CN110257682A - A kind of preparation method of high entropy alloy material and its coating - Google Patents
A kind of preparation method of high entropy alloy material and its coating Download PDFInfo
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- CN110257682A CN110257682A CN201910604637.4A CN201910604637A CN110257682A CN 110257682 A CN110257682 A CN 110257682A CN 201910604637 A CN201910604637 A CN 201910604637A CN 110257682 A CN110257682 A CN 110257682A
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- 239000000956 alloy Substances 0.000 title claims abstract description 62
- 238000000576 coating method Methods 0.000 title claims abstract description 26
- 239000011248 coating agent Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 41
- 238000005253 cladding Methods 0.000 claims abstract description 39
- 239000000843 powder Substances 0.000 claims abstract description 24
- 238000002844 melting Methods 0.000 claims abstract description 18
- 230000008018 melting Effects 0.000 claims abstract description 18
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 15
- 239000011159 matrix material Substances 0.000 claims abstract description 15
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 15
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 15
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 15
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000005498 polishing Methods 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000004372 laser cladding Methods 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 8
- 238000002156 mixing Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 41
- 230000003647 oxidation Effects 0.000 description 7
- 229910001069 Ti alloy Inorganic materials 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 230000001590 oxidative effect Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 3
- 230000008520 organization Effects 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 244000137852 Petrea volubilis Species 0.000 description 2
- 230000003026 anti-oxygenic effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010288 cold spraying Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
-
- 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
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
- C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
- C23C24/106—Coating with metal alloys or metal elements only
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
The present invention discloses the preparation method of a kind of high entropy alloy material and its coating, belongs to laser melting and coating technique field.AlNbMoVCr high entropy alloy material of the present invention is made of Al, Nb, Mo, V and Cr metal powder, and wherein the molar ratio of Al, Nb, Mo, V and Cr are 1.5:1:1:1:1.Coating the preparation method comprises the following steps: Al, Nb, Mo, V and Cr metal powder are obtained AlNbMoVCr high-entropy alloy powder after mixing；AlNbMoVCr high-entropy alloy powder is preset at pretreatment matrix surface and forms preformed layer, processes to obtain high-entropy alloy cladding layer by laser melting coating after dry.The cladding layer that laser melting coating obtains in the present invention has good macro morphology, and coating and matrix reach good metallurgical bonding and have the characteristics that high rigidity and high pyro-oxidation resistance.
Description
Technical field
The preparation method of a kind of high entropy alloy material of the present invention and its coating, belongs to the Laser Surface Modification Technology of titanium alloy
Field.
Background technique
Since specific strength is high, specific modulus is high, biocompatibility is preferable and has the characteristics that preferable corrosion resistance, titanium is closed
Gold is widely used in the fields such as space flight and aviation, ocean development, health care, machine-building and derived energy chemical, light at present
There is more excellent comprehensive performance in matter high-strength material.But its disadvantage is also more obvious, use reach 600 DEG C and its with
When upper, titanium alloy material can fail because vigorous oxidation occurs.
And for improving titanium alloy high-temperature antioxygenic property, currently used method has surface modified.It mainly has: ion
Injection method, spray coating method (cold spraying, thermal spraying, plasma spraying), vapour deposition process, coating process (hot dip, plating, chemical plating),
Laser cladding etc..Above method is all mainly to prepare high-temperature oxidation resistant layer in titanium alloy surface, with obstruct titanium alloy substrate with
The contact of oxidizing atmosphere and increase titanium alloy aoxidize resistance to improve its antioxygenic property.And with other several surface modification sides
Method is compared, laser cladding have preparation efficiency high (the high rate of heat addition and high cooldown rate), matrix heat affected area be small, coating with
The advantages that substrate combinating strength is high, coating layer thickness is adjustable, cladding layer material selectable range is wide.
Different from traditional material based on a kind of element, supplemented by oligo-element, high-entropy alloy is current newly-developed
Multi-principal elements alloy.In general, high-entropy alloy pivot number n >=5, and every kind of metal element content is between 5-35%.This element
Content is according to equal atomic ratios or connects novel alloy made of near atomic ratio configuration, since element can be enhanced in its high entropy
Between dissolve each other inhibit it is complicated mutually and the generation of a large amount of intermetallic compounds；And the performance of high-entropy alloy is by a variety of pivots
Element collective effect determines.
Summary of the invention
The purpose of the present invention is to provide a kind of novel high entropy alloy materials, are made of Al, Nb, Mo, V, Cr metal powder,
Wherein the molar ratio of Al, Nb, Mo, V and Cr are 1.5:1:1:1:1, and each component powders partial size is 47 μm ~ 88 μm, each component
Purity is all larger than equal to 99.9%.
Another object of the present invention is to provide the high entropy alloy materials to be used to prepare coating process, passes through preset high entropy
Alloy material is in matrix surface, then makes high entropy alloy material and matrix surface via laser melting coating while melting, and quickly solidify
Low at dilution rate, and matrix is at metallurgical bonding and high-entropy alloy pivot diffusivity is low, the weaker high entropy alloy coating of segregation, specifically
Steps are as follows:
(1) removing oxide layer is removed into substrate polishing, is then cleaned by ultrasonic with alcohol clean；
(2) Al, Nb, Mo, V and Cr metal powder are uniformly mixed and carry out vacuum sphere mill (2h or more) and obtain AlNbMoVCr high
Entropy alloy powder, powder diameter are 170 ~ 320 mesh；
(3) by the AlNbMoVCr high-entropy alloy powder of step (2) be preset at pretreatment matrix surface formed preformed layer (with a thickness of
0.5 ~ 1.2mm), it is then dried, then obtain high-entropy alloy cladding layer through laser melting coating.
Pretreating substrates are TC4(Ti6-Al4-V in step (1) of the present invention) or industrial pure titanium TA2.
Dry condition in step (3) of the present invention are as follows: constant temperature handles 6 ~ 10h at being 80 ~ 100 DEG C in temperature.
In step (3) of the present invention in laser cladding process: laser power be 3500 ~ 4000W, scanning speed be 300 ~
500mm/min, spot diameter are 3.0 ~ 5.0mm, and defocusing amount is 15 ~ 30mm, and protective gas is argon gas, and gas flow is 6 ~ 10L/
min 。
Step (3) the of the present invention preformed layer with a thickness of 0.5 ~ 1.2mm.
Beneficial effects of the present invention:
(1) present invention in AlNbMoVCr high entropy alloy material metallurgical bonding is reached by laser melting coating and matrix, make matrix and
The bond strength of cladding layer has obtained greatly improving, and matrix thermal deformation is small, and dilution rate is low, and parts scrap rate is relatively low.
(2) the AlNbMoVCr high entropy alloy material in the present invention is tissue via in the cladding layer formed after laser melting coating
The uniform dendrite of structure, and cladding layer has high rigidity and excellent high-temperature oxidation resistance.
(3) cladding of the AlNbMoVCr high entropy alloy material in the present invention on different substrate materials by being obtained after laser melting coating
Layer all has high rigidity and excellent high-temperature oxidation resistance.
Detailed description of the invention
Fig. 1 is high-entropy alloy cladding organization chart in embodiment 1；
Fig. 2 is high-entropy alloy cladding organization chart in embodiment 1；
Fig. 3 is high-entropy alloy cladding layer XRD spectra in embodiment 1；
Fig. 4 is that high-entropy alloy cladding layer hardness compares figure in embodiment 1；
High-entropy alloy cladding layer oxidizing dynamics curve compares figure in the position Fig. 5 embodiment 1.
Specific embodiment
Invention is further described in detail With reference to embodiment, but protection scope of the present invention and unlimited
In the content.
Embodiment 1
A kind of AlNbMoVCr high entropy alloy material, be made of Al, Nb, Mo, V, Cr metal powder, and wherein Al, Nb, Mo, V, Cr rub
That ratio are as follows: 1.5:1:1:1:1.
The preparation method of AlNbMoVCr high entropy alloy material cladding layer in this example, the specific steps are as follows:
(1) removing oxide layer is removed into substrate TC4 polishing, is then cleaned by ultrasonic with alcohol clean.
(2) load weighted Al, Nb, Mo, V and Cr metal powder is uniformly mixed and carry out vacuum sphere mill 2h it is derived above
AlNbMoVCr high-entropy alloy powder.
(3) the AlNbMoVCr high-entropy alloy powder of step (2) is preset at the pretreatment surface matrix TC4 and forms preformed layer,
It is subsequently placed in vacuum oven, constant temperature handles 10h at being 80 DEG C in temperature, then obtains high-entropy alloy cladding through laser melting coating
Layer, wherein the laser power of laser melting coating is 3500W, scanning speed 500mm/min, spot diameter 5.0mm, and defocusing amount is
30mm, protective gas are argon gas, gas flow 10L/min.
High-entropy alloy cladding layer is polishing to metallographic requirement with high power sand paper after this example laser melting coating, is clapped with SEM
Observation is taken the photograph, it is as shown in Figure 1 and Figure 2 to obtain organization chart, from Fig. 1, Fig. 2 it is found that cladding layer and matrix are well combined, and cladding layer group
Densification is knitted, without obvious hole defect.
X-ray diffraction is carried out to cladding layer using X-ray diffractometer (XRD), cladding layer diffracting spectrum is obtained, such as Fig. 3 institute
Show, by XRD spectra it is found that can obtain single BCC phase by laser melting coating, cladding layer is the conjunction of high entropy after illustrating laser melting coating
Gold.
Using the microhardness of microhardness tester measurement high-entropy alloy cladding layer, at clad layer surface different distance
It takes and a little measures, and be compared with AlNbMoV high-entropy alloy cladding layer, AlNbMoVTi high-entropy alloy cladding layer, as a result such as
Shown in Fig. 4, as can be seen from Figure 4, AlNbMoVCr high-entropy alloy cladding layer hardness compared with other two kinds of high-entropy alloy cladding layers has
It significantly improves.
Using the high-temperature oxidation resistance of tube type resistance furnace measurement AlNbMoVCr high-entropy alloy cladding layer, test temperature 800
DEG C, testing time 120h obtains oxidizing dynamics curve, and with AlNbMoV high-entropy alloy cladding layer and AlNbMoVTi high
The oxidizing dynamics curve of entropy alloy cladding layer is compared to obtain Fig. 5, as seen from Figure 5 compared with substrate TC4,
The high-temperature oxidation resistance of AlNbMoVCr high-entropy alloy cladding layer is close with AlNbMoVTi high-entropy alloy cladding layer, but with
AlNbMoV high-entropy alloy cladding layer is compared to being significantly improved, and compared with substrate TC4, AlNbMoVCr high-entropy alloy cladding layer is mentioned
It is 4.89 times high.
Embodiment 2
A kind of AlNbMoVCr high entropy alloy material, be made of Al, Nb, Mo, V, Cr metal powder, and wherein Al, Nb, Mo, V, Cr rub
That ratio are as follows: 1.5:1:1:1:1.
The preparation method of AlNbMoVCr high entropy alloy material cladding layer in this example, the specific steps are as follows:
(1) removing oxide layer is removed into the polishing of substrate industrial pure titanium TA2, is then cleaned by ultrasonic with alcohol clean.
(2) load weighted Al, Nb, Mo, V and Cr metal powder is uniformly mixed and carry out vacuum sphere mill 2h it is derived above
AlNbMoVCr high-entropy alloy powder.
(3) the AlNbMoVCr high-entropy alloy powder of step (2) is preset at pretreatment matrix industrial pure titanium TA2 surface shape
It at preformed layer, is subsequently placed in vacuum oven, constant temperature handles 6h at being 100 DEG C in temperature, then obtains high entropy through laser melting coating
Alloy cladding layer, wherein the laser power of laser melting coating be 4000W, scanning speed 300mm/min, spot diameter 3.0mm,
Defocusing amount is 30mm, and protective gas is argon gas, and gas flow is 6 ~ 10L/min.
High-entropy alloy cladding layer is polishing to metallographic requirement with high power sand paper after the present embodiment laser melting coating, is clapped with SEM
Observation is taken the photograph, finds to reach metallurgical bonding between cladding layer and matrix, bond strength is high and microstructure of surface cladding layer is fine and close, without obvious cavity
Defect；Single BCC phase is obtained in XRD material phase analysis, and performance all obtains in hardness test and high-temperature oxidation resistance test
Effectively promoted.
Claims (8)
1. a kind of high entropy alloy material, it is characterised in that: be made of Al, Nb, Mo, V, Cr metal powder, wherein Al, Nb, Mo, V
Molar ratio with Cr is 1.5:1:1:1:1.
2. high entropy alloy material according to claim 1, it is characterised in that: each component powders partial size is 47 μm ~ 88 μm.
3. high entropy alloy material according to claim 1, it is characterised in that: each compositional purity is all larger than equal to 99.9%.
4. high entropy alloy material described in claim 1 is used to prepare coating process, which is characterized in that specific step is as follows:
(1) removing oxide layer is removed into substrate polishing, is then cleaned by ultrasonic with alcohol clean；
(2) Al, Nb, Mo, V and Cr metal powder are uniformly mixed and carry out vacuum sphere and grind to obtain AlNbMoVCr high-entropy alloy powder
End, powder diameter are 170 ~ 320 mesh；
(3) by the AlNbMoVCr high-entropy alloy powder of step (2) be preset at pretreatment matrix surface formed preformed layer, then into
Row is dried, then obtains high-entropy alloy cladding layer through laser melting coating.
5. preparation method according to claim 4, it is characterised in that: step (1) pretreating substrates are TC4 or industrially pure titanium
TA2。
6. preparation method according to claim 4, it is characterised in that: dry condition in step (3) are as follows: temperature be 80 ~
Constant temperature handles 6 ~ 10h at 100 DEG C.
7. preparation method according to claim 4, it is characterised in that: in step (3) in laser cladding process: laser power is
3500 ~ 4000W, scanning speed are 300 ~ 500mm/min, and spot diameter is 3.0 ~ 5.0mm, and defocusing amount is 15 ~ 30mm, protect gas
Body is argon gas, and gas flow is 6 ~ 10L/min.
8. preparation method according to claim 4, it is characterised in that: step (3) preformed layer with a thickness of 0.5 ~ 1.2mm.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111139471A (en) * | 2020-02-10 | 2020-05-12 | 重庆理工大学 | Method for preparing superhard Zr on surface of zirconium alloyxMethod for CrCoFeNi high-entropy alloy coating |
| CN111318805A (en) * | 2020-02-14 | 2020-06-23 | 江苏大学 | Laser welding method for high-entropy alloy with preset powder |
| CN112226758A (en) * | 2020-09-17 | 2021-01-15 | 北京科技大学 | Wear-resistant anti-oxidation high-entropy alloy coating and preparation method thereof |
| US20220097133A1 (en) * | 2020-09-29 | 2022-03-31 | Kunming University Of Science And Technology | High entropy alloy powder for laser cladding and application method thereof |
| CN114717546A (en) * | 2020-12-21 | 2022-07-08 | 武汉苏泊尔炊具有限公司 | Cooking utensil and preparation method thereof |
| CN114807935A (en) * | 2022-03-31 | 2022-07-29 | 河北科技大学 | Magnesium alloy composite material and preparation method thereof |
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| CN115852361A (en) * | 2022-12-07 | 2023-03-28 | 哈尔滨工业大学 | Wear-resistant high-entropy alloy coating for material surface protection and preparation method thereof |
| CN116024480A (en) * | 2023-01-10 | 2023-04-28 | 昆明理工大学 | High-entropy alloy material and preparation method thereof |
| CN116121618A (en) * | 2023-01-10 | 2023-05-16 | 昆明理工大学 | Light high-entropy alloy coating and preparation method thereof |
| CN116200739A (en) * | 2023-03-03 | 2023-06-02 | 昆明理工大学 | In-situ autogenous Al 2 O 3 Reinforced high-entropy alloy coating and preparation method thereof |
| BE1030353B1 (en) * | 2022-03-17 | 2023-10-16 | Univ Kunming Science & Technology | HIGH-ENTROPY ALLOY MATERIAL AND METHOD FOR PRODUCING A COATING BY USING THE SAME |
| CN116970943A (en) * | 2023-08-10 | 2023-10-31 | 齐鲁工业大学(山东省科学院) | High-entropy alloy coating synergistically enhanced by double Laves phase elements and preparation method thereof |
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| CN111139471A (en) * | 2020-02-10 | 2020-05-12 | 重庆理工大学 | Method for preparing superhard Zr on surface of zirconium alloyxMethod for CrCoFeNi high-entropy alloy coating |
| CN111139471B (en) * | 2020-02-10 | 2021-11-12 | 重庆理工大学 | Method for preparing superhard Zr on surface of zirconium alloyxMethod for CrCoFeNi high-entropy alloy coating |
| CN111318805A (en) * | 2020-02-14 | 2020-06-23 | 江苏大学 | Laser welding method for high-entropy alloy with preset powder |
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| US20220097133A1 (en) * | 2020-09-29 | 2022-03-31 | Kunming University Of Science And Technology | High entropy alloy powder for laser cladding and application method thereof |
| US11850659B2 (en) * | 2020-09-29 | 2023-12-26 | Kunming University Of Science And Technology | High entropy alloy powder for laser cladding and application method thereof |
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| CN114807884A (en) * | 2021-01-18 | 2022-07-29 | 武汉苏泊尔炊具有限公司 | Preparation method of cooking appliance and cooking appliance |
| BE1030353B1 (en) * | 2022-03-17 | 2023-10-16 | Univ Kunming Science & Technology | HIGH-ENTROPY ALLOY MATERIAL AND METHOD FOR PRODUCING A COATING BY USING THE SAME |
| CN114807935B (en) * | 2022-03-31 | 2023-11-17 | 河北科技大学 | Magnesium alloy composite material and preparation method thereof |
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Application publication date: 20190920 |