CN117655352A - A method for depositing refractory high-entropy alloy coating on CMC surface via dual-pass powder feeding - Google Patents
A method for depositing refractory high-entropy alloy coating on CMC surface via dual-pass powder feeding Download PDFInfo
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Abstract
The invention relates to a method for depositing refractory high-entropy alloy coating on CMC surface by double-way powder feeding, which adopts a laser melting deposition process, deposits Si connecting layer on the surface of silicon carbide fiber reinforced silicon carbide substrate in advance, and deposits Al powder and refractory high-entropy alloy powder into Al by double-way powder feeding 0.15 A refractory high-entropy alloy coating of CrMoTaTi. The book is provided withThe invention adopts a double-way powder feeding mode to solve the problems of volatilization loss of Al and Cr and difficult mixing of Al powder when spherical high-entropy alloy powder is prepared, and the interface between a coating and a matrix is smooth through the adjustment of technological parameters, the thickness of the coating is uniform, the structure is compact, the defects of coating holes, cracking and the like are obviously reduced, excellent oxidation resistance and high temperature resistance are further obtained, and the compact alumina protective film generated after constant-temperature oxidation of the coating is the only oxide film capable of completely protecting the matrix at present, and the working condition adaptability is excellent.
Description
Technical Field
The invention relates to a method for depositing refractory high-entropy alloy coating on the surface of CMC (CMC) by double-path powder feeding, and particularly belongs to the technical field of additive manufacturing of metal materials.
Background
The silicon carbide fiber reinforced silicon carbide base material (CMC) is one kind of ceramic base composite material with silicon carbide fiber as reinforcing body and silicon carbide as matrix. The material has the characteristics of low density, excellent high-temperature mechanical property, excellent oxidation resistance, corrosion resistance, wear resistance and the like, and is regarded as a main candidate material of a new generation of high thrust-weight ratio aeroengine high-temperature parts. However, the material has performance degradation phenomenon in a high-temperature vapor environment, and can generate water-oxygen corrosion, so that the application of CMC in the aerospace field is limited to a great extent.
The adoption of the Environment Barrier Coating (EBC) can effectively resist the water-oxygen corrosion of the complex environment to the ceramic matrix composite material by the hot end component of the CMC material, and improve the high-temperature stability of the ceramic matrix composite material. The environmental barrier coating has good heat insulation, oxidation resistance and corrosion resistance, is one of the most advanced high-temperature thermal protection coatings at present, and is widely applied to the industries of aviation, aerospace, automobiles, large-scale thermal power generation and the like. However, most of the EBC coatings developed today are 250-350 μm thick and of non-uniform thickness. For the EBC coating, the domestic technical maturity and manufacturing maturity are not high enough, and the use of the hot end component of the aeroengine in China is severely limited.
Refractory high entropy alloyRHEA) is an innovative ultra-high temperature metal material. They are typically made of alloys of three or more refractory elements (e.g., cr, mo, ta, hf, nb, V, W) with some other elements (e.g., al, si, co, ni and Ti) in equimolar or near equimolar proportions. Refractory elements are added, so that on one hand, the density of the refractory high-entropy alloy is reduced, and meanwhile, the high-temperature oxidation resistance of the material is improved. However, poor oxidation resistance is a serious disadvantage of common high-entropy alloys, and most high-entropy alloys are difficult to grow protective oxides at high temperatures. Currently, refractory high-entropy alloys of AlCrMoTaTi system are the only refractory high-entropy alloys demonstrated at 1300 o C or more can generate compact Al 2 O 3 An oxide film, and a high-entropy alloy having complete oxidation resistance. Because the high-entropy alloy has excellent oxidation resistance under the ultra-high temperature condition, the high-entropy alloy can be considered to be applied to the surface of a ceramic matrix composite for protection, but RHEA spherical powder is difficult to prepare, cr and Al volatilize in a large amount in the powder preparation process, the Al density is small, the high-entropy alloy is difficult to be uniformly mixed with Cr powder and spherical RHEA powder, and the double-way powder feeding mode can uniformly mix the Al powder with small density, the Cr powder with similar density and the RHEA spherical powder in the powder feeding process so as to compensate the volatilization loss of Al and Cr in the powder preparation process of the spherical RHEA powder.
Disclosure of Invention
Aiming at the defects of the existing refractory high-entropy alloy coating preparation method, the invention aims to provide a method for depositing a refractory high-entropy coating on the surface of CMC by double-path powder feeding, so as to solve the problems of volatilization loss of Al and Cr and difficult mixing of Al powder when preparing refractory high-entropy alloy powder, and prepare the Al with compact structure, flat interface, thin and uniform thickness 0.15 The CrMoTaTi refractory high-entropy alloy coating has excellent ultrahigh-temperature oxidation resistance.
In order to achieve the aim, the invention discloses a method for depositing refractory high-entropy alloy coating on the surface of CMC by double-way powder feeding, which adopts a laser melting deposition process, deposits Si connecting layer on the surface of silicon carbide fiber reinforced silicon carbide substrate in advance, and deposits Al powder and refractory high-entropy alloy powder into Al by double-way powder feeding 0.15 A refractory high-entropy alloy coating of crmotiti;
the method specifically comprises the following steps:
step 1: uniformly mixing spherical high-entropy alloy powder with Cr powder to obtain refractory high-entropy alloy powder;
wherein, the atomic percentage of the spherical high-entropy alloy powder is as follows: al:4.3at.%, cr:5.7 at.% and Mo:31.4 at.%, ta:30.2 at.%, ti:28.4 at.%; the addition amount of Cr powder accounts for 13 wt percent of the refractory high-entropy alloy powder;
step 2: polishing the surface of the silicon carbide fiber reinforced silicon carbide substrate by adopting 320# abrasive paper, respectively ultrasonically cleaning the silicon carbide fiber reinforced silicon carbide substrate by using water and absolute ethyl alcohol, and then drying the silicon carbide fiber reinforced silicon carbide substrate;
step 3: the refractory high-entropy alloy powder, si powder and Al powder are respectively 120-140 o Drying at the temperature C for 12 hours, and naturally cooling to room temperature for standby;
step 4: installing the silicon carbide fiber reinforced silicon carbide substrate treated in the step 2 below a laser emitter and fixing the silicon carbide fiber reinforced silicon carbide substrate by using a steel plate;
step 5: adding the Si powder processed in the step 3 into a powder feeder of laser additive manufacturing equipment, starting the laser additive manufacturing equipment, and setting laser melting deposition process parameters; under the protection of argon, si powder is formed on the surface of the silicon carbide fiber reinforced silicon carbide substrate in a layer-by-layer melting way through a laser beam, and an Si connecting layer is obtained on the surface of the silicon carbide fiber reinforced silicon carbide substrate;
step 6: cleaning up the residual Si powder in the powder feeder, respectively adding the Al powder and refractory high-entropy alloy powder into two powder feeders of laser additive manufacturing equipment, and respectively carrying out two-way powder feeding through a first powder feeding channel and a second powder feeding channel; setting laser melting deposition process parameters, melting refractory high-entropy alloy powder and Al powder by a laser beam under the protection of argon, and depositing Al on the surface of the Si connecting layer of the silicon carbide fiber reinforced silicon carbide substrate 0.15 A refractory high-entropy alloy coating of CrMoTaTi.
In the step 5, the laser melting deposition process parameters are as follows: the laser power is 400-600W, the scanning speed is 1200-1800mm/min, the scanning interval is 0.5 mm, the thickness of each layer is 0.5 mm, the rotating speed of the powder feeder is 0.15-0.25r/min, the powder feeding gas flow is 4-8 rad/min, the deposition layer number is 2, the defocusing amount is 4-6mm, the light spot diameter is 1-3mm, and the gas flow of argon is controlled to be 15L/min.
In the step 6, the laser melting deposition process parameters are as follows: the laser power is 700-900W, the scanning speed is 1000-1500 mm/min, the scanning interval is 0.7 mm, the thickness of each layer is 0.5 mm, the rotating speed of the first powder feeder channel is 0.08-0.12r/min, the rotating speed of the second powder feeder channel is 0.12-0.18r/min, the powder feeding gas flow is 4-8 rad/min, the deposition layer number is 1 layer, the defocusing amount is 4-6mm, the light spot diameter is 1-3mm, and the flow rate of argon is controlled to be 15L/min.
The invention has the beneficial effects that: the invention adopts a double-way powder feeding mode to solve the problems of volatilization loss of Al and Cr and difficult mixing of Al powder when refractory high-entropy alloy powder is prepared, and through adjustment of laser additive manufacturing process parameters, the interface between a coating and a substrate is effectively promoted to be smooth, the thickness of the coating is uniform, the structure is compact, the defects of coating holes, cracking and the like are obviously reduced, excellent oxidation resistance and high temperature resistance are further obtained, and a compact aluminum oxide protection film generated by constant-temperature oxidation of the coating is the only oxide film capable of completely protecting the substrate at present, and the working condition adaptability is excellent.
Drawings
Fig. 1: the invention discloses a technological process schematic diagram of laser additive manufacturing of refractory high-entropy alloy coating;
fig. 2: the electron microscope topography of the refractory high-entropy alloy powder is shown in the specification;
fig. 3: the interface diagram of the refractory high-entropy alloy coating is obtained by melting refractory high-entropy alloy powder when the laser power is 700W;
fig. 4: the invention provides a refractory high-entropy alloy coating interface diagram obtained by melting refractory high-entropy alloy powder when the laser power is 800W;
fig. 5: the invention discloses an electron microscope morphology graph of a refractory high-entropy alloy coating after oxidation.
Detailed Description
Example 1
The method for depositing the refractory high-entropy alloy coating on the surface of CMC through double-path powder feeding comprises the following specific processes:
(1) Preparation and treatment of powders
Refractory high-entropy alloy powder for laser additive manufacturing is obtained by mixing spherical high-entropy alloy powder (RHEA) and Cr powder, and is shown in fig. 2 when observed under an electron microscope. Wherein the RHEA powder is prepared by plasma spheroidization, and comprises the following components in percentage by atom: 4.3at.%, cr:5.7 at.% and Mo:31.4 at.%, ta:30.2 at.%, ti:28.4 at.% composition; the addition amount of Cr powder accounts for 13 wt percent of the refractory high-entropy alloy powder. And respectively loading refractory high-entropy alloy powder, si powder and Al powder into a drying oven, heating to 120-140 ℃ for drying treatment for 12 hours, and cooling to room temperature for standby.
(2) Pretreatment of silicon carbide fiber reinforced silicon carbide substrate
Cutting a silicon carbide fiber reinforced silicon carbide substrate into samples with the thickness of 1mm, the length of 5mm and the width of 5mm by using a diamond wire saw cutting method, polishing the surface of the silicon carbide fiber reinforced silicon carbide substrate by using 320# abrasive paper, respectively ultrasonically cleaning with water and absolute ethyl alcohol, drying, installing the silicon carbide fiber reinforced silicon carbide substrate below a laser emitter manufactured by laser additive manufacturing, and fixing by using a steel plate.
(3) Silicon carbide fiber reinforced silicon carbide substrate surface deposited Si connecting layer
Starting laser additive manufacturing equipment, under the protection of argon, melting and forming Si powder layer by layer on the surface of the silicon carbide fiber reinforced silicon carbide substrate by laser beams, and obtaining an Si connecting layer on the surface of the silicon carbide fiber reinforced silicon carbide substrate.
The set laser melting deposition process parameters are as follows: the laser power is 500W, the scanning speed is 1500mm/min, the scanning interval is 0.5 mm, the thickness of each layer is 0.5 mm, the rotating speed of the powder feeder is 0.2r/min, the powder feeding gas flow is 6rad/min, the deposition layer number is 2 layers, the defocusing amount is 5mm, the light spot diameter is 2mm, and the gas flow of argon is controlled to be 15L/min.
(4) Depositing refractory high-entropy alloy coating on surface of Si connecting layer
And cleaning up the residual Si powder in the powder feeder, respectively adding the Al powder and the refractory high-entropy alloy powder into two powder feeders of laser additive manufacturing equipment, and respectively carrying out two-way powder feeding through a first powder feeding channel and a second powder feeding channel, wherein the two-way powder feeding process flow is shown in figure 1.
Under the protection of argon, melting refractory high-entropy alloy powder and Al powder by a laser beam, and depositing Al on the surface of the Si connecting layer of the silicon carbide fiber reinforced silicon carbide substrate 0.15 A CrMoTaTi refractory high-entropy alloy coating.
The set laser melting deposition process parameters are as follows: the power is 700W or 800W, the scanning speed is 1200 mm/min, the scanning interval is 0.7 mm, each layer thickness is 0.5 mm, the defocusing amount is 5mm, the light spot diameter is 2mm, the rotating speed of a first powder feeding channel is 0.11 r/min, the rotating speed of a second powder feeding channel is 0.15 r/min, the powder feeding gas flow is 6rad/min, the deposition layer number is 1 layer, and the flow rate of argon is controlled to be 15L/min.
(5) Constant temperature oxidation evaluation of refractory high entropy alloy coatings
Surface deposition of Al with 800# sandpaper 0.15 Polishing a silicon carbide fiber reinforced silicon carbide sample of the CrMoTaTi refractory high-entropy alloy coating, sequentially carrying out ultrasonic cleaning by using water and absolute ethyl alcohol, drying, observing under a scanning electron microscope, and obtaining Al with power of 700W and 800W 0.15 The interface of the CrMoTaTi refractory high-entropy alloy coating is shown in figures 3 and 4, the interface between the coating and the matrix is flat, the thickness is uniform, the thickness is about 150 mu m, the defects such as cracks and the like are avoided, and the structure is compact; thereafter, the sample was placed in a clean corundum crucible and placed in a muffle furnace for 1400 o C, carrying out constant-temperature oxidation for 20h, sequentially polishing the obtained oxidized sample by using 800# abrasive paper, 1000# abrasive paper, 1500# abrasive paper and 2000# abrasive paper, sequentially polishing the oxidized sample by using W2.5 abrasive paste, W1.5 abrasive paste and W0.5 abrasive paste, flushing the polished surface by using clear water, soaking the polished surface by using alcohol for 1-2 min to remove redundant abrasive paste or impurities, drying, and evaluating the thickness and the continuity of an oxide layer by using a Scanning Electron Microscope (SEM). As shown in FIG. 5, the electron microscope image of the oxidized layer after constant temperature oxidation is that the oxidized layer is continuous, has thinner and uniform thickness and excellent oxidation resistance and high temperature resistance, and the alumina protective layer is the only oxidized film capable of completely protecting the substrate at present.
Claims (3)
1. Method for depositing refractory high-entropy alloy coating on CMC surface through double-path powder feedingThe method is characterized in that: the method adopts a laser melting deposition process, deposits an Si connecting layer on the surface of a silicon carbide fiber reinforced silicon carbide substrate in advance, and deposits Al powder and refractory high-entropy alloy powder into Al in a double-path powder feeding mode 0.15 A refractory high-entropy alloy coating of crmotiti;
the method specifically comprises the following steps:
step 1: uniformly mixing spherical high-entropy alloy powder with Cr powder to obtain refractory high-entropy alloy powder;
wherein, the atomic percentage of the spherical high-entropy alloy powder is as follows: al:4.3at.%, cr:5.7 at.% and Mo:31.4 at.%, ta:30.2 at.%, ti:28.4 at.%; the addition amount of Cr powder accounts for 13 wt percent of the refractory high-entropy alloy powder;
step 2: polishing the surface of the silicon carbide fiber reinforced silicon carbide substrate by adopting 320# abrasive paper, respectively ultrasonically cleaning the silicon carbide fiber reinforced silicon carbide substrate by using water and absolute ethyl alcohol, and then drying the silicon carbide fiber reinforced silicon carbide substrate;
step 3: the refractory high-entropy alloy powder, si powder and Al powder are respectively 120-140 o Drying at the temperature C for 12 hours, and naturally cooling to room temperature for standby;
step 4: installing the silicon carbide fiber reinforced silicon carbide substrate treated in the step 2 below a laser emitter and fixing the silicon carbide fiber reinforced silicon carbide substrate by using a steel plate;
step 5: adding the Si powder processed in the step 3 into a powder feeder of laser additive manufacturing equipment, starting the laser additive manufacturing equipment, and setting laser melting deposition process parameters; under the protection of argon, si powder is formed on the surface of the silicon carbide fiber reinforced silicon carbide substrate in a layer-by-layer melting way through a laser beam, and an Si connecting layer is obtained on the surface of the silicon carbide fiber reinforced silicon carbide substrate;
step 6: cleaning up the residual Si powder in the powder feeder, respectively adding the Al powder and refractory high-entropy alloy powder into two powder feeders of laser additive manufacturing equipment, and respectively carrying out two-way powder feeding through a first powder feeding channel and a second powder feeding channel; setting laser melting deposition process parameters, melting refractory high-entropy alloy powder and Al powder by a laser beam under the protection of argon, and depositing a silicon carbide fiber reinforced silicon carbide substrate on the surface of an Si connecting layer to form the compositionAl 0.15 A refractory high-entropy alloy coating of CrMoTaTi.
2. The method for depositing refractory high-entropy alloy coating on the surface of CMC by two-way powder delivery according to claim 1, wherein: in the step 5, the laser melting deposition process parameters are as follows: the laser power is 400-600W, the scanning speed is 1200-1800mm/min, the scanning interval is 0.5 mm, the thickness of each layer is 0.5 mm, the rotating speed of the powder feeder is 0.15-0.25r/min, the powder feeding gas flow is 4-8 rad/min, the deposition layer number is 2, the defocusing amount is 4-6mm, the light spot diameter is 1-3mm, and the gas flow of argon is controlled to be 15L/min.
3. The method for depositing refractory high-entropy alloy coating on the surface of CMC by two-way powder delivery according to claim 1, wherein: in the step 6, the laser melting deposition process parameters are as follows: the laser power is 700-900W, the scanning speed is 1000-1500 mm/min, the scanning interval is 0.7 mm, the thickness of each layer is 0.5 mm, the rotating speed of the first powder feeder channel is 0.08-0.12r/min, the rotating speed of the second powder feeder channel is 0.12-0.18r/min, the powder feeding gas flow is 4-8 rad/min, the deposition layer number is 1 layer, the defocusing amount is 4-6mm, the light spot diameter is 1-3mm, and the flow rate of argon is controlled to be 15L/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN118326393A (en) * | 2024-04-08 | 2024-07-12 | 南昌航空大学 | A method for preparing a refractory high entropy alloy coating for C/C composite materials |
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