CN113046690A - Mo-Si-B/TiN composite coating and preparation method thereof - Google Patents
Mo-Si-B/TiN composite coating and preparation method thereof Download PDFInfo
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- CN113046690A CN113046690A CN202110265206.7A CN202110265206A CN113046690A CN 113046690 A CN113046690 A CN 113046690A CN 202110265206 A CN202110265206 A CN 202110265206A CN 113046690 A CN113046690 A CN 113046690A
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- 229910008423 Si—B Inorganic materials 0.000 title claims abstract description 162
- 238000000576 coating method Methods 0.000 title claims abstract description 85
- 239000011248 coating agent Substances 0.000 title claims abstract description 84
- 239000002131 composite material Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title abstract description 22
- 238000009792 diffusion process Methods 0.000 claims abstract description 62
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000011159 matrix material Substances 0.000 claims abstract description 48
- 238000000034 method Methods 0.000 claims abstract description 22
- 230000008569 process Effects 0.000 claims abstract description 13
- 229910045601 alloy Inorganic materials 0.000 claims description 85
- 239000000956 alloy Substances 0.000 claims description 85
- 229910020010 Nb—Si Inorganic materials 0.000 claims description 33
- 239000000843 powder Substances 0.000 claims description 28
- 239000002994 raw material Substances 0.000 claims description 22
- 230000004888 barrier function Effects 0.000 claims description 19
- 239000000758 substrate Substances 0.000 claims description 19
- 238000002844 melting Methods 0.000 claims description 14
- 230000008018 melting Effects 0.000 claims description 14
- 230000015572 biosynthetic process Effects 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 238000000151 deposition Methods 0.000 claims description 12
- 238000005498 polishing Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000003786 synthesis reaction Methods 0.000 claims description 10
- 230000008021 deposition Effects 0.000 claims description 9
- 239000000126 substance Substances 0.000 claims description 9
- 238000005137 deposition process Methods 0.000 claims description 8
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 8
- 229910052681 coesite Inorganic materials 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 229910052682 stishovite Inorganic materials 0.000 claims description 7
- 229910052905 tridymite Inorganic materials 0.000 claims description 7
- 229910015503 Mo5Si3 Inorganic materials 0.000 claims description 6
- 229910020968 MoSi2 Inorganic materials 0.000 claims description 6
- 230000007480 spreading Effects 0.000 claims description 6
- 238000003892 spreading Methods 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910015425 Mo2B5 Inorganic materials 0.000 claims description 4
- 238000000137 annealing Methods 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 230000006698 induction Effects 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000004544 sputter deposition Methods 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 239000013077 target material Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 244000137852 Petrea volubilis Species 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 abstract description 36
- 238000007254 oxidation reaction Methods 0.000 abstract description 36
- 239000003963 antioxidant agent Substances 0.000 abstract description 8
- 230000003078 antioxidant effect Effects 0.000 abstract description 8
- 230000006872 improvement Effects 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 113
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 229910052593 corundum Inorganic materials 0.000 description 7
- 238000001878 scanning electron micrograph Methods 0.000 description 7
- 229910001845 yogo sapphire Inorganic materials 0.000 description 7
- 239000011247 coating layer Substances 0.000 description 5
- 238000002490 spark plasma sintering Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 229910001029 Hf alloy Inorganic materials 0.000 description 1
- 229910016006 MoSi Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/028—Physical treatment to alter the texture of the substrate surface, e.g. grinding, polishing
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
- B22F2007/042—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal characterised by the layer forming method
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- Optics & Photonics (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a Mo-Si-B/TiN composite coating and a preparation method thereof, wherein the Mo-Si-B/TiN composite coating consists of a TiN diffusion-resistant layer and a Mo-Si-B mixed layer, and the TiN diffusion-resistant layer can completely prevent the mutual diffusion of elements in the coating and a matrix in the preparation process; after being oxidized for 100 hours at the high temperature of 1200-1300 ℃, the weight is increased by 0.52mg/cm through oxidation3～0.78mg/cm3Forming crystalline SiO on the surface of the Mo-Si-B mixed layer2And a mixed layer of amorphous borosilicate for preventingThe Mo-Si-B mixed layer is further oxidized, and the TiN diffusion-resistant layer can effectively inhibit mutual diffusion between the Mo-Si-B mixed layer and the matrix in the oxidation process, so that enough antioxidant elements are ensured in the Mo-Si-B/TiN composite coating, and the improvement of the antioxidant life of the Mo-Si-B/TiN composite coating is facilitated.
Description
Technical Field
The invention relates to the technical field of ultrahigh-temperature alloy coating materials, in particular to a Mo-Si-B/TiN composite coating and a preparation method thereof.
Background
Nb-Si based alloys have the advantages of high melting point, low density, and high strength at high temperatures, which makes them potentially a new generation of structural materials for aircraft engines. However, the Nb-Si based alloy has poor oxidation resistance, which hinders its use. The oxidation resistance of the alloy can be improved to a certain extent by adding oxidation resistant elements such as Cr, Al, Ti, Hf and the like, but the mechanical properties such as fracture toughness, creep property and the like of the alloy can be sacrificed, so that the preparation of the protective coating with excellent oxidation resistance on the surface of the Nb-Si-based alloy is an effective method for improving the oxidation resistance of the Nb-Si-based alloy.
The Mo-Si-B alloy has excellent oxidation resistance and is expected to become an oxidation resistant coating material. The addition of B can lead the Mo-Si-B coating to form a compact glassy borosilicate layer with better fluidity and excellent oxidation resistance in the oxidation process. However, the existing research shows that the Mo-Si-B coating and the Nb-Si-based alloy are easy to generate serious interdiffusion, Si in the Mo-Si-B coating diffuses to a matrix, so that the Si content in the Mo-Si-B coating is reduced, and MoSi is reduced to a certain extent when the Si content is reduced2The phase degenerates into brittle phase (Mo) with poor oxidation resistance5Si3Phase), no more dense oxide film can be formed, and brittle compatibility is prone to crack formation, all of which accelerate Mo-Si-B coating failure. Therefore, to extend the life of Mo-Si-B coatings, it is highly desirable to inhibit interdiffusion between the Mo-Si-B coating and the substrate.
Disclosure of Invention
In view of the above, the invention provides a Mo-Si-B/TiN composite coating and a preparation method thereof, which are used for inhibiting mutual diffusion between a Mo-Si-B mixed layer and a matrix and prolonging the service life of the coating.
The invention provides a Mo-Si-B/TiN composite coating, which comprises the following components: a TiN diffusion-resistant layer and a Mo-Si-B mixed layer which are sequentially stacked on the Nb-Si base alloy substrate; wherein the content of the first and second substances,
the Mo-Si-B mixed layer comprises SiO2、MoSi2And Mo5Si3Three phases, further comprising MoB phase or Mo2B5And (4) phase(s).
In one possible implementation manner, in the Mo-Si-B/TiN composite coating provided by the invention, the Nb-Si-based alloy matrix is an Nb-16Si-22Ti-17Cr-2Al-2Hf matrix.
In a possible implementation manner, in the Mo-Si-B/TiN composite coating provided by the invention, the thickness of the TiN diffusion-resistant layer is 2-6 μm.
In one possible implementation manner, in the Mo-Si-B/TiN composite coating provided by the invention, the thickness of the Mo-Si-B mixed layer is 85-980 μm.
The invention also provides a preparation method of the Mo-Si-B/TiN composite coating, which comprises the following steps:
s1: taking Nb-Si-Ti-Cr-Al-Hf hexahydric alloy as a first synthetic raw material, sequentially carrying out non-consumable vacuum arc melting and induction melting on the first synthetic raw material to obtain an Nb-Si-based alloy ingot, annealing at 1250 ℃ for a preset time t, and cutting the Nb-Si-based alloy ingot into a wafer sample with the diameter of 8-12 mm and the thickness of 2-3 mm as a matrix; wherein, t is more than 0h and less than or equal to 60 h;
s2: selecting an alloy element with a nominal chemical component of Mo-nSi-mB as a second synthesis raw material, carrying out non-consumable vacuum arc melting on the second synthesis raw material to obtain a Mo-Si-B alloy ingot, mechanically crushing the Mo-Si-B alloy ingot to obtain Mo-Si-B alloy powder, and carrying out ball milling on the Mo-Si-B alloy powder by using a planetary ball mill to obtain Mo-Si-B alloy powder with the particle size of 2-4 mu m; wherein the value range of n is 52-62, and the value range of m is 5-15;
s3: sequentially polishing the substrate by using 60#, 150#, 400#, 800#, 1000# and 1500# water grinding sand paper, polishing the surface of the polished substrate by using a polishing machine, mounting the polished substrate on a fixture of a magnetron sputtering device, mounting a TiN target material, and ensuring that the vacuum degree before deposition is 2 multiplied by 10-4Pa, introducing 20sccmAr and 0 sccm-5 sccmN in the deposition process2Depositing to obtain a TiN layer, wherein the vacuum degree in the deposition process is 0.5Pa, the rotation speed of the matrix is 3 r/min-7 r/min, the sputtering power is 250W, and the deposition time is 6 h-40 h;
s4: uniformly spreading Mo-Si-B alloy powder with the mass of 0.23-0.40 g at the bottom of a graphite mould with the diameter of 10-14 mm, placing a matrix deposited with a TiN layer at the middle position above the Mo-Si-B alloy powder, filling a gap between the side surface of the matrix and the mould with the Mo-Si-B alloy powder with the mass of 0.15-0.40 g, uniformly spreading the Mo-Si-B alloy powder with the mass of 0.23-0.40 g above the matrix, performing discharge plasma sintering, heating to 1300-1350 ℃ from room temperature, wherein the heating process lasts for 15min, the pressure is 5MPa in the heating process, the temperature is kept for 5min at 1300-1350 ℃, the pressure is 40-50 MPa in the heat preservation process, cooling along with the furnace, and the range of the pressure P in the cooling process is 0MPa < P < 15 MPa.
In one possible implementation manner, in the preparation method of the Mo-Si-B/TiN composite coating provided by the invention, in step S1, the alloy element with the atomic percentage of Nb-16Si-22Ti-17Cr-2Al-2Hf is used as the first synthetic raw material.
In a possible implementation manner, in the preparation method of the Mo-Si-B/TiN composite coating provided by the invention, in step S2, an alloy element with the atomic percentage of Mo-62Si-5B is selected as a second synthesis raw material.
According to the Mo-Si-B/TiN composite coating and the preparation method thereof provided by the invention, the Mo-Si-B/TiN composite coating consists of the TiN diffusion-resistant layer and the Mo-Si-B mixed layer, the TiN diffusion-resistant layer is arranged between the Mo-Si-B mixed layer and the Nb-Si-based alloy matrix, and the TiN diffusion-resistant layer can completely prevent the mutual diffusion of elements in the coating and the matrix in the preparation process; after the Mo-Si-B/TiN composite coating is oxidized for 100 hours at the high temperature of 1200-1300 ℃, the oxidation weight is increased by 0.52mg/cm3～0.78mg/cm3Forming continuous and compact crystalline SiO on the surface of the Mo-Si-B mixed layer2And the amorphous borosilicate mixed layer can prevent the Mo-Si-B mixed layer from being further oxidized, and the TiN diffusion-resistant layer can effectively inhibit mutual diffusion between the Mo-Si-B mixed layer and a matrix in the oxidation process, so that enough antioxidant elements are ensured in the Mo-Si-B/TiN composite coating, and the Mo-Si-B/TiN composite coating is beneficial to prolonging the antioxidant life of the Mo-Si-B/TiN composite coating. The Mo-Si-B/TiN composite coating is prepared on the Nb-Si-based alloy substrate by adopting the process of combining the magnetron sputtering technology with the spark plasma sintering technology。
Drawings
FIG. 1 is a schematic structural diagram of a Mo-Si-B/TiN composite coating prepared according to the present invention;
FIG. 2 is a sectional SEM image of a prepared state of a conventional Mo-Si-B coating layer without a TiN diffusion barrier layer;
FIG. 3 is a cross-sectional SEM image of a prior Mo-Si-B coating after oxidation without preparing a TiN diffusion barrier layer;
FIG. 4 shows a conventional Al-bearing belt2O3A cross-sectional SEM image of a prepared state of a Mo-Si-B coating of the diffusion barrier layer;
FIG. 5 shows a conventional Al-bearing belt2O3A cross-sectional SEM image of the Mo-Si-B coating of the diffusion barrier layer after oxidation;
FIG. 6 is a schematic structural diagram of a Mo-Si-B/TiN composite coating provided by the invention after oxidation;
FIG. 7 is a surface SEM and cross-sectional SEM images of TiN diffusion barrier layers prepared on Nb-Si based alloy substrates in example 1 of the present invention;
FIG. 8 is a sectional SEM photograph of a Mo-Si-B/TiN composite coating layer prepared in example 1 of the invention;
FIG. 9 is a cross-sectional SEM image of the Mo-Si-B/TiN composite coating layer prepared in example 1 of the invention after oxidation;
FIG. 10 is a distribution diagram of the main elements of the Mo-Si-B/TiN composite coating layer prepared in the example 1 of the invention after oxidation.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only illustrative and are not intended to limit the present invention.
The invention provides a Mo-Si-B/TiN composite coating, as shown in figure 1, comprising: a TiN diffusion-resistant layer and a Mo-Si-B mixed layer which are sequentially stacked on the Nb-Si base alloy substrate; wherein the content of the first and second substances,
the Mo-Si-B mixed layer comprises SiO2、MoSi2And Mo5Si3Three phases, further including MoB phase or Mo2B5The phase, i.e. the Mo-Si-B mixed layer, comprising SiO2、MoSi2、Mo5Si3And MoB four phases, or the Mo-Si-B mixed layer comprises SiO2、MoSi2、Mo5Si3And Mo2B5And (4) four phases.
According to the Mo-Si-B/TiN composite coating provided by the invention, the TiN diffusion-resistant layer is added between the Nb-Si-based alloy matrix and the Mo-Si-B mixed layer, TiN still has chemical inertness and high melting point at high temperature, all elements are difficult to diffuse in TiN, and the thermal expansion coefficients of TiN, Nb-Si alloy and Mo-Si-B coating are similar, so that the combination of the TiN coating and the Nb-Si-based alloy matrix is facilitated, and the TiN coating can become an excellent diffusion-resistant layer. The TiN diffusion barrier completely prevented the formation of the interdiffusion region during the as-prepared process.
For the Mo-Si-B coating samples without TiN diffusion barrier, the preparation states are Mo-Si-B outer layer, (Mo, X')5Si3Layer, (Nb, X)5Si3Four layers of Nb-Si substrate, shown in FIG. 3, after oxidation, oxide layer, Mo-Si-B outer layer, (Mo, X')5Si3Layer, (Nb, X)5Si3Five layers of layers and Nb-Si matrix, both as prepared and after oxidation (Mo, X')5Si3Layer sum (Nb, X)5Si3Inter-diffusion regions of layers. For with Al2O3Mo-Si-B coating sample of diffusion barrier layer, as shown in FIG. 4, prepared as Mo-Si-B outer layer, Al2O3Three layers of Nb-Si substrate, shown in FIG. 5, after oxidation, are an oxide layer, an outer layer of Mo-Si-B, (Mo, X')5Si3Layer of Al2O3Layer, (Nb, X)5Si3Six layers of Nb-Si matrix, both as prepared and after oxidation (Mo, X')5Si3Layer sum (Nb, X)5Si3Inter-diffusion regions of layers. According to the Mo-Si-B/TiN composite coating provided by the invention, the TiN diffusion-resistant layer completely hinders the formation of the interdiffusion region in the preparation state (as shown in figure 1), and after the TiN diffusion-resistant layer is oxidized for 100 hours at the high temperature of 1200-1300 ℃, the diffusion of Si is effectively reduced, so that the interdiffusion region is not formed by (Mo, X')5Si3Layer sum (Nb, X)5Si3Layer two-layer compositionBut only (Nb, X)5Si3Layer one layer, as shown in FIG. 6, completely suppressed samples that had not been prepared with TiN diffusion barrier layer and had Al2O3(Mo, X') in Mo-Si-B coating sample of diffusion barrier layer5Si3Forming a layer; furthermore, a continuous and dense crystalline SiO is formed on the surface of the Mo-Si-B mixed layer2The amorphous borosilicate mixed layer can effectively prevent oxygen from diffusing to the Nb-Si-based alloy matrix, improve the oxidation resistance of the Nb-Si-based alloy matrix and increase the oxidation weight by 0.52mg/cm3～0.78mg/cm3And the oxidation resistance is excellent.
In the specific implementation, in the Mo-Si-B/TiN composite coating provided by the invention, the Nb-Si-based alloy matrix is preferably an Nb-16Si-22Ti-17Cr-2Al-2Hf matrix.
In the specific implementation, in the Mo-Si-B/TiN composite coating provided by the invention, the thickness of the TiN diffusion-resistant layer can be controlled within the range of 2-6 μm.
In the specific implementation, in the Mo-Si-B/TiN composite coating provided by the invention, the thickness of the Mo-Si-B mixed layer can be controlled within the range of 85-980 μm.
Based on the same inventive concept, the invention also provides a preparation method of the Mo-Si-B/TiN composite coating, which comprises the following steps:
s1: taking Nb-Si-Ti-Cr-Al-Hf hexahydric alloy as a first synthetic raw material, sequentially carrying out non-consumable vacuum arc melting and induction melting on the first synthetic raw material to obtain an Nb-Si-based alloy ingot, annealing at 1250 ℃ for a preset time t, and cutting the Nb-Si-based alloy ingot into a wafer sample with the diameter of 8-12 mm and the thickness of 2-3 mm as a matrix; wherein, t is more than 0h and less than or equal to 60 h;
s2: selecting an alloy element with a nominal chemical component of Mo-nSi-mB as a second synthesis raw material, carrying out non-consumable vacuum arc melting on the second synthesis raw material to obtain a Mo-Si-B alloy ingot, mechanically crushing the Mo-Si-B alloy ingot to obtain Mo-Si-B alloy powder, and carrying out ball milling on the Mo-Si-B alloy powder by using a planetary ball mill to obtain Mo-Si-B alloy powder with the particle size of 2-4 mu m; wherein the value range of n is 52-62, and the value range of m is 5-15;
s3: in turn usingPolishing the base body with water mill sandpaper of 60#, 150#, 400#, 800#, 1000# and 1500#, polishing the surface of the polished base body with a polishing machine, mounting the polished base body on a fixture of a magnetron sputtering device, mounting TiN target material, and ensuring that the vacuum degree before deposition is 2 multiplied by 10-4Pa, introducing 20sccmAr and 0 sccm-5 sccmN in the deposition process2Depositing to obtain a TiN layer, wherein the vacuum degree in the deposition process is 0.5Pa, the rotation speed of the matrix is 3 r/min-7 r/min, the sputtering power is 250W, and the deposition time is 6 h-40 h;
s4: uniformly spreading Mo-Si-B alloy powder with the mass of 0.23-0.40 g at the bottom of a graphite mould with the diameter of 10-14 mm, placing a matrix deposited with a TiN layer at the middle position above the Mo-Si-B alloy powder, filling a gap between the side surface of the matrix and the mould with the Mo-Si-B alloy powder with the mass of 0.15-0.40 g, uniformly spreading the Mo-Si-B alloy powder with the mass of 0.23-0.40 g above the matrix, performing discharge plasma sintering, heating to 1300-1350 ℃ from room temperature, wherein the heating process lasts for 15min, the pressure is 5MPa in the heating process, the temperature is kept for 5min at 1300-1350 ℃, the pressure is 40-50 MPa in the heat preservation process, cooling along with the furnace, and the range of the pressure P in the cooling process is 0MPa < P < 15 MPa.
In concrete practice, in the step S1 of the method for preparing the Mo-Si-B/TiN composite coating provided by the invention, the alloy element with the atomic percentage of Nb-16Si-22Ti-17Cr-2Al-2Hf is preferably used as the first synthetic raw material. Of course, other suitable atomic percentages of Nb-Si-Ti-Cr-Al-Hf alloy elements may be selected as the first synthetic raw material, and are not limited herein.
In concrete practice, in the step S2 of the method for preparing the Mo-Si-B/TiN composite coating provided by the invention, the alloy element with the Mo-62Si-5B atom percentage is preferably used as the second synthetic raw material. Of course, other suitable atomic percentages of the Mo-Si-B alloy elements can be selected as the second synthesis raw material, and are not limited herein.
The specific implementation of the preparation method of the Mo-Si-B/TiN composite coating provided by the invention is described in detail by a specific example.
Example 1:
first, the preparation of the matrix.
Selecting alloy elements with nominal chemical components of Nb-16Si-22Ti-17Cr-2Al-2Hf (atomic percentage, at%) as first synthesis raw materials, sequentially using non-consumable vacuum arc melting and induction melting to obtain Nb-Si-based alloy ingots, annealing at 1250 ℃ for 50 hours, and cutting the alloy ingots into wafer samples with the diameters of 12mm and the thicknesses of 2mm as substrates.
The second step is that: and preparing a Mo-Si-B mixed layer material.
Selecting an alloy element with nominal chemical components of Mo-62Si-5B (atomic percentage, at%) as a second synthesis raw material, performing non-consumable vacuum arc melting to obtain a Mo-Si-B alloy ingot, performing mechanical crushing on the Mo-Si-B alloy ingot to obtain Mo-Si-B alloy powder, and performing ball milling on the Mo-Si-B alloy powder by using a planetary ball mill to obtain the Mo-Si-B alloy powder with the particle size of 2-4 mu m.
And thirdly, preparing the TiN diffusion-resistant layer.
And (3) sequentially polishing the matrix prepared in the first step by using 60#, 150#, 400#, 800#, 1000# and 1500# water-mill sandpaper, polishing the surface by using a polishing machine, mounting the treated matrix on a clamp of magnetron sputtering equipment, and performing magnetron sputtering to prepare the TiN diffusion-resistant layer by using TiN targets as the deposition targets.
Magnetron sputtering parameters were as follows: the backing vacuum (i.e. the vacuum before deposition) was 2X 10-4Pa, introducing 20sccmAr and 1sccmN in the deposition process2The vacuum degree in the deposition process is 0.5Pa, the autorotation speed of the matrix is 5r/min, the sputtering power is 250W, and the deposition time is 30 h.
The surface SEM and the cross-sectional SEM of the TiN diffusion barrier layer prepared on the Nb-Si based alloy substrate are respectively shown in (a) and (b) of fig. 7, and the TiN diffusion barrier layer is dense columnar crystal, free of pores and cracks. For with Al2O3Mo-Si-B coating sample of diffusion barrier layer, Al2O3The diffusion barrier is porous.
The fourth step: and (4) performing spark plasma sintering to obtain the composite coating.
0.29g of Mo-Si-B alloy powder is uniformly spread at the bottom of a graphite mold with the diameter of 14mm, a matrix with a TiN diffusion-resistant layer is placed at the middle position above the Mo-Si-B alloy powder, a gap between the side surface of the matrix and the mold is filled with 0.4g of Mo-Si-B alloy powder, 0.29g of Mo-Si-B alloy powder is uniformly spread above the matrix, and then spark plasma sintering is carried out.
The spark plasma sintering parameters were as follows: heating from room temperature to 1350 deg.C, maintaining the temperature at 1350 deg.C under 5MPa for 15min, maintaining the temperature at 1350 deg.C under 50MPa for 5min, and cooling with furnace under 10 MPa.
The SEM image of the cross section of the prepared Mo-Si-B/TiN composite coating is shown in FIG. 8, and as can be seen from FIG. 8, no interdiffusion region exists between the prepared Mo-Si-B mixed layer and the matrix, and the TiN diffusion-resistant layer completely hinders the diffusion of Si element in the Mo-Si-B mixed layer to the matrix in the preparation process.
SEM analysis of the Mo-Si-B/TiN composite coating prepared by the method in example 1 of the invention shows that the Mo-Si-B mixed layer has the thickness of 980 mu m and comprises MoSi2、Mo5Si3、SiO2And the thickness of the TiN diffusion-resistant layer is 5.4 mu m, no interdiffusion region exists between the Mo-Si-B mixed layer and the matrix, and a coating preparation state without the TiN diffusion-resistant layer has a interdiffusion region of 4 mu m, which shows that the interdiffusion phenomenon of the Mo-Si-B/TiN composite coating prepared by the method in the embodiment 1 of the invention in the preparation process is effectively inhibited, so that enough antioxidant elements are ensured in the Mo-Si-B/TiN composite coating, and the improvement of the antioxidant life of the Mo-Si-B/TiN composite coating is facilitated.
After the Mo-Si-B/TiN composite coating prepared by the method in the embodiment 1 of the invention is oxidized for 100 hours at the high temperature of 1200-1300 ℃, the oxidation weight is increased by 0.78mg/cm3The surface of the Mo-Si-B mixed layer forms continuous compact crystalline state SiO2And an amorphous borosilicate mixed layer for preventing further oxidation of the Mo-Si-B mixed layer, and SEM observation of the cross section after oxidation, as shown in FIG. 9, the composite coating layer is formed by an oxide layer, a Mo-Si-B mixed layer, a TiN diffusion-resistant layer and (Nb, X)5Si3Layer four layer composition, Mo-Si-B coating samples not appearing like unpainted TiN diffusion barrier and with Al2O3SiO Dispersion in Mo-Si-B coating samples of diffusion barrier layers2Facies (Mo, X')5Si3Layer, diffusion of elements during oxidation only results in (Nb, X')5Si3The presence of layers, the interdiffusion zone consisting of (Nb, X) only5Si3Layer by layer. FIG. 10 is a diagram showing the distribution of the main elements of the Mo-Si-B/TiN composite coating after oxidation, and the TiN diffusion-resistant layer completely inhibits the diffusion of the Mo element in the Mo-Si-B mixed layer to the substrate and the diffusion of the Nb, Ti and Cr elements in the substrate to the Mo-Si-B mixed layer.
The thickness of the interdiffusion region formed after the oxidation of the Mo-Si-B/TiN composite coating in the embodiment 1 of the invention is 11 μm, which is much smaller than the thickness of the interdiffusion region formed after the oxidation of the Mo-Si-B coating without preparing TiN diffusion-resistant layer in the figure 3, which is 26 μm, and the Mo-Si-B coating with Al in the figure 52O3The thickness of the Mo-Si-B coating of the diffusion barrier layer in the interdiffusion region after oxidation was 17 μm, which indicates that the TiN diffusion barrier layer effectively inhibits interdiffusion of the Mo-Si-B mixed layer and the elements in the matrix.
According to the Mo-Si-B/TiN composite coating and the preparation method thereof provided by the invention, the Mo-Si-B/TiN composite coating consists of the TiN diffusion-resistant layer and the Mo-Si-B mixed layer, the TiN diffusion-resistant layer is arranged between the Mo-Si-B mixed layer and the Nb-Si-based alloy matrix, and the TiN diffusion-resistant layer can completely prevent the mutual diffusion of elements in the Mo-Si-B mixed layer and the matrix in the preparation process; after the Mo-Si-B/TiN composite coating is oxidized for 100 hours at the high temperature of 1200-1300 ℃, the oxidation weight is increased by 0.52mg/cm3～0.78mg/cm3Forming continuous and compact crystalline SiO on the surface of the Mo-Si-B mixed layer2And the amorphous borosilicate mixed layer can prevent the Mo-Si-B mixed layer from being further oxidized, and the TiN diffusion-resistant layer can effectively inhibit mutual diffusion between the Mo-Si-B mixed layer and a matrix in the oxidation process, so that enough antioxidant elements are ensured in the Mo-Si-B/TiN composite coating, and the Mo-Si-B/TiN composite coating is beneficial to prolonging the antioxidant life of the Mo-Si-B/TiN composite coating. The Mo-Si-B/TiN composite coating is prepared on the Nb-Si-based alloy substrate by adopting a process of combining a magnetron sputtering technology and a spark plasma sintering technology.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (7)
1. A Mo-Si-B/TiN composite coating, which is characterized by comprising: a TiN diffusion-resistant layer and a Mo-Si-B mixed layer which are sequentially stacked on the Nb-Si base alloy substrate; wherein the content of the first and second substances,
the Mo-Si-B mixed layer comprises SiO2、MoSi2And Mo5Si3Three phases, further including MoB phase or Mo2B5And (4) phase(s).
2. The Mo-Si-B/TiN composite coating according to claim 1, wherein the Nb-Si based alloy matrix is a Nb-16Si-22Ti-17Cr-2Al-2Hf matrix.
3. The Mo-Si-B/TiN composite coating of claim 1, wherein the TiN diffusion barrier layer has a thickness of 2 μ ι η to 6 μ ι η.
4. The Mo-Si-B/TiN composite coating according to claim 1, wherein the thickness of the Mo-Si-B mixed layer is 85 μm to 980 μm.
5. A method for preparing the Mo-Si-B/TiN composite coating according to any one of claims 1 to 4, characterized by comprising the following steps:
s1: taking Nb-Si-Ti-Cr-Al-Hf hexahydric alloy as a first synthetic raw material, sequentially carrying out non-consumable vacuum arc melting and induction melting on the first synthetic raw material to obtain an Nb-Si-based alloy ingot, annealing at 1250 ℃ for a preset time t, and cutting the Nb-Si-based alloy ingot into a wafer sample with the diameter of 8-12 mm and the thickness of 2-3 mm as a matrix; wherein, t is more than 0h and less than or equal to 60 h;
s2: selecting an alloy element with a nominal chemical component of Mo-nSi-mB as a second synthesis raw material, carrying out non-consumable vacuum arc melting on the second synthesis raw material to obtain a Mo-Si-B alloy ingot, mechanically crushing the Mo-Si-B alloy ingot to obtain Mo-Si-B alloy powder, and carrying out ball milling on the Mo-Si-B alloy powder by using a planetary ball mill to obtain Mo-Si-B alloy powder with the particle size of 2-4 mu m; wherein the value range of n is 52-62, and the value range of m is 5-15;
s3: sequentially polishing the substrate by using 60#, 150#, 400#, 800#, 1000# and 1500# water grinding sand paper, polishing the surface of the polished substrate by using a polishing machine, mounting the polished substrate on a fixture of a magnetron sputtering device, mounting a TiN target material, and ensuring that the vacuum degree before deposition is 2 multiplied by 10-4Pa, introducing 20sccmAr and 0 sccm-5 sccmN in the deposition process2Depositing to obtain a TiN layer, wherein the vacuum degree in the deposition process is 0.5Pa, the rotation speed of the matrix is 3 r/min-7 r/min, the sputtering power is 250W, and the deposition time is 6 h-40 h;
s4: uniformly spreading Mo-Si-B alloy powder with the mass of 0.23-0.40 g at the bottom of a graphite mould with the diameter of 10-14 mm, placing a matrix deposited with a TiN layer at the middle position above the Mo-Si-B alloy powder, filling a gap between the side surface of the matrix and the mould with the Mo-Si-B alloy powder with the mass of 0.15-0.40 g, uniformly spreading the Mo-Si-B alloy powder with the mass of 0.23-0.40 g above the matrix, performing discharge plasma sintering, heating to 1300-1350 ℃ from room temperature, wherein the heating process lasts for 15min, the pressure is 5MPa in the heating process, the temperature is kept for 5min at 1300-1350 ℃, the pressure is 40-50 MPa in the heat preservation process, cooling along with the furnace, and the range of the pressure P in the cooling process is 0MPa < P < 15 MPa.
6. The method of preparing a Mo-Si-B/TiN composite coating according to claim 5, wherein in step S1, the alloy element with the atomic percentage of Nb-16Si-22Ti-17Cr-2Al-2Hf is used as the first synthetic raw material.
7. The method of preparing a Mo-Si-B/TiN composite coating according to claim 5, wherein in step S2, the second synthetic raw material is selected as the alloy element with the atomic percentage of Mo-62 Si-5B.
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