CN104928512B - The preparation method of super coarse-grain tungsten-cobalt hard alloy - Google Patents
The preparation method of super coarse-grain tungsten-cobalt hard alloy Download PDFInfo
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Abstract
A kind of preparation method of super coarse-grain tungsten-cobalt hard alloy comprising following processing step: ingredient, drying, preheating, wet mixing, drying, mixes binder, granulation, compression moulding and vacuum low-pressure integral sintering at wet-milling；The mass ratio of selection cobalt powder and tungsten carbide powder progress mix when ingredient, cobalt powder and tungsten carbide powder is 2.4~2.6: 97.4~97.6；Mixture after preheating is added into metal cobalt powder and Co2W4C nano particle, the mass ratio of cobalt and tungsten carbide in mixture is that the additional amount of 8~13: 87~92, Co2W4C nano particle will reach the mass ratio 1: 0.045~0.055 for making the cobalt in mixture Yu Co2W4C nano particle.The present invention is by adopting the above-described technical solution, compared with prior art, the WC mean grain size of the hard alloy of preparation reaches 4.0~5.2 μm, and bending strength reaches 3000~3400MPa, hardness HRA88.0~90.8.
Description
Technical field
The present invention relates to a kind of preparation method of hard alloy, especially a kind of preparation side of super coarse-grain tungsten-cobalt hard alloy
Method.
Background technique
With the continuous development of hard carbide industry, the requirement to its raw material WC powder (i.e. tungsten carbide powder) is higher and higher.It is special
It is not the preparation of super thick type hard alloy, there are strict requirements to the granularity of WC powder, currently, the aggregation extent of WC powder is higher, powder
Last granularity is not coarse enough, and coarseness WC powder all has WC particle aggregation.Due to the presence of aggregation, it be easy to cause Fei Shi flat
Equal granularity is big, and the illusion that actual particle size is partially thin.In addition the combination tightness of aggregation is different, thus increases high-quality hard
The manufacture difficulty of alloy makes hard metal article difficult unification for accomplishing height in wearability and toughness.And the WC powder of import
The big height of cost, is unfavorable for domestic large-scale production.So what is generallyd use at present burns through wet-milling, drying, compression moulding, vacuum
The crystal grain maximum of the coarse-grain tungsten-cobalt hard alloy of the processes such as knot production is also between 3.2~4.0 μm.Bending strength 2600~
3000MPa, hardness Hv301150~1320, intensity and microhardness matching are poor, and comprehensive performance is lower, especially the height of alloy
Warm hardness and elevated temperature strength be not high, and shock resistance and heat resistanceheat resistant flow ability are poor, and hardly possible is suitble to work under high temperature environment, restricts significantly
The application range of hard alloy.
Summary of the invention
A kind of system of super coarse-grain tungsten-cobalt hard alloy is provided the purpose of the present invention is overcoming the above-mentioned insufficient of the prior art
Preparation Method reaches 4.0~5.2 μm by the WC mean grain size of the hard alloy of its preparation, and bending strength reaches 3000~
3400MPa, hardness HRA88.0~90.8, it can be achieved that alloy strength and microhardness matched well, so that hard metal article is existed
The unification for reaching height in wearability and toughness improves the synthesis service performance of alloy.
The technical scheme is that a kind of preparation method of super coarse-grain tungsten-cobalt hard alloy comprising following technique step
Rapid: ingredient, drying, preheating, wet mixing, drying, mixes binder, granulation, compression moulding and vacuum low-pressure integration burning at wet-milling
Knot；The mass ratio of selection cobalt powder and tungsten carbide powder progress mix when ingredient, cobalt powder and tungsten carbide powder is 2.4~2.6:
97.4~97.6, it is 13.0~18.5 μm of Coarse Grain Tungsten Carbide that tungsten carbide powder, which selects Fsss granularity, and the granularity of cobalt powder is 1.4
~2.0 μm；Wet-milling is ball milling；It is dried after wet-milling, the mixture obtained after dry carries out preheating；After preheating
Mixture add metal cobalt powder and Co2W4C nano particle, the additional amount of cobalt powder will reach the cobalt and carbonization made in mixture
The mass ratio of tungsten is 8~13: 87~92, Co2W4The additional amount of C nano particle will reach the cobalt and Co made in mixture2W4C
The mass ratio of nano particle is 1: 0.045~0.055.
The preferred technical solution of the present invention is: the ball-milling medium when wet-milling is acetone, and the ratio between ball material is 3: 1, solid-liquid
The ratio between be 5: 1, the wet-milling time be 7~12 hours.
The further optimal technical scheme of the present invention is: the preheating is to reach 700~850 through heating in 3~4 hours
DEG C, then keep the temperature 55~65 minutes.
The further optimal technical scheme of the present invention is: added in the mixture after preheating metal cobalt powder and
Co2W458~62 DEG C of progress wet mixing 3.5~4.5 hours are heated to after C nano particle.
The also further optimal technical scheme of the present invention is: the maximum temperature of the vacuum low-pressure integral sintering is 1440
~1460 DEG C.
The also further optimal technical scheme of the present invention is: the mass ratio of selection cobalt powder and tungsten carbide powder is when ingredient
2.5:97.5；It is 13.5~15.5 μm of Coarse Grain Tungsten Carbide that tungsten carbide powder, which selects Fsss granularity,；It will be mixed after preheating
It closes material and adds metal cobalt powder and Co2W4C nano particle, the additional amount of cobalt powder will reach the cobalt and tungsten carbide made in mixture
Mass ratio is 9~11.5: 88.5~91, Co2W4The additional amount of C nano particle will reach the cobalt and Co made in mixture2W4C
The mass ratio of nano particle is 1: 0.048~0.052.
The explanation of primary symbols or title that the present invention uses:
WC: tungsten carbide；
Fsss granularity: Fsss Full Name in English is Fisher Sub-sieve Sizer, i.e. the granularity of " Fei Shi sieve " measurement；
Co: cobalt；
WC powder: tungsten carbide powder.
Compared with the prior art, the invention has the following features:
The present invention uses Fsss granularity for 13.0~18.5 μm of common coarse-grained WC powder and quality percentage close to monocrystalline
1.4~2.0 μm of metal Co powder of granularity than 2.5%；Increased preheating process improves WC particle by the package journey of cobalt simultaneously
Degree slows down the irregular of WC grain in sintering process and grows up, WC is made to keep the pattern before sintering；It is aided with the allotment of wet mixing process
At mixing Co in target cobalt amount and cobalt2W4C nano particle can enhance Binder Phase, alleviate the crack propagation of alloy in use,
So that the average particle size of WC in finally obtained extra-coarse grained carbide alloy is reached 4.0~5.2 μm, toughness is high, and crystallize it is complete,
Defect is few, microstrain is small, and subgrain is coarse uniformly, microhardness is high, and wearability and toughness are greatly improved,
Bending strength has reached 3000~3400MPa, and hardness has reached HRA88.0~90.8, realizes the good of intensity and microhardness
Good matching, so that alloy comprehensive performance be made greatly to improve；Since the super coarse-grain hard alloy of high tenacity of the invention passes through control
Cobalt and Co2W4The mixed ratio of C nano particle had both enhanced the intensity of Binder Phase and had improved intergranular microstructure, and improved alloy
Toughness and wearability more significantly improve the thermal shock resistance of alloy, so that being closed by the super coarse-grain hard of high tenacity of the invention
The quality such as mine, digging tool shield knife, the pick of gold manufacture are stablized, and service life extends 30% or more, greatly
Expand the use scope of hard alloy.
In order to illustrate more clearly of the present invention, following embodiment is enumerated, but it is without any restrictions to the range of invention.
Specific embodiment
Embodiment 1:
A kind of preparation method of super coarse-grain tungsten-cobalt hard alloy comprising following processing step: ingredient, wet-milling, drying, pre-
Burning processing, drying, mixes binder, granulation, compression moulding and vacuum low-pressure integral sintering at wet mixing；When ingredient select cobalt powder and
Tungsten carbide powder (i.e. WC powder), the mass ratio of cobalt powder and tungsten carbide powder are 2.5: 97.5, and tungsten carbide powder selection Fsss granularity is
13.0~13.5 μm of Coarse Grain Tungsten Carbide, the granularity of cobalt powder are 1.4~2.0 μm；Wet-milling is ball milling, ball-milling medium third
Ketone, the ratio between ball material are 3: 1, and the ratio between solid-liquid is 5: 1, and the wet-milling time is 7 hours；It is dried after wet-milling, what is obtained after dry is mixed
It closes material and carries out preheating, preheating reaches 700~850 DEG C through heating in 4 hours, then keeps the temperature 60 minutes；After preheating
Mixture add metal cobalt powder and Co2W4C nano particle, the additional amount of cobalt powder will reach the cobalt and carbonization made in mixture
The mass ratio of tungsten be 8: 92 (to include first with the mass ratio of cobalt powder and tungsten carbide powder be 2.5: 97.5 ratio
The cobalt powder of addition, that is to say, that the cobalt powder being specifically added will meet the sum of cobalt powder being added twice and the mass ratio of tungsten carbide is
8: 92, following embodiment is synonymous with this), Co2W4The additional amount of C nano particle will reach the cobalt and Co made in mixture2W4C receives
The mass ratio of rice grain is 1: 0.045, and is heated to 60 DEG C of wet mixings 4 hours；Again through drying, mix binder, pelletize, be pressed into
Type, vacuum low-pressure integral sintering, the maximum temperature of vacuum low-pressure integral sintering are 1460 DEG C.
By the super coarse-grain tungsten-cobalt hard alloy of the high tenacity obtained through this embodiment, (compact dimensions are 6.5*5.25*20 μm
Standardized product) 100, sample detected, obtain that WC mean grain size is 4.0 μm, average bending strength is 3000MPa, flat
Equal hardness is HRA90.8.
Embodiment 2:
A kind of preparation method of super coarse-grain tungsten-cobalt hard alloy comprising following processing step: ingredient, wet-milling, drying, pre-
Burning processing, drying, mixes binder, granulation, compression moulding and vacuum low-pressure integral sintering at wet mixing；When ingredient select cobalt powder and
Tungsten carbide powder (i.e. WC powder), the mass ratio of cobalt powder and tungsten carbide powder are 2.4: 97.6, and tungsten carbide powder selection Fsss granularity is
13.5~15.5 μm of Coarse Grain Tungsten Carbide, the granularity of cobalt powder are 1.4~2.0 μm；Wet-milling is ball milling, ball-milling medium third
Ketone, the ratio between ball material are 3: 1, and the ratio between solid-liquid is 5: 1, and the wet-milling time is 8 hours；It is dried after wet-milling, what is obtained after dry is mixed
It closes material and carries out preheating, preheating reaches 800 DEG C through heating in 4 hours, then keeps the temperature 60 minutes；By the mixing after preheating
Material adds metal cobalt powder and Co2W4C nano particle, the additional amount of cobalt powder will reach the matter for making cobalt and tungsten carbide in mixture
The ratio between amount is 9: 91, Co2W4The additional amount of C nano particle will reach the cobalt and Co made in mixture2W4The quality of C nano particle
The ratio between be 1: 0.048, and be heated to 60 DEG C of wet mixings 4 hours；Again through drying, mix binder, granulation, compression moulding, vacuum low-pressure
Integral sintering, the maximum temperature of vacuum low-pressure integral sintering are 1450 DEG C.
By the super coarse-grain tungsten-cobalt hard alloy of the high tenacity obtained through this embodiment, (compact dimensions are 6.5*5.25*20 μm
Standardized product) 100, sample detected, obtain that WC mean grain size is 4.5 μm, average bending strength is 3200MPa, flat
Equal hardness is HRA89.5.
Embodiment 3:
A kind of preparation method of super coarse-grain tungsten-cobalt hard alloy comprising following processing step: ingredient, wet-milling, drying, pre-
Burning processing, drying, mixes binder, granulation, compression moulding and vacuum low-pressure integral sintering at wet mixing；When ingredient select cobalt powder and
Tungsten carbide powder (i.e. WC powder), the mass ratio of cobalt powder and tungsten carbide powder are 2.6: 97.4, and tungsten carbide powder selection Fsss granularity is
15.5~17.2 μm of Coarse Grain Tungsten Carbide, the granularity of cobalt powder are 1.4~2.0 μm；Wet-milling is ball milling, ball-milling medium third
Ketone, the ratio between ball material are 3: 1, and the ratio between solid-liquid is 5: 1, and the wet-milling time is 9 hours；It is dried after wet-milling, what is obtained after dry is mixed
It closes material and carries out preheating, preheating reaches 750 DEG C through heating in 4 hours, then keeps the temperature 60 minutes；By the mixing after preheating
Material adds metal cobalt powder and Co2W4C nano particle, the additional amount of cobalt powder will reach the matter for making cobalt and tungsten carbide in mixture
The ratio between amount is 9.5: 90.5, Co2W4The additional amount of C nano particle will reach the cobalt and Co made in mixture2W4C nano particle
Mass ratio is 1: 0.050, and is heated to 58~62 DEG C of wet mixings 4 hours；Again through drying, mix binder, granulation, compression moulding,
Vacuum low-pressure integral sintering, the maximum temperature of vacuum low-pressure integral sintering are 1450 DEG C.
By the super coarse-grain tungsten-cobalt hard alloy of the high tenacity obtained through this embodiment, (compact dimensions are 6.5*5.25*20 μm
Standardized product) 100, sample detected, obtain that WC mean grain size is 4.8 μm, average bending strength is 3200MPa, flat
Equal hardness is HRA89.0.
Embodiment 4:
A kind of preparation method of super coarse-grain tungsten-cobalt hard alloy comprising following processing step: ingredient, wet-milling, drying, pre-
Burning processing, drying, mixes binder, granulation, compression moulding and vacuum low-pressure integral sintering at wet mixing；When ingredient select cobalt powder and
Tungsten carbide powder (i.e. WC powder), the mass ratio of cobalt powder and tungsten carbide powder are 2.5: 97.5, and tungsten carbide powder selection Fsss granularity is
17.2~18.0 μm of Coarse Grain Tungsten Carbide, the granularity of cobalt powder are 1.4~2.0 μm；Wet-milling is ball milling, ball-milling medium third
Ketone, the ratio between ball material are 3: 1, and the ratio between solid-liquid is 5: 1, and the wet-milling time is 10 hours；It is dried after wet-milling, what is obtained after dry is mixed
It closes material and carries out preheating, preheating reaches 700 DEG C through heating in 3 hours, then keeps the temperature 55~65 minutes；
Mixture after preheating is added into metal cobalt powder and Co2W4The additional amount of C nano particle, cobalt powder will reach
Make the mass ratio 11.5: 88.5 of the cobalt and tungsten carbide in mixture, Co2W4The additional amount of C nano particle, which will reach, to be made to mix
Cobalt and Co in material2W4The mass ratio of C nano particle is 1: 0.052, and is heated to 58~62 DEG C of wet mixings 4 hours；Again through dry
It is dry, mix binder, granulation, compression moulding, vacuum low-pressure integral sintering, the maximum temperature of vacuum low-pressure integral sintering is
1450℃。
By the super coarse-grain tungsten-cobalt hard alloy of the high tenacity obtained through this embodiment, (compact dimensions are 6.5*5.25*20 μm
Standardized product) 100, sample detected, obtain that WC mean grain size is 5.2 μm, average bending strength is 3400MPa, flat
Equal hardness is HRA88.5.
Embodiment 5:
A kind of preparation method of super coarse-grain tungsten-cobalt hard alloy comprising following processing step: ingredient, wet-milling, drying, pre-
Burning processing, drying, mixes binder, granulation, compression moulding and vacuum low-pressure integral sintering at wet mixing；When ingredient select cobalt powder and
Tungsten carbide powder (i.e. WC powder), the mass ratio of cobalt powder and tungsten carbide powder are 2.5: 97.5, and tungsten carbide powder selection Fsss granularity is
18.0~18.5 μm of Coarse Grain Tungsten Carbide, the granularity of cobalt powder are 1.4~2.0 μm；Wet-milling is ball milling, ball-milling medium third
Ketone, the ratio between ball material are 3: 1, and the ratio between solid-liquid is 5: 1, and the wet-milling time is 12 hours；It is dried after wet-milling, what is obtained after dry is mixed
It closes material and carries out preheating, preheating reaches 700 DEG C through heating in 3 hours, then keeps the temperature 60 minutes；By the mixing after preheating
Material adds metal cobalt powder and Co2W4C nano particle, the additional amount of cobalt powder will reach the matter for making cobalt and tungsten carbide in mixture
The ratio between amount is 13: 87, Co2W4The additional amount of C nano particle will reach the cobalt and Co made in mixture2W4The quality of C nano particle
The ratio between be 1: 0.055, and be heated to 60 DEG C of wet mixings 3.5~4.5 hours；Again through drying, mix binder, granulation, compression moulding, true
Empty low pressure integral sintering, the maximum temperature of vacuum low-pressure integral sintering are 1440 DEG C.
By the super coarse-grain tungsten-cobalt hard alloy of the high tenacity obtained through this embodiment, (compact dimensions are 6.5*5.25*20 μm
Standardized product) 100, sample detected, obtain that WC mean grain size is 5.0 μm, average bending strength is 3300MPa, flat
Equal hardness is HRA88.0.
Claims (1)
1. a kind of preparation method of super coarse-grain tungsten-cobalt hard alloy, it is characterized in that comprising the technical steps that: ingredient, is done wet-milling
Dry, preheating, drying, mixes binder, granulation, compression moulding and vacuum low-pressure integral sintering at wet mixing；Cobalt is selected when ingredient
The mass ratio of powder and tungsten carbide powder is 2.5: 97.5；It is 13.5~15.5 μm of coarse granule carbon that tungsten carbide powder, which selects Fsss granularity,
Change tungsten powder；The granularity of cobalt powder is 1.4~2.0 μm；Wet-milling is ball milling；Be dried after wet-milling, the mixture obtained after dry into
Row preheating；
Mixture after preheating is added into metal cobalt powder and Co2W4C nano particle, the additional amount of cobalt powder will reach and make to mix
The mass ratio for closing cobalt and tungsten carbide in material is 9~11.5: 88.5~91, Co2W4The additional amount of C nano particle will reach and make
Cobalt and Co in mixture2W4The mass ratio of C nano particle is 1: 0.048~0.052；
The ball-milling medium when wet-milling is acetone, and the ratio between ball material is 3: 1, and the ratio between solid-liquid is 5: 1, and the wet-milling time is 7~12 small
When；
The preheating is to reach 700~850 DEG C through heating in 3~4 hours, then keep the temperature 55~65 minutes；
Metal cobalt powder and Co are added in mixture after preheating2W4It is wet that 58~62 DEG C of progress are heated to after C nano particle
It is 3.5~4.5 hours mixed；
The maximum temperature of the vacuum low-pressure integral sintering is 1440~1460 DEG C.
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| CN201510386912.1A CN104928512B (en) | 2010-11-13 | 2010-11-13 | The preparation method of super coarse-grain tungsten-cobalt hard alloy |
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| CN201010553047.2A CN101985717B (en) | 2010-11-13 | 2010-11-13 | Method for preparing high-tenacity super-coarse-grained tungsten and cobalt hard alloy |
| CN201510386912.1A CN104928512B (en) | 2010-11-13 | 2010-11-13 | The preparation method of super coarse-grain tungsten-cobalt hard alloy |
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| CN201510386946.0A Pending CN104962770A (en) | 2010-11-13 | 2010-11-13 | Preparation method of crude crystal tungsten-cobalt alloy |
| CN201510386912.1A Expired - Fee Related CN104928512B (en) | 2010-11-13 | 2010-11-13 | The preparation method of super coarse-grain tungsten-cobalt hard alloy |
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| CN201510386946.0A Pending CN104962770A (en) | 2010-11-13 | 2010-11-13 | Preparation method of crude crystal tungsten-cobalt alloy |
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| CN102676902B (en) * | 2012-05-15 | 2014-02-19 | 赣州海盛钨钼集团有限公司 | Ultra-thick hard alloy, and preparation method and application thereof |
| CN102965534A (en) * | 2012-11-13 | 2013-03-13 | 中南大学 | Preparation method of hard alloy with ultra-coarse grains on surface |
| CN103866173B (en) * | 2014-03-06 | 2016-08-17 | 西安交通大学 | A kind of Hardmetal materials of pick cutter head for coal-winning machine and preparation method thereof |
| CN104388719A (en) * | 2014-10-29 | 2015-03-04 | 株洲硬质合金集团有限公司 | Preparation method of uniform coarse-grain hard alloy |
| CN105779844B (en) * | 2016-03-11 | 2019-01-22 | 中国神华能源股份有限公司 | A kind of nano hard alloy and preparation method thereof |
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| CN106636836A (en) * | 2017-01-22 | 2017-05-10 | 四川理工学院 | Preparation method of ultra-coarse hard alloy |
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| CN108274005B (en) * | 2018-02-08 | 2019-09-13 | 合肥工业大学 | A method of low cobalt, ultra-fine cemented carbide bar are prepared with nanometer WC-Co composite powder |
| CN109468517A (en) * | 2018-12-29 | 2019-03-15 | 株洲硬质合金集团有限公司 | A kind of preparation method and application of pile foundation engineering hard alloy |
| CN110385430B (en) * | 2019-08-21 | 2022-02-08 | 西迪技术股份有限公司 | 3D printed powder material |
| CN113669057B (en) * | 2021-08-06 | 2022-05-10 | 中国矿业大学 | Diamond composite cutting pick and low-temperature activation liquid-phase sintering process thereof |
| CN113699406A (en) * | 2021-08-30 | 2021-11-26 | 四川轻化工大学 | High-strength and high-toughness extra-coarse-grain WC hard alloy with average grain size larger than 8 microns and preparation method thereof |
| CN113857474A (en) * | 2021-09-01 | 2021-12-31 | 河海大学 | Preparation method of WC surface-coated Co powder added with Ce element |
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Also Published As
| Publication number | Publication date |
|---|---|
| CN101985717A (en) | 2011-03-16 |
| CN104962770A (en) | 2015-10-07 |
| CN101985717B (en) | 2015-07-01 |
| CN104928512A (en) | 2015-09-23 |
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