CN109371307A - It is a kind of using high-entropy alloy powder as the preparation method of the WC base cemented carbide of binder - Google Patents
It is a kind of using high-entropy alloy powder as the preparation method of the WC base cemented carbide of binder Download PDFInfo
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- CN109371307A CN109371307A CN201811445236.0A CN201811445236A CN109371307A CN 109371307 A CN109371307 A CN 109371307A CN 201811445236 A CN201811445236 A CN 201811445236A CN 109371307 A CN109371307 A CN 109371307A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/08—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on tungsten carbide
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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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/067—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds comprising a particular metallic binder
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Abstract
The present invention provides a kind of using high-entropy alloy powder as the preparation method of the WC base cemented carbide of binder, its binder is high-entropy alloy powder, it is made of elemental metals iron, cobalt, chromium, nickel, aluminium, vanadium, titanium, copper, zirconium, manganese etc., does not add other such as carbon, boron, silicon element and metallic compound etc..In above-mentioned hard alloy preparation method raw material components and component weight percentage be high-entropy alloy powder binder be 6 ~ 30%, WC powder be 70 ~ 94%.Above-mentioned hard alloy step of preparation process are as follows: (1) preparation of high-entropy alloy powder binder；(2) mixing；(3) sinter molding.WC base cemented carbide is prepared using three kinds of different sintering methods, and shows good mechanical property.
Description
Technical field
The present invention relates to cermet material fields, more particularly to a kind of using high-entropy alloy powder as the WC base of binder
The preparation method of hard alloy.
Background technique:
The one kind of hard alloy as cermet material, be using refractory metal hard compounds as base, using metal as binder,
Using the high rigidity of powder metallurgy process preparation, high abrasion resisting material.Not only had the toughness of metal but also had both the high-strength of ceramics
Degree, while cemented carbide exhibits go out preferable wearability, make it be widely used in manufacturing processing industry, main application has cutting
Processing, percussion tool, wear-and corrosion-resistant components, die casting etc..
Further further investigation now with researchers to cermet, not only has carbide base, boronation also occurs
Object and nitride hard phase, but still being most widely used with carbide, and be mainly with tungsten carbide in carbide hard phase
Main, WC base cemented carbide keeps its application most because of the advantages that its high rigidity, high abrasion, high compressive strength.In WC base cemented carbide
Common Binder Phase mainly has Co, Fe, Ni etc., can usually add different grain refiners according to demand and pursue mentioning for performance
It is high.But the study found that addition Fe, the hard alloy comprehensive performance of Ni Binder Phase preparation is not fine.Moreover, Abroad in Recent Years
There is certain radiation to Co in-depth study discovery Co in person, prolonged use can generate the health of the mankind in production
Certain harm, while Co is as national strategy resource, it is expensive.In high-end manufacture, possesses and adapt to that high speed, height cuts
The cutter material for cutting processing is particularly important, so the research high tool for cutting machining of high speed becomes emphasis, scholars strive for
Seek new mode improving performance, for example add TiC, VC, CrC etc. or other rare earth elements in WC, but adds these
Ingredient be all it is a small amount of, fail the performance for significantly alterring hard alloy.
High-entropy alloy has just become a hot spot and has obtained numerous scholars' favor since being suggested.According to Taiwan's scholars leaf
It is luxuriant professor propose high-entropy alloy definition: be made of 5 kinds and the above element, the content of every kind of element between 5%-35%,
With simple solid solution structure, such as face-centred cubic structure (FCC), body-centered cubic structure (BCC).Compared to conventional alloys, high entropy
More pivot effects that alloy has, such as the high entropy effect in terms of thermodynamics, slow diffusion effect in terms of dynamics, structure side
The distortion of lattice effect in face, the cocktail effect of aspect of performance.The four of high-entropy alloy are big, and effect rush forms it into single solid solution
The structure of body, and then excellent performance is shown, such as high hardness and corrosion resistance, resistance to oxidation high-temperature behavior.Given this present invention will
Single Co, which is substituted, as binder using high-entropy alloy powder prepares WC base cemented carbide.
The Chinese patent CN100526490 Invention Announce is a kind of hard with high-entropy alloy binder and double carbide sintering
The production method of matter alloy, but its claim is that double carbide and Binder Phase metal are packed into ball grinding cylinder to carry out high energy ball
Mill, what is obtained is the composite powder containing Binder Phase.Then addition paraffin carries out low energy ball milling as forming agent and wetting agent.This
Preparation method fails to give full play to high-entropy alloy because high-entropy alloy binder does not realize alloying sufficiently before mixing and sintering
Characteristic.
The present invention uses mechanical alloying that pure metal powder is carried out high-energy ball milling, realizes alloying first, obtains single
Then the high-entropy alloy of solid solution structure prepares WC base cemented carbide using three kinds of different sintering processings.
Summary of the invention
The shortcomings that in order to overcome existing Binder Phase, the present invention provide one kind using WC as hard phase, have single solid solution knot
The high-entropy alloy powder of structure is Binder Phase, substitutes one or both original metal and makees binder, and uses three kinds of different burnings
Knot mode prepares WC base cemented carbide.
The technical solution adopted by the present invention to solve the technical problems is:
It is a kind of using high-entropy alloy powder as the preparation method of the WC base cemented carbide of binder, the Binder Phase of hard alloy is prior
Preparation single solid solution structure high-entropy alloy powder, hard phase WC, which mainly includes following element: iron, cobalt,
The metallic elements such as nickel, chromium, titanium, vanadium, manganese, zirconium, aluminium, between 5%-35%, hard phase is the content of each element in Binder Phase
The quality of WC, hard phase and Binder Phase is 100% than summation, and specific preparation method includes the following steps:
One) high-entropy alloy powder of single solid solution structure is prepared
Five kinds or five kinds or more of metal simple-substance powder is weighed, the content (atomic ratio) of every kind of element is 5 ~ 35%, powder size ruler
Very little is 325 ~ 2000 mesh, and load weighted metal powder is fitted into ball grinder, is packed into hard alloy by 8:1 ~ 15:1 ratio of grinding media to material
Abrading-ball, the mechanical milling process controlling agent that 1-3wt% is added further according to weight metal carry out ball milling, reduce powder and send out in mechanical milling process
Raw food weldering phenomenon, rotational speed of ball-mill are 200 ~ 300rpm；Ball milling total time according under X-ray diffraction equipment detection formed it is single
Subject to body-centered or face-centered cubic crystal structure.The metal simple-substance powder includes iron, cobalt, nickel, chromium, titanium, vanadium, manganese, zirconium, aluminium etc..
Two) mixing: WC powder and high-entropy alloy powder are packed into ball grinder, wherein 70 ~ 94 wt % of WC powder, high-entropy alloy powder
6 ~ 30wt% of end；It is packed into abrading-ball mixing by 6:1 ~ 10:1 ratio of grinding media to material, and pours into alcoholic solution, is mixed 10 ~ 72 hours, rotational speed of ball-mill
For 150 ~ 200rpm, vacuum is sieved after dry and saves backup；
Three) it is sintered: by the way of vacuum-sintering, vacuum heating-press sintering or discharge plasma sintering that uniformly mixed material is high
Temperature is sintered to hard alloy.
Further to improve, the step 1) in mechanical milling process controlling agent be normal heptane
Further to improve, the step 3) in vacuum-sintering concrete mode are as follows: according to step 2) preparation shines mixture
The amount of material is mixed into the forming agent paraffin of 0.5 ~ 3wt% thereto, and heat drying sieving is reloaded into die cavity, is pressed into green compact；It will pressure
Base is packed into vacuum sintering furnace, is evacuated to 1x10-1Pa dewaxes at 250 ~ 650 DEG C, is then gradually heated to 1100 ~ 1300 DEG C admittedly
Phase sintering, 1300 ~ 1500 DEG C after heat preservation 0.5 ~ 1.5 hour, are passed through argon gas to 0.5-5MPa, then keep the temperature 0.2 ~ 1 at such a temperature
Hour, finally cool to room temperature with the furnace, i.e. acquisition hard alloy.
It is further to improve, 5 ~ 10 DEG C/min of heating rate
Further to improve, the step 3) in vacuum heating-press sintering concrete mode are as follows: by step 2) preparation according to mixing
Material is packed into graphite jig, is put into vacuum hotpressing stove, is evacuated to 5.0x10-3Pa is gradually heated to 900 ~ 1100 DEG C, starts
Precharge, pressure are set pressure 40 ~ 60%, are continuously heating to 1200 DEG C, and pressure adds to setting pressure, are warming up to sintering temperature
1250-1500 DEG C of degree keeps the temperature 0.5 ~ 2h, finally cools to room temperature with the furnace, i.e. acquisition hard alloy.
Further to improve, heating rate is 5 ~ 10 DEG C/min.
It is further to improve, pressure is set as 15MPa.
Further to improve, the step 3) in discharge plasma sintering concrete mode are as follows: by step 2) preparation
It is packed into graphite jig according to mixed material, is put into vacuum discharge plasma agglomeration furnace, is evacuated to 5.0x10-3Pa is filled with nitrogen,
1400 DEG C of sintering temperature are warming up to, 10-30min is kept the temperature, pressure is 10-40Mpa in sintering process, finally cools to room with the furnace
Temperature is obtained using high-entropy alloy powder as the WC base cemented carbide of binder.
Further to improve, heating rate is 130 ~ 150 DEG C/min.
Compared with the prior art, the advantages of the present invention are as follows:
(1) three kinds of sintering processings provided by the invention must can effectively reduce WC during the sintering process and aoxidize, and because of portion
Divide sintering processing pressurization that can obtain fine and close micro- heterogeneous microstructure.To obtain preferable mechanical property.
(2) present invention using FeCoCrNiAl high-entropy alloy powder as binder, instead of single cobalt as binder,
While product can be made to obtain higher hardness, the cost of binder is reduced.
(3) the FeCoCrNiAl high-entropy alloy powder that the present invention uses has good as binder, the high-entropy alloy
The WC base cemented carbide of high temperature oxidation resistance and wearability, preparation has better oxidation resistent susceptibility during the cutting process.
The positive effect of the present invention is: the WC base cemented carbide prepared using the high-entropy alloy of single structure as adhesive,
Hardness changes in 1600HV-1820HV, and has preferable wearability, abrasion loss 1.0x10 at room temperature-3, there is hardness
Height, the excellent performances such as wearability is good.
Detailed description of the invention
Fig. 1 is the SEM figure of the WC-Co hard alloy microscopic structure prepared under vacuum-sintering；
Fig. 2 is the SEM figure of the WC base cemented carbide microscopic structure prepared under 1 vacuum-sintering of example.
Specific embodiment
[embodiment 1]
Five kinds of elements such as Fe, Co, Cr, Ni, Al are taken, by equimolar ratio 1:1:1:1:1, weighing total amount is 80g, is packed into ball grinder
In, the ball milling controlling agent normal heptane reagent of 2ml is added, ratio of grinding media to material 15:1, rotational speed of ball-mill 250rpm carry out the high energy of 60h
Ball milling obtains the high-entropy alloy powder of mechanical alloying.The WC powder of 10% high-entropy alloy powder 90% is weighed by quality proportioning
It is fitted into ball grinder, adds the alcoholic solution of 50ml, ball grinder is put into progress low energy ball milling, rotational speed of ball-mill in planetary ball mill
For 150rpm, ratio of grinding media to material is that then progress discharging vacuum drying saves backup 8:1..Using vacuum-sintering mode.Weigh 80g powder
End adds 1.2% paraffin as forming agent, blank is pressed into using 6.3t press, then in 500 DEG C of progress degreasings, through degreasing
It is sintered under vacuum conditions at 1400 DEG C after processing, and measures its performance.Its hardness surveyed is 1825HV, is higher by work of the same race
Using Co as adhesive hard alloy 230 under skill.From figure 2 it can be seen that comparing Fig. 1, high-entropy alloy powder exists as Binder Phase
WC grain growing up to polygon is inhibited to a certain extent, and crystal grain is obviously reduced than WC-Co hard alloy.
[embodiment 2]
Five kinds of elements such as Fe, Co, Cr, Ni, Al are taken, by equimolar ratio 1:1:1:1:1, weighing total amount is 80g, is packed into ball grinder
In, the ball milling controlling agent normal heptane reagent of 2ml is added, ratio of grinding media to material 15:1, rotational speed of ball-mill 250rpm carry out the high energy of 60h
Ball milling obtains the high-entropy alloy powder of mechanical alloying.The WC powder of 10% high-entropy alloy powder 90% is weighed by quality proportioning
It is fitted into ball grinder, adds the alcoholic solution of 50ml, ball grinder is put into progress low energy ball milling, rotational speed of ball-mill in planetary ball mill
For 150rpm, ratio of grinding media to material is that then progress discharging vacuum drying saves backup 8:1..Using vacuum heating-press sintering mode.It weighs
80g powder, is fitted into graphite jig, pressurizes lower 1400 DEG C of 15Mpa be sintered to obtain sample under vacuum conditions, and measure it
Performance, hardness 1850HV.
[embodiment 3]
Five kinds of elements such as Fe, Co, Cr, Ni, Al are taken, by equimolar ratio 1:1:1:1:1, weighing total amount is 80g, is packed into ball grinder
In, the ball milling controlling agent normal heptane reagent of 2ml is added, ratio of grinding media to material 15:1, rotational speed of ball-mill 250rpm carry out the high energy of 60h
Ball milling obtains the high-entropy alloy powder of mechanical alloying.The WC powder of 10% high-entropy alloy powder 90% is weighed by quality proportioning
It is fitted into ball grinder, adds the alcoholic solution of 50ml, ball grinder is put into progress low energy ball milling, rotational speed of ball-mill in planetary ball mill
For 150rpm, ratio of grinding media to material is that then progress discharging vacuum drying saves backup 8:1..Using discharge plasma sintering mode.It weighs
80g powder, is fitted into graphite jig, and pressure is sintered to obtain sample under vacuum conditions for lower 1400 DEG C of 40Mpa, and measures
Its performance, hardness 1900HV.
Claims (9)
1. a kind of using high-entropy alloy powder as the preparation method of the WC base cemented carbide of binder, which is characterized in that including as follows
Step:
One) high-entropy alloy powder of single solid solution structure is prepared: the metal simple-substance powder of five kinds or five kinds of weighing or more, every kind
The atom percentage content of element is 5 ~ 35%, and load weighted metal powder is packed by powder size having a size of 325 ~ 2000 mesh
In ball grinder, it is packed into hard alloy abrading-ball by 8:1 ~ 15:1 ratio of grinding media to material, the mechanical milling process of 1-3wt% is added further according to weight metal
Controlling agent carries out ball milling, and rotational speed of ball-mill is 200 ~ 300rpm；In mechanical milling process, appropriate powder is taken to be detected with X-ray diffractometer, gold
Belonging to after powder forms single solid solution structure terminates ball milling, obtains high-entropy alloy powder;The metal simple-substance include iron, cobalt, nickel,
Chromium, titanium, vanadium, manganese, zirconium, aluminium；
Two) mixing: being packed into ball grinder for WC powder and high-entropy alloy powder, wherein 70 ~ 94 wt % of WC powder, and high-entropy alloy powder 6 ~
30wt%；It is packed into abrading-ball mixing by 6:1 ~ 10:1 ratio of grinding media to material, and pours into alcoholic solution, is mixed 10 ~ 72 hours, rotational speed of ball-mill 150
~ 200rpm is sieved after dry vacuum and saves backup；
Three) it is sintered: by the way of vacuum-sintering, vacuum heating-press sintering or discharge plasma sintering that uniformly mixed material is high
Temperature is sintered to hard alloy.
2. it is as described in claim 1 a kind of using high-entropy alloy powder as the preparation method of the WC base cemented carbide of binder,
Be characterized in that, the step 1) in mechanical milling process controlling agent be normal heptane reagent.
3. it is as described in claim 1 a kind of using high-entropy alloy powder as the preparation method of the WC base cemented carbide of binder,
Be characterized in that, the step 3) in vacuum-sintering concrete mode are as follows: according to step 2) preparation the amount according to mixed material to
It is wherein mixed into the forming agent paraffin of 0.5 ~ 3wt%, heat drying sieving is reloaded into die cavity, is pressed into green compact；Green compact is packed into true
Empty sintering furnace, is evacuated to 1x10-1Pa dewaxes at 250 ~ 650 DEG C, is then gradually heated to 1100 ~ 1300 DEG C of solid-phase sinterings,
1300 ~ 1500 DEG C after heat preservation 0.5 ~ 1.5 hour, are passed through argon gas to 0.5-5MPa, then keep the temperature 0.2 ~ 1 hour, most at such a temperature
After cool to room temperature with the furnace, i.e., acquisition hard alloy.
4. it is as claimed in claim 3 a kind of using high-entropy alloy powder as the preparation method of the WC base cemented carbide of binder,
It is characterized in that, 5 ~ 10 DEG C/min of heating rate.
5. it is as described in claim 1 a kind of using high-entropy alloy powder as the preparation method of the WC base cemented carbide of binder,
Be characterized in that, the step 3) in vacuum heating-press sintering concrete mode are as follows: by step 2) preparation mixed material be packed into stone
Black mold, is put into vacuum hotpressing stove, is evacuated to 5.0x10-3Pa is gradually heated to 900 ~ 1100 DEG C, starts precharge, pressure
Power is set pressure 40 ~ 60%, is continuously heating to 1200 DEG C, pressure adds to setting pressure, is warming up to sintering temperature 1250-
1500 DEG C, 0.5 ~ 2h is kept the temperature, finally cools to room temperature with the furnace, is i.e. acquisition hard alloy.
6. it is as claimed in claim 5 a kind of using high-entropy alloy powder as the preparation method of the WC base cemented carbide of binder,
It is characterized in that, heating rate is 5 ~ 10 DEG C/min.
7. it is as claimed in claim 5 a kind of using high-entropy alloy powder as the preparation method of the WC base cemented carbide of binder,
It is characterized in that, sets pressure as 10-50MPa.
8. it is as described in claim 1 a kind of using high-entropy alloy powder as the preparation method of the WC base cemented carbide of binder,
Be characterized in that, the step 3) in discharge plasma sintering concrete mode are as follows: by step 2) preparation according to mixed material fill
Enter graphite jig, is put into vacuum discharge plasma agglomeration furnace, is evacuated to 5.0x10-3Pa is filled with nitrogen, is warming up to sintering temperature
1250-1500 DEG C of degree keeps the temperature 10-30min, and pressure is 10-40MPa in sintering process, finally cools to room temperature with the furnace, that is, obtains
Using high-entropy alloy powder as the WC base cemented carbide of binder.
9. it is as claimed in claim 8 a kind of using high-entropy alloy powder as the preparation method of the WC base cemented carbide of binder,
It is characterized in that, heating rate is 130 ~ 150 DEG C/min.
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| CN110205533A (en) * | 2019-07-12 | 2019-09-06 | 南方科技大学 | Hard alloy and preparation method and application thereof |
| CN110423930A (en) * | 2019-08-21 | 2019-11-08 | 福建工程学院 | A kind of high entropy ceramic-metal composite of Ultra-fine Grained and preparation method thereof |
| CN110629133A (en) * | 2019-09-30 | 2019-12-31 | 成都工业学院 | Carbon fiber- (Ti, V) (C, N) hard alloy and preparation method thereof |
| CN110735076A (en) * | 2019-09-04 | 2020-01-31 | 广东工业大学 | high-entropy metal ceramics and preparation method and application thereof |
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| CN114406267A (en) * | 2021-12-08 | 2022-04-29 | 西安理工大学 | Method for connecting CuW and CuCr materials through high-entropy alloy infiltration |
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| US11718899B1 (en) | 2022-03-01 | 2023-08-08 | Hefei University Of Technology | Preparation method of cemented carbide with iron, cobalt and copper medium-entropy alloy as binding phase |
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