CN109434122A - Without metallic binding phase Talide composite material and preparation method - Google Patents
Without metallic binding phase Talide composite material and preparation method Download PDFInfo
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- CN109434122A CN109434122A CN201811472697.7A CN201811472697A CN109434122A CN 109434122 A CN109434122 A CN 109434122A CN 201811472697 A CN201811472697 A CN 201811472697A CN 109434122 A CN109434122 A CN 109434122A
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- 239000002131 composite material Substances 0.000 title claims abstract description 111
- 241001080061 Talides Species 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims description 8
- 238000005245 sintering Methods 0.000 claims abstract description 86
- 238000000227 grinding Methods 0.000 claims abstract description 68
- 239000000843 powder Substances 0.000 claims abstract description 65
- 238000000498 ball milling Methods 0.000 claims abstract description 54
- 238000002156 mixing Methods 0.000 claims abstract description 47
- 239000000203 mixture Substances 0.000 claims description 85
- 238000010438 heat treatment Methods 0.000 claims description 71
- 239000002994 raw material Substances 0.000 claims description 51
- 239000000463 material Substances 0.000 claims description 38
- 238000001816 cooling Methods 0.000 claims description 36
- 229910052799 carbon Inorganic materials 0.000 claims description 32
- 239000002270 dispersing agent Substances 0.000 claims description 23
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 21
- 239000010936 titanium Substances 0.000 claims description 21
- 229910052719 titanium Inorganic materials 0.000 claims description 21
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims description 21
- 238000004321 preservation Methods 0.000 claims description 18
- 230000001681 protective effect Effects 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 4
- 238000003701 mechanical milling Methods 0.000 claims description 3
- 125000003158 alcohol group Chemical group 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims 1
- 229910045601 alloy Inorganic materials 0.000 abstract description 56
- 239000000956 alloy Substances 0.000 abstract description 56
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 abstract description 38
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 31
- 229910002804 graphite Inorganic materials 0.000 abstract description 16
- 239000010439 graphite Substances 0.000 abstract description 16
- 229910052751 metal Inorganic materials 0.000 abstract description 7
- 239000002184 metal Substances 0.000 abstract description 7
- 230000007704 transition Effects 0.000 abstract description 5
- 150000001247 metal acetylides Chemical class 0.000 abstract description 4
- 230000001133 acceleration Effects 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 230000018984 mastication Effects 0.000 abstract description 3
- 238000010077 mastication Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 107
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 60
- 229910052786 argon Inorganic materials 0.000 description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 16
- 230000008859 change Effects 0.000 description 15
- 238000001514 detection method Methods 0.000 description 15
- 238000005498 polishing Methods 0.000 description 15
- 238000007789 sealing Methods 0.000 description 15
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 15
- 229910052721 tungsten Inorganic materials 0.000 description 15
- 239000010937 tungsten Substances 0.000 description 15
- 238000005406 washing Methods 0.000 description 15
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005551 mechanical alloying Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910009043 WC-Co Inorganic materials 0.000 description 1
- 229910000905 alloy phase Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process 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
- 229910052742 iron Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- 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
- B22F3/1017—Multiple heating or additional steps
-
- 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
-
- 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
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/042—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling using a particular milling fluid
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention belongs to technical field of composite materials, are related to a kind of no metallic binding phase Talide composite material, and Talide composite material is trielement composite material, including WC and TiC0.4, further include VC, NbC or TaC, each group is divided into equimolar ratio, granular size 100nm.Carbide powder after ball milling is packed into graphite grinding tool after mixing, carries out discharge plasma sintering, and sintering pressure 30-50MPa 1400-1800 DEG C of sintering temperature, keeps the temperature 10-30min, is made without metallic binding phase Talide composite material.The present invention utilizes TiC0.4In vacancy can reduce sintering temperature acceleration of sintering, on this basis with the complex sintered formation of tungsten carbide and other transition group refractory carbides without metal adhesive tungsten carbide composite, the shortcomings that overcoming the hot mastication of traditional WC hard alloy leads to performance failure, its hardness and fracture toughness are improved simultaneously, solves the problems, such as transition group carbide compared with hard-to-sinter.
Description
Technical field
The invention belongs to technical field of composite materials, are related to a kind of no metallic binding phase Talide composite material
And preparation method thereof.
Background technique
With the continuous development that WC hard alloy is applied in related industry, the requirement to its performance is higher and higher, therefore develops
Simultaneously there is the novel WC hard alloy of high rigidity and high tenacity to seem extremely important out.But it is either traditional or super
Thin and nanocrystalline WC base cemented carbide is to be combined by metal phase (such as Co, Ni, Fe) and provide enough fractures by metal phase
Toughness, Vickers hardness are about 16GPa, and fracture toughness is 8~14MPam1/2.Exactly because however also metallic binding phase is deposited
The performance of WC hard alloy is restricted, and is hampering its application in high temperature, high speed and strong corrosive environment.Without gold
Belonging to Binder Phase WC hard alloy is a kind of novel WC hard alloy developed in recent years, by pure WC or WC and various metal carbides
Composition.Since it is without the metallic binding phases such as Co, Ni, no metallic binding phase WC hard alloy and traditional WC-Co hard alloy phase
Than having better polishability, higher hardness, deformation resistance and corrosion resistance.Kuo-Ming Tsai uses the WC after refinement
Powder obtains the pure WC cemented carbide sintered body that relative density is 95.1%, Vickers using GPS sintering technology at 1860 DEG C
Hardness is 17GPa, fracture toughness 5.97MPam1/2.It is improved compared with conventional rigid alloy rigidity, toughness decreases, still
Deformation resistance, corrosion resistance, oxidation resistance etc. increase [Kuo-MingTsai.The effect
ofconsolidationparameters on the mechanicalproperties ofbinderless tungsten
carbide.International Journal ofRefractory Metals and HardMaterials[J],2011,
29:188-201]。
Summary of the invention
In view of the deficiencies of the prior art, the non-stoichiometric TiC that the present invention prepares mechanical alloying method (MA)0.4With
It is hard without metallic binding phase tungsten carbide using discharge plasma sintering (SPS) preparation that the powder such as WC, NbC, VC of refinement carry out mixing
Matter alloy composite materials, utilize TiC0.4In vacancy can reduce sintering temperature acceleration of sintering, on this basis with tungsten carbide and its
The complex sintered formation of his transition group refractory carbides overcomes traditional WC hard alloy without metal adhesive tungsten carbide composite
Hot mastication causes the shortcomings that performance failure, while improving its hardness and fracture toughness.
The present invention is implemented as follows:
A kind of no metallic binding phase Talide composite material, the Talide composite material are three
First composite material, including WC and TiC0.4, further include VC, NbC or TaC, each group is divided into equimolar ratio, granular size 100nm.
Preferably, WC, VC and TiC0.4Molar ratio be 1:1:1, mass fraction 61.5%, 19.7% and 18.8%.
Preferably, WC, NbC and TiC0.4Molar ratio be 1:1:1, mass fraction is respectively 54.1%, 29.3% and
16.6%.
Preferably, WC, TaC and TiC0.4Molar ratio be 1:1:1, mass fraction is respectively 43.7%, 43.0% and
13.3%.
Preferably, the TiC0.4It is prepared by the titanium carbide powder and titanium valve of molar ratio 4:6.
A kind of preparation method of above-mentioned no metallic binding phase Talide composite material comprising following step
It is rapid:
S1, ball is carried out after dispersing agent is added in the titanium carbide powder of default molar ratio and the raw material powder of titanium valve composition
The TiC of 100nm is made in mill, ratio of grinding media to material 20:1, revolving speed 600r/min, ball milling 21h0.4；
S2, by TaC, NbC and VC it is one such with WC powder equimolar than carrying out ball mill mixing, ratio of grinding media to material 10:1,
Revolving speed is 300r/min, and the mixture of 100nm is obtained after ball milling 10h；
S3, the TiC for obtaining step S10.4The mixture obtained with step S2, than carrying out mixing, is filled out with equimolar after mixing
Enter and carries out discharge plasma sintering in grinding tool, sintering pressure 30-50MPa, 1400-1800 DEG C of sintering temperature, soaking time 10-
30min, it is cooling that when cooling, is filled with protective gas, is made without metallic binding phase Talide composite material.
Preferably, the dispersing agent is alcohol, and the dispersing agent of 0.1mL is added in the raw material powder of every 10g.
Preferably, step S1, the mechanical milling process of S2 and S3 is all made of two kinds of WC sintered carbide balls of 8mm and 5mm.
Preferably, step S3 mixing revolving speed is 300r/min, mixing time 10h.
Preferably, the discharge plasma sintering process of step S3 specifically: with the heating rate of 110 DEG C/min from room temperature liter
To 571 DEG C, 600 DEG C are raised to from 571 DEG C with the heating rate of 30 DEG C/min, in 600 DEG C of heat preservation 5min, with the liter of 100 DEG C/min
Warm rate is raised to 1300 DEG C from 600 DEG C, then respectively with 80 DEG C/min, 70 DEG C/min, 50 DEG C/min, 30 DEG C/min, 15 DEG C/min
Heating rate be raised to 1400 DEG C, 1500 DEG C, 1600 DEG C, 1700 DEG C, 1800 DEG C respectively from 1300 DEG C, protected after reaching sintering temperature
Warm 10-30min.
Compared with prior art, the invention has the following advantages:
The non-stoichiometric TiC that the present invention prepares mechanical alloying method (MA)0.4With the powder such as WC, NbC, VC of refinement
End carries out mixing using discharge plasma sintering (SPS) preparation without metallic binding phase Talide composite material, utilizes
TiC0.4In vacancy can reduce sintering temperature acceleration of sintering, on this basis with tungsten carbide and other transition group refractory carbides
Complex sintered formation overcomes the hot mastication of traditional WC hard alloy that performance is caused to be lost without metal adhesive tungsten carbide composite
The shortcomings that effect, while its hardness and fracture toughness are improved, solve the problems, such as transition group carbide compared with hard-to-sinter.
Specific embodiment
It will be detailed below exemplary embodiment of the present invention, feature and aspect of performance.
A kind of no metallic binding phase Talide composite material, Talide composite material are multiple for ternary
Condensation material, including WC and TiC0.4, further include VC, NbC or TaC, each group is divided into equimolar ratio, granular size 100nm.WC,VC
And TiC0.4Molar ratio be 1:1:1, mass fraction 61.5%, 19.7% and 18.8%.WC, NbC and TiC0.4Molar ratio
For 1:1:1, mass fraction is respectively 54.1%, 29.3% and 16.6%.WC, TaC and TiC0.4Molar ratio be 1:1:1, quality
Score is respectively 43.7%, 43.0% and 13.3%.
TiC0.4It is prepared by the titanium carbide powder and titanium valve of molar ratio 4:6.
A kind of preparation method of above-mentioned no metallic binding phase Talide composite material comprising following step
It is rapid:
S1, after alcohol is added as dispersing agent in the raw material powder of titanium carbide powder and the titanium valve composition of default molar ratio
Ball milling, ratio of grinding media to material 20:1, revolving speed 600r/min are carried out, the TiC of 100nm is made in ball milling 21h0.4；
S2, by TaC, NbC and VC it is one such with WC powder equimolar than carrying out ball mill mixing, ratio of grinding media to material 10:1,
Revolving speed is 300r/min, and the mixture of 100nm is obtained after ball milling 10h；
S3, the TiC for obtaining step S10.4With equimolar than progress mixing, revolving speed is the mixture obtained with step S2
300r/min, mixing time 10h are inserted in grinding tool after mixing and are carried out discharge plasma sintering, sintering pressure 30-50MPa,
1400-1800 DEG C of sintering temperature, 571 DEG C are raised to from room temperature with the heating rate of 110 DEG C/min, with the heating rate of 30 DEG C/min
600 DEG C are raised to from 571 DEG C, in 600 DEG C of heat preservation 5min, is raised to 1300 DEG C from 600 DEG C with the heating rate of 100 DEG C/min, then divide
It is not raised to respectively with 80 DEG C/min, 70 DEG C/min, 50 DEG C/min, 30 DEG C/min, the heating rate of 15 DEG C/min from 1300 DEG C
1400 DEG C, 1500 DEG C, 1600 DEG C, 1700 DEG C, 1800 DEG C reach and keep the temperature 10-30min after sintering temperature, and when cooling is filled with protection
Gas cooling is made without metallic binding phase Talide composite material.
Preferably, the dosage of dispersing agent is the dispersing agent that 0.1mL is added in the raw material powder of every 10g.
Preferably, step S1, the mechanical milling process of S2 and S3 is all made of two kinds of WC sintered carbide balls of 8mm and 5mm.
Embodiment 1
The WC composite material for preparing 20g is as shown in the table using the dosage of composition of raw materials:
Table 1 prepares the composition of raw materials table of 20g tungsten carbide composite
S1, the alcohol that 0.1mL is added in the raw material powder of the titanium valve composition of the titanium carbide powder and 5.45g of 4.55g are made
To be put into hard alloy tank after dispersing agent, ratio of grinding media to material 20:1, ball-milling medium is that diameter is 8mm and the sintered carbide ball of 5mm,
It is put into the operating cavity body of ball mill after carrying out gas washing repeatedly in glove box transitional storehouse, gases used is argon gas, covers sealing
Lid, guarantee are managed to take out under interior ar gas environment and be put into ball mill, and after rotational speed of ball-mill 600r/min, ball milling 21h, TiC is made0.4；
S2, it the VC powder of the WC of 12.29g and 3.95g is put into WC hard alloy tank carries out ball mill mixing, ratio of grinding media to material is
The mixture of the WC and VC of 100nm are obtained after 10:1, ball milling 10h；
S3, the TiC by 3.76g0.4After carrying out mixing on high energy ball mill with the mixture of the WC and VC of step S2, fill out
Enter and carry out discharge plasma sintering in the graphite grinding tool of 20mm, grinding tool is placed on sintering platform, is filled with argon gas protection gas, pressurizes,
Sintering pressure is 30MPa, is raised to 571 DEG C from room temperature with the heating rate of 110 DEG C/min, with the heating rate of 30 DEG C/min from
571 DEG C are raised to 600 DEG C, in 600 DEG C of heat preservation 5min, are raised to 1300 DEG C from 600 DEG C with the heating rate of 100 DEG C/min, then with 80
DEG C/heating rate of min from 1300 DEG C be raised to 1400 DEG C after, keep the temperature 30min, it is cooling that when cooling is filled with protective gas, and carbon is made
Change tungsten hard alloy composite material.
Tissue and performance detection, gained sintering will be carried out after the sintered tungsten carbide composite sample sanding and polishing of SPS
Block technical parameter is as follows:
The performance parameter of composite sinter in 2 embodiment 1 of table
Embodiment 2
The WC composite material for preparing 20g is as shown in the table using the dosage of composition of raw materials:
Table 3 prepares the composition of raw materials table of 20g tungsten carbide composite
S1, the alcohol that 0.1mL is added in the raw material powder of the titanium valve composition of the titanium carbide powder and 5.45g of 4.55g are made
To be put into hard alloy tank after dispersing agent, ratio of grinding media to material 20:1, ball-milling medium is that diameter is 8mm and the sintered carbide ball of 5mm,
It is put into the operating cavity body of ball mill after carrying out gas washing repeatedly in glove box transitional storehouse, gases used is argon gas, covers sealing
Lid, guarantee are managed to take out under interior ar gas environment and be put into ball mill, and after rotational speed of ball-mill 600r/min, ball milling 21h, TiC is made0.4；
S2, it the VC powder of the WC of 12.29g and 3.95g is put into WC hard alloy tank carries out ball mill mixing, ratio of grinding media to material is
The mixture of the WC and VC of 100nm are obtained after 10:1, ball milling 10h；
S3, the TiC by 3.76g0.4After carrying out mixing on high energy ball mill with the mixture of the WC and VC of step S2, fill out
Enter and carry out discharge plasma sintering in the graphite grinding tool of 20mm, grinding tool is placed on sintering platform, is filled with argon gas protection gas, pressurizes,
Sintering pressure is 40MPa, is raised to 571 DEG C from room temperature with the heating rate of 110 DEG C/min, with the heating rate of 30 DEG C/min from
571 DEG C are raised to 600 DEG C, in 600 DEG C of heat preservation 5min, are raised to 1300 DEG C from 600 DEG C with the heating rate of 100 DEG C/min, then with 70
DEG C/heating rate of min from 1300 DEG C be raised to 1500 DEG C after, keep the temperature 20min, it is cooling that when cooling is filled with protective gas, and carbon is made
Change tungsten hard alloy composite material.
Tissue and performance detection, gained sintering will be carried out after the sintered tungsten carbide composite sample sanding and polishing of SPS
Block technical parameter is as follows:
The performance parameter of composite sinter in 4 embodiment 2 of table
Embodiment 3
The WC composite material for preparing 20g is as shown in the table using the dosage of composition of raw materials:
Table 5 prepares the composition of raw materials table of 20g tungsten carbide composite
S1, the alcohol that 0.1mL is added in the raw material powder of the titanium valve composition of the titanium carbide powder and 5.45g of 4.55g are made
To be put into hard alloy tank after dispersing agent, ratio of grinding media to material 20:1, ball-milling medium is that diameter is 8mm and the sintered carbide ball of 5mm,
It is put into the operating cavity body of ball mill after carrying out gas washing repeatedly in glove box transitional storehouse, gases used is argon gas, covers sealing
Lid, guarantee are managed to take out under interior ar gas environment and be put into ball mill, and after rotational speed of ball-mill 600r/min, ball milling 21h, TiC is made0.4；
S2, it the VC powder of the WC of 12.29g and 3.95g is put into WC hard alloy tank carries out ball mill mixing, ratio of grinding media to material is
The mixture of the WC and VC of 100nm are obtained after 10:1, ball milling 10h；
S3, the TiC by 3.76g0.4After carrying out mixing on high energy ball mill with the mixture of the WC and VC of step S2, fill out
Enter and carry out discharge plasma sintering in the graphite grinding tool of 20mm, grinding tool is placed on sintering platform, is filled with argon gas protection gas, pressurizes,
Sintering pressure is 50MPa, is raised to 571 DEG C from room temperature with the heating rate of 110 DEG C/min, with the heating rate of 30 DEG C/min from
571 DEG C are raised to 600 DEG C, in 600 DEG C of heat preservation 5min, are raised to 1300 DEG C from 600 DEG C with the heating rate of 100 DEG C/min, then with 50
DEG C/heating rate of min from 1300 DEG C be raised to 1600 DEG C after, keep the temperature 10min, it is cooling that when cooling is filled with protective gas, and carbon is made
Change tungsten hard alloy composite material.
Tissue and performance detection, gained sintering will be carried out after the sintered tungsten carbide composite sample sanding and polishing of SPS
Block technical parameter is as follows:
The performance parameter of composite sinter in 6 embodiment 3 of table
Embodiment 4
The WC composite material for preparing 20g is as shown in the table using the dosage of composition of raw materials:
Table 7 prepares the composition of raw materials table of 20g tungsten carbide composite
S1, the alcohol that 0.1mL is added in the raw material powder of the titanium valve composition of the titanium carbide powder and 5.45g of 4.55g are made
To be put into hard alloy tank after dispersing agent, ratio of grinding media to material 20:1, ball-milling medium is that diameter is 8mm and the sintered carbide ball of 5mm,
It is put into the operating cavity body of ball mill after carrying out gas washing repeatedly in glove box transitional storehouse, gases used is argon gas, covers sealing
Lid, guarantee are managed to take out under interior ar gas environment and be put into ball mill, and after rotational speed of ball-mill 600r/min, ball milling 21h, TiC is made0.4；
S2, it the VC powder of the WC of 12.29g and 3.95g is put into WC hard alloy tank carries out ball mill mixing, ratio of grinding media to material is
The mixture of the WC and VC of 100nm are obtained after 10:1, ball milling 10h；
S3, the TiC by 3.76g0.4After carrying out mixing on high energy ball mill with the mixture of the WC and VC of step S2, fill out
Enter and carry out discharge plasma sintering in the graphite grinding tool of 20mm, grinding tool is placed on sintering platform, is filled with argon gas protection gas, pressurizes,
Sintering pressure is 50MPa, is raised to 571 DEG C from room temperature with the heating rate of 110 DEG C/min, with the heating rate of 30 DEG C/min from
571 DEG C are raised to 600 DEG C, in 600 DEG C of heat preservation 5min, are raised to 1300 DEG C from 600 DEG C with the heating rate of 100 DEG C/min, then with 30
DEG C/heating rate of min from 1300 DEG C be raised to 1700 DEG C after, keep the temperature 30min, it is cooling that when cooling is filled with protective gas, and carbon is made
Change tungsten hard alloy composite material.
Tissue and performance detection, gained sintering will be carried out after the sintered tungsten carbide composite sample sanding and polishing of SPS
Block technical parameter is as follows:
The performance parameter of composite sinter in 8 embodiment 4 of table
Embodiment 5
The WC composite material for preparing 20g is as shown in the table using the dosage of composition of raw materials:
Table 9 prepares the composition of raw materials table of 20g tungsten carbide composite
S1, the alcohol that 0.1mL is added in the raw material powder of the titanium valve composition of the titanium carbide powder and 5.45g of 4.55g are made
To be put into hard alloy tank after dispersing agent, ratio of grinding media to material 20:1, ball-milling medium is that diameter is 8mm and the sintered carbide ball of 5mm,
It is put into the operating cavity body of ball mill after carrying out gas washing repeatedly in glove box transitional storehouse, gases used is argon gas, covers sealing
Lid, guarantee are managed to take out under interior ar gas environment and be put into ball mill, and after rotational speed of ball-mill 600r/min, ball milling 21h, TiC is made0.4；
S2, it the VC powder of the WC of 12.29g and 3.95g is put into WC hard alloy tank carries out ball mill mixing, ratio of grinding media to material is
The mixture of the WC and VC of 100nm are obtained after 10:1, ball milling 10h；
S3, the TiC by 3.76g0.4After carrying out mixing on high energy ball mill with the mixture of the WC and VC of step S2, fill out
Enter and carry out discharge plasma sintering in the graphite grinding tool of 20mm, grinding tool is placed on sintering platform, is filled with argon gas protection gas, pressurizes,
Sintering pressure is 40MPa, is raised to 571 DEG C from room temperature with the heating rate of 110 DEG C/min, with the heating rate of 30 DEG C/min from
571 DEG C are raised to 600 DEG C, in 600 DEG C of heat preservation 5min, are raised to 1300 DEG C from 600 DEG C with the heating rate of 100 DEG C/min, then with 15
DEG C/heating rate of min from 1300 DEG C be raised to 1800 DEG C after, keep the temperature 10min, it is cooling that when cooling is filled with protective gas, and carbon is made
Change tungsten hard alloy composite material.
Tissue and performance detection, gained sintering will be carried out after the sintered tungsten carbide composite sample sanding and polishing of SPS
Block technical parameter is as follows:
The performance parameter of composite sinter in 10 embodiment 5 of table
Embodiment 6
The WC composite material for preparing 20g is as shown in the table using the dosage of composition of raw materials:
Table 11 prepares the composition of raw materials table of 20g tungsten carbide composite
S1, the alcohol that 0.1mL is added in the raw material powder of the titanium valve composition of the titanium carbide powder and 5.45g of 4.55g are made
To be put into hard alloy tank after dispersing agent, ratio of grinding media to material 20:1, ball-milling medium is that diameter is 8mm and the sintered carbide ball of 5mm,
It is put into the operating cavity body of ball mill after carrying out gas washing repeatedly in glove box transitional storehouse, gases used is argon gas, covers sealing
Lid, guarantee are managed to take out under interior ar gas environment and be put into ball mill, and after rotational speed of ball-mill 600r/min, ball milling 21h, TiC is made0.4；
S2, it the NbC powder of the WC of 10.83g and 5.86g is put into WC hard alloy tank carries out ball mill mixing, ratio of grinding media to material
For 10:1, the mixture of the WC and NbC of 100nm are obtained after ball milling 10h；
S3, the TiC by 3.31g0.4After carrying out mixing on high energy ball mill with the mixture of the WC and NbC of step S2, fill out
Enter and carry out discharge plasma sintering in the graphite grinding tool of 20mm, grinding tool is placed on sintering platform, is filled with argon gas protection gas, pressurizes,
Sintering pressure is 30MPa, is raised to 571 DEG C from room temperature with the heating rate of 110 DEG C/min, with the heating rate of 30 DEG C/min from
571 DEG C are raised to 600 DEG C, in 600 DEG C of heat preservation 5min, are raised to 1300 DEG C from 600 DEG C with the heating rate of 100 DEG C/min, then with 80
DEG C/heating rate of min from 1300 DEG C be raised to 1400 DEG C after, keep the temperature 10min, it is cooling that when cooling is filled with protective gas, and carbon is made
Change tungsten hard alloy composite material.
Tissue and performance detection, gained sintering will be carried out after the sintered tungsten carbide composite sample sanding and polishing of SPS
Block technical parameter is as follows:
The performance parameter of composite sinter in 12 embodiment 6 of table
Embodiment 7
The WC composite material for preparing 20g is as shown in the table using the dosage of composition of raw materials:
Table 13 prepares the composition of raw materials table of 20g tungsten carbide composite
S1, the alcohol that 0.1mL is added in the raw material powder of the titanium valve composition of the titanium carbide powder and 5.45g of 4.55g are made
To be put into hard alloy tank after dispersing agent, ratio of grinding media to material 20:1, ball-milling medium is that diameter is 8mm and the sintered carbide ball of 5mm,
It is put into the operating cavity body of ball mill after carrying out gas washing repeatedly in glove box transitional storehouse, gases used is argon gas, covers sealing
Lid, guarantee are managed to take out under interior ar gas environment and be put into ball mill, and after rotational speed of ball-mill 600r/min, ball milling 21h, TiC is made0.4；
S2, it the NbC powder of the WC of 10.83g and 5.86g is put into WC hard alloy tank carries out ball mill mixing, ratio of grinding media to material
For 10:1, the mixture of the WC and NbC of 100nm are obtained after ball milling 10h；
S3, the TiC by 3.31g0.4After carrying out mixing on high energy ball mill with the mixture of the WC and NbC of step S2, fill out
Enter and carry out discharge plasma sintering in the graphite grinding tool of 20mm, grinding tool is placed on sintering platform, is filled with argon gas protection gas, pressurizes,
Sintering pressure is 40MPa, is raised to 571 DEG C from room temperature with the heating rate of 110 DEG C/min, with the heating rate of 30 DEG C/min from
571 DEG C are raised to 600 DEG C, in 600 DEG C of heat preservation 5min, are raised to 1300 DEG C from 600 DEG C with the heating rate of 100 DEG C/min, then with 70
DEG C/heating rate of min from 1300 DEG C be raised to 1500 DEG C after, keep the temperature 20min, it is cooling that when cooling is filled with protective gas, and carbon is made
Change tungsten hard alloy composite material.
Tissue and performance detection, gained sintering will be carried out after the sintered tungsten carbide composite sample sanding and polishing of SPS
Block technical parameter is as follows:
The performance parameter of composite sinter in 14 embodiment 7 of table
Embodiment 8
The WC composite material for preparing 20g is as shown in the table using the dosage of composition of raw materials:
Table 15 prepares the composition of raw materials table of 20g tungsten carbide composite
S1, the alcohol that 0.1mL is added in the raw material powder of the titanium valve composition of the titanium carbide powder and 5.45g of 4.55g are made
To be put into hard alloy tank after dispersing agent, ratio of grinding media to material 20:1, ball-milling medium is that diameter is 8mm and the sintered carbide ball of 5mm,
It is put into the operating cavity body of ball mill after carrying out gas washing repeatedly in glove box transitional storehouse, gases used is argon gas, covers sealing
Lid, guarantee are managed to take out under interior ar gas environment and be put into ball mill, and after rotational speed of ball-mill 600r/min, ball milling 21h, TiC is made0.4；
S2, it the NbC powder of the WC of 10.83g and 5.86g is put into WC hard alloy tank carries out ball mill mixing, ratio of grinding media to material
For 10:1, the mixture of the WC and NbC of 100nm are obtained after ball milling 10h；
S3, the TiC by 3.31g0.4After carrying out mixing on high energy ball mill with the mixture of the WC and NbC of step S2, fill out
Enter and carry out discharge plasma sintering in the graphite grinding tool of 20mm, grinding tool is placed on sintering platform, is filled with argon gas protection gas, pressurizes,
Sintering pressure is 50MPa, is raised to 571 DEG C from room temperature with the heating rate of 110 DEG C/min, with the heating rate of 30 DEG C/min from
571 DEG C are raised to 600 DEG C, in 600 DEG C of heat preservation 5min, are raised to 1300 DEG C from 600 DEG C with the heating rate of 100 DEG C/min, then with 50
DEG C/heating rate of min from 1300 DEG C be raised to 1600 DEG C after, keep the temperature 30min, it is cooling that when cooling is filled with protective gas, and carbon is made
Change tungsten hard alloy composite material.
Tissue and performance detection, gained sintering will be carried out after the sintered tungsten carbide composite sample sanding and polishing of SPS
Block technical parameter is as follows:
The performance parameter of composite sinter in 16 embodiment 8 of table
Embodiment 9
The WC composite material for preparing 20g is as shown in the table using the dosage of composition of raw materials:
Table 17 prepares the composition of raw materials table of 20g tungsten carbide composite
S1, the alcohol that 0.1mL is added in the raw material powder of the titanium valve composition of the titanium carbide powder and 5.45g of 4.55g are made
To be put into hard alloy tank after dispersing agent, ratio of grinding media to material 20:1, ball-milling medium is that diameter is 8mm and the sintered carbide ball of 5mm,
It is put into the operating cavity body of ball mill after carrying out gas washing repeatedly in glove box transitional storehouse, gases used is argon gas, covers sealing
Lid, guarantee are managed to take out under interior ar gas environment and be put into ball mill, and after rotational speed of ball-mill 600r/min, ball milling 21h, TiC is made0.4；
S2, it the NbC powder of the WC of 10.83g and 5.86g is put into WC hard alloy tank carries out ball mill mixing, ratio of grinding media to material
For 10:1, the mixture of the WC and NbC of 100nm are obtained after ball milling 10h；
S3, the TiC by 3.31g0.4After carrying out mixing on high energy ball mill with the mixture of the WC and NbC of step S2, fill out
Enter and carry out discharge plasma sintering in the graphite grinding tool of 20mm, grinding tool is placed on sintering platform, is filled with argon gas protection gas, pressurizes,
Sintering pressure is 30MPa, is raised to 571 DEG C from room temperature with the heating rate of 110 DEG C/min, with the heating rate of 30 DEG C/min from
571 DEG C are raised to 600 DEG C, in 600 DEG C of heat preservation 5min, are raised to 1300 DEG C from 600 DEG C with the heating rate of 100 DEG C/min, then with 30
DEG C/heating rate of min from 1300 DEG C be raised to 1700 DEG C after, keep the temperature 20min, it is cooling that when cooling is filled with protective gas, and carbon is made
Change tungsten hard alloy composite material.
Tissue and performance detection, gained sintering will be carried out after the sintered tungsten carbide composite sample sanding and polishing of SPS
Block technical parameter is as follows:
The performance parameter of composite sinter in 18 embodiment 9 of table
Embodiment 10
The WC composite material for preparing 20g is as shown in the table using the dosage of composition of raw materials:
Table 19 prepares the composition of raw materials table of 20g tungsten carbide composite
S1, the alcohol that 0.1mL is added in the raw material powder of the titanium valve composition of the titanium carbide powder and 5.45g of 4.55g are made
To be put into hard alloy tank after dispersing agent, ratio of grinding media to material 20:1, ball-milling medium is that diameter is 8mm and the sintered carbide ball of 5mm,
It is put into the operating cavity body of ball mill after carrying out gas washing repeatedly in glove box transitional storehouse, gases used is argon gas, covers sealing
Lid, guarantee are managed to take out under interior ar gas environment and be put into ball mill, and after rotational speed of ball-mill 600r/min, ball milling 21h, TiC is made0.4；
S2, it the NbC powder of the WC of 10.83g and 5.86g is put into WC hard alloy tank carries out ball mill mixing, ratio of grinding media to material
For 10:1, the mixture of the WC and NbC of 100nm are obtained after ball milling 10h；
S3, the TiC by 3.31g0.4After carrying out mixing on high energy ball mill with the mixture of the WC and NbC of step S2, fill out
Enter and carry out discharge plasma sintering in the graphite grinding tool of 20mm, grinding tool is placed on sintering platform, is filled with argon gas protection gas, pressurizes,
Sintering pressure is 30MPa, is raised to 571 DEG C from room temperature with the heating rate of 110 DEG C/min, with the heating rate of 30 DEG C/min from
571 DEG C are raised to 600 DEG C, in 600 DEG C of heat preservation 5min, are raised to 1300 DEG C from 600 DEG C with the heating rate of 100 DEG C/min, then with 30
DEG C/heating rate of min from 1300 DEG C be raised to 1700 DEG C after, keep the temperature 20min, it is cooling that when cooling is filled with protective gas, and carbon is made
Change tungsten hard alloy composite material.
Tissue and performance detection, gained sintering will be carried out after the sintered tungsten carbide composite sample sanding and polishing of SPS
Block technical parameter is as follows:
The performance parameter of composite sinter in 20 embodiment 10 of table
Embodiment 11
The WC composite material for preparing 20g is as shown in the table using the dosage of composition of raw materials:
Table 21 prepares the composition of raw materials table of 20g tungsten carbide composite
S1, the alcohol that 0.1mL is added in the raw material powder of the titanium valve composition of the titanium carbide powder and 5.45g of 4.55g are made
To be put into hard alloy tank after dispersing agent, ratio of grinding media to material 20:1, ball-milling medium is that diameter is 8mm and the sintered carbide ball of 5mm,
It is put into the operating cavity body of ball mill after carrying out gas washing repeatedly in glove box transitional storehouse, gases used is argon gas, covers sealing
Lid, guarantee are managed to take out under interior ar gas environment and be put into ball mill, and after rotational speed of ball-mill 600r/min, ball milling 21h, TiC is made0.4；
S2, it the TaC powder of the WC of 8.73g and 8.60g is put into WC hard alloy tank carries out ball mill mixing, ratio of grinding media to material is
The mixture of the WC and TaC of 100nm are obtained after 10:1, ball milling 10h；
S3, the TiC by 2.67g0.4After carrying out mixing on high energy ball mill with the mixture of the WC and TaC of step S2, fill out
Enter and carry out discharge plasma sintering in the graphite grinding tool of 20mm, grinding tool is placed on sintering platform, is filled with argon gas protection gas, pressurizes,
Sintering pressure is 30MPa, is raised to 571 DEG C from room temperature with the heating rate of 110 DEG C/min, with the heating rate of 30 DEG C/min from
571 DEG C are raised to 600 DEG C, in 600 DEG C of heat preservation 5min, are raised to 1300 DEG C from 600 DEG C with the heating rate of 100 DEG C/min, then with 80
DEG C/heating rate of min from 1300 DEG C be raised to 1400 DEG C after, keep the temperature 10min, it is cooling that when cooling is filled with protective gas, and carbon is made
Change tungsten hard alloy composite material.
Tissue and performance detection, gained sintering will be carried out after the sintered tungsten carbide composite sample sanding and polishing of SPS
Block technical parameter is as follows:
The performance parameter of composite sinter in 22 embodiment 11 of table
Embodiment 12
The WC composite material for preparing 20g is as shown in the table using the dosage of composition of raw materials:
Table 23 prepares the composition of raw materials table of 20g tungsten carbide composite
S1, the alcohol that 0.1mL is added in the raw material powder of the titanium valve composition of the titanium carbide powder and 5.45g of 4.55g are made
To be put into hard alloy tank after dispersing agent, ratio of grinding media to material 20:1, ball-milling medium is that diameter is 8mm and the sintered carbide ball of 5mm,
It is put into the operating cavity body of ball mill after carrying out gas washing repeatedly in glove box transitional storehouse, gases used is argon gas, covers sealing
Lid, guarantee are managed to take out under interior ar gas environment and be put into ball mill, and after rotational speed of ball-mill 600r/min, ball milling 21h, TiC is made0.4；
S2, it the TaC powder of the WC of 8.73g and 8.60g is put into WC hard alloy tank carries out ball mill mixing, ratio of grinding media to material is
The mixture of the WC and TaC of 100nm are obtained after 10:1, ball milling 10h；
S3, the TiC by 2.67g0.4After carrying out mixing on high energy ball mill with the mixture of the WC and TaC of step S2, fill out
Enter and carry out discharge plasma sintering in the graphite grinding tool of 20mm, grinding tool is placed on sintering platform, is filled with argon gas protection gas, pressurizes,
Sintering pressure is 40MPa, is raised to 571 DEG C from room temperature with the heating rate of 110 DEG C/min, with the heating rate of 30 DEG C/min from
571 DEG C are raised to 600 DEG C, in 600 DEG C of heat preservation 5min, are raised to 1300 DEG C from 600 DEG C with the heating rate of 100 DEG C/min, then with 70
DEG C/heating rate of min from 1300 DEG C be raised to 1500 DEG C after, keep the temperature 20min, it is cooling that when cooling is filled with protective gas, and carbon is made
Change tungsten hard alloy composite material.
Tissue and performance detection, gained sintering will be carried out after the sintered tungsten carbide composite sample sanding and polishing of SPS
Block technical parameter is as follows:
The performance parameter of composite sinter in 24 embodiment 12 of table
Embodiment 13
The WC composite material for preparing 20g is as shown in the table using the dosage of composition of raw materials:
Table 25 prepares the composition of raw materials table of 20g tungsten carbide composite
S1, the alcohol that 0.1mL is added in the raw material powder of the titanium valve composition of the titanium carbide powder and 5.45g of 4.55g are made
To be put into hard alloy tank after dispersing agent, ratio of grinding media to material 20:1, ball-milling medium is that diameter is 8mm and the sintered carbide ball of 5mm,
It is put into the operating cavity body of ball mill after carrying out gas washing repeatedly in glove box transitional storehouse, gases used is argon gas, covers sealing
Lid, guarantee are managed to take out under interior ar gas environment and be put into ball mill, and after rotational speed of ball-mill 600r/min, ball milling 21h, TiC is made0.4；
S2, it the TaC powder of the WC of 8.73g and 8.60g is put into WC hard alloy tank carries out ball mill mixing, ratio of grinding media to material is
The mixture of the WC and TaC of 100nm are obtained after 10:1, ball milling 10h；
S3, the TiC by 2.67g0.4After carrying out mixing on high energy ball mill with the mixture of the WC and TaC of step S2, fill out
Enter and carry out discharge plasma sintering in the graphite grinding tool of 20mm, grinding tool is placed on sintering platform, is filled with argon gas protection gas, pressurizes,
Sintering pressure is 50MPa, is raised to 571 DEG C from room temperature with the heating rate of 110 DEG C/min, with the heating rate of 30 DEG C/min from
571 DEG C are raised to 600 DEG C, in 600 DEG C of heat preservation 5min, are raised to 1300 DEG C from 600 DEG C with the heating rate of 100 DEG C/min, then with 50
DEG C/heating rate of min from 1300 DEG C be raised to 1600 DEG C after, keep the temperature 30min, it is cooling that when cooling is filled with protective gas, and carbon is made
Change tungsten hard alloy composite material.
Tissue and performance detection, gained sintering will be carried out after the sintered tungsten carbide composite sample sanding and polishing of SPS
Block technical parameter is as follows:
The performance parameter of composite sinter in 26 embodiment 13 of table
Embodiment 14
The WC composite material for preparing 20g is as shown in the table using the dosage of composition of raw materials:
Table 27 prepares the composition of raw materials table of 20g tungsten carbide composite
S1, the alcohol that 0.1mL is added in the raw material powder of the titanium valve composition of the titanium carbide powder and 5.45g of 4.55g are made
To be put into hard alloy tank after dispersing agent, ratio of grinding media to material 20:1, ball-milling medium is that diameter is 8mm and the sintered carbide ball of 5mm,
It is put into the operating cavity body of ball mill after carrying out gas washing repeatedly in glove box transitional storehouse, gases used is argon gas, covers sealing
Lid, guarantee are managed to take out under interior ar gas environment and be put into ball mill, and after rotational speed of ball-mill 600r/min, ball milling 21h, TiC is made0.4；
S2, it the TaC powder of the WC of 8.73g and 8.60g is put into WC hard alloy tank carries out ball mill mixing, ratio of grinding media to material is
The mixture of the WC and TaC of 100nm are obtained after 10:1, ball milling 10h；
S3, the TiC by 2.67g0.4After carrying out mixing on high energy ball mill with the mixture of the WC and TaC of step S2, fill out
Enter and carry out discharge plasma sintering in the graphite grinding tool of 20mm, grinding tool is placed on sintering platform, is filled with argon gas protection gas, pressurizes,
Sintering pressure is 30MPa, is raised to 571 DEG C from room temperature with the heating rate of 110 DEG C/min, with the heating rate of 30 DEG C/min from
571 DEG C are raised to 600 DEG C, in 600 DEG C of heat preservation 5min, are raised to 1300 DEG C from 600 DEG C with the heating rate of 100 DEG C/min, then with 30
DEG C/heating rate of min from 1300 DEG C be raised to 1700 DEG C after, keep the temperature 20min, it is cooling that when cooling is filled with protective gas, and carbon is made
Change tungsten hard alloy composite material.
Tissue and performance detection, gained sintering will be carried out after the sintered tungsten carbide composite sample sanding and polishing of SPS
Block technical parameter is as follows:
The performance parameter of composite sinter in 28 embodiment 14 of table
Embodiment 15
The WC composite material for preparing 20g is as shown in the table using the dosage of composition of raw materials:
Table 29 prepares the composition of raw materials table of 20g tungsten carbide composite
S1, the alcohol that 0.1mL is added in the raw material powder of the titanium valve composition of the titanium carbide powder and 5.45g of 4.55g are made
To be put into hard alloy tank after dispersing agent, ratio of grinding media to material 20:1, ball-milling medium is that diameter is 8mm and the sintered carbide ball of 5mm,
It is put into the operating cavity body of ball mill after carrying out gas washing repeatedly in glove box transitional storehouse, gases used is argon gas, covers sealing
Lid, guarantee are managed to take out under interior ar gas environment and be put into ball mill, and after rotational speed of ball-mill 600r/min, ball milling 21h, TiC is made0.4；
S2, it the TaC powder of the WC of 8.73g and 8.60g is put into WC hard alloy tank carries out ball mill mixing, ratio of grinding media to material is
The mixture of the WC and TaC of 100nm are obtained after 10:1, ball milling 10h；
S3, the TiC by 2.67g0.4After carrying out mixing on high energy ball mill with the mixture of the WC and TaC of step S2, fill out
Enter and carry out discharge plasma sintering in the graphite grinding tool of 20mm, grinding tool is placed on sintering platform, is filled with argon gas protection gas, pressurizes,
Sintering pressure is 40MPa, is raised to 571 DEG C from room temperature with the heating rate of 110 DEG C/min, with the heating rate of 30 DEG C/min from
571 DEG C are raised to 600 DEG C, in 600 DEG C of heat preservation 5min, are raised to 1300 DEG C from 600 DEG C with the heating rate of 100 DEG C/min, then with 15
DEG C/heating rate of min from 1300 DEG C be raised to 1800 DEG C after, keep the temperature 20min, it is cooling that when cooling is filled with protective gas, and carbon is made
Change tungsten hard alloy composite material.
Tissue and performance detection, gained sintering will be carried out after the sintered tungsten carbide composite sample sanding and polishing of SPS
Block technical parameter is as follows:
The performance parameter of composite sinter in 30 embodiment 15 of table
To sum up, the consistency of Talide composite material prepared by the present invention is 78.9~99.1%, and hardness is
10.11~22.32GPa, fracture toughness are 5.15~6.50MPa/m1/2, it has excellent performance.
Finally, it should be noted that above-described each embodiment is merely to illustrate technical solution of the present invention, rather than it is limited
System；Although the present invention is described in detail referring to the foregoing embodiments, those skilled in the art should understand that: its
It can still modify to technical solution documented by previous embodiment, or part of or all technical features are carried out
Equivalent replacement；And these modifications or substitutions, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution
Range.
Claims (10)
1. a kind of no metallic binding phase Talide composite material, it is characterised in that: the Talide is multiple
Condensation material is trielement composite material, including WC and TiC0.4, further include VC, NbC or TaC, each group is divided into equimolar ratio, and particle is big
Small is 100nm.
2. no metallic binding phase Talide composite material according to claim 1, it is characterised in that: WC, VC
And TiC0.4Molar ratio be 1:1:1, mass fraction 61.5%, 19.7% and 18.8%.
3. no metallic binding phase Talide composite material according to claim 1, it is characterised in that: WC, NbC
And TiC0.4Molar ratio be 1:1:1, mass fraction is respectively 54.1%, 29.3% and 16.6%.
4. no metallic binding phase Talide composite material according to claim 1, it is characterised in that: WC, TaC
And TiC0.4Molar ratio be 1:1:1, mass fraction is respectively 43.7%, 43.0% and 13.3%.
5. no metallic binding phase Talide composite material according to claim 1, it is characterised in that: described
TiC0.4It is prepared by the titanium carbide powder and titanium valve of molar ratio 4:6.
6. a kind of preparation side without metallic binding phase Talide composite material as described in Claims 1 to 5 is any
Method, it is characterised in that: itself the following steps are included:
S1, ball milling, ball are carried out after dispersing agent is added in the titanium carbide powder of default molar ratio and the raw material powder of titanium valve composition
The TiC of 100nm is made than being 20:1, revolving speed 600r/min, ball milling 21h in material0.4；
S2, one such by TaC, NbC and VC and WC powder equimolar is than carrying out ball mill mixing, ratio of grinding media to material 10:1, revolving speed
For 300r/min, the mixture of 100nm is obtained after ball milling 10h；
S3, the TiC for obtaining step S10.4The mixture obtained with step S2, than carrying out mixing, inserts mill after mixing with equimolar
Carry out discharge plasma sintering in tool, sintering pressure 30-50MPa, 1400-1800 DEG C of sintering temperature, soaking time 10-
30min, it is cooling that when cooling, is filled with protective gas, is made without metallic binding phase Talide composite material.
7. no metallic binding phase Talide composite material according to claim 6, it is characterised in that: described point
Powder is alcohol, and the dispersing agent of 0.1mL is added in the raw material powder of every 10g.
8. no metallic binding phase Talide composite material according to claim 6, it is characterised in that: step
The mechanical milling process of S1, S2 and S3 are all made of two kinds of WC sintered carbide balls of 8mm and 5mm.
9. no metallic binding phase Talide composite material according to claim 6, it is characterised in that: step S3
Mixing revolving speed is 300r/min, mixing time 10h.
10. no metallic binding phase Talide composite material according to claim 6, it is characterised in that: step
The discharge plasma sintering process of S3 specifically: 571 DEG C are raised to from room temperature with the heating rate of 110 DEG C/min, with 30 DEG C/min
Heating rate be raised to 600 DEG C from 571 DEG C, in 600 DEG C of heat preservation 5min, be raised to the heating rate of 100 DEG C/min from 600 DEG C
1300 DEG C, then respectively with 80 DEG C/min, 70 DEG C/min, 50 DEG C/min, 30 DEG C/min, the heating rate of 15 DEG C/min from 1300 DEG C
It is raised to 1400 DEG C, 1500 DEG C, 1600 DEG C, 1700 DEG C, 1800 DEG C respectively, keeps the temperature 10-30min after reaching sintering temperature.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110606745A (en) * | 2019-09-25 | 2019-12-24 | 燕山大学 | Metal-free binder phase tungsten carbide hard alloy composite material and preparation method thereof |
| CN111471908A (en) * | 2020-05-09 | 2020-07-31 | 燕山大学 | TiCx-combined nanocrystalline WC-based hard alloy composite material and preparation method thereof |
| CN113620713A (en) * | 2021-09-07 | 2021-11-09 | 燕山大学 | WC/VCxHard material, method for the production thereof and use thereof |
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| CN115652166B (en) * | 2022-11-04 | 2024-03-08 | 安徽尚欣晶工新材料科技有限公司 | Superhard hard alloy material for ultrahigh-pressure water jet knife and preparation method thereof |
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