CN108060322A - The preparation method of hard high-entropy alloy composite material - Google Patents
The preparation method of hard high-entropy alloy composite material Download PDFInfo
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- CN108060322A CN108060322A CN201711284615.1A CN201711284615A CN108060322A CN 108060322 A CN108060322 A CN 108060322A CN 201711284615 A CN201711284615 A CN 201711284615A CN 108060322 A CN108060322 A CN 108060322A
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- 239000000956 alloy Substances 0.000 title claims abstract description 54
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 53
- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 115
- 238000005245 sintering Methods 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 26
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 238000005275 alloying Methods 0.000 claims abstract description 15
- 238000000498 ball milling Methods 0.000 claims abstract description 14
- 239000011159 matrix material Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- 238000003701 mechanical milling Methods 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 7
- 230000002708 enhancing effect Effects 0.000 abstract description 2
- 239000011651 chromium Substances 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 238000004663 powder metallurgy Methods 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- 229910001315 Tool steel Inorganic materials 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 230000000717 retained effect Effects 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000007780 powder milling Methods 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 238000007723 die pressing method Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- UFGZSIPAQKLCGR-UHFFFAOYSA-N chromium carbide Chemical compound [Cr]#C[Cr]C#[Cr] UFGZSIPAQKLCGR-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000007499 fusion processing Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 229910003470 tongbaite Inorganic materials 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical group [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- 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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- 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
Abstract
The invention discloses a kind of preparation methods of hard high-entropy alloy composite material, comprise the following steps：(1) superhard material powder, alloying element powder are chosen as raw material, wherein, the alloying element powder is selected from the alloy powder of Fe powder, Co powder, Cr powder, Ni powder, Mn powder and foregoing arbitrary three kinds or three kinds or more element compositions；The superhard material powder is selected from one or more of WC alloyed powders, BN powder, bortz powder；(2) raw material chosen in step (1) is subjected to ball-milling treatment, obtains fine grain powder；(3) the fine grain powder is subjected to discharge plasma sintering, furnace cooling, gained sintering block is hard high-entropy alloy composite material.The present invention as matrix, adds in the superhard particles such as WC, cube BN as enhancing phase using the high-entropy alloy of the excellent plasticities such as FeCoCrNiMn, while so that the product is obtained very high rigidity, reduces the cost, the density of product and preparation difficulty of the high entropy raw material of hard.
Description
Technical field
It is compound that hard high-entropy alloy is prepared the invention belongs to field of alloy material more particularly to a kind of use powder metallurgic method
The method of material.
Background technology
Powder metallurgy tool steel has the advantages such as high intensity, high rigidity and wearability, in mold, cutting tool, roll etc.
Field is widely used general.But due to such material contain more than alloying element species and carbide form it is complicated, micro- group
Knit, the control of the pattern of phase structure and carbide particle it is difficult.Simultaneously as the plasticity of powder metallurgy tool steel is low, toughness is poor,
Difficulty is big in terms of the preparation processing of tool and mould.By the matrix composition for changing tool steel, it is possible to improve its plasticity.High-entropy alloy
Alloying element content it is also higher, but species is relatively fewer, and phase constitution is simple in structure, good toughness, can be used as tool steel
Potential basis material.In addition, high-entropy alloy generally has the characteristics that high temperature oxidation resisting, on high-entropy alloy component base, lead to
Crossing addition or precipitation hard carbide in situ, exploitation high-wearing feature, the tool die material of high tenacity resistance to high temperature oxidation has non-
Often important engineering significance.
Hard high-entropy alloy of the prior art is mainly prepared using refractory metal elements, such as MoTaWNbV,
WMoNbZr, TaNbVZr etc..Although this kind of high-entropy alloy also has higher hardness, the cost of material used is high and material is close
Spend larger, material melting point is high, it is big to prepare energy consumption, has challenge to Preparation equipment.
At present, the preparation of more pivot high-entropy alloy blocks is mainly using the method for vacuum melting.But hard material is molten
Point is general very high, and the method for melting is difficult to melt, such as WC hard phases, and the energy expenditure of fusion process is also very big.In addition,
Thermal expansion and condensation can be generated in casting process, it is big so as to cause as cast condition high-entropy alloy block internal stress；Also, the high entropy of as cast condition
The defects of alloy grain size is larger, and internal component segregation is notable, gap and shrinkage cavity is more, this also affects the high entropy of as cast condition and closes
The performance of gold；In addition as cast condition high-entropy alloy majority brittleness is larger, so as to limit further applying for alloy.Powder metallurgical technique has
Have the advantages that technological process is short, equipment investment is small, energy expenditure is small.Powder metallurgical technique can prepare the hard of hard alloy etc
Composite material.Therefore PM technique is also one of potential technology for preparing hard high-entropy alloy.Conventional powder metallurgy
In technique, forming technology generally use die pressing, but there is friction in die pressing forming process between powder and die wall, and hard
Grain has very high hardness so that green compact have the defects of porosity is high made from die forming, so as to cause the mechanical property of finished product
It can be relatively low；Moreover, the sintering time usually after mill pressure is longer, material inner tissue phenomenon of growing up is apparent, so as to reduce material
Mechanical property.
The content of the invention
The technical problems to be solved by the invention are to overcome the shortcomings of to mention in background above technology and defect, provide one
The method that kind prepares hard high-entropy alloy composite material using powder metallurgic method.
In order to solve the above technical problems, technical solution proposed by the present invention is：
A kind of preparation method of hard high-entropy alloy composite material, comprises the following steps：
(1) choose superhard material powder, alloying element powder is raw material, wherein, the alloying element powder be selected from Fe powder, Co powder,
The alloy powder that Cr powder, Ni powder, Mn powder and foregoing arbitrary three kinds or more elements form；The superhard material powder is selected from WC alloys
One or more of powder, BN powder, bortz powder；
(2) raw material chosen in step (1) is subjected to ball-milling treatment, obtains fine grain powder；
(3) the fine grain powder is subjected to discharge plasma sintering, furnace cooling, gained sintering block is the high entropy of hard
Alloy composite materials.
Above-mentioned preparation method, it is preferred that in the raw material, the atom content of superhard material powder is not higher than 70%.
Above-mentioned preparation method, it is preferred that the granularity of the superhard material powder is the mesh of -200 mesh~-600, the alloy member
The granularity of plain powder is the mesh of -200 mesh~-300.
Above-mentioned preparation method, it is preferred that in step (2), mechanical milling process carries out under the protection of inert gas, and ball milling turns
Speed 240~280r/min, 5~10h of Ball-milling Time, the matrix powder grain size after ball milling is at 30~40 μm.
Above-mentioned preparation method, it is preferred that in step (3), the pressure control during discharge plasma sintering is 30MPa
~40MPa, sintering temperature are 900 DEG C~1200 DEG C, and the sintered heat insulating time is 15min~30min.
Above-mentioned preparation method, it is preferred that in step (3), discharge plasma sintering is sintered using graphite jig；The stone
The ratio of height to diameter of black mold is 1: 8~1: 1.
Compared with prior art, the advantage of the invention is that：
(1) product of high-compactness can be obtained during preparation method of the invention using discharge plasma sintering, is burnt
The knot time is short, and tiny microstructure can remain caused by mechanical milling process, so that material possesses higher mechanical property
Energy；In addition sintering velocity is fast, and the processes element diffusion is low, the superhard material particle of addition can preferably be retained in matrix
It is interior, so as to increase substantially the hardness of material.
(2) it is super to add in WC, cube BN etc. using the high-entropy alloy of the excellent plasticities such as FeCoCrNiMn as matrix by the present invention
Grit is as enhancing phase, while so that the product is obtained very high rigidity, reduce the cost of the high entropy raw material of hard, product it is close
Degree is with preparing difficulty.
(3) present invention has good plasticity, toughness and better resistance to high temperature oxidation using matrixes such as FeCoCrNiMn
Property, the hard high-entropy alloy being prepared into inherits the good characteristic of matrix；The superhard particles of addition significantly improve material
Hardness makes it possess comprehensive performance more better than mould steel.
Description of the drawings
Fig. 1 is the process flow chart that the present invention prepares hard high-entropy alloy composite material.
Fig. 2 is the pass that hardness changes with carbide additive amount in high-entropy alloy composite material prepared by the embodiment of the present invention 1
It is curve.
Fig. 3 is the SEM photograph of high-entropy alloy composite material prepared by the embodiment of the present invention 1.
Specific embodiment
For the ease of understanding the present invention, done more entirely below in conjunction with Figure of description and preferred embodiment to inventing herein
Face meticulously describes, but protection scope of the present invention is not limited to specific examples below.
Unless otherwise defined, all technical terms used hereinafter are generally understood meaning phase with those skilled in the art
Together.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention's
Protection domain.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1：
A kind of preparation method of the hard high-entropy alloy composite material of the present invention, process flow chart as shown in Figure 1, including
Following steps：
(1) choose the alloying element powder that granularity is the WC powder of -280 mesh and granularity is -300 mesh (oxygen content is less than 0.3%)
For raw material, the atomic ratio of WC powder and metallic element powder is 3: 7, Fe powder, Cr powder, Ni powder, the atomic ratio of Co powder in metallic element powder
For 1：1：1：1；Wherein, other impurity are free of in alloying element powder outside a small amount of inevitably impurity oxygen element, in raw material not
Containing the other elements ingredient in addition to WC powder, Fe powder, Cr powder, Ni powder, Co powder；
(2) raw material powder that step (1) obtains is fitted into ball grinder, using planetary ball mill and hard alloy ball milling
Tank when ball milling 5 is small under the speed of 250r/s, obtains fine grain powder, and mechanical milling process carries out under the protection of argon gas, obtains grain size
3540 μm or so of fine grain powder；
(3) fine grain powder made from step (2) is carried out discharge plasma sintering (to be sintered using graphite jig, graphite mo(u)ld
The ratio of height to diameter of tool is 1:2), the pressure control during discharge plasma sintering is 30MPa, and sintering temperature is 1000 DEG C, heating
Speed be 100 DEG C/min, soaking time 15min, sintering process nitrogen atmosphere protection under carry out；After furnace cooling is completed in sintering
The sintering block of gained is hard high-entropy alloy composite material.Hard high-entropy alloy composite material carries out wire cutting processing, obtains
To the hard powder metallurgy workpieces of various shape, to adapt to the demand of different product.
The present embodiment product is tested by drainage, the consistency for measuring the hard high-entropy alloy composite material is
98%, hardness (Vickers) 760HV (test result is as shown in Figure 2).
(A is height to powder metallurgy hard high-entropy alloy composite material SEM photograph manufactured in the present embodiment in Fig. 3 as shown in Figure 3
Entropy phase；B is tungsten carbide phase；C1 and C2 is chromium carbide phase), as seen from Figure 3, hard high-entropy alloy composite wood manufactured in the present embodiment
The compactness of material is good, and tissue is comparatively fine, and distributed mutually is uniform, and superhard WC particle is preferably retained in high entropy matrix.
The elongation percentage of the hard high-entropy alloy composite material stretching experiment is 9%, fracture toughness 1324kJ/m2；Sample exists
Under 973K, after aoxidizing 4h in air atmosphere, sample quality increases as 0.0013mg/mm2。
Embodiment 2：
A kind of preparation method of the hard high-entropy alloy composite material of the present invention, process flow chart as shown in Figure 1, including
Following steps：
(1) (oxygen content is less than the alloying element powder that selection granularity is -600 purpose cube BN powder and granularity is -300 mesh
0.3%) for raw material, the atomic ratio of BN powder and metallic element powder is 4: 6, Fe powder in metallic element powder, Cr powder, Ni powder, Co powder
Atomic ratio is 1：1：1：1；Wherein, other impurity are free of in addition to a small amount of inevitably impurity oxygen element in alloying element powder, it is former
Without the other elements ingredient in addition to BN powder, Fe powder, Cr powder, Ni powder, Co powder in material；
(2) raw material powder that step (1) obtains is fitted into ball grinder, using planetary ball mill and hard alloy ball milling
Tank when ball milling 7 is small under the speed of 240r/s, obtains fine grain powder, and mechanical milling process carries out under the protection of argon gas, obtains grain size
For 35 μm or so of fine grain powder；
(3) fine grain powder made from step (2) is carried out discharge plasma sintering (to be sintered using graphite jig, graphite mo(u)ld
The ratio of height to diameter of tool is 2:3), the pressure control during discharge plasma sintering is 40MPa, and sintering temperature is 1100 DEG C, heating
Speed be 130 DEG C/min, soaking time 20min, sintering process nitrogen atmosphere protection under carry out；After furnace cooling is completed in sintering
The sintering block of gained is hard high-entropy alloy composite material.Hard high-entropy alloy composite material carries out wire cutting processing, obtains
To the hard powder metallurgy workpieces of various shape, to adapt to the demand of different product.
The present embodiment product is tested by drainage, the consistency for measuring the hard high-entropy alloy composite material is
98%, hardness (Vickers) 960HV, the elongation percentage of stretching experiment is 8%, fracture toughness 1203kJ/m2；Sample is at 973k, empty
After aoxidizing 4h in gas atmosphere, sample quality increases as 0.0017mg/mm2。
The compactness of hard high-entropy alloy composite material manufactured in the present embodiment is good, and tissue is comparatively fine, and distributed mutually is equal
Even, superhard BN particles are preferably retained in high entropy matrix.
Embodiment 3：
A kind of preparation method of the hard high-entropy alloy composite material of the present invention, process flow chart as shown in Figure 1, including
Following steps：
(1) (oxygen content is less than the alloying element powder that selection granularity is the bortz powder of -400 mesh and granularity is -300 mesh
0.3%) it is raw material, the atomic ratio of bortz powder and metallic element powder is 2: 8, Fe powder, Cr powder, Ni powder, Co in metallic element powder
The atomic ratio of powder is 1：1：1：1；Wherein, be free of in alloying element powder in addition to a small amount of inevitably impurity oxygen element other miscellaneous
Matter, without the other elements ingredient in addition to bortz powder, Fe powder, Cr powder, Ni powder, Co powder in raw material；
(2) raw material powder that step (1) obtains is fitted into ball grinder, using planetary ball mill and hard alloy ball milling
Tank when ball milling 6 is small under the speed of 260r/s, obtains fine grain powder, and mechanical milling process carries out under the protection of argon gas, obtains grain size
For 35 μm or so of fine grain powder；
(3) fine grain powder made from step (2) is carried out discharge plasma sintering (to be sintered using graphite jig, graphite mo(u)ld
The ratio of height to diameter of tool is 1：2), the pressure control during discharge plasma sintering is 35MPa, and sintering temperature is 1050 DEG C, heating
Speed be 150 DEG C/min, soaking time 25min, sintering process nitrogen atmosphere protection under carry out；After furnace cooling is completed in sintering
The sintering block of gained is hard high-entropy alloy composite material.Hard high-entropy alloy composite material carries out wire cutting processing, obtains
To the hard powder metallurgy workpieces of various shape, to adapt to the demand of different product.
The present embodiment product is tested by drainage, the consistency for measuring the hard high-entropy alloy composite material is
98%, hardness (Vickers) 830HV, the elongation percentage of stretching experiment is 11%, fracture toughness 1456kJ/m2；The sample is in 973K
Under, after aoxidizing 4h in air atmosphere, sample quality increases as 0.0011mg/mm2。
The compactness of hard high-entropy alloy composite material manufactured in the present embodiment is good, and tissue is comparatively fine, and distributed mutually is equal
Even, ultrahard diamond particle is preferably retained in high entropy matrix.
Claims (6)
1. a kind of preparation method of hard high-entropy alloy composite material, which is characterized in that comprise the following steps：
(1) choose superhard material powder, alloying element powder is raw material, wherein, the alloying element powder be selected from Fe powder, Co powder, Cr powder,
The alloy powder of Ni powder, Mn powder and foregoing arbitrary three kinds or more element compositions；The superhard material powder is selected from WC alloyed powders, BN
One or more of powder, bortz powder；
(2) raw material chosen in step (1) is subjected to ball-milling treatment, obtains fine grain powder；
(3) the fine grain powder is subjected to discharge plasma sintering, furnace cooling, gained sintering block is hard high-entropy alloy
Composite material.
2. preparation method as described in claim 1, which is characterized in that in the raw material, the molar content of superhard material powder is not
Higher than 70%.
3. preparation method as described in claim 1, which is characterized in that the granularity of the superhard material powder is -200 mesh~-600
Mesh, the granularity of the alloying element powder are the mesh of -200 mesh~-300.
4. preparation method as described in claim 1, which is characterized in that in step (2), mechanical milling process is in the protection of inert gas
Lower progress, 240~280r/min of rotational speed of ball-mill, 5~10h of Ball-milling Time, the matrix powder grain size after ball milling is at 30~40 μm.
5. such as Claims 1 to 4 any one of them preparation method, which is characterized in that in step (3), discharge plasma sintering
For 30MPa~40MPa, sintering temperature is 900 DEG C~1200 DEG C for pressure control in the process, the sintered heat insulating time for 15min~
30min。
6. such as Claims 1 to 4 any one of them preparation method, which is characterized in that in step (3), discharge plasma sintering
It is sintered using graphite jig；The ratio of height to diameter of the graphite jig is 1: 8~1: 1.
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| CN108842106A (en) * | 2018-07-13 | 2018-11-20 | 中南大学 | A kind of gauge ring and its preparation method and application |
| CN108941546A (en) * | 2018-06-15 | 2018-12-07 | 燕山大学 | A kind of high-entropy alloy combination cubic boron nitride superhard composite material and preparation method |
| CN109082550A (en) * | 2018-07-12 | 2018-12-25 | 上海交通大学 | The nickel-base composite material and preparation method thereof of nano-ceramic particle 3D net distribution |
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| CN109295399A (en) * | 2018-12-10 | 2019-02-01 | 西南交通大学 | A kind of high-damping high entropy alloy material and preparation method thereof |
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