CN113025951B - Molybdenum alloy containing antioxidant composite coating and preparation method thereof - Google Patents
Molybdenum alloy containing antioxidant composite coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a molybdenum alloy containing an antioxidant composite coating and a preparation method thereof, relates to the technical field of high-temperature alloy thermal protection, and comprises a molybdenum alloy matrix and a composite coating on the surface of the molybdenum alloy matrix, wherein the composite coating at least comprises (Mo, X) Si2Phase of (Cr, X) Si2The composite coating may also have a two-layer structure, the outer layer of which comprises at least (Mo, X) Si2Phase of (Cr, X) Si2The inner layer at least comprises (Mo, X)5Si3Phase (1); wherein, (Mo, X) Si2Wherein X represents Cr, Ti or W, (Cr, X) Si2Wherein X represents Mo, Ti or W, the preparation method comprises the preparation of a molybdenum alloy matrix and the preparation of a composite coating on the alloy surface by co-infiltration, the invention combines matrix alloying and surface modification, and the (Mo, X) Si is prepared by the alloying and compounding method and the method of jointly modifying a silicide coating by a multilayer structure2‑(Cr,X)Si2The molybdenum alloy protected by the base composite coating has excellent medium-temperature and high-temperature oxidation resistance.
Description
Technical Field
The invention relates to the technical field of high-temperature alloy thermal protection, in particular to a molybdenum alloy containing an antioxidant composite coating and a preparation method thereof.
Background
The molybdenum and the alloy thereof have the advantages of high melting point, low resistivity, high thermal conductivity, low thermal expansion coefficient, high-temperature strength and the like, and are key materials for preparing rocket nozzles, nozzle throat liners, radiation shields, heat shields, heating elements and the likeHas wide application prospect in the fields of aerospace, nuclear industry, machinery, metallurgy and the like. However, molybdenum and molybdenum alloys are rapidly oxidized to volatile MoO in an air environment above 600 deg.C3Severely restricting the use of the material as a high-temperature material.
At present, the high-temperature oxidation resistance of molybdenum mainly comprises alloying and surface modification. The alloying method is to add antioxidant alloy elements (such as zirconium, chromium and aluminum) into molybdenum, and in the high-temperature oxidation process, the antioxidant alloy elements are selectively oxidized, so that the oxidation rate of the molybdenum is slowed down to a certain extent. However, the alloying method has certain limitation in improving the high-temperature oxidation resistance, and a dense and continuous protective oxide film cannot be formed on the surface of the molybdenum alloy by only adding alloying elements. The surface modification can give consideration to the oxidation resistance and the mechanical property of the alloy, and the oxidation resistance of the matrix metal is obviously improved. Silicide coatings (e.g. MoSi)2Etc.) has the advantages of high melting point, good thermal stability, excellent oxidation resistance, self-healing capability and the like, and is a high-temperature oxidation-resistant coating system which is most widely applied to the surface of refractory metals. According to the current research situation at home and abroad, the silicide coating prepared on the surface of the molybdenum alloy has the main problems that: (1) single MoSi2Although the coating has excellent high-temperature oxidation resistance, the coating has poor high-temperature oxidation resistance, and the coating can generate 'moulding' pulverization oxidation at 400-600 ℃; (2) MoSi2The difference of the thermal expansion coefficients between the coating and the matrix is large, cracks are easily generated in the coating and at the joint of the coating and the matrix interface, so that the coating fails and the thermal shock resistance is poor; (3) MoSi2SiO formed on the surface of the oxidized coating2The membrane has good fluidity at high temperature and thus insufficient resistance to gas scouring. The development trend of molybdenum and molybdenum alloy high-temperature oxidation resistant coatings is that the molybdenum and molybdenum alloy high-temperature oxidation resistant coatings have excellent oxidation resistance, thermal shock resistance and gas scouring resistance at a wider use temperature. However, there is no established method for simultaneously solving the above problems.
Disclosure of Invention
The invention aims to solve at least one technical problem in the prior art and provides a molybdenum alloy containing an antioxidant composite coating and a preparation method thereof.
The technical solution of the invention is as follows:
a molybdenum alloy containing an oxidation-resistant composite coating, comprising a molybdenum alloy substrate and a composite coating on the surface of the molybdenum alloy substrate, wherein the composite coating at least comprises (Mo, X) Si2Phase of (Cr, X) Si2Phase(s) of each other.
Preferably, the composite coating is a double-layer structure, and the outer layer at least comprises (Mo, X) Si2Phase of (Cr, X) Si2The inner layer at least comprises (Mo, X)5Si3And (4) phase(s).
Preferably, the outer layer and/or the inner layer further comprises Al2O3Phase, (Mo, X) Si2Wherein X represents Cr, Ti or W, (Cr, X) Si2Wherein X represents Mo, Ti or W.
Preferably, the molybdenum alloy matrix comprises the following composition: 10 to 30at% Cr, 0 to 15at% Al, 0 to 30at% W, 0 to 15at% Ti, and the balance Mo.
The invention also discloses a preparation method of the molybdenum alloy containing the antioxidant composite coating, which comprises the steps of alloying the substrate to obtain a molybdenum alloy substrate, and then preparing the composite coating on the molybdenum alloy substrate to reduce the difference of the thermal expansion coefficients of the molybdenum alloy substrate and the composite coating. The method specifically comprises the following steps:
the method comprises the following steps: mixing Mo powder, Cr powder, Al powder, W powder and Ti powder in proportion, putting the mixture into a ball mill for ball milling, drying, sequentially performing compression molding on the dried powder, and sintering at low pressure to obtain a molybdenum alloy matrix;
step two: polishing, burnishing, polishing and cleaning the molybdenum alloy matrix in the step one, placing the molybdenum alloy matrix in a tube furnace, and introducing NH into the furnace tube3Keeping the temperature at 800-1200 ℃ for 2-5 h at a flow rate of 100-300 ml/min, and then cooling along with the furnace;
step three: mixing silicon powder, sodium fluoride powder, sodium fluosilicate powder and alumina powder according to a certain proportion, and performing ball milling to obtain penetrant powder;
step four: filling the infiltration agent powder obtained in the step three into an alumina crucible, embedding the molybdenum alloy matrix obtained in the step one into the infiltration agent powder obtained in the step three, and covering the crucible with a coverWith combined use of Al2O3Sealing the slurry prepared by the powder and the silica sol; and (3) placing the sealed crucible into a high-temperature tube furnace, heating to 1000-1300 ℃ under the protection of argon, preserving the temperature for 15-30 h, and cooling along with the furnace to obtain the molybdenum alloy containing the composite coating.
Preferably, in the first step, the specific conditions of ball milling are as follows: the ball-material ratio is 5-10: 1, the rotating speed is 100-200 r/min, and the ball milling time is 10-40 h.
Preferably, in the step one, the temperature of low-pressure sintering is 1600-1800 ℃, and the temperature is kept for 2-5 hours.
Preferably, in the third step, the penetrant powder is prepared by uniformly mixing the following raw materials in percentage by mass: 20-30% of silicon powder, 2-6% of sodium fluoride powder, 1-3% of sodium fluosilicate powder, 56-70% of alumina powder and 0-5% of yttrium oxide powder.
Preferably, the purity of the silicon powder, the sodium fluoride powder, the sodium fluosilicate powder, the yttrium oxide powder and the aluminum oxide is not lower than 99.0%.
Preferably, in the third step, the ball milling is specifically performed for 1-3 hours by a planetary ball mill at a speed of 100-250 r/min.
The invention has at least one of the following beneficial effects:
(1) the invention adopts the combination of matrix alloying and surface modification, and the alloying and compounding method and the method of multilayer structure combined modification silicide coating to prepare (Mo, X) Si2-(Cr,X)Si2The molybdenum alloy protected by the base composite coating has excellent medium-temperature and high-temperature oxidation resistance.
(2) The invention adopts alloying of the matrix and simultaneously prepares the composite coating on the surface thereof, thus reducing the difference of the thermal expansion coefficients of the matrix and the composite coating, forming a compact coating with good interface bonding and improving the thermal shock resistance of the material; (Mo, X) Si prepared on surface of molybdenum alloy by pack cementation2-(Cr,X)Si2The base composite coating is compact and uniform, and the combination of the matrix and the coating is good. SiO formed on the surface of the alloy during oxidation2·Al2O3The protective film has larger viscosity and is beneficial to the anti-scouring capability of the material.
(3) The method has the advantages of simple process, convenient operation, low cost, high yield, high efficiency and the like, is suitable for industrial popularization and application, and has important practical value for preparing high-temperature hot end parts in the fields of aerospace, nuclear industry, machinery, metallurgy and the like.
Drawings
FIG. 1 is a graph of the oxidation weight gain at 1300 ℃ after Si-Y co-doping of different substrates of molybdenum-based alloys alone (examples 1-4);
FIG. 2 is a sectional structure of Mo-30Cr-10Al-5W alloy coating, wherein (a) Si is infiltrated alone (example 3 sample), (b) Si-Y is infiltrated (example 4 sample);
FIG. 3 is a surface texture of Mo-30Cr-10Al-5W alloy after Si-Y co-cementation oxidized for 280 hours at 1300 ℃ (sample of example 4);
FIG. 4 is a graph of the oxidation rate of weight gain for Mo-30Cr-10Al-5W alloy after Si-Y co-cementation, oxidized at 500 deg.C and 900 deg.C for 80 hours (sample of example 4).
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
to verify the effect of the invention, (Mo, X) Si was prepared on the surface of the alloy by two-step method using different base alloys2-(Cr,X)Si2And carrying out a cyclic oxidation test for 80-280 h on the composite coating under the atmospheric environment at the temperature of 500-1300 ℃.
Example 1:
the method comprises the following steps: preparation of Mo-based alloy
Mixing materials according to the proportion of 85 at% of Mo and 15at% of Cr, wet grinding by adopting a planetary ball mill, wherein the ball-material ratio is 5:1, the rotating speed is 120r/min, the ball milling time is 30 hours, and after the ball milling is finished, putting the powder into a vacuum drying oven for drying. And then putting the dried powder into a cold isostatic pressing die for pressing and molding. And (3) sintering the pressed sample at 1600 ℃ and 0.6Mpa under low pressure, and keeping the temperature for 3 hours to prepare the Mo-15Cr matrix alloy.
Step two: preparing (Mo, X) Si on the surface of the alloy obtained in the step one2-(Cr,X)Si2Base composite coating
And gradually grinding and polishing the alloy surface by using 240#, 400#, 600# and 1000# silicon carbide abrasive paper, ultrasonically cleaning in absolute ethyl alcohol, and drying. Placing the treated sample in an alumina crucible, placing the alumina crucible in a tube furnace, and introducing NH into the tube furnace3And keeping the temperature at 1000 ℃ for 3 hours at the flow of 200ml/min for surface nitriding treatment, and obtaining a nitride transition layer on the alloy surface after the heat preservation is finished. Mixing silicon powder, sodium fluoride powder, sodium fluosilicate powder and alumina powder according to a certain proportion, and then carrying out ball milling for 2 hours at 150 revolutions per minute by a planetary ball mill to obtain penetrant powder; wherein the purity of the silicon powder, the sodium fluoride powder, the sodium fluosilicate powder and the aluminum oxide is not lower than 99.0 percent; wherein, 25 wt% of silicon powder, 4 wt% of sodium fluoride powder, 2 wt% of sodium fluosilicate powder and 69 wt% of alumina powder. Filling the penetrant powder into an alumina crucible, burying the Mo-15Cr matrix alloy subjected to surface nitriding treatment in the penetrant powder, covering the crucible cover and using Al2O3Sealing the slurry prepared by the powder and the silica sol; placing the sealed crucible in a high-temperature tube furnace, heating to 1200 ℃ under the protection of argon, and preserving heat for 20 hours to finish Si infiltration treatment to obtain (Mo, Cr) Si2-(Cr,Mo)Si2A composite coating; the sample after the Si infiltration treatment is subjected to a 150-hour cyclic oxidation experiment at 1300 ℃ in an atmospheric environment, the surface oxide film is compact and complete, the peeling phenomenon is avoided, and the oxidation weight gain rate is 0.43% (refer to figure 1).
Example 2:
the method comprises the following steps: preparation of Mo-based alloy
Proportioning according to the proportion of 75 at% of Mo and 25 at% of Cr, wet grinding by adopting a planetary ball mill, wherein the ball-material ratio is 5:1, the rotating speed is 120r/min, the ball milling time is 30h, and after the ball milling is finished, putting the powder into a vacuum drying oven for drying. And then putting the dried powder into a cold isostatic pressing die for pressing and molding. And (3) sintering the pressed sample at 1600 ℃ and 0.6Mpa under low pressure, and keeping the temperature for 3 hours to prepare the Mo-25Cr matrix alloy.
Step two: preparing (Mo, X) Si on the surface of the alloy obtained in the step one2-(Cr,X)Si2Base composite coating
The alloy surface is gradually treated by 240#, 400#, 600# and 1000# silicon carbide sand paperGrinding and polishing, ultrasonically cleaning in absolute ethyl alcohol, and drying. Placing the treated sample in an alumina crucible, placing the alumina crucible in a tube furnace, and introducing NH into the tube furnace3And the flow is 200ml/min, the surface nitriding treatment is carried out at the temperature of 1000 ℃ for 3 hours, and a nitride transition layer is obtained on the surface of the alloy after the heat preservation is finished. Mixing silicon powder, sodium fluoride powder, sodium fluosilicate powder and alumina powder according to a certain proportion, and then carrying out ball milling for 2 hours at 150 revolutions per minute by a planetary ball mill to obtain penetrant powder; wherein the purity of the silicon powder, the sodium fluoride powder, the sodium fluosilicate powder and the aluminum oxide is not lower than 99.0 percent; wherein, the silicon powder accounts for 25 wt%, the sodium fluoride powder accounts for 4 wt%, the sodium fluosilicate powder accounts for 2 wt%, and the alumina powder accounts for 69 wt%. Filling the penetrant powder into an alumina crucible, burying the Mo-25Cr matrix alloy subjected to surface nitriding treatment in the penetrant powder, covering the crucible cover and using Al2O3Sealing the slurry prepared by the powder and the silica sol; placing the sealed crucible in a high-temperature tube furnace, heating to 1200 ℃ under the protection of argon, and preserving heat for 20 hours to finish Si infiltration treatment to obtain (Mo, Cr) Si2-(Cr,Mo)Si2A composite coating; and (3) performing a 150-hour cyclic oxidation experiment on the sample subjected to the Si infiltration treatment at 1300 ℃ in an atmospheric environment, wherein the surface oxide film is compact and complete, the peeling phenomenon is avoided, and the oxidation weight gain rate is 0.36% (refer to figure 1).
Example 3:
the method comprises the following steps: preparation of Mo-based alloy
Preparing materials according to the proportion of 30at% Cr, 10 at% Al, 5at% W and the balance Mo, wet-grinding by adopting a planetary ball mill, wherein the ball-material ratio is 5:1, the rotating speed is 120r/min, the ball-milling time is 30h, and after the ball-milling is finished, putting the powder into a vacuum drying oven for drying. And then putting the dried powder into a cold isostatic pressing die for pressing and molding. And (3) sintering the pressed sample at 1600 ℃ and 0.6Mpa under low pressure, and keeping the temperature for 3 hours to prepare the Mo-30Cr-10Al-5W matrix alloy.
Step two: preparing (Mo, X) Si on the surface of the alloy obtained in the step one2-(Cr,X)Si2Base composite coating
The surface of the molybdenum base alloy is gradually ground and polished by 240#, 400#, 600# and 1000# silicon carbide abrasive paper in the absence of waterUltrasonically cleaning in ethanol and drying. Placing the treated sample in an alumina crucible, placing the alumina crucible in a tube furnace, and introducing NH into the tube furnace3And the flow is 200ml/min, the surface nitriding treatment is carried out at the temperature of 1000 ℃ for 3 hours, and a nitride transition layer is obtained on the surface of the alloy after the heat preservation is finished. Mixing silicon powder, sodium fluoride powder, sodium fluosilicate powder and alumina powder according to a certain proportion, and then carrying out ball milling for 2 hours at 150 revolutions per minute by a planetary ball mill to obtain penetrant powder; wherein the purity of the silicon powder, the sodium fluoride powder, the sodium fluosilicate powder and the aluminum oxide is not lower than 99.0 percent; wherein, 25 wt% of silicon powder, 4 wt% of sodium fluoride powder, 2 wt% of sodium fluosilicate powder and 69 wt% of alumina powder. Filling Si penetrant powder into an alumina crucible, burying the Mo-30Cr-10Al-5W matrix alloy subjected to surface nitriding treatment in the penetrant powder, covering the crucible and using Al2O3Sealing the slurry prepared by the powder and the silica sol; placing the sealed crucible in a high-temperature tube furnace, heating to 1200 ℃ under the protection of argon, and preserving heat for 20 hours to finish Si infiltration treatment to obtain (Mo, X) Si2-(Cr,X)Si2The thickness of the base composite coating is 307 μm (refer to fig. 2 a). The sample after the Si infiltration treatment is subjected to a 150-hour cyclic oxidation experiment in an atmospheric environment at 1300 ℃, the surface oxide film is compact and complete, the peeling phenomenon is avoided, and the oxidation weight gain rate is-0.03% (refer to figure 1).
Example 4:
the method comprises the following steps: preparation of Mo-based alloy
Preparing materials according to the proportion of 30at% Cr, 10 at% Al, 5at% W and the balance Mo, wet-grinding by adopting a planetary ball mill, wherein the ball-material ratio is 5:1, the rotating speed is 120r/min, the ball-milling time is 30h, and after the ball-milling is finished, putting the powder into a vacuum drying oven for drying. And then putting the dried powder into a cold isostatic pressing die for pressing and molding. And sintering the pressed sample at 1600 ℃ under low pressure, and keeping the temperature for 3 hours to prepare the Mo-30Cr-10Al-5W matrix alloy.
Step two: preparing (Mo, X) Si on the alloy surface obtained in the step one by Si-Y co-infiltration2-(Cr,X)Si2Base composite coating
Gradually treating the surface of the molybdenum matrix alloy by using 240#, 400#, 600# and 1000# silicon carbide sand paperGrinding and polishing, ultrasonically cleaning in absolute ethyl alcohol, and drying. Placing the treated sample in an alumina crucible, placing the alumina crucible in a tube furnace, and introducing NH into the tube furnace3And the flow is 200ml/min, the surface nitriding treatment is carried out at the temperature of 1000 ℃ for 3 hours, and a nitride transition layer is obtained on the surface of the alloy after the heat preservation is finished. Mixing silicon powder, sodium fluoride powder, sodium fluosilicate powder, yttrium oxide powder and alumina powder according to a certain proportion, and then carrying out ball milling for 2 hours at 150 revolutions per minute by a planetary ball mill to obtain Si-Y co-infiltration agent powder; wherein the purity of the silicon powder, the sodium fluoride powder, the sodium fluosilicate powder, the yttrium oxide powder and the aluminum oxide is not lower than 99.0 percent; wherein, the silicon powder accounts for 25 wt%, the sodium fluoride powder accounts for 4 wt%, the sodium fluosilicate powder accounts for 2 wt%, the yttrium oxide powder accounts for 3 wt%, and the aluminum oxide powder accounts for 66 wt%. Filling Si-Y co-infiltration agent powder into an alumina crucible, burying the Mo-30Cr-10Al-5W matrix alloy subjected to surface nitriding in the infiltration agent powder, covering the crucible and using Al2O3Sealing the slurry prepared by the powder and the silica sol; and (3) placing the sealed crucible into a high-temperature tube furnace, heating to 1200 ℃ under the protection of argon, and preserving heat for 20 hours to obtain the Y modified composite coating.
The thickness of the Y modified composite coating is 488 mu m, the Y modified composite coating is of a double-layer structure, and the outer layer is mainly (Mo, X) Si2+(Cr,X)Si2+Al2O3The inner layer is mainly (Mo, X)5Si3+Al2O3Phase (see fig. 2 b). When the sample subjected to Si-Y co-permeation is subjected to a 280-hour cyclic oxidation experiment in an atmosphere environment at 1300 ℃, the surface oxide film is compact and complete, the peeling phenomenon is avoided, and the oxidation weight gain rate is only 0.35% (refer to figure 1). FIG. 3 shows the microscopic appearance of the oxide film on the surface of the alloy after the alloy is oxidized for 280h at 1300 ℃ in the atmospheric environment, wherein the oxide film is mainly composed of dense SiO2·Al2O3Film and Cr distributed thereon2O3And Y2O3And (4) forming. The sample after Si-Y co-permeation is subjected to 80h cyclic oxidation experiments at 900 ℃ and 500 ℃ in the atmospheric environment, the oxidation weight gain rates are only 0.14% and 0.02% respectively (refer to figure 4), and no 'Pesting' pulverization oxidation occurs. (Mo, X) Si2-(Cr,X)Si2The molybdenum-based alloy protected by the base composite coating is 500-130 DEGThe antioxidant has excellent antioxidant performance and good stability within the temperature range of 0 ℃.
Simultaneously using a single MoSi2The bulk material as a control was found to be completely powdered by oxidation at 500 ℃ for 48h, whereas examples 1 to 4 show, on the one hand, a combination of alloying of the matrix and modification of the coating, in which the coating structure is (Mo, X) Si2-(Cr,X)Si2/(Mo,X)5Si3The composite coating reduces the difference of the thermal expansion coefficients of the two, and can form a compact coating with good interface combination; on the other hand, referring to the attached figure 1, the alloy in the embodiment undergoes cyclic oxidation times of 31 times (total oxidation time is 280 hours) at 1300 ℃, the surface is compact and complete, no stripping occurs, and the excellent thermal shock resistance can be shown.
In the description of the embodiments of the present invention, it should be understood that "-" and "-" indicate the same range of two numerical values, and the range includes the endpoints. For example: "A-B" means a range of greater than or equal to A and less than or equal to B. "A to B" means a range of not less than A and not more than B.
In the description of the embodiments of the present invention, the term "and/or" herein is only one kind of association relationship describing an associated object, and means that there may be three relationships, for example, a and/or B, and may mean: a exists alone, A and B exist simultaneously, and B exists alone. In addition, the character "/" herein generally indicates that the former and latter related objects are in an "or" relationship.
The above description is only a preferred embodiment of the present invention, and the technical solutions that achieve the objects of the present invention by basically the same means are all within the protection scope of the present invention.
Claims (5)
1. The preparation method of the molybdenum alloy containing the antioxidant composite coating is characterized by comprising the following steps:
the method comprises the following steps: mixing Mo powder, Cr powder, Al powder, W powder and Ti powder in proportion, putting the mixture into a ball mill for ball milling, drying, sequentially performing compression molding on the dried powder, and sintering at low pressure to obtain a molybdenum alloy matrix;
step two: polishing, burnishing and cleaning the molybdenum alloy matrix in the step one, placing the molybdenum alloy matrix in a tube furnace, and introducing NH into the furnace tube3Keeping the temperature at 800-1200 ℃ for 2-5 h at a flow rate of 100-300 ml/min, and then cooling along with the furnace;
step three: mixing silicon powder, sodium fluoride powder, sodium fluosilicate powder and alumina powder according to a certain proportion, and performing ball milling to obtain penetrant powder;
step four: filling the infiltration agent powder obtained in the step three into an alumina crucible, embedding the molybdenum alloy matrix obtained in the step one into the infiltration agent powder obtained in the step three, covering the crucible and using Al2O3Sealing the slurry prepared by the powder and the silica sol; placing the sealed crucible in a high-temperature tube furnace, heating to 1000-1300 ℃ under the protection of argon, preserving heat for 15-30 h, and cooling along with the furnace to obtain a molybdenum alloy containing a composite coating;
the molybdenum alloy comprises a molybdenum alloy substrate and a composite coating on the surface of the molybdenum alloy substrate, and the composite coating at least comprises (Mo, X) Si2Phase of (Cr, X) Si2Phase (1); the composite coating is of a double-layer structure, and the outer layer at least comprises (Mo, X) Si2Phase of (Cr, X) Si2The inner layer at least comprises (Mo, X)5Si3Phase (1); the molybdenum alloy matrix comprises the following components: 10-30 at% Cr, 0-15 at% Al, 0-30 at% W, 0-15 at% Ti, and the balance Mo; the (Mo, X) Si2Wherein X represents Cr, Ti or W, (Cr, X) Si2Wherein X represents Mo, Ti or W.
2. The preparation method of the molybdenum alloy containing the oxidation-resistant composite coating according to claim 1, wherein in the first step, the specific conditions of ball milling are as follows: the ball-material ratio is 5-10: 1, the rotating speed is 100-200 r/min, and the ball milling time is 10-40 h.
3. The preparation method of the molybdenum alloy containing the antioxidant composite coating according to claim 1, wherein in the first step, the temperature of low-pressure sintering is 1600-1800 ℃ and the temperature is kept for 2-5 h.
4. The preparation method of the molybdenum alloy containing the antioxidant composite coating according to claim 1, wherein in the third step, the penetrant powder is prepared by ball-milling and uniformly mixing the following raw materials in percentage by mass: 20-30% of silicon powder, 2-6% of sodium fluoride powder, 1-3% of sodium fluosilicate powder, 56-70% of alumina powder and 0-5% of yttrium oxide powder.
5. The preparation method of the molybdenum alloy containing the antioxidant composite coating according to claim 1, wherein in the third step, the ball milling is performed for 1-3 hours at a speed of 100-250 r/min by using a planetary ball mill.
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| CN114182251B (en) * | 2021-11-09 | 2023-09-12 | 北京神箭空天科技有限公司 | High-temperature protective coating for jet pipe of aerospace vehicle engine as well as preparation method and application thereof |
| CN114686740B (en) * | 2022-04-02 | 2022-10-04 | 太原理工大学 | High-temperature wear-resistant molybdenum alloy coating and preparation method thereof |
| CN114875355B (en) * | 2022-04-20 | 2023-08-18 | 西安致远航空科技有限公司 | Preparation process of composite protective coating on surface of die |
| CN115505891A (en) * | 2022-09-15 | 2022-12-23 | 核工业理化工程研究院 | Tantalum surface composite coating and preparation method thereof |
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