CN116815113A - Yttrium modified refractory high-entropy silicide coating and preparation method thereof - Google Patents
Yttrium modified refractory high-entropy silicide coating and preparation method thereof Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 98
- 239000011248 coating agent Substances 0.000 title claims abstract description 93
- 229910021332 silicide Inorganic materials 0.000 title claims abstract description 78
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 229910052727 yttrium Inorganic materials 0.000 title claims abstract description 58
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 98
- 239000000956 alloy Substances 0.000 claims abstract description 98
- 239000000843 powder Substances 0.000 claims abstract description 74
- 239000011159 matrix material Substances 0.000 claims abstract description 45
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 42
- 230000003647 oxidation Effects 0.000 claims abstract description 42
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 42
- 230000000149 penetrating effect Effects 0.000 claims abstract description 42
- 238000005475 siliconizing Methods 0.000 claims abstract description 26
- 238000002679 ablation Methods 0.000 claims abstract description 23
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 19
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 10
- 238000007789 sealing Methods 0.000 claims abstract description 10
- 239000012298 atmosphere Substances 0.000 claims abstract description 9
- 229910052758 niobium Inorganic materials 0.000 claims description 27
- 229910052721 tungsten Inorganic materials 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 26
- 239000003870 refractory metal Substances 0.000 claims description 20
- 239000000126 substance Substances 0.000 claims description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000004140 cleaning Methods 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 13
- 238000002844 melting Methods 0.000 claims description 11
- 230000008018 melting Effects 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 11
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 238000005520 cutting process Methods 0.000 claims description 9
- 238000005238 degreasing Methods 0.000 claims description 9
- 239000004615 ingredient Substances 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 238000005498 polishing Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 238000011065 in-situ storage Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 230000004584 weight gain Effects 0.000 claims description 4
- 235000019786 weight gain Nutrition 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 description 14
- 238000004321 preservation Methods 0.000 description 13
- 238000009792 diffusion process Methods 0.000 description 8
- 239000007789 gas Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 229910004298 SiO 2 Inorganic materials 0.000 description 6
- 238000000498 ball milling Methods 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000003064 anti-oxidating effect Effects 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000012190 activator Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910004525 TaCr Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- 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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
- C23C10/34—Embedding in a powder mixture, i.e. pack cementation
- C23C10/52—Embedding in a powder mixture, i.e. pack cementation more than one element being diffused in one step
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Abstract
The invention discloses an yttrium modified refractory high-entropy silicide coating and a preparation method thereof, wherein the yttrium modified refractory high-entropy silicide coating has excellent oxidation resistance at 1450 ℃ and ultra-high temperature ablation resistance at 2100 ℃, and the preparation method comprises the following steps: (1) preparing a penetrating agent: the penetrating agent consists of the following components in percentage by mass: 25 to 35 percent of Si powder, 2 to 8%Y 2 O 3 Powder, 3-5% NaF powder and Al 2 O 3 Powder balance; (2) Embedding and compacting a NbMoTaW refractory high-entropy alloy matrix into a crucible filled with a penetrating agent, covering and sealing the crucible, and carrying out embedding and siliconizing treatment on the NbMoTaW refractory high-entropy alloy matrix in an inert atmosphere at 900-1200 ℃ for 3-24 h; obtaining yttrium modified refractory high entropy silicide (NbMoTaW) Si on the surface of NbMoTaW refractory high entropy alloy 2 And (3) coating.
Description
Technical Field
The invention relates to an yttrium modified refractory high-entropy silicide coating and a preparation method thereof.
Background
The high-entropy alloy is an alloy composed of a plurality of metal elements in equimolar or near equimolar ratio. The high-entropy alloy has excellent mechanical, friction and wear resistance, corrosion resistance and high temperature resistance and is one of the most potential novel materials. The refractory high-entropy alloy composed of refractory metal elements Nb, mo, ta, W, V, hf and the like has stable structure and excellent high-temperature mechanical properties, for example, the compressive yield strength of the NbMoTaW refractory high-entropy alloy can still reach 405MPa at 1600 ℃.
However, refractory high-entropy alloys have poor oxidation resistance at medium and high temperatures, greatly restricting their engineering applications in high-temperature aerobic environments. Therefore, for refractory high-entropy alloys used in the high-temperature field, modification is needed to improve the high-temperature oxidation resistance. Currently, the main approaches for improving the high-temperature performance of materials are divided into two types, including alloy component design and surface oxidation-resistant coating. Liu et al (J.alloy.Compd., 2014, 583:162-169) research found NbCrMoTiAl 0.5 ，NbCrMoTiVAl 0.5 ，NbCrMoTiVAl 0. 5Si 0.3 And NbCrMoVAl 0.5 The refractory high-entropy alloy has a single-phase BCC solid solution structure, oxidation kinetics in the air at 1300 ℃ follow a linear rule, and the addition of Ti and Al can effectively improve the oxidation resistance of the refractory high-entropy alloy. However, the addition of antioxidation elements such as silicon (Si), aluminum (Al), chromium (Cr) and the like to the refractory metal alloy tends to form a hard brittle phase (NbCr) 2 、TaCr 2 、Nb 3 Al), alloy workability is drastically reduced when the doping element ratio exceeds a threshold value, and thus there is a limitation; in addition, the melting point of the added element is lower, so that the high-temperature mechanical property of the refractory high-entropy alloy is often reduced.
The surface coating method can maintain the room temperature and high temperature mechanical properties of the alloy matrix and simultaneously remarkably improve the high temperature oxidation resistance of the material. Shi et al (int. J. Refract)Met.H.,2021, 98:105562) a micro-arc oxidation (MAO) film was prepared on the surface of AlTiCrVZr refractory high entropy alloy. Al in MAO coating 2 O 3 、Cr 2 O 3 And SiO 2 The iso-oxides inhibit diffusion of oxygen into the matrix and volatilization of V element, but the oxidation temperature studied in this work was only 800 ℃. Han et al (Materials, 2020, 13:3592) prepared Si-20Cr-20Fe coatings on MonbTaTiW refractory high entropy alloys by slurry sintering, which silicide coatings were effective in improving oxidation of the alloys at 1000 ℃ and 1300 ℃. However, the silicide coating prepared by the slurry melting method has a large number of pores, which affect the antioxidation effect of the coating. In the existing research on the surface antioxidation coating of the refractory high-entropy alloy, the oxidation temperature is low and the research on the oxidation behavior is not long-term.
Disclosure of Invention
The invention aims to: the invention aims to provide an yttrium modified refractory high-entropy silicide coating and a preparation method thereof, and the method can form the yttrium modified refractory high-entropy silicide coating on the surface of an NbMoTaW refractory high-entropy alloy, so that the high-temperature oxidation resistance and the ultrahigh-temperature ablation resistance of the NbMoTaW refractory high-entropy alloy can be effectively improved.
The technical scheme is as follows: the yttrium modified refractory high entropy silicide coating comprises the chemical composition of [ NbMoTaW (Y)]Si 2 The method comprises the steps of carrying out a first treatment on the surface of the The content of Nb, mo, ta, W atom percent is a, the content of a is more than or equal to 5% and less than or equal to 10%, the content of b is Y, the content of b is more than or equal to 0.2% and less than or equal to 4.5%, the content of Si is c, and the content of c is more than or equal to 64% and less than or equal to 69%; the yttrium modified refractory high-entropy silicide coating has a hexagonal C40 crystal structure and is formed by in-situ reaction on the surface of the NbMoTaW refractory high-entropy alloy; high-temperature oxidation at 1450 ℃ for 24 hours is less than 3.5mg/cm 2 The mass ablation rate after 180s of ablation at 2100 ℃ is only 0.014-0.1mg/s, and the limit ablation temperature reaches 2200 ℃.
The preparation method of the yttrium modified refractory high-entropy silicide coating comprises the following steps:
(1) Preparing a penetrating agent: the penetrating agent consists of the following components in percentage by mass: 25 to 35 percent of Si powder, 2 to 8%Y 2 O 3 3 to 5 percent of powderNaF powder and Al 2 O 3 Powder balance;
(2) Embedding and compacting a NbMoTaW refractory high-entropy alloy matrix into a crucible filled with a penetrating agent, covering and sealing the crucible, and carrying out embedding and siliconizing treatment on the NbMoTaW refractory high-entropy alloy matrix in an inert atmosphere at 900-1200 ℃ for 3-24 h; obtaining yttrium modified refractory high entropy silicide (NbMoTaW) Si on the surface of NbMoTaW refractory high entropy alloy 2 And (3) coating.
Wherein in the step (1), si powder and Y are mixed 2 O 3 Powder, naF powder, al 2 O 3 The powder and the grinding balls are placed in a ball mill, and the ball mill is evenly mixed for 6 to 8 hours.
In the step (2), refractory metal simple substance Nb, mo, ta, W with equal molar ratio is taken as ingredients, and an oxide film on the metal surface is removed firstly; then preparing NbMoTaW refractory high-entropy alloy cast ingots by adopting a vacuum arc melting method; and sequentially carrying out linear cutting, degreasing, polishing and cleaning on the high-entropy alloy cast ingot to obtain the NbMoTaW refractory high-entropy alloy matrix. The purity of the refractory metal element Nb, mo, ta, W feedstock was 99.9wt.%.
In the step (2), the NbMoTaW refractory high-entropy alloy matrix is buried in a crucible filled with the penetrating agent and compacted, so that the thickness of the penetrating agent covered on each surface of the alloy matrix is not less than 10mm.
Wherein in the step (2), al is added to 2 O 3 Powder and silica sol in the mass-volume ratio of 1.5g:1mL of the mixture is mixed and prepared into slurry, and the crucible cover is sealed by adopting the slurry.
In the step (2), the inert atmosphere is an argon protection atmosphere.
Wherein, in the step (2), the heating rate is 10 ℃/min.
In the step (2), the NbMoTaW refractory high-entropy alloy matrix is subjected to embedding siliconizing treatment in an inert atmosphere at 1000 ℃ for 12 hours. Yttrium modified (NbMoTaW) Si 2 The optimal embedding siliconizing temperature of the coating is 1000 ℃ and the time is 12 hours.
In the step (2), the cooling rate in the process of cooling to room temperature after embedding siliconizing treatment is 5 ℃/min.
During the embedding siliconizing process, si reacts with an activator (NaF) to form a plurality of gas fluorides SiF through the reaction formula 1 x (1.ltoreq.x.ltoreq.4), e.g. SiF 4 、SiF 3 、SiF 2 And SiF; y is Y 2 O 3 React with an activator (NaF) to form a gaseous fluoride YF 3 (equation 2); driven by chemical potential gradients, these SiFs x And YF 3 Diffusion to the substrate surface occurs through interstices between the infiltrant powder particles. SiF (SiF) x And YF 3 Disproportionation reactions respectively take place to form the activity [ Si ] at atomic scale]And Activity [ Y ]](equations 3 and 4), partial Activity [ Y ]]With SiF x Substitution reaction promoting Activity [ Si ]]The formation (reaction formula 5), in addition, active Y atoms are adsorbed on the surface of the refractory high-entropy alloy matrix and diffuse inwards, and as the size of the Y atoms is slightly larger than that of the NbMoTaW refractory high-entropy alloy, the Y forms a substitutional solid solution with the matrix alloy, so that lattice distortion is increased, a larger channel is provided for Si to diffuse inwards, and active Si atoms are adsorbed on the surface of the refractory high-entropy alloy matrix and diffuse inwards to react with the high-entropy alloy to form a refractory high-entropy silicide coating (reaction formula 7).
Si(s)+xNaF(l)→SiF x (g) +xNa (g) equation 1
Y 2 O 3 (s)+6NaF(l)→2YF 3 (g)+3Na 2 O(s) equation 2
(x+1)SiF x (g)→xSiF x-1 (g)+[Si](s) equation 3
2YF 3 (g)→2[Y](s)+3F 2 (g) Reaction 4
x[Y](s)+3SiF x (g)→xYF 3 (g)+3[Si](s) equation 5
NbMoTaW+ [ Y ] →NbMoTaW (Y) equation 6
NbMoTaW(Y)+2[Si]→[NbMoTaW(Y)]Si 2 Equation 7.
Yttrium modified refractory high entropy silicide (NbMoTaW) Si grown in situ on refractory high entropy alloy substrate surface 2 The coating, yttrium can effectively promote Si diffusion penetration, increase the diffusion rate of Si in the matrix alloy, and form a refractory high-entropy silicide coating with fine and uniform grains. The refractory high entropy silicide has improved yttrium due to delayed diffusion and selective oxidationThe adhesiveness of the oxide film improves its anti-peeling ability. The yttrium modified refractory high-entropy silicide coating has excellent high-temperature heat stability at 1450 ℃, and the refractory high-entropy silicide coating is subjected to preferential oxidation of Si to form continuous and compact SiO on the surface 2 Film, simultaneously forming Y 2 O 3 ，Y 2 O 3 And SiO in oxide film 2 React to form Y 2 Si 2 O 7 Stabilizing the structure of the oxide film and protecting the NbMoTaW refractory high-entropy alloy matrix from oxidation for more than 24 hours at 1450 ℃.
The beneficial effects are that: compared with the prior art, the invention has the following remarkable advantages: (1) The yttrium modified refractory high entropy silicide (NbMoTaW) Si prepared by the invention 2 The coating grows on the surface of the NbMoTaW refractory high-entropy alloy in situ, and the coating is tightly combined with the matrix and is not easy to crack and fall off; (2) The yttrium in the penetrating agent can provide more diffusion channels for silicon in the embedding and siliconizing process, so that the diffusion growth of Si and NbMoTaW refractory high-entropy alloy matrix is accelerated; yttrium modified refractory high entropy silicide (NbMoTaW) Si 2 The coating can obviously improve the high-temperature oxidation resistance of NbMoTaW refractory high-entropy alloy at more than 1450 ℃, and the yttrium modified refractory high-entropy silicide (NbMoTaW) Si 2 Surface SiO of coating at high temperature 2 The oxide film is continuous and compact and can be self-repaired; the coating has stable structure at high temperature, and the surface oxide film is continuous and compact, so that the oxidation resistance of the coating can be maintained for a long time (more than 24 h); (3) Yttrium modified refractory high entropy silicide (NbMoTaW) Si 2 The coating can obviously improve the ablation resistance of NbMoTaW refractory high-entropy alloy above 2000 ℃, the coating remains intact after 180s of ablation at 2100 ℃, the sample has a pit after 100s of ablation at 2200 ℃, and yttrium in the coating can promote SiO 2 The oxide film forms and retards oxidation of oxygen to the refractory high entropy silicide layer.
Drawings
FIG. 1 is an XRD pattern for yttrium-modified refractory high entropy silicide coatings obtained in examples 1-4;
FIG. 2 is a surface SEM image of the yttrium modified refractory high entropy silicide coating obtained in example 3 after 24 hours of oxidation at 1450 ℃;
FIG. 3 is a surface XRD pattern of the yttrium modified refractory high entropy silicide coating obtained in example 3 after 24 hours of oxidation at 1450 ℃;
FIG. 4 is a cross-sectional SEM elemental profile of the yttrium modified refractory high entropy silicide coating obtained in example 3 after 24h oxidation at 1450 ℃;
FIG. 5 is a surface SEM image of the refractory high entropy silicide coating obtained in comparative example 3 after 24 hours of oxidation at 1450 ℃;
FIG. 6 is a plot of ablated surface temperature versus ablation time at 2100℃and 2200℃for the yttrium-modified refractory high entropy silicide coating obtained in example 3;
FIG. 7 is a macroscopic photograph of the surface of the yttrium-modified refractory high entropy silicide coating obtained in example 3 after ablation at 2100℃and 2200 ℃.
Detailed Description
Example 1
The preparation method of the yttrium modified refractory high-entropy silicide coating comprises the following steps:
(1) Taking refractory metal simple substance Nb, mo, ta, W with equal molar ratio as ingredients, and firstly removing an oxide film on the metal surface; then preparing NbMoTaW refractory high-entropy alloy cast ingots by adopting a vacuum arc melting method; sequentially performing linear cutting, degreasing, polishing and cleaning on the high-entropy alloy cast ingot to obtain a NbMoTaW refractory high-entropy alloy matrix; the purity of the refractory metal simple substance Nb, mo, ta, W raw material is 99.9wt.%;
(2) Preparing a penetrating agent: the penetrating agent consists of the following components in percentage by mass: 30% Si powder, 2%Y 2 O 3 Powder, 5% NaF powder and 63% Al 2 O 3 Powder; mixing the Si powder and Y in the formula amount 2 O 3 Powder, naF powder, al 2 O 3 Placing the powder and the grinding balls in a ball mill, and uniformly mixing the powder and the grinding balls after ball milling for 6 hours;
(3) Embedding an NbMoTaW refractory high-entropy alloy matrix into Al filled with a penetrating agent 2 O 3 The crucible is compacted, so that the thickness of penetrating agent covered on each surface of NbMoTaW refractory high-entropy alloy matrix is not less than 10mm, the crucible is covered and silica sol and Al are adopted 2 O 3 Sealing the slurry prepared by the powder, placing the sealed crucible in a high-temperature tube furnace for embedding and siliconizing treatment, and heating along with the furnace under the protection of argon gas at the heating rate of10 ℃/min, the heat preservation temperature is 1200 ℃, the temperature is kept for 3 hours, then the temperature is reduced along with the furnace, and the temperature reduction rate is 5 ℃/min;
(4) Taking out the sample after embedding siliconizing cooled to room temperature, and ultrasonically cleaning to obtain a product of NbMoTaW refractory high-entropy alloy with yttrium modified refractory high-entropy silicide (NbMoTaW) Si on the surface 2 And (3) coating.
The yttrium modified refractory high entropy silicide (NbMoTaW) Si of the invention 2 The coating contains Nb, mo, ta, W atom% 6.92%, 6.95%, 7.57%, 9.65%, Y atom% 0.74% and Si atom% 68.18%.
Example 2
The preparation method of the yttrium modified refractory high-entropy silicide coating comprises the following steps:
(1) Taking refractory metal simple substance Nb, mo, ta, W with equal molar ratio as ingredients, and firstly removing an oxide film on the metal surface; then preparing NbMoTaW refractory high-entropy alloy cast ingots by adopting a vacuum arc melting method; sequentially performing linear cutting, degreasing, polishing and cleaning on the high-entropy alloy cast ingot to obtain a NbMoTaW refractory high-entropy alloy matrix; the purity of the refractory metal simple substance Nb, mo, ta, W raw material is 99.9wt.%;
(2) Preparing a penetrating agent: the penetrating agent consists of the following components in percentage by mass: 25% Si powder, 8%Y 2 O 3 Powder, 3% NaF powder and 64% Al 2 O 3 Powder; mixing the Si powder and Y in the formula amount 2 O 3 Powder, naF powder, al 2 O 3 Placing the powder and the grinding balls in a ball mill, and uniformly mixing the powder and the grinding balls after ball milling for 6 hours;
(3) Embedding an NbMoTaW refractory high-entropy alloy matrix into Al filled with a penetrating agent 2 O 3 The crucible is compacted, so that the thickness of penetrating agent covered on each surface of NbMoTaW refractory high-entropy alloy matrix is not less than 10mm, the crucible is covered and silica sol and Al are adopted 2 O 3 Sealing the slurry prepared by the powder, placing the sealed crucible in a high-temperature tube furnace for embedding and siliconizing treatment, heating along with the furnace under the protection of argon gas, wherein the heating rate is 10 ℃/min, the heat preservation temperature is 900 ℃, and cooling along with the furnace after heat preservation for 24 hours, and the cooling rate is 5 ℃/min;
(4) Taking out the sample after embedding siliconizing cooled to room temperature, and ultrasonically cleaning to obtain a product of NbMoTaW refractory high-entropy alloy with yttrium modified refractory high-entropy silicide (NbMoTaW) Si on the surface 2 And (3) coating.
The yttrium modified refractory high entropy silicide (NbMoTaW) Si of the invention 2 The Nb, mo, ta, W atomic percent content in the coating is 6.82 percent, 6.65 percent, 7.10 percent and 8.75 percent respectively, the Y atomic percent content is 4.11 percent, and the Si atomic percent content is 66.57 percent.
Example 3
The preparation method of the yttrium modified refractory high-entropy silicide coating comprises the following steps:
(1) Taking refractory metal simple substance Nb, mo, ta, W with equal molar ratio as ingredients, and firstly removing an oxide film on the metal surface; then preparing NbMoTaW refractory high-entropy alloy cast ingots by adopting a vacuum arc melting method; sequentially performing linear cutting, degreasing, polishing and cleaning on the high-entropy alloy cast ingot to obtain a NbMoTaW refractory high-entropy alloy matrix; the purity of the refractory metal simple substance Nb, mo, ta, W raw material is 99.9wt.%;
(2) Preparing a penetrating agent: the penetrating agent consists of the following components in percentage by mass: 30% Si powder, 4%Y 2 O 3 Powder, 5% NaF powder and 61% Al 2 O 3 Powder; mixing the Si powder and Y in the formula amount 2 O 3 Powder, naF powder, al 2 O 3 Placing the powder and the grinding balls in a ball mill, and uniformly mixing the powder and the grinding balls after ball milling for 6 hours;
(3) Embedding an NbMoTaW refractory high-entropy alloy matrix into Al filled with a penetrating agent 2 O 3 The crucible is compacted, so that the thickness of penetrating agent covered on each surface of NbMoTaW refractory high-entropy alloy matrix is not less than 10mm, the crucible is covered and silica sol and Al are adopted 2 O 3 Sealing the slurry prepared by the powder, placing the sealed crucible in a high-temperature tube furnace for embedding and siliconizing treatment, heating along with the furnace under the protection of argon gas, wherein the heating rate is 10 ℃/min, the heat preservation temperature is 1000 ℃, and cooling along with the furnace after 12h of heat preservation, and the cooling rate is 5 ℃/min;
(4) Taking out the sample after embedding siliconizing cooled to room temperature, and performing ultrasonic cleaningWashing, and obtaining a product of NbMoTaW refractory high-entropy alloy with yttrium modified refractory high-entropy silicide (NbMoTaW) Si on the surface 2 And (3) coating.
The yttrium modified refractory high entropy silicide (NbMoTaW) Si of the invention 2 The Nb, mo, ta, W atomic percent content in the coating is 7.33 percent, 7.54 percent, 7.69 percent and 8.65 percent respectively, the Y atomic percent content is 2.03 percent, and the Si atomic percent content is 66.76 percent.
Example 4
The preparation method of the yttrium modified refractory high-entropy silicide coating comprises the following steps:
(1) Taking refractory metal simple substance Nb, mo, ta, W with equal molar ratio as ingredients, and firstly removing an oxide film on the metal surface; then preparing NbMoTaW refractory high-entropy alloy cast ingots by adopting a vacuum arc melting method; sequentially performing linear cutting, degreasing, polishing and cleaning on the high-entropy alloy cast ingot to obtain a NbMoTaW refractory high-entropy alloy matrix; the purity of the refractory metal simple substance Nb, mo, ta, W raw material is 99.9wt.%;
(2) Preparing a penetrating agent: the penetrating agent consists of the following components in percentage by mass: 35% Si powder, 6%Y 2 O 3 Powder, 5% NaF powder and 54% Al 2 O 3 Powder; mixing the Si powder and Y in the formula amount 2 O 3 Powder, naF powder, al 2 O 3 Placing the powder and the grinding balls in a ball mill, and uniformly mixing the powder and the grinding balls for 8 hours;
(3) Embedding an NbMoTaW refractory high-entropy alloy matrix into Al filled with a penetrating agent 2 O 3 The crucible is compacted, so that the thickness of penetrating agent covered on each surface of NbMoTaW refractory high-entropy alloy matrix is not less than 10mm, the crucible is covered and silica sol and Al are adopted 2 O 3 Sealing the slurry prepared by the powder, placing the sealed crucible in a high-temperature tube furnace for embedding and siliconizing treatment, heating along with the furnace under the protection of argon gas, wherein the heating rate is 10 ℃/min, the heat preservation temperature is 1000 ℃, and cooling along with the furnace after 12h of heat preservation, and the cooling rate is 5 ℃/min;
(4) Taking out the sample after embedding siliconizing cooled to room temperature, and ultrasonically cleaning to obtain the product of NbMoTaW refractory high-entropy alloy with yttrium modified refractory high-entropy siliconizing surfaceObject (NbMoTaW) Si 2 And (3) coating.
The yttrium modified refractory high entropy silicide (NbMoTaW) Si of the invention 2 The Nb, mo, ta, W atomic percent content in the coating is 5.96 percent, 7.14 percent, 6.25 percent and 8.24 percent respectively, the Y atomic percent content is 3.41 percent, and the Si atomic percent content is 69.00 percent.
Comparative example 1
A preparation method of an yttrium modified refractory high-entropy silicide coating comprises the following steps:
(1) Taking refractory metal simple substance Nb, mo, ta, W with equal molar ratio as ingredients, and firstly removing an oxide film on the metal surface; then preparing NbMoTaW refractory high-entropy alloy cast ingots by adopting a vacuum arc melting method; sequentially performing linear cutting, degreasing, polishing and cleaning on the high-entropy alloy cast ingot to obtain a NbMoTaW refractory high-entropy alloy matrix; the purity of the refractory metal simple substance Nb, mo, ta, W raw material is 99.9wt.%;
(2) Preparing a penetrating agent: the penetrating agent consists of the following components in percentage by mass: 30% Si powder, 4%Y 2 O 3 Powder, 5% NaF powder and 61% Al 2 O 3 Powder; mixing the Si powder and Y in the formula amount 2 O 3 Powder, naF powder, al 2 O 3 Placing the powder and the grinding balls in a ball mill, and uniformly mixing the powder and the grinding balls after ball milling for 6 hours;
(3) Embedding an NbMoTaW refractory high-entropy alloy matrix into Al filled with a penetrating agent 2 O 3 The crucible is compacted, so that the thickness of penetrating agent covered on each surface of NbMoTaW refractory high-entropy alloy matrix is not less than 10mm, the crucible is covered and silica sol and Al are adopted 2 O 3 Sealing the slurry prepared by the powder, placing the sealed crucible in a high-temperature tube furnace for embedding and siliconizing treatment, heating along with the furnace under the protection of argon gas, wherein the heating rate is 10 ℃/min, the heat preservation temperature is 1500 ℃, and cooling along with the furnace after 12h of heat preservation, and the cooling rate is 5 ℃/min;
(4) Taking out the sample after embedding siliconizing cooled to room temperature, and ultrasonically cleaning to obtain a product of NbMoTaW refractory high-entropy alloy with yttrium modified refractory high-entropy silicide (NbMoTaW) Si on the surface 2 And (3) coating.
The yttrium modified refractory high-entropy siliconCompound (NbMoTaW) Si 2 The coating contains Nb, mo, ta, W atom% 6.01%, 5.14%, 5.71%, 9.21%, Y atom% 2.51% and Si atom% 71.42%.
Comparative example 2
A preparation method of an yttrium modified refractory high-entropy silicide coating comprises the following steps:
(1) Taking refractory metal simple substance Nb, mo, ta, W with equal molar ratio as ingredients, and firstly removing an oxide film on the metal surface; then preparing NbMoTaW refractory high-entropy alloy cast ingots by adopting a vacuum arc melting method; sequentially performing linear cutting, degreasing, polishing and cleaning on the high-entropy alloy cast ingot to obtain a NbMoTaW refractory high-entropy alloy matrix; the purity of the refractory metal simple substance Nb, mo, ta, W raw material is 99.9wt.%;
(2) Preparing a penetrating agent: the penetrating agent consists of the following components in percentage by mass: 30% Si powder, 10% Y 2 O 3 Powder, 5% NaF powder and 61% Al 2 O 3 Powder; mixing the Si powder and Y in the formula amount 2 O 3 Powder, naF powder, al 2 O 3 Placing the powder and the grinding balls in a ball mill, and uniformly mixing the powder and the grinding balls after ball milling for 6 hours;
(3) Embedding an NbMoTaW refractory high-entropy alloy matrix into Al filled with a penetrating agent 2 O 3 The crucible is compacted, so that the thickness of penetrating agent covered on each surface of NbMoTaW refractory high-entropy alloy matrix is not less than 10mm, the crucible is covered and silica sol and Al are adopted 2 O 3 Sealing the slurry prepared by the powder, placing the sealed crucible in a high-temperature tube furnace for embedding and siliconizing treatment, heating along with the furnace under the protection of argon gas, wherein the heating rate is 10 ℃/min, the heat preservation temperature is 1000 ℃, and cooling along with the furnace after 12h of heat preservation, and the cooling rate is 5 ℃/min;
(4) Taking out the sample after embedding siliconizing cooled to room temperature, and ultrasonically cleaning to obtain a product of NbMoTaW refractory high-entropy alloy with yttrium modified refractory high-entropy silicide (NbMoTaW) Si on the surface 2 And (3) coating.
The yttrium modified refractory high entropy silicide (NbMoTaW) Si 2 Nb, mo, ta, W atom percent of the coating is 6.94 percent, 6.51 percent,8.24%, 8.25%, and the content of Y atom% is 4.64%, and the content of Si atom% is 65.42%.
Comparative example 3
A method for preparing a refractory high entropy silicide coating, comprising the steps of:
(1) Taking refractory metal simple substance Nb, mo, ta, W with equal molar ratio as ingredients, and firstly removing an oxide film on the metal surface; then preparing NbMoTaW refractory high-entropy alloy cast ingots by adopting a vacuum arc melting method; sequentially performing linear cutting, degreasing, polishing and cleaning on the high-entropy alloy cast ingot to obtain a NbMoTaW refractory high-entropy alloy matrix; the purity of the refractory metal simple substance Nb, mo, ta, W raw material is 99.9wt.%;
(2) Preparing a penetrating agent: the penetrating agent consists of the following components in percentage by mass: 30% Si powder, 5% NaF powder and 65% Al 2 O 3 Powder; mixing the Si powder, naF powder and Al powder in the formula amount 2 O 3 Placing the powder and the grinding balls in a ball mill, and uniformly mixing the powder and the grinding balls after ball milling for 6 hours;
(3) Embedding an NbMoTaW refractory high-entropy alloy matrix into Al filled with a penetrating agent 2 O 3 The crucible is compacted, so that the thickness of penetrating agent covered on each surface of NbMoTaW refractory high-entropy alloy matrix is not less than 10mm, the crucible is covered and silica sol and Al are adopted 2 O 3 Sealing the slurry prepared by the powder, placing the sealed crucible in a high-temperature tube furnace for embedding and siliconizing treatment, heating along with the furnace under the protection of argon gas, wherein the heating rate is 10 ℃/min, the heat preservation temperature is 1000 ℃, and cooling along with the furnace after 12h of heat preservation, and the cooling rate is 5 ℃/min;
(4) Taking out the sample after embedding siliconizing cooled to room temperature, and ultrasonically cleaning to obtain a product of NbMoTaW refractory high-entropy alloy with refractory high-entropy silicide (NbMoTaW) Si on the surface 2 And (3) coating.
The refractory high entropy silicide (NbMoTaW) Si 2 The coating contains Nb, mo, ta, W atom percent 5.74%, 6.24%, 9.91% and 11.35%, Y atom percent 0 and Si atom percent 66.76%.
Testing the yttrium-modified refractory high entropy siliconizing prepared in examples 1-4 Using an X-ray diffractometerThe structure of the coating is shown in FIG. 1, and all the yttrium-modified refractory high-entropy silicide coating samples prepared are single-phase structures, corresponding to (NbMoTaW) Si 2 。
The yttrium-modified refractory high-entropy silicide coatings prepared in examples 1 to 4 were subjected to static oxidation at 1450 ℃ using a high-temperature box furnace, the oxidation weight increase per unit area after 24 hours of oxidation is shown in Table 1, and the minimum oxidation weight increase of the yttrium-modified refractory high-entropy silicide coating in example 3 is only 1.92mg/cm 2 Has optimal oxidation resistance.
TABLE 1
The yttrium-modified refractory high entropy silicide coating in example 3 was up to 58 μm thick. The surface appearance of the sample after 24h oxidation at 1450 ℃ is shown in figure 2, and the surface is continuous and compact SiO 2 And (3) a film. Example 3 XRD analysis of the sample surface after 24h of oxidation at 1450℃ as shown in FIG. 3, the oxidized surface of the yttrium-modified refractory high entropy silicide coating was free of SiO 2 In addition, there is also a factor Y 2 O 3 And SiO in oxide film 2 Y formed by the reaction 2 Si 2 O 7 Can stabilize SiO 2 The role of the oxide film structure. The morphology analysis of the cross section of the sample oxidized for 24 hours at 1450 ℃ in example 3 is carried out, and the result is shown in figure 4, wherein thermal growth cracks appear after the high-temperature oxidation of the yttrium modified refractory high-entropy silicide coating, and SiO is formed on the surface of the yttrium modified refractory high-entropy silicide coating 2 The oxide film has self-repairing capability, fills up cracks and blocks oxygen diffusion, so that the coating has excellent oxidation resistance.
The yttrium modified refractory high-entropy silicide coating in comparative example 1 has a thickness of 500 μm, and has a large number of cracks due to the overlarge thermal stress generated by the coating due to the overhigh preparation temperature, and the unit oxidation weight of the coating reaches 54.48mg/cm after static oxidation for 10 hours at 1450 DEG C 2 Without protection, the substrate begins to oxidize.
Comparative example 2 yttrium modified refractory high entropy silicide coating thickness was 46 μm when Y 2 O 3 The powder is added in excessive amount, and the excessive active yttrium atoms are inThe surface of the matrix is piled up, so that Si is blocked from diffusing into the NbMoTaW refractory high-entropy alloy, and the growth of the coating is inhibited. After static oxidation at 1450℃for 2h, the weight per unit area of oxidation increases by about 1.85mg/cm 2 . The yttrium on the surface of the coating reacts with oxygen quickly, which causes obvious oxidation weight gain and is unfavorable for forming continuous and compact SiO 2 Oxidation film, oxidation weight gain reaches 4.94mg/cm after 24 hours of oxidation 2 。
The refractory high entropy silicide coating of comparative example 3 had a thickness of only 31 μm and was about half that of the yttrium-modified refractory high entropy silicide coating of example 3. Insufficient coating thickness will not provide longer protection to the substrate. The unit area oxidation weight gain of the refractory high-entropy silicide coating after 24h oxidation at 1450 ℃ is obviously increased to 3.7mg/cm 2 The surface morphology of the oxidized sample after 24 hours is shown in figure 5, and more refractory metal oxide and SiO appear on the oxidized surface 2 The membrane is destroyed, severely affecting its long-term oxidation at 1450 ℃.
An ablation experiment is carried out on the yttrium modified refractory high-entropy silicide coating prepared in the embodiment 3 by adopting a plasma ablation method, a change curve of the surface temperature of a sample along with ablation time is shown in figure 6, a macroscopic photograph of the surface of the sample after ablation is shown in figure 7, the coating remains intact after ablation for 180s at 2100 ℃, the mass ablation rate is only 0.014mg/s, the sample has ablation pits after ablation for 100s at 2200 ℃, and the mass ablation rate is-2.075 mg/s. Illustrating that the yttrium-modified refractory high-entropy silicide coating prepared in example 3 has ultra-high temperature ablation resistance.
Claims (10)
1. The preparation method of the yttrium modified refractory high-entropy silicide coating is characterized by comprising the following steps of:
(1) Preparing a penetrating agent: the penetrating agent consists of the following components in percentage by mass: 25 to 35 percent of Si powder, 2 to 8%Y 2 O 3 Powder, 3-5% NaF powder and Al 2 O 3 Powder balance;
(2) Embedding and compacting a NbMoTaW refractory high-entropy alloy matrix into a crucible filled with a penetrating agent, covering and sealing the crucible, and carrying out embedding and siliconizing treatment on the NbMoTaW refractory high-entropy alloy matrix in an inert atmosphere at 900-1200 ℃ for 3-24 h; in NbMoTThe surface of the aW refractory high-entropy alloy is obtained to obtain yttrium modified refractory high-entropy silicide (NbMoTaW) Si 2 And (3) coating.
2. The method of preparing a yttrium-modified refractory high entropy silicide coating as claimed in claim 1, wherein: in the step (1), si powder and Y 2 O 3 Powder, naF powder, al 2 O 3 The powder and the grinding balls are placed in a ball mill, and the ball mill is evenly mixed for 6 to 8 hours.
3. The method of preparing a yttrium-modified refractory high entropy silicide coating as claimed in claim 1, wherein: in the step (2), refractory metal simple substance Nb, mo, ta, W with equal molar ratio is taken as ingredients, and an oxide film on the metal surface is removed firstly; then preparing NbMoTaW refractory high-entropy alloy cast ingots by adopting a vacuum arc melting method; and sequentially carrying out linear cutting, degreasing, polishing and cleaning on the high-entropy alloy cast ingot to obtain the NbMoTaW refractory high-entropy alloy matrix.
4. The method of preparing a yttrium-modified refractory high entropy silicide coating as claimed in claim 1, wherein: in the step (2), the NbMoTaW refractory high-entropy alloy matrix is buried in a crucible filled with the penetrating agent and compacted, so that the thickness of the penetrating agent covered on each surface of the alloy matrix is not less than 10mm.
5. The method of preparing a yttrium-modified refractory high entropy silicide coating as claimed in claim 1, wherein: in the step (2), silica sol and Al are adopted 2 O 3 The slurry prepared by the powder seals the crucible cover.
6. The method of preparing a yttrium-modified refractory high entropy silicide coating as recited in claim 5, wherein: al (Al) 2 O 3 Powder and silica sol in the mass-volume ratio of 1.5g:1mL of the mixture was mixed to prepare a slurry.
7. The method of preparing a yttrium-modified refractory high entropy silicide coating as claimed in claim 1, wherein: in the step (2), the inert atmosphere is an argon protection atmosphere.
8. The method of preparing a yttrium-modified refractory high entropy silicide coating as claimed in claim 1, wherein: in the step (2), the heating rate of the embedding siliconizing treatment is not higher than 10 ℃/min, and the cooling rate is not higher than 5 ℃/min.
9. The method of preparing a yttrium-modified refractory high entropy silicide coating as claimed in claim 2, wherein: in the step (2), the NbMoTaW refractory high-entropy alloy matrix is subjected to embedding siliconizing treatment in an inert atmosphere at 1000 ℃ for 12 hours.
10. The yttrium-modified refractory high-entropy silicide coating prepared by the preparation method as claimed in claim 1, wherein the yttrium-modified refractory high-entropy silicide coating has a chemical composition of [ NbMoTaW (Y)]Si 2 The method comprises the steps of carrying out a first treatment on the surface of the The content of Nb, mo, ta, W atom percent is a, the content of a is more than or equal to 5% and less than or equal to 10%, the content of b is Y atom percent, the content of b is more than or equal to 0.2% and less than or equal to 4.5%, the content of Si atom percent is c, and the content of c is more than or equal to 65% and less than or equal to 69%; the yttrium modified refractory high-entropy silicide coating has a hexagonal C40 crystal structure and is formed by in-situ reaction on the surface of the NbMoTaW refractory high-entropy alloy; the weight gain is less than 3.5mg/cm after 24 hours of high-temperature oxidation at 1450 DEG C 2 The mass ablation rate after 180s of ablation at 2100 ℃ is only 0.014-0.1mg/s, and the limit ablation temperature reaches 2200 ℃.
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