CN106319260B - A kind of high-melting-point high-entropy alloy and its coating production - Google Patents
A kind of high-melting-point high-entropy alloy and its coating production Download PDFInfo
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- CN106319260B CN106319260B CN201610840448.3A CN201610840448A CN106319260B CN 106319260 B CN106319260 B CN 106319260B CN 201610840448 A CN201610840448 A CN 201610840448A CN 106319260 B CN106319260 B CN 106319260B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- 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
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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
- 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
Abstract
The present invention relates to new alloy material technical field there is provided a kind of high-melting-point high-entropy alloy, constitute as CoCrMoNbTi；The atomic molar ratio of said components is：(0.8~1.1):(0.8~1.1):(0.8~1.1):(0.8~1.1):(0~1.1)；Selected Co, Cr, Mo, Nb and Ti material purity is not less than 99%；Additionally provide the preparation method of a kind of above-mentioned alloy block material and laser cladding coating.Beneficial effects of the present invention are：The high-entropy alloy has simple body-centered cubic structure, is provided simultaneously with very high intensity and heat endurance, and excellent in mechanical performance can meet the higher performance requirement to material, the particularly requirement of high-temperature behavior in modern industry；The preparation of the high-entropy alloy coating, promotes and has expanded the application field of high-entropy alloy；Preparation method is simple, easy, possess wide application prospect.
Description
Technical field
The present invention relates to technical field of alloy material, more particularly to a kind of high-melting-point high-entropy alloy and its coating preparation side
Method.
Background technology
The proposition of high-entropy alloy theory, is that the research of alloy material opens new approach.High-entropy alloy generally comprises 5 kinds
Or more than 5 kinds of constituent element, and every kind of element atomic ratio between 5%-35%.Due to high entropic effect, rubbed containing atom is waited
You ratio or closely atomic molar than multicomponent alloy do not form baroque weld metal zone brittle intermetallic thing phase, on the contrary can
Simple solid solution structure is formed, assigns alloy excellent combination property.Particularly pass through several high-melting-point alloys in recent years
The high-melting-point high-entropy alloy that organic assembling is designed and developed is significantly improved in associated high-temperature aspect of performance than conventional high-temperature alloy, should
With having a extensive future, one of focus branch studied as high-entropy alloy.
CN201510010329.0 discloses a kind of method of regulation and control AlCoCrFeNi high-entropy alloy tissues, in atmospheric environment
It is lower that AlCoCrFeNi high-entropy alloys are coated with covering, tissue morphology is changed by high undercooling rapid solidification, by obtaining
The big degree of supercooling of AlCoCrFeNi high-entropy alloys is with organization of regulation control pattern in experimentation.
CN201310161152.5 discloses a kind of preparation method of the coating of high-entropy alloy containing amorphous nano-crystalline, available for making
Standby combination property superior high-entropy alloy coating and block materials.
CN200810063807.4 discloses a kind of high-entropy alloy-base composite material and preparation method thereof, composite it is hard
The performances such as degree, intensity before being combined all than significantly improving.
All without reference to high-melting-point high-entropy alloy and its preparation in above-mentioned material.
The content of the invention
The purpose of the present invention is exactly to overcome the deficiencies in the prior art there is provided a kind of high-melting-point high-entropy alloy, using vacuum
Electric arc melting Technology design have developed the high-melting-point high-entropy alloy of CoCrMoNbTi systems, it is determined that the composition range of alloy and molten
Sweetening process, tests the institutional framework and correlated performance of alloy.It is prepared for simultaneously by laser melting and coating technique and plasma spray technology
High-melting-point high-entropy alloy coating, it is determined that preparation technology of coating and linked groups' performance, is that practical application has paved road.
A kind of high-melting-point high-entropy alloy of the present invention, is constituted as CoCrMoNbTi；The atomic molar ratio of said components is：Co:
Cr:Mo:Nb:Ti=(0.8~1.1):(0.8~1.1):(0.8~1.1):(0.8~1.1):(0~1.1).
Further, when preparing the high-melting-point high-entropy alloy, selected Co, Cr, Mo, Nb and Ti raw material are pure
Spend for 99%~99.99%.
Present invention also offers a kind of preparation method of above-mentioned high-melting-point high-entropy alloy block materials, comprise the following steps：
Step 1: Co, Cr, Mo, Nb, Ti raw material surface cleaning, remove oxide；
Step 2: Co, Cr, Mo, Nb, Ti are according to mol ratio (0.8~1.1):(0.8~1.1):(0.8~1.1):(0.8
~1.1):(0~1.1) proportioning is weighed；
Step 3: the raw material configured is placed in the water cooled copper mould in vacuum non-consumable tungsten electrode arc smelting furnace, to electricity
Air pressure is 0~6 × 10 in arc stove evacuation, electric arc furnaces-3Pa；Technical argon is then charged with electromagnetic oven, pressure reaches 0.4~
0.6 atmospheric pressure；
Step 4: in fusion process, after each alloy melting, electric arc retention time 30-60s will after alloy block is cooled down
It overturns, so repeatedly 3~5 times or more；After the uniform melting of alloy, taking-up produces the high-melting-point high-entropy alloy.
Present invention also offers a kind of preparation method of above-mentioned high-melting-point high-entropy alloy laser cladding coating, including following step
Suddenly：
Step 1: the powder of the high-melting-point high-entropy alloy is mixed in omnidirectional planetary ball mill, rotational speed of ball-mill
For 140-160r/min, the time is 14-16h, well mixed powder is placed on plain steel, pre-set thickness is 600-
800um；
Step 2: carrying out multiple tracks cladding with superpower laser, laser power is 2.3~2.7kW, and sweep speed is 300-
600mm/min, spot diameter is 3~4mm, and overlapping rate is 25%~40%, blanketing with inert gas during cladding.
Further, the rotational speed of ball-mill in step one is 150r/min, and the pre-set thickness of alloy powder is 700um.
Further, the inert gas in step 2 is Ar.
Beneficial effects of the present invention are：The high-entropy alloy has simple body-centered cubic structure, is provided simultaneously with very high strong
Degree and heat endurance, excellent in mechanical performance, can meet the higher performance requirement to material, particularly high-temperature behavior in modern industry
Requirement；The preparation of the high-entropy alloy coating, promotes and has expanded the application field of high-entropy alloy；Preparation method is simple, easy,
Possesses wide application prospect.
Brief description of the drawings
Fig. 1 show the X ray diffracting spectrum of CoCrMoNbTi high-entropy alloys in the embodiment of the present invention 1.
Fig. 2 show the ESEM back scattering photo of CoCrMoNbTi high-entropy alloys in embodiment 1.
Fig. 3 show the ESEM back scattering photo of CoCrMoNbTi high-entropy alloys coating interface in embodiment 2.
Embodiment
The specific embodiment of the invention is described in detail below in conjunction with specific accompanying drawing.It should be noted that in following embodiments
The combination of the technical characteristic or technical characteristic of description is not construed as isolated, and they can be mutually combined so as to reaching
To superior technique effect.In the accompanying drawing of following embodiments, the identical label that each accompanying drawing occurs represent identical feature or
Person's part, can be applied in not be the same as Example.
A kind of high-melting-point high-entropy alloy of the embodiment of the present invention, the composition of the high-melting-point high-entropy alloy is CoCrMoNbTi；
The atomic molar ratio of said components is：(0.8-1.1)：(0.8-1.1)：(0.8-1.1)：(0.8-1.1)：(0-1.1).
When preparing the high-melting-point high-entropy alloy, selected Co, Cr, Mo, Nb and Ti material purity is not low
In 99%, preferably 99%~99.99%.
A kind of preparation method of above-mentioned high-melting-point high-entropy alloy block materials, comprises the following steps：
Step 1: Co, Cr, Mo, Nb, Ti raw material surface cleaning, remove oxide；
Step 2: Co, Cr, Mo, Nb, Ti are according to mol ratio (0.8~1.1):(0.8~1.1):(0.8~1.1):(0.8
~1.1):(0~1.1) proportioning is weighed；
Step 3: the raw material configured is placed in the water cooled copper mould in vacuum non-consumable tungsten electrode arc smelting furnace, to electricity
Air pressure is 0~6 × 10 in arc stove evacuation, electric arc furnaces-3Pa；Technical argon is then charged with electromagnetic oven, pressure reaches 0.4~
0.6 atmospheric pressure；
Step 4: in fusion process, after each alloy melting, electric arc retention time 30-60s will after alloy block is cooled down
It overturns, so repeatedly 3~5 times or more；After the uniform melting of alloy, taking-up produces the high-melting-point high-entropy alloy.
A kind of preparation method of above-mentioned high-melting-point high-entropy alloy laser cladding coating, comprises the following steps：
Step 1: the powder of the high-melting-point high-entropy alloy is mixed in omnidirectional planetary ball mill, rotational speed of ball-mill
For 140-160r/min, the time is 14-16h, well mixed powder is placed on plain steel, pre-set thickness is 600-
800um；
Step 2: carrying out multiple tracks cladding with superpower laser, laser power is 2.3~2.7kW, and sweep speed is 300-
600mm/min, spot diameter is 3~4mm, and overlapping rate is 25%~40%, blanketing with inert gas during cladding.
It is preferred that, the rotational speed of ball-mill in step one is 150r/min, and the pre-set thickness of alloy powder is 700um；Step 2
In inert gas be Ar.
Embodiment 1
The present embodiment high-melting-point high-entropy alloy preparation process is as follows：
Raw material prepares：By Co, Cr, Mo, Nb and Ti block material mechanically scale removal, according to molar ratio
Co:Cr:Mo:Nb:Ti=1:1:1:1:1:0.4 carries out accurate weighing proportioning, is cleaned up in alcohol with ultrasonic oscillation；
Alloy melting：Using vacuum non-consumable arc furnace molten alloy；The raw material mixed is placed in vacuum arc melting
In water cooled copper mould in stove, to electric arc stove evacuation, after vacuum reaches 5 × 10-3Pa, technical argon is filled with until in stove
Pressure reaches half of atmospheric pressure；After each molten alloy fusing, electric arc retention time 45s；Again by crucible after alloy is cooled down
Alloy turn-over continue melting, be so repeated 4 times, with ensure alloy be well mixed.
The institutional framework of alloy and performance evaluation are as follows：
X-ray diffraction (XRD) result：Sample is cut into after 10 × 10 × 10mm squares using wire cutting, by sample table
Carefully ground with 150#, 400#, 800#, 1200#, 1500# and 2000# abrasive paper for metallograph successively in face.Use X-ray diffractometer pair
Metallographic sample progress crystal species analysis, scanning step 0.01/s, the θ of scanning angle 2 scope is from 10 ° to 90 °.Test result is as schemed
Shown in 1.
ESEM (SEM) result：Sample is cut into after 10 × 10 × 10mm squares with wire cutting, through 150#, 400#,
800#, 1200#, 1500# and 2000# abrasive paper for metallograph are carefully ground, and after mechanical polishing, use ESEM back scattering mould
Formula observes alloy structure.Test result is as shown in Figure 2.
Fabric analysis finds that the alloy is made up of simple BCC solid solutions, as shown in Figure 1；Alloy structure is by typically setting
Dendrite and interdendritic structure composition, as shown in Figure 2.It can be seen that, alloy structure is in typical high-entropy alloy tissue characteristic.
Microhardness：The microhardness of alloy is determined using 401MVD digital displays micro Vickers, before hardness test,
Alloy sample is carefully ground using the abrasive paper for metallograph through 150#, 400#, 800#, 1200#, 1500# and 2000#, and carries out machine
Tool is polished.The load loaded during experiment is 500g, keeps 15s.Each sample 7 points of random test, are removed minimum and maximum
After data, the average value of remaining 5 data points is taken as the microhardness value of the alloy, as shown in table 1.
The microhardness of high-melting-point high-entropy alloy in the embodiment 1 of table 1
With the room temperature Compressive Mechanical Properties of the Material Testing Machine beta alloys of MTS 809, specimen size is φ 3mm × 6mm, should
Variable Rate is 1 × 10-4s-1, alloy is with very high fracture strength, up to 1780MPa；Cash and break for fragility in compression process
Split.Hot compression test is carried out on Gleeble-1500 hot modeling test machines, deformation temperature is 600~1300 DEG C, strain rate
For 0.001~0.1s-1, deflection is 30%~60%.Sample is heated to 8~12 DEG C/s speed to carry out after preset temperature
Compression, can be obtained in the case where 1200 DEG C are high temperature compressed, and alloy compression strength is up to 680MPa, and compressive plastic deformation amount is more than 35%,
With excellent elevated temperature strength and pyroplastic deformability's ability.
Embodiment 2
Preparing for the present embodiment high-melting-point high-entropy alloy laser cladding coating is as follows：
Raw material prepares：Co powder, Cr powder, Mo powder, Nb powder and Ti powder are entered into composition proportion according to the molar ratio of embodiment 1,
The powder of various elements is weighed using electronic balance, the powder configured is placed in omnidirectional planetary ball mill and mixed, if
Rotating speed is determined for 150r/min, the time is 15h, obtain well mixed powder；
Matrix processing：45 steel matrix surfaces are polished smooth with sand paper, is then once cleaned and beaten with absolute ethyl alcohol and acetone
Matrix after mill, finally carries out blasting treatment, obtains the matrix of surface coarsening；
It is prepared by coating：The mixed-powder that step one is obtained is placed on 45 firm matrixes, obtains the thick fore-put powders of about 700um
Layer, multiple tracks cladding is carried out using laser, and laser power used is 2.3~2.7kW, and sweep speed is 300~600mm/
Min, spot diameter is 3~4mm, with inert gas Ar gas shieldeds during cladding.The present invention is prepared thick using laser melting and coating technique
The matrix surface of change obtains the high-entropy alloy coating of high comprehensive performance.
The tissue of high-entropy alloy laser cladding coating and performance evaluation：
X-ray diffraction (XRD) result：Coating sample is cut into after 10 × 10 × 10mm squares using wire cutting, will be applied
Layer surface is carefully ground using 150#, 400#, 800#, 1200#, 1500# and 2000# abrasive paper for metallograph successively.Spread out using X-ray
Penetrate instrument to metallographic sample carry out crystal species analysis, scanning step 0.01/s, the θ of scanning angle 2 scope is from 10 ° to 90 °.Obtain high
Entropy alloy thing is made up of simple body-centered cubic BCC solid solution.
ESEM (SEM) result：Sample is cut into after 10 × 10 × 10mm squares with wire cutting, through 150#, 400#,
800#, 1200#, 1500# and 2000# abrasive paper for metallograph are carefully ground, and after mechanical polishing, use ESEM back scattering mould
Formula observes coating interface tissue.Obtain high-entropy alloy thing phase composition as shown in Figure 3.
Coating hardness is tested：The microhardness of alloy, hardness test are determined using 401MVD digital displays micro Vickers
Before, alloy sample is carefully ground using the abrasive paper for metallograph through 150#, 400#, 800#, 1200#, 1500# and 2000#, gone forward side by side
Row mechanical polishing.The load loaded during experiment is 500g, keeps 15s.Each sample 7 points of random test, are removed maximum and most
After small data, the average value of remaining 5 data points is taken as the microhardness value of the alloy.
High-entropy alloy coating is obtained using laser melting and coating technique in the present embodiment, as can be seen that height from Fig. 3 scanning figure
Entropy alloy coat is uniform dendrite tissue, has obvious transition zone between coating and matrix, is well combined, because of coating cladding
Heat transfer direction is different from pyroconductivity, and coating diverse location dendrite morphology is different.High entropy adds up to the coating surface hardness such as institute of table 2
Show, coating has reached 859.46HV after laser melting coating0.5。
The microhardness of high-melting-point high-entropy alloy laser cladding layer in the embodiment 2 of table 2
Beneficial effects of the present invention are：The high-entropy alloy has simple body-centered cubic structure, is provided simultaneously with very high strong
Degree and heat endurance, excellent in mechanical performance, can meet the higher performance requirement to material, particularly high-temperature behavior in modern industry
Requirement；The preparation of the high-entropy alloy coating, promotes and has expanded the application field of high-entropy alloy；Preparation method is simple, easy,
Possesses wide application prospect.
Although having been presented for several embodiments of the present invention herein, it will be appreciated by those of skill in the art that
Without departing from the spirit of the invention, the embodiments herein can be changed.Above-described embodiment be it is exemplary, no
The restriction of interest field of the present invention should be used as using the embodiments herein.
Claims (6)
1. a kind of high-melting-point high-entropy alloy, it is characterised in that the composition of the high-melting-point high-entropy alloy is CoCrMoNbTi；It is above-mentioned
The atomic molar ratio of component is：Co:Cr:Mo:Nb:Ti=(0.8~1.1):(0.8~1.1):(0.8~1.1):(0.8~
1.1):(0~1.1)；Wherein, not including Co:Cr:Mo:Nb:Ti=(0.8~1.1):(0.8~1.1):(0.8~1.1):
(0.8~1.1):0.
2. high-melting-point high-entropy alloy as claimed in claim 1, it is characterised in that when preparing the high-melting-point high-entropy alloy,
Selected Co, Cr, Mo, Nb and Ti material purity is 99%~99.99%.
3. a kind of preparation method of high-melting-point high-entropy alloy block materials as claimed in claim 1 or 2, it is characterised in that bag
Include following steps：
Step 1: Co, Cr, Mo, Nb, Ti raw material surface cleaning, remove oxide；
Step 2: Co, Cr, Mo, Nb, Ti are according to mol ratio (0.8~1.1):(0.8~1.1):(0.8~1.1):(0.8~
1.1):(0~1.1) proportioning is weighed；Wherein, not including Co:Cr:Mo:Nb:Ti=(0.8~1.1):(0.8~1.1):(0.8~
1.1):(0.8~1.1):0；
Step 3: the raw material configured is placed in the water cooled copper mould in vacuum non-consumable tungsten electrode arc smelting furnace, to electric arc furnaces
Vacuumize, air pressure is 0~6 × 10 in electric arc furnaces-3Pa；Technical argon is then charged with electromagnetic oven, pressure reaches 0.4~0.6
Individual atmospheric pressure；
Step 4: in fusion process, after each alloy melting, 30~60s of electric arc retention time is turned over after after alloy block cooling
Turn, so repeatedly 3~5 times；After the uniform melting of alloy, taking-up produces the high-melting-point high-entropy alloy.
4. a kind of preparation method of high-melting-point high-entropy alloy laser cladding coating as claimed in claim 1 or 2, its feature exists
In comprising the following steps：
Step 1: the powder of the high-melting-point high-entropy alloy is mixed in omnidirectional planetary ball mill, rotational speed of ball-mill is 140
~160r/min, the time is 14~16h, and well mixed powder is placed on plain steel, and pre-set thickness is 600-800 μm
；
Step 2: carrying out multiple tracks cladding with superpower laser, laser power is 2.3~2.7kW, and sweep speed is 300-
600mm/min, spot diameter is 3~4mm, and overlapping rate is 25%~40%, blanketing with inert gas during cladding.
5. preparation method as claimed in claim 4, it is characterised in that the rotational speed of ball-mill in step one is 150r/min, alloy
The pre-set thickness of powder is 700 μm.
6. preparation method as claimed in claim 4, it is characterised in that the inert gas in step 2 is Ar.
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| CN108103495B (en) * | 2017-12-12 | 2020-08-25 | 贵州交通职业技术学院 | High-temperature-resistant high-entropy alloy tool steel coating material and preparation method of coating |
| RU2790708C1 (en) * | 2022-04-19 | 2023-02-28 | Федеральное государственное автономное образовательное учреждение высшего образования "Белгородский государственный национальный исследовательский университет" (НИУ "БелГУ") | High-entropy alloy and method of its deformation-heat treatment |
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| CN109628819A (en) * | 2019-01-18 | 2019-04-16 | 湘潭大学 | A kind of VTiCuHfZr high-entropy alloy and preparation method thereof |
| CN110000515A (en) * | 2019-05-24 | 2019-07-12 | 中国矿业大学 | A kind of high-entropy alloy CoCrCuFeNi laser re cast layer and preparation method thereof |
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| CN114606419A (en) * | 2022-02-22 | 2022-06-10 | 中国科学院宁波材料技术与工程研究所 | Refractory high-entropy alloy composite material and preparation method thereof |
| CN114752931A (en) * | 2022-04-06 | 2022-07-15 | 中国科学院宁波材料技术与工程研究所 | Refractory high-entropy alloy composite coating and preparation method and application thereof |
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| US20020159914A1 (en) * | 2000-11-07 | 2002-10-31 | Jien-Wei Yeh | High-entropy multielement alloys |
| US9150945B2 (en) * | 2011-10-27 | 2015-10-06 | Ut-Battelle, Llc | Multi-component solid solution alloys having high mixing entropy |
| CN104120325B (en) * | 2014-07-04 | 2017-01-18 | 北京科技大学 | Low thermal expansion coefficient NaMxAlySiz high entropy alloy and preparation method thereof |
| CN105671392B (en) * | 2014-11-19 | 2017-11-03 | 北京科技大学 | A kind of TiZrHfNb base high-entropy alloys of nitrogen reinforcing and preparation method thereof |
| CN105296836B (en) * | 2015-11-17 | 2017-12-08 | 北京科技大学 | A kind of N with SMExMyHigh-entropy alloy and preparation method thereof |
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| CN108103495B (en) * | 2017-12-12 | 2020-08-25 | 贵州交通职业技术学院 | High-temperature-resistant high-entropy alloy tool steel coating material and preparation method of coating |
| RU2790708C1 (en) * | 2022-04-19 | 2023-02-28 | Федеральное государственное автономное образовательное учреждение высшего образования "Белгородский государственный национальный исследовательский университет" (НИУ "БелГУ") | High-entropy alloy and method of its deformation-heat treatment |
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