powder for a thermal spray transition layer according to any one of claims 1 to 6.
9. A high temperature resistant refractory metal matrix protective layer characterized by: the protective layer comprises a transition layer and a coating, the transition layer is prepared by utilizing the powder for the thermal spraying transition layer in the claim 8 through a thermal spraying process, and the coating is a silicon-based coating, an oxide coating or a rare earth oxide coating.
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