CN108624772A - Ultra-fine Grained tungsten carbide base carbide alloy material and preparation method thereof - Google Patents
Ultra-fine Grained tungsten carbide base carbide alloy material and preparation method thereof Download PDFInfo
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- CN108624772A CN108624772A CN201810671837.7A CN201810671837A CN108624772A CN 108624772 A CN108624772 A CN 108624772A CN 201810671837 A CN201810671837 A CN 201810671837A CN 108624772 A CN108624772 A CN 108624772A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- 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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- 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
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Abstract
The invention discloses a kind of Ultra-fine Grained tungsten carbide base carbide alloy materials and preparation method thereof.The Ultra-fine Grained tungsten carbide base carbide alloy includes cobalt 8%, tungsten carbide 90.2%~90.8%, vanadium carbide 0.2%~0.8%, cubic boron nitride 1% by weight percentage.The present invention uses discharge plasma sintering technique, and under vacuum atmosphere protection, with persistently overheating to 1250~1300 DEG C of the heating rate of 100 ± 20 DEG C/min, control pressure is 30 ± 2Mpa, and Ultra-fine Grained tungsten carbide base carbide alloy is made.The hard alloy of the present invention not only has higher hardness, while also good toughness, and the highest sample hardness of comprehensive performance reaches 20.17 ± 0.20GPa, and fracture toughness reaches 12.18 ± 0.2MPa.m1/2, hardness improves 10~20% compared with YG8 hard alloy commercial now, and fracture toughness improves 10%~18%.
Description
Technical field
The invention belongs to discharge plasma sintering (SPS) field of material technology, are related to a kind of Ultra-fine Grained tungsten carbide-base hard
Alloy material and preparation method thereof.
Background technology
Tungsten carbide (WC) based hard alloy material is a kind of high rigidity, high-wearing feature, corrosion resistant material, is suitable for height
The operating mode of the bad environments such as temperature, friction, heavy duty, is also used for the fields such as aerospace component, bearing, high speed cutting tool.When
When crystallite dimension drops to submicrometer scale, intensity, hardness, toughness and the wearability of cemented carbide material can obtain larger
Range improves.Ultra-fine cemented carbide of the size in 0.1~0.6 μ m has while having higher hardness and wearability
There is excellent toughness, there is broader practice foreground.Currently, the conventional sintering technique of WC base cemented carbides mainly has：Reaction is burnt
Knot, pressureless sintering, gas pressure sintering, hot pressed sintering and HIP sintering.But there are many drawbacks for conventional sintering：Equipment and maintenance
It is with high costs；Mode of heating using heat radiation, heat transfer can cause the temperature gradient in material larger, and material internal is easy production
Raw residual stress；Long preparation period, efficiency is low, is unfavorable for the batch production of material.
SPS sintering technologies are a kind of economic, energy saving, efficient, environmentally friendly sintering processings, reduction fast with temperature rate
Sintering temperature, purification particle surface, improve consistency, soaking time it is short can the advantages that.SPS sintering technologies are applied to ceramics
As soon as field of material preparation has become a popular topic in recent years, for WC base cemented carbides, there has also been many at this stage
Open report.(S.G.Huang, K.Vanmeensel, Tailored sintering of VC-doped the WC-Co of document 1
cemented carbides by pulsed electric current sintering,Int J Refract Mater
Hard Mater.26 (2008) 256-262.) WC+12wt.%Co+0.9wt.%VC hard alloy is prepared, existed using SPS technologies
The hardness of 1240 DEG C of heat preservation 2min, hard alloy are 17.3GPa, fracture toughness 9.1MPa.m1/2, crystallite dimension is 0.17 μm,
But the Cemented Carbide Hardness and fracture toughness are relatively low.(Lan Sun, ChengchangJia, the Effects of of document 2
Cr3C2additions on the densification,graingrowth and properties of ultrafine
WC–11Co compositesby spark plasma sintering,Int J Refract MaterHard Mater.26
(2008) 357-361.) WC+11wt.%Co+0.6wt.%Cr is prepared3C2Hard alloy is kept the temperature using SPS technologies at 1200 DEG C
5min, material density obtained are 98.4%, and hardness is 18GPa or so, fracture toughness 13.MPa.m1/2Left and right.It is obtained
For material since more Co is added, toughness is preferable, but material hardness reduces.Document 3 (XIAO Dai-hong, HE
Yue-hui,Effect of VC and NbC additions on microstructure and properties
ofultrafine WC-10Co cemented carbides,Trans.Nonferrous Met.Soc.China.19(2009)
The sintering of hard alloy is studied in 1520-152), 60min, research hair are kept the temperature at 1400 DEG C by inhibitor of VC and NbC
The addition of existing inhibitor can effective crystal grain thinning, the wherein inhibition of VC is best.But both of the above is added then can simultaneously
Cause the decline of performance.
From the foregoing, it will be observed that the sintering process of hard alloy is still not perfect at present, the performance difference for preparing material is bigger, and
And SPS will be intended to be sintered out the higher hard alloy of toughness in existing report, to be usually added and largely cohere phase, this will certainly
The decline for causing hardness has the material preparation of high rigidity and high tenacity also fewer simultaneously under low cobalt state.Therefore to hard
The SPS sintering process of matter alloy is studied and is subject to perfect, optimizes inhibitor and reinforced phase content to improving hard alloy power
It learns performance and its industrialization is promoted to be of great significance.
Invention content
The purpose of the present invention is to provide a kind of Ultra-fine Grained tungsten carbide base carbide alloy materials and preparation method thereof.The material
It is suitable inhibitor (vanadium carbide) and reinforced phase (cubic boron nitride) to be added in tungsten carbide matrix, and inhibit by controlling
The ratio of agent and reinforced phase makes material with the excellent mechanical property of high rigidity and high tenacity.
Realize that the technical solution of the object of the invention is as follows：
Ultra-fine Grained tungsten carbide base carbide alloy material, by weight percentage, including following component：Cobalt (Co) 8%, carbonization
Tungsten (WC) 90.2%~90.8%, vanadium carbide (VC) 0.2%~0.8%, cubic boron nitride (cBN) 1%.
Further, the present invention also provides the preparation methods of above-mentioned Ultra-fine Grained tungsten carbide base carbide alloy material, using height
Energy-efficient sintering technology is imitated, by optimizing the technological parameters such as sintering temperature, soaking time, realization is prepared in a short time to be had
The cemented carbide material of higher comprehensive mechanical property, includes the following steps：
Step 1, Co, WC, VC and cBN powder are weighed in proportion, are mixed, at room temperature using absolute ethyl alcohol as concussion medium,
Carry out ultrasonic vibration, stirring, mixed powder；
Step 2, mixed powder is dried, is ground, sieving；
Step 3, the powder of sieving is directly poured into mold, carries out precompressed；
Step 4, it in vacuum environment, using discharge plasma sintering process, is held with the heating rate of 100 ± 20 DEG C/min
Continuous to be warming up to 1250~1300 DEG C, control pressure is 30 ± 2Mpa, heat preservation, subsequent furnace cooling, obtained Ultra-fine Grained tungsten carbide-base
Hard alloy.
In step 1, the concussion incorporation time is 2~3 hours.
In step 2, the drying temperature is 100~120 DEG C, and the mesh number of sieve is 100 mesh.
In step 3, the precompressed pressure is 10~30Mpa, and the dwell time is 2~4min.
In step 4, it is evacuated to 5~8pa and forms vacuum environment, soaking time is 4~6min, preferably 5min.
Compared with prior art, the present invention its remarkable advantage is：
(1) compared with hard alloy on the market, crystal grain is more tiny, and crystallite dimension keeps 238~248nm, is ultra-fine
Cemented carbide；
(2) it by the synergistic effect of inhibitor and reinforced phase, uses the Ultra-fine Grained hard that SPS sintering technologies are prepared and closes
Gold utensil has excellent mechanical property and a heterogeneous microstructure, the wherein highest sample hardness of comprehensive performance up to 20.17 ± 0.20GPa,
Fracture toughness is up to 12.18 ± 0.02MPa.m1/2, hardness improves 10~20% compared with YG8 hard alloy commercial now, breaks
It splits toughness and improves 10%~18%.
Specific implementation mode
The present invention is described in further details with reference to embodiment.
Embodiment 1
Co 8%, WC90.8%, VC 0.2%, cBN 1% carry out dispensing by weight percent, are to be situated between with absolute ethyl alcohol
Matter is put into concussion in boronation conical flask plus stirs 2 hours, and in due course addition clear water is to ensure water temperature always during earthquake
In room temperature；Grinding is dried after concussion mixing, and is sieved with 100 mesh sieve, the mixed-powder prepared is added directly into graphite jig,
Pressurize 3 minutes under 10Mpa pressure；The green compact pressed through in advance is put into attemperator to be placed in discharge plasma sintering stove, it will
Vacuum state in furnace chamber, pressure to 6pa, application pressure are 30Mpa；Sample is heated with the heating rate of 100 DEG C/min
To 1300 DEG C, 5min, then furnace cooling are kept the temperature.After tested, consistency is the 98.3% of material, Vickers hardness 20.17
± 0.2GPa, fracture toughness are 12.18 ± 0.2MPa.m1/2, average grain size 246nm.
Embodiment 2
Co 8%, WC 90.5%, VC 0.5%, cBN 1% carry out dispensing by weight percent, are to be situated between with absolute ethyl alcohol
Matter is put into concussion in boronation conical flask plus stirs 2 hours, and in due course addition clear water is to ensure water temperature always during earthquake
In room temperature；Grinding is dried after concussion mixing, and is sieved with 100 mesh sieve, the mixed-powder prepared is added directly into graphite jig,
Pressurize 3 minutes under 10Mpa pressure；The green compact pressed through in advance is put into attemperator to be placed in discharge plasma sintering stove, it will
Vacuum state in furnace chamber, pressure to 6pa, application pressure are 30Mpa；Sample is heated with the heating rate of 100 DEG C/min
To 1300 DEG C, 5min, then furnace cooling are kept the temperature.After tested, consistency is the 97.4% of material, Vickers hardness 19.86
± 0.2GPa, fracture toughness are 10.62 ± 0.2MPa.m1/2, average grain size 241nm.
Embodiment 3
Co 8%, WC 90.2%, VC 0.8%, cBN 1% carry out dispensing by weight percent, are to be situated between with absolute ethyl alcohol
Matter is put into concussion in boronation conical flask plus stirs 2 hours, and in due course addition clear water is to ensure water temperature always during earthquake
In room temperature；Grinding is dried after concussion mixing, and is sieved with 100 mesh sieve, the mixed-powder prepared is added directly into graphite jig,
Pressurize 3 minutes under 10Mpa pressure；The green compact pressed through in advance is put into attemperator to be placed in discharge plasma sintering stove, it will
Vacuum state in furnace chamber, pressure to 6pa, application pressure are 30Mpa；Sample is heated with the heating rate of 100 DEG C/min
To 1300 DEG C, 5min, then furnace cooling are kept the temperature.After tested, consistency is the 96.8% of material, Vickers hardness 20.48
± 0.15GPa, fracture toughness are 10.78 ± 0.1MPa.m1/2, average grain size 238nm.
Embodiment 4
Co 8%, WC 90.8%, VC 0.2%, cBN 1% carry out dispensing by weight percent, are to be situated between with absolute ethyl alcohol
Matter is put into concussion in boronation conical flask plus stirs 2 hours, and in due course addition clear water is to ensure water temperature always during earthquake
In room temperature；Grinding is dried after concussion mixing, and is sieved with 100 mesh sieve, the mixed-powder prepared is added directly into graphite jig,
Pressurize 3 minutes under 10Mpa pressure；The green compact pressed through in advance is put into attemperator to be placed in discharge plasma sintering stove, it will
Vacuum state in furnace chamber, pressure to 6pa, application pressure are 28Mpa；Sample is heated to the heating rate of 80 DEG C/min
1250 DEG C, keep the temperature 5min, then furnace cooling.After tested, consistency is the 98.2% of material, Vickers hardness is 19.99 ±
0.2GPa, fracture toughness are 11.99 ± 0.1MPa.m1/2, average grain size 244nm.
Embodiment 5
Co 8%, WC 90.2%, VC 0.8%, cBN 1% carry out dispensing by weight percent, are to be situated between with absolute ethyl alcohol
Matter is put into concussion in boronation conical flask plus stirs 2 hours, and in due course addition clear water is to ensure water temperature always during earthquake
In room temperature；Grinding is dried after concussion mixing, and is sieved with 100 mesh sieve, the mixed-powder prepared is added directly into graphite jig,
Pressurize 3 minutes under 30Mpa pressure；The green compact pressed through in advance is put into attemperator to be placed in discharge plasma sintering stove, it will
Vacuum state in furnace chamber, pressure to 6pa, application pressure are 32Mpa；Sample is heated with the heating rate of 120 DEG C/min
To 1300 DEG C, 5min, then furnace cooling are kept the temperature.After tested, consistency is the 97.3% of material, Vickers hardness 19.93
± 0.2GPa, fracture toughness are 10.95 ± 0.1MPa.m1/2, average grain size 235nm.
Comparative example 1
Co 8%, WC 82.8%, VC 0.2%, cBN 9% carry out dispensing by weight percent, are to be situated between with absolute ethyl alcohol
Matter is put into concussion in boronation conical flask plus stirs 2 hours, and in due course addition clear water is to ensure water temperature always during earthquake
In room temperature；Grinding is dried after concussion mixing, and is sieved with 100 mesh sieve, the mixed-powder prepared is added directly into graphite jig,
Pressurize 3 minutes under 10Mpa pressure；The green compact pressed through in advance is put into attemperator to be placed in discharge plasma sintering stove, it will
Vacuum state in furnace chamber, pressure to 6pa, application pressure are 28Mpa；Sample is heated to the heating rate of 80 DEG C/min
1250 DEG C, keep the temperature 5min, then furnace cooling.After tested, consistency is the 90.0% of material, Vickers hardness is 10.74 ±
0.15GPa, fracture toughness are 9.8 ± 0.1MPa.m1/2, average grain size 240nm.
This comparative example illustrates that excessive cBN can be such that the densification degree of hard alloy quickly reduces, due to existing in material
A large amount of hole, so that its hardness and toughness can all become very poor.
Comparative example 2
Co 8%, WC 82%, VC 1%, the progress of cBN 1% dispensing are put using absolute ethyl alcohol as medium by weight percent
Enter concussion in boronation conical flask plus stir 2 hours, in due course addition clear water is to ensure water temperature always in room during earthquake
Temperature；Grinding is dried after concussion mixing, and is sieved with 100 mesh sieve, the mixed-powder prepared is added directly into graphite jig,
Pressurize 3 minutes under 10Mpa pressure；The green compact pressed through in advance is put into attemperator to be placed in discharge plasma sintering stove, by stove
Intracavitary vacuum state, pressure to 6pa, application pressure are 32Mpa；Sample is heated to the heating rate of 120 DEG C/min
1300 DEG C, keep the temperature 5min, then furnace cooling.After tested, consistency is the 92.8% of material, Vickers hardness is 18.3 ±
0.25GPa, fracture toughness are 8.0 ± 0.2MPa.m1/2, average grain size 243nm.
This comparative example illustrates that excessive VC can be such that the densification degree of hard alloy reduces, a large amount of due to existing in material
Hole, so that its hardness and toughness reduce.
Claims (6)
1. Ultra-fine Grained tungsten carbide base carbide alloy material, which is characterized in that by weight percentage, including following component：Cobalt
8%, tungsten carbide 90.2%~90.8%, vanadium carbide 0.2%~0.8%, cubic boron nitride 1%.
2. the preparation method of Ultra-fine Grained tungsten carbide base carbide alloy material according to claim 1, which is characterized in that including
Following steps：
Step 1, cobalt, tungsten carbide, vanadium carbide and cubic boron nitride powder are weighed in proportion, are mixed, are made at room temperature with absolute ethyl alcohol
To shake medium, ultrasonic vibration, stirring, mixed powder are carried out；
Step 2, mixed powder is dried, is ground, sieving；
Step 3, the powder of sieving is directly poured into mold, carries out precompressed；
Step 4, it in vacuum environment, using discharge plasma sintering process, is persistently risen with the heating rate of 100 ± 20 DEG C/min
For temperature to 1250~1300 DEG C, control pressure is 30 ± 2Mpa, heat preservation, subsequent furnace cooling, obtained Ultra-fine Grained tungsten carbide-base hard
Alloy.
3. the preparation method of Ultra-fine Grained tungsten carbide base carbide alloy material according to claim 1, which is characterized in that step
In 1, the concussion incorporation time is 2~3 hours.
4. the preparation method of Ultra-fine Grained tungsten carbide base carbide alloy material according to claim 1, which is characterized in that step
In 2, the drying temperature is 100~120 DEG C, and the mesh number of sieve is 100 mesh.
5. the preparation method of Ultra-fine Grained tungsten carbide base carbide alloy material according to claim 1, which is characterized in that step
In 3, the precompressed pressure is 10~30Mpa, and the dwell time is 2~4min.
6. the preparation method of Ultra-fine Grained tungsten carbide base carbide alloy material according to claim 1, which is characterized in that step
In 4, it is evacuated to 5~8pa and forms vacuum environment, soaking time is 4~6min.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110157969A (en) * | 2019-07-10 | 2019-08-23 | 合肥工业大学 | A kind of preparation method of the super thick Talide containing trace cobalt |
| CN110253028A (en) * | 2019-07-16 | 2019-09-20 | 湖南伊澍智能制造有限公司 | A kind of self-lubricating 3D printing alloy powder and preparation method thereof |
| CN110373593A (en) * | 2019-07-01 | 2019-10-25 | 南京理工大学 | A kind of titanium carbonitride based composite metal ceramic material microwave sintering process |
| CN111088450A (en) * | 2020-01-07 | 2020-05-01 | 北京科技大学 | Rare earth-added ultrafine-grained high-toughness WC-10Co hard alloy material and preparation method thereof |
| CN113059157A (en) * | 2021-03-09 | 2021-07-02 | 南京理工大学 | Method for sintering superfine crystal WC-based hard alloy special-shaped cutter under SPS pressure |
| FR3120636A1 (en) | 2021-03-15 | 2022-09-16 | Sintermat | Method for manufacturing tungsten carbide parts and material obtained based on SPS sintering of tungsten carbide |
| CN115725885A (en) * | 2021-08-30 | 2023-03-03 | 四川大学 | Gradient YG hard alloy material for mold and preparation method |
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| CN110373593A (en) * | 2019-07-01 | 2019-10-25 | 南京理工大学 | A kind of titanium carbonitride based composite metal ceramic material microwave sintering process |
| CN110157969A (en) * | 2019-07-10 | 2019-08-23 | 合肥工业大学 | A kind of preparation method of the super thick Talide containing trace cobalt |
| CN110253028A (en) * | 2019-07-16 | 2019-09-20 | 湖南伊澍智能制造有限公司 | A kind of self-lubricating 3D printing alloy powder and preparation method thereof |
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| CN113059157A (en) * | 2021-03-09 | 2021-07-02 | 南京理工大学 | Method for sintering superfine crystal WC-based hard alloy special-shaped cutter under SPS pressure |
| FR3120636A1 (en) | 2021-03-15 | 2022-09-16 | Sintermat | Method for manufacturing tungsten carbide parts and material obtained based on SPS sintering of tungsten carbide |
| WO2022195215A1 (en) | 2021-03-15 | 2022-09-22 | Sintermat | Process for manufacturing tungsten carbide parts and resulting material based on sps sintering of tungsten carbide |
| CN115725885A (en) * | 2021-08-30 | 2023-03-03 | 四川大学 | Gradient YG hard alloy material for mold and preparation method |
| CN115725885B (en) * | 2021-08-30 | 2023-10-27 | 四川大学 | Gradient YG hard alloy material for mold and preparation method |
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