CN106319260A - Preparation method for high-melting-point and high-entropy alloy and coating thereof - Google Patents
Preparation method for high-melting-point and high-entropy alloy and coating thereof Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 104
- 239000011248 coating agent Substances 0.000 title claims abstract description 32
- 238000000576 coating method Methods 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 13
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 11
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 238000004372 laser cladding Methods 0.000 claims abstract description 8
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims description 18
- 230000008018 melting Effects 0.000 claims description 14
- 238000002844 melting Methods 0.000 claims description 14
- 238000010891 electric arc Methods 0.000 claims description 10
- 238000005253 cladding Methods 0.000 claims description 9
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 238000003723 Smelting Methods 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
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- 230000008901 benefit Effects 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract 1
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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
-
- 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
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Abstract
The invention relates to the technical field of novel alloy materials, and provides a high-melting-point and high-entropy alloy. The composition of the high-melting-point and high-entropy alloy is CoCrMoNbTi; the atomic mole ratio of the components is (0.8 to 1.1): (0.8 to 1.1): (0.8 to 1.1): (0.8 to 1.1): (0 to 1.1); and the purities of the selected raw materials of Co, Cr, Mo, Nb and Ti are all not lower than 99%. The invention further provides a preparation method for the abovementioned alloy block material and a laser cladding coating. The high-entropy alloy and the preparation method, which are disclosed by the invention, have the following beneficial benefits: the high-entropy alloy is simple in body-centred cubic structure, great in strength and heat stability, excellent in mechanical property, and capable of meeting higher performance requirements on materials in the modern industry, and in particular, meeting high-temperature performance requirements; preparation for the high-entropy alloy coating promotes and expands the application fields of the high-entropy alloy; and the preparation method is simple and practicable, and wide in application prospect.
Description
Technical field
The present invention relates to novel alloy field of material technology, prepare particularly to a kind of high-melting-point high-entropy alloy and coating thereof
Method.
Background technology
The proposition of high-entropy alloy theory, the research for alloy material opens new approach.High-entropy alloy generally comprises 5 kinds
Or the constituent element of more than 5 kinds, and the atomic ratio of every kind of element is between 5%-35%.Due to high entropic effect, contain and wait atom to rub
The multicomponent alloy of that ratio or nearly atomic molar ratio does not form baroque brittle intermetallic thing phase, on the contrary can
Form simple solid solution structure, give the combination property that alloy is excellent.The most in recent years by several high-melting-point alloys
The high-melting-point high-entropy alloy that organic assembling is designed and developed is significantly improved than conventional high-temperature alloy at associated high-temperature aspect of performance, should
With having a extensive future, become one of focus branch of high-entropy alloy research.
CN201510010329.0 disclose a kind of regulate and control AlCoCrFeNi high-entropy alloy tissue method, in atmospheric environment
AlCoCrFeNi high-entropy alloy is coated with by lower covering, changes tissue morphology by high undercooling rapid solidification, by obtaining
The degree of supercooling that in experimentation, AlCoCrFeNi high-entropy alloy is big is with organization of regulation control pattern.
CN201310161152.5 discloses a kind of preparation method containing amorphous nano-crystalline high-entropy alloy coating, can be used for making
The high-entropy alloy coating superior for combination property and block materials.
CN200810063807.4 discloses a kind of high-entropy alloy-base composite material and preparation method thereof, composite hard
The performances such as degree, intensity all significantly improve before compound.
All without reference to high-melting-point high-entropy alloy and preparation thereof in above-mentioned material.
Summary of the invention
The purpose of the present invention overcomes the deficiencies in the prior art exactly, it is provided that a kind of high-melting-point high-entropy alloy, uses vacuum
Electric arc melting Technology design have developed the high-melting-point high-entropy alloy of the novel system of CoCrMoNbTi, it is determined that the composition range of alloy
And smelting technology, test organizational structure and the correlated performance of alloy.Simultaneously by laser melting and coating technique and plasma spray technology system
For high-melting-point high-entropy alloy coating, it is determined that preparation technology of coating and linked groups's performance, for the actual application of novel alloy
Pave road.
One high-melting-point high-entropy alloy of the present invention, consists of 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 described high-melting-point high-entropy alloy, the raw material of selected Co, Cr, Mo, Nb and Ti is pure
Degree is 99%～99.99%.
Present invention also offers the preparation method of a kind of above-mentioned high-melting-point high-entropy alloy block materials, comprise the steps:
Step one, 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) weigh proportioning；
In step 3, the water cooled copper mould raw material configured being placed in vacuum non-consumable tungsten electrode arc smelting furnace, to electricity
Arc stove evacuation, electric arc furnace internal gas pressure is 0～6 × 10-3Pa；Be then charged with technical argon in electromagnetic oven, pressure reach 0.4～
0.6 atmospheric pressure；
In step 4, fusion process, after each alloy melting, electric arc retention time 30-60s, will after alloy block cools down
Its upset, so repeat 3～5 times or more than；After the uniform melting of alloy, take out and i.e. obtain described high-melting-point high-entropy alloy.
Present invention also offers the preparation method of a kind of above-mentioned high-melting-point high-entropy alloy laser cladding coating, including walking as follows
Rapid:
Step one, the powder body of described 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, is placed on plain steel by the powder body of mix homogeneously, and pre-set thickness is 600-
800um；
Step 2, carrying out multiple tracks cladding with superpower laser, laser power is 2.3～2.7kW, and scanning 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 noble gas in step 2 is Ar.
The invention have the benefit that this high-entropy alloy has simple body-centered cubic structure, be provided simultaneously with the highest strong
Degree and heat stability, excellent in mechanical performance, can meet the higher performance requirement to material, particularly high-temperature behavior in modern industry
Requirement；The preparation of this high-entropy alloy coating, promotes and has expanded the application of high-entropy alloy；Preparation method is simple, easy,
Possesses wide application prospect.
Accompanying drawing explanation
Fig. 1 show the X ray diffracting spectrum of CoCrMoNbTi high-entropy alloy in the embodiment of the present invention 1.
Fig. 2 show the scanning electron microscope back scattering photo of CoCrMoNbTi high-entropy alloy in embodiment 1.
Fig. 3 show the scanning electron microscope back scattering photo of CoCrMoNbTi high-entropy alloy coating interface in embodiment 2.
Detailed description of the invention
The specific embodiment of the invention is described in detail below in conjunction with concrete accompanying drawing.It should be noted that, in following embodiment
The technical characteristic described or the combination of technical characteristic are not construed as isolating, and they can be mutually combined thus reach
To superior technique effect.In the accompanying drawing of following embodiment, the identical label that each accompanying drawing is occurred represent identical feature or
Person's parts, can be applicable in different embodiment.
Embodiment of the present invention one high-melting-point high-entropy alloy, described high-melting-point high-entropy alloy consist of 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 described high-melting-point high-entropy alloy, the material purity of selected Co, Cr, Mo, Nb and Ti is the lowest
In 99%, preferably 99%～99.99%.
The preparation method of a kind of above-mentioned high-melting-point high-entropy alloy block materials, comprises the steps:
Step one, 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) weigh proportioning；
In step 3, the water cooled copper mould raw material configured being placed in vacuum non-consumable tungsten electrode arc smelting furnace, to electricity
Arc stove evacuation, electric arc furnace internal gas pressure is 0～6 × 10-3Pa；Be then charged with technical argon in electromagnetic oven, pressure reach 0.4～
0.6 atmospheric pressure；
In step 4, fusion process, after each alloy melting, electric arc retention time 30-60s, will after alloy block cools down
Its upset, so repeat 3～5 times or more than；After the uniform melting of alloy, take out and i.e. obtain described high-melting-point high-entropy alloy.
The preparation method of a kind of above-mentioned high-melting-point high-entropy alloy laser cladding coating, comprises the steps:
Step one, the powder body of described 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, is placed on plain steel by the powder body of mix homogeneously, and pre-set thickness is 600-
800um；
Step 2, carrying out multiple tracks cladding with superpower laser, laser power is 2.3～2.7kW, and scanning speed is 300-
600mm/min, spot diameter is 3～4mm, and overlapping rate is 25%～40%, blanketing with inert gas during cladding.
Preferably, 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 noble 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, cleans up with ultrasonic wave concussion in ethanol；
Alloy melting: use 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 furnace evacuation, after vacuum reaches 5 × 10-3Pa, it is filled with technical argon until in stove
Pressure reaches half atmospheric pressure；Every time after molten alloy fusing, electric arc retention time 45s；Again by crucible after alloy cools down
Alloy turn-over continue melting, be so repeated 4 times, to ensure alloy mix homogeneously.
Organizational structure and the performance evaluation of alloy are as follows:
X-ray diffraction (XRD) result: after utilizing line cutting that sample is cut into 10 × 10 × 10mm square, by sample table
Face is carefully ground with the abrasive paper for metallograph of 150#, 400#, 800#, 1200#, 1500# and 2000# successively.Use X-ray diffractometer pair
Metallographic sample carries out crystal species analysis, scanning step 0.01/s, and the scope of scanning angle 2 θ is from 10 ° to 90 °.Test result such as figure
Shown in 1.
Scanning electron microscope (SEM) result: with line cutting sample is cut into 10 × 10 × 10mm square after, through 150#, 400#,
The abrasive paper for metallograph of 800#, 1200#, 1500# and 2000# carefully grinds, and after mechanical polishing, uses scanning electron microscope back scattering mould
Formula observes alloy structure.Test result is as shown in Figure 2.
Fabric analysis finds, this alloy is made up of, as shown in Figure 1 simple BCC solid solution；Alloy structure is by typically setting
Dendrite and interdendritic structure composition, as shown in Figure 2.Visible, alloy structure is typical high-entropy alloy tissue characteristic.
Microhardness: use 401MVD digital display micro Vickers to measure the microhardness of alloy, before hardness test,
Use the abrasive paper for metallograph through 150#, 400#, 800#, 1200#, 1500# and 2000# carefully to grind alloy sample, and carry out machine
Tool polishes.The load loaded during test is 500g, keeps 15s.7 points of each sample random test, remove minimum and maximum
After data, take the meansigma methods microhardness value as this alloy of 5 data points of residue, as shown in table 1.
The microhardness of high-melting-point high-entropy alloy laser cladding layer in table 1 embodiment 1
With the room temperature Compressive Mechanical Properties of MTS 809 Material Testing Machine beta alloy, specimen size is φ 3mm × 6mm, should
Variable Rate is 1 × 10-4s-1, alloy has the highest fracture strength, up to 1780MPa；Compression process is cashed and breaks for fragility
Split.Carrying out hot compression test on Gleeble-1500 hot modeling test machine, deformation temperature is 600～1300 DEG C, strain rate
It is 0.001～0.1s-1, deflection is 30%～60%.Carry out after sample being heated to preset temperature with the speed of 8～12 DEG C/s
Compression, can high temperature compressed at 1200 DEG C under, Alloy Anti Compressive Strength is up to 680MPa, and compressive plastic deformation amount is more than 35%,
There is elevated temperature strength and pyroplastic deformability's ability of excellence.
Embodiment 2
Preparing of the present embodiment high-melting-point high-entropy alloy laser cladding coating is as follows:
Raw material prepares: according to the molar ratio of embodiment 1, Co powder, Cr powder, Mo powder, Nb powder and Ti powder are entered composition proportion,
Use electronic balance to weigh the powder of various element, mix in the powder configured is placed in omnidirectional planetary ball mill, if
Determining rotating speed is 150r/min, and the time is 15h, it is thus achieved that the powder of mix homogeneously；
Matrix processes: polished smooth on 45 steel matrix surfaces with sand paper, then once cleans with dehydrated alcohol and acetone and beats
Matrix after mill, finally carries out blasting treatment, obtains the matrix of surface coarsening；
Prepared by coating: mixed-powder step one obtained is placed on 45 firm matrixes, obtains the thick fore-put powder of about 700um
Layer, uses laser instrument to carry out multiple tracks cladding, and laser power used is 2.3～2.7kW, and scanning speed is 300～600mm/
Min, spot diameter is 3～4mm, with noble gas Ar gas shielded during cladding.The present invention uses laser melting and coating technique to prepare slightly
The matrix surface changed 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: after utilizing line cutting that coating sample is cut into 10 × 10 × 10mm square, will be coated with
Layer surface uses the abrasive paper for metallograph of 150#, 400#, 800#, 1200#, 1500# and 2000# carefully to grind successively.Use X-ray is spread out
Penetrating instrument and metallographic sample carries out crystal species analysis, scanning step 0.01/s, the scope of scanning angle 2 θ is from 10 ° to 90 °.Obtain height
Entropy alloy thing is made up of simple body-centered cubic BCC solid solution.
Scanning electron microscope (SEM) result: with line cutting sample is cut into 10 × 10 × 10mm square after, through 150#, 400#,
The abrasive paper for metallograph of 800#, 1200#, 1500# and 2000# carefully grinds, and after mechanical polishing, uses scanning electron microscope back scattering mould
Formula observes coating interface tissue.Obtain high-entropy alloy thing phase composition as shown in Figure 3.
Coating hardness is tested: use 401MVD digital display micro Vickers to measure the microhardness of alloy, hardness test
Before, use the abrasive paper for metallograph through 150#, 400#, 800#, 1200#, 1500# and 2000# carefully to grind alloy sample, go forward side by side
Row mechanical polishing.The load loaded during test is 500g, keeps 15s.7 points of each sample random test, remove maximum and
After little data, take the meansigma methods microhardness value as this alloy of 5 data points of residue.
The present embodiment utilize laser melting and coating technique obtain high-entropy alloy coating, it can be seen that high from the scanning figure of Fig. 3
Entropy alloy coat is uniform dendrite tissue, has obvious transition zone, be well combined between coating and matrix, because of coating cladding
Conduction of heat direction is different from pyroconductivity, and coating diverse location dendrite morphology is different.High entropy adds up to coating surface hardness such as table 2 institute
Showing, after laser melting coating, coating has reached 859.46HV0.5。
The microhardness of high-melting-point high-entropy alloy laser cladding layer in table 2 embodiment 2
The invention have the benefit that this high-entropy alloy has simple body-centered cubic structure, be provided simultaneously with the highest strong
Degree and heat stability, excellent in mechanical performance, can meet the higher performance requirement to material, particularly high-temperature behavior in modern industry
Requirement；The preparation of this high-entropy alloy coating, promotes and has expanded the application 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 is exemplary, no
Should be using the embodiments herein as the restriction of interest field of the present invention.
Claims (6)
1. a high-melting-point high-entropy alloy, it is characterised in that described high-melting-point high-entropy alloy consist of CoCrMoNbTi；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).
2. high-melting-point high-entropy alloy as claimed in claim 1, it is characterised in that when preparing described high-melting-point high-entropy alloy,
The material purity of selected Co, Cr, Mo, Nb and Ti is 99%～99.99%.
3. the preparation method of a 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 one, 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) weigh proportioning；
In step 3, the water cooled copper mould raw material configured being placed in vacuum non-consumable tungsten electrode arc smelting furnace, to electric arc furnace
Evacuation, electric arc furnace internal gas pressure is 0～6 × 10-3Pa；Being then charged with technical argon in electromagnetic oven, pressure reaches 0.4～0.6
Individual atmospheric pressure；
In step 4, fusion process, after each alloy melting, the electric arc retention time 30～60s, turned over after alloy block cools down
Turn, so repeat 3～5 times；After the uniform melting of alloy, take out and i.e. obtain described high-melting-point high-entropy alloy.
4. a preparation method for high-melting-point high-entropy alloy laser cladding coating as claimed in claim 1 or 2, its feature exists
In, comprise the steps:
Step one, being mixed in omnidirectional planetary ball mill by the powder body of described high-melting-point high-entropy alloy, rotational speed of ball-mill is 140
～160r/min, the time is 14～16h, is placed on plain steel by the powder body of mix homogeneously, and pre-set thickness is 600-800um；
Step 2, carrying out multiple tracks cladding with superpower laser, laser power is 2.3～2.7kW, and scanning 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 body is 700um.
6. preparation method as claimed in claim 4, it is characterised in that the noble gas in step 2 is Ar.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108103495A (en) * | 2017-12-12 | 2018-06-01 | 田兴强 | A kind of preparation method of high temperature resistant high-entropy alloy tool steel coating material and coating |
| 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 |
| 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 |
| CN114645237A (en) * | 2020-12-21 | 2022-06-21 | 武汉苏泊尔炊具有限公司 | Cooking utensil 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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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108103495A (en) * | 2017-12-12 | 2018-06-01 | 田兴强 | A kind of preparation method of high temperature resistant high-entropy alloy tool steel coating material and coating |
| 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 |
| CN114645237A (en) * | 2020-12-21 | 2022-06-21 | 武汉苏泊尔炊具有限公司 | Cooking utensil and preparation method thereof |
| 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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