CN106083113A - A kind of cBN toughness reinforcing WC composite and preparation method thereof - Google Patents
A kind of cBN toughness reinforcing WC composite and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to technical field of alloy material, disclose a kind of cBN toughness reinforcing WC composite and preparation method thereof.Described composite is by the WC, the cBN of 0.01～0.25wt.% of 99.75～99.99wt.% and inevitable trace impurity composition.Described preparation method is: WC powder body, cBN and organic solvent is placed in ball mill and carries out wet ball-milling, prepares ball milling slurry；Sieve after ball milling slurry is dried removing solvent, it is thus achieved that the composite powder of particle size≤300 μm；Then composite powder is placed in sintering curing in mould shape, obtains the cBN toughness reinforcing WC composite of soap-free emulsion polymeization phase.Composite of the present invention is a kind of WC composite of not containing any metallic binding phase toughness reinforcing by cBN, has the highest hardness, wearability, antioxygenic property and preferable toughness, is suitable as cutter material or mold materials.
Description
Technical field
The invention belongs to technical field of alloy material, be specifically related to a kind of cBN toughness reinforcing WC composite and preparation method thereof.
Background technology
WC-Co hard alloy, is a kind of common, important hard alloy kind (YG series), is widely used in existing
For cutter material, wear-resisting, corrosion-resistant and exotic material field, there is the title of the tooth of modern industry.Pure WC material is difficult to sintering
Densification, even if densified sintering product, sintering temperature also tends to more than 2000 DEG C, and the highest sintering temperature is also one to equipment itself
After planting infringement, and sintering, fracture toughness only has～4MPa m1/2.A kind of Binder Phase when Co sinters as WC, has non-to WC
The best wettability, can make WC sintering temperature be reduced to～1400 DEG C simultaneously, and during sintering, Co becomes liquid phase, is greatly increased WC particle
Diffusion rate, makes densified sintering product, after sintering the usual fracture toughness of tungsten carbide composite～12MPa m1/2.But, Co provides
The distribution in the world in source is the most unbalanced, and the Co resource of China is most deficient, heavy dependence import so that the supply of Co raw material
There is also a lot of unstable factor.Co is as a kind of binding agent simultaneously, reduces the hardness of WC material, corrosion resistance and high temperature resistant
Property, limit the application under some extreme Service Environment of the WC material.Therefore, the non-adherent of a kind of common wide material sources is found
The material of phase substitutes Co, breaks away from external dependence, and the hardness and the high-temperature behavior that improve WC series hard alloy just seem simultaneously
Extremely important.
At present in the research to soap-free emulsion polymeization phase WC material, improve its fracture toughness frequently with two kinds of means.One is logical
Cross the mode of crystal grain refinement, it is possible to simultaneously work as improving the effect of hardness and fracture toughness；Two is to add ceramic phase particles/fibre
Tie up, or the phase transformation of ceramic phase improves its fracture toughness.CBN (cubic boron nitride) is the diamond-like stone material of a kind of high rigidity
Material, is usually used in manufacturing cutter and abrasive material.But the most not yet there is the report using cBN particulate reinforcement WC composite.
Summary of the invention
In place of solving the shortcoming and defect of above prior art, the primary and foremost purpose of the present invention is to provide a kind of cBN
Toughness reinforcing WC composite.
Another object of the present invention is to provide the above-mentioned cBN preparation method of toughness reinforcing WC composite.
The object of the invention is achieved through the following technical solutions:
A kind of cBN toughness reinforcing WC composite, by the WC of 99.75～99.99wt.%, the cBN of 0.01～0.25wt.% with
And inevitably trace impurity forms.
The preparation method of above-mentioned cBN toughness reinforcing WC composite, including following preparation process:
(1) WC powder body, cBN and organic solvent are placed in ball mill carry out wet ball-milling, prepare ball milling slurry；
(2) sieve after ball milling slurry is dried removing solvent, it is thus achieved that the composite powder of particle size≤300 μm；
(3) step (2) gained composite powder being placed in sintering curing in mould shape, the cBN obtaining soap-free emulsion polymeization phase is toughness reinforcing
WC composite.
Preferably, the organic solvent described in step (1) is ethanol.
Preferably, dry the referring to described in step (2) is dried to solvent residues quality≤1%.
Preferably, the sintering described in step (3) refers to use discharge plasma sintering technique to be sintered；Concrete sintering
Condition is as follows:
Sintering current type is DC pulse current；
Sintering pressure: 30～50MPa；
Sintering atmosphere: coarse vacuum≤6Pa；
Heating rate: 50～300 DEG C/min；
Sintering temperature: 1650～1850 DEG C；
Temperature retention time: 0～10min.
Preparation method and the gained composite of the present invention have the advantage that and beneficial effect:
(1) present invention uses WC powder body that particle diameter is thinner and adds trace cBN and be prepared for cBN toughness reinforcing WC composite；Carefully
The particulate reinforcement mechanism of little WC grain and cBN, while being favorably improved matrix material toughness, keeps matrix material itself
High rigidity；
(2) the WC composite that prepared by the present invention is that a kind of WC of not containing any metallic binding phase toughness reinforcing by cBN is multiple
Condensation material, it has the highest hardness, wearability, antioxygenic property and preferable toughness, be suitable as cutter material or
Mold materials；
(3) the WC composite that prepared by the present invention does not contains Co, and compared with tradition WC-Co hard alloy, it is possible not only to
Reduce cost, it is also possible to save rare and have strategic Co resource, it is even more important that cBN used in the present invention is
Through preferable commercialization, wide material sources.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of embodiment 1 gained cBN toughness reinforcing WC composite.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention do not limit
In this.
Embodiment 1
A kind of cBN toughness reinforcing WC composite of the present embodiment, is prepared via a method which:
(1) by 99.9g WC (0.2 μm, purity > 99.9%, Xuzhou victory innovative material Science and Technology Ltd.), 0.1gcBN
(0.1 μm, purity > 99.9%, Guangzhou Ke Siman grinds company limited), pour in 250ml hard alloy tank, add ethanol and make
For solvent (volume of gained mixed slurry is less than the 2/3 of ball grinder volume), obtain mixed slurry；Will be equipped with mixed slurry
Ball grinder is placed on planetary ball mill and carries out wet ball-milling (rotating speed 180r/min, Ball-milling Time is 30h), obtains ball milling slurry
Material；
(2) ball milling slurry is placed in vacuum drying oven it is dried to solvent residues amount≤1%, take out the powder after drying and grind
Broken, sieve, it is thus achieved that the composite powder of particle size≤300 μm；
(3) take 28g composite powder and put into internal diameterAnd external diameterCylindrical shape graphite jig in, powder
Material, die and drift the most all separate with graphite paper so that the demoulding, be also coated with outside die the graphite felt of one layer of 10mm thickness with
Reduce heat radiation loss；Will be equipped with the graphite jig of composite powder to be placed in discharge plasma sintering stove and be sintered, obtain nothing
Binder Phase cBN toughness reinforcing WC composite.Described sintering parameter is: sintering current type is DC pulse current, and sintering atmosphere is
Coarse vacuum (≤6Pa), sintering pressure is 30MPa, and heating rate is 100 DEG C/min, and thermometric mode is infrared measurement of temperature (>=570
DEG C), sintering temperature is 1700 DEG C, temperature retention time 0min.
The present embodiment gained cBN toughness reinforcing WC composite is calculated relative density after measuring the test of its Archimedes method
It is 98.1%；Using Vickers and set load 10kg power test hardness, hardness is HV1024.7GPa；According to Vickers hardness
Impression, uses indentation method to be calculated fracture toughness 7.8Mpa m1/2。
The XRD spectra of the present embodiment gained cBN toughness reinforcing WC composite as it is shown in figure 1, appeared in figure diffraction maximum be
WC phase.
Embodiment 2
A kind of cBN toughness reinforcing WC composite of the present embodiment, is prepared via a method which:
Step (1)～(2) are same as in Example 1；
(3) take 28g composite powder and put into internal diameterAnd external diameterCylindrical shape graphite jig in, powder
Material, die and drift the most all separate with graphite paper so that the demoulding, be also coated with outside die the graphite felt of one layer of 10mm thickness with
Reduce heat radiation loss；Will be equipped with the graphite jig of composite powder to be placed in discharge plasma sintering stove and be sintered, obtain nothing
Binder Phase cBN toughness reinforcing WC composite.Described sintering parameter is: sintering current type is DC pulse current, and sintering atmosphere is
Coarse vacuum (≤6Pa), sintering pressure is 30MPa, and heating rate is 100 DEG C/min, and thermometric mode is infrared measurement of temperature (>=570
DEG C), sintering temperature is 1700 DEG C, temperature retention time 10min.
The present embodiment gained cBN toughness reinforcing WC composite is 98.9% through its relative density of survey calculation, and hardness is HV10
24.5GPa, fracture toughness 7.95Mpa m1/2。
Embodiment 3
A kind of cBN toughness reinforcing WC composite of the present embodiment, is prepared via a method which:
Step (1)～(2) are same as in Example 1；
(3) take 28g composite powder and put into internal diameterAnd external diameterCylindrical shape graphite jig in, powder
Material, die and drift the most all separate with graphite paper so that the demoulding, be also coated with outside die the graphite felt of one layer of 10mm thickness with
Reduce heat radiation loss；Will be equipped with the graphite jig of composite powder to be placed in discharge plasma sintering stove and be sintered, obtain nothing
Binder Phase cBN toughness reinforcing WC composite.Described sintering parameter is: sintering current type is DC pulse current, and sintering atmosphere is
Coarse vacuum (≤6Pa), sintering pressure is 50MPa, and heating rate is 300 DEG C/min, and thermometric mode is infrared measurement of temperature (>=570
DEG C), sintering temperature is 1800 DEG C, temperature retention time 0min.
The present embodiment gained cBN toughness reinforcing WC composite is 98.5% through its relative density of survey calculation, and hardness is HV10
24.9GPa, fracture toughness 7.66Mpa m1/2。
Embodiment 4
A kind of cBN toughness reinforcing WC composite of the present embodiment, is prepared via a method which:
Step (1)～(2) are same as in Example 1；
(3) take 28g composite powder and put into internal diameterAnd external diameterCylindrical shape graphite jig in, powder
Material, die and drift the most all separate with graphite paper so that the demoulding, be also coated with outside die the graphite felt of one layer of 10mm thickness with
Reduce heat radiation loss；Will be equipped with the graphite jig of composite powder to be placed in discharge plasma sintering stove and be sintered, obtain nothing
Binder Phase cBN toughness reinforcing WC composite.Described sintering parameter is: sintering current type is DC pulse current, and sintering atmosphere is
Coarse vacuum (≤6Pa), sintering pressure is 30MPa, and heating rate is 100 DEG C/min, and thermometric mode is infrared measurement of temperature (>=570
DEG C), thermometric focus point is positioned at bottom outer mold wall centre bore, and away from mould inner wall 7.5mm, sintering temperature is 1800 DEG C, insulation
Time 5min.
The present embodiment gained cBN toughness reinforcing WC composite is 98.7% through its relative density of survey calculation, and hardness is HV10
25.2GPa, fracture toughness 7.58Mpa m1/2。
Embodiment 5
A kind of cBN toughness reinforcing WC composite of the present embodiment, is prepared via a method which:
Step (1)～(2) are same as in Example 1；
(3) take 28g composite powder and put into internal diameterAnd external diameterCylindrical shape graphite jig in, powder
Material, die and drift the most all separate with graphite paper so that the demoulding, be also coated with outside die the graphite felt of one layer of 10mm thickness with
Reduce heat radiation loss；Will be equipped with the graphite jig of composite powder to be placed in discharge plasma sintering stove and be sintered, obtain nothing
Binder Phase cBN toughness reinforcing WC composite.Described sintering parameter is: sintering current type is DC pulse current, and sintering atmosphere is
Coarse vacuum (≤6Pa), sintering pressure is 50MPa, and heating rate is 100 DEG C/min, and thermometric mode is infrared measurement of temperature (>=570
DEG C), thermometric focus point is positioned at bottom outer mold wall centre bore, and away from mould inner wall 7.5mm, sintering temperature is 1800 DEG C, insulation
Time 0min.
The present embodiment gained cBN toughness reinforcing WC composite is 98.5% through its relative density of survey calculation, and hardness is HV10
24.8GPa, fracture toughness 7.74Mpa m1/2。
Embodiment 6
A kind of cBN toughness reinforcing WC composite of the present embodiment, is prepared via a method which:
Step (1)～(2) are same as in Example 1；
(3) take 28g composite powder and put into internal diameterAnd external diameterCylindrical shape graphite jig in, powder
Material, die and drift the most all separate with graphite paper so that the demoulding, be also coated with outside die the graphite felt of one layer of 10mm thickness with
Reduce heat radiation loss；Will be equipped with the graphite jig of composite powder to be placed in discharge plasma sintering stove and be sintered, obtain nothing
Binder Phase cBN toughness reinforcing WC composite.Described sintering parameter is: sintering current type is DC pulse current, and sintering atmosphere is
Coarse vacuum (≤6Pa), sintering pressure is 30MPa, and heating rate is 100 DEG C/min, and thermometric mode is infrared measurement of temperature (>=570
DEG C), thermometric focus point is positioned at bottom outer mold wall centre bore, and away from mould inner wall 7.5mm, sintering temperature is 1850 DEG C, insulation
Time 5min.
The present embodiment gained cBN toughness reinforcing WC composite is 98.2% through its relative density of survey calculation, and hardness is HV10
25.3GPa, fracture toughness 7.46Mpa m1/2。
Embodiment 7
A kind of cBN toughness reinforcing WC composite of the present embodiment, is prepared via a method which:
Step (1)～(2) are same as in Example 1；
(3) take 28g composite powder and put into internal diameterAnd external diameterCylindrical shape graphite jig in, powder
Material, die and drift the most all separate with graphite paper so that the demoulding, be also coated with outside die the graphite felt of one layer of 10mm thickness with
Reduce heat radiation loss；Will be equipped with the graphite jig of composite powder to be placed in discharge plasma sintering stove and be sintered, obtain nothing
Binder Phase cBN toughness reinforcing WC composite.Described sintering parameter is: sintering current type is DC pulse current, and sintering atmosphere is
Coarse vacuum (≤6Pa), sintering pressure is 50MPa, and heating rate is 50 DEG C/min, and thermometric mode is infrared measurement of temperature (>=570 DEG C),
Thermometric focus point is positioned at bottom outer mold wall centre bore, and away from mould inner wall 7.5mm, sintering temperature is 1850 DEG C, temperature retention time
0min。
The present embodiment gained cBN toughness reinforcing WC composite is 98.8% through its relative density of survey calculation, and hardness is HV10
24.4GPa, fracture toughness 7.42Mpa m1/2。
Embodiment 8
A kind of cBN toughness reinforcing WC composite of the present embodiment, is prepared via a method which:
(1) by 99.99g WC (0.2 μm, purity > 99.9%, Xuzhou victory innovative material Science and Technology Ltd.), 0.01g
CBN (0.1 μm, purity > 99.9%, Guangzhou Ke Siman grinds company limited), pour in 250ml hard alloy tank, add second
Alcohol, as solvent (volume of gained mixed slurry is less than the 2/3 of ball grinder volume), obtains mixed slurry；Will be equipped with mixing slurry
The ball grinder of material is placed on planetary ball mill and carries out wet ball-milling (rotating speed 180r/min, Ball-milling Time is 30h), obtains ball milling
Slurry；
Step (2)～(3) are same as in Example 1.
The present embodiment gained cBN toughness reinforcing WC composite is 98.9% through its relative density of survey calculation, and hardness is HV10
24.8GPa, fracture toughness 7.5Mpa m1/2。
Embodiment 9
A kind of CNTs toughness reinforcing WC composite of the present embodiment, is prepared via a method which:
(1) by 99.75g WC (0.2 μm, purity > 99.9%, Xuzhou victory innovative material Science and Technology Ltd.), 0.25g
CBN (0.1 μm, purity > 99.9%, Guangzhou Ke Siman grinds company limited), pour in 250ml hard alloy tank, add second
Alcohol, as solvent (volume of gained mixed slurry is less than the 2/3 of ball grinder volume), obtains mixed slurry；Will be equipped with mixing slurry
The ball grinder of material is placed on planetary ball mill and carries out wet ball-milling (rotating speed 180r/min, Ball-milling Time is 30h), obtains ball milling
Slurry；
Step (2)～(3) are same as in Example 1.
The present embodiment gained cBN toughness reinforcing WC composite is 98.8% through its relative density of survey calculation, and hardness is HV10
24.5GPa, fracture toughness 7.96Mpa m1/2。
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-described embodiment
Limit, the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify,
All should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (5)
1. a cBN toughness reinforcing WC composite, it is characterised in that: described composite by 99.75～99.99wt.% WC,
The cBN of 0.01～0.25wt.% and inevitable trace impurity composition.
2. the preparation method of a kind of cBN toughness reinforcing WC composite described in claim 1, it is characterised in that include following preparation step
Rapid:
(1) WC powder body, cBN and organic solvent are placed in ball mill carry out wet ball-milling, prepare ball milling slurry；
(2) sieve after ball milling slurry is dried removing solvent, it is thus achieved that the composite powder of particle size≤300 μm；
(3) wet grinding composite powder is placed in sintering curing in mould shape, obtains the cBN toughness reinforcing WC composite of soap-free emulsion polymeization phase.
The preparation method of a kind of cBN the most according to claim 2 toughness reinforcing WC composite, it is characterised in that: in step (1)
Described organic solvent is ethanol.
The preparation method of a kind of cBN the most according to claim 2 toughness reinforcing WC composite, it is characterised in that: in step (2)
Described dry referring to is dried to solvent residues quality≤1%.
The preparation method of a kind of cBN the most according to claim 2 toughness reinforcing WC composite, it is characterised in that: in step (3)
Described sintering refers to use discharge plasma sintering technique to be sintered；Concrete sintering condition is as follows:
Sintering current type is DC pulse current；
Sintering pressure: 30～50MPa；
Sintering atmosphere: coarse vacuum≤6Pa；
Heating rate: 50～300 DEG C/min；
Sintering temperature: 1650～1850 DEG C；
Temperature retention time: 0～10min.
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| CN106834778B (en) * | 2017-01-03 | 2018-09-28 | 崇义恒毅陶瓷复合材料有限公司 | Hard alloy and preparation method |
| CN106946570A (en) * | 2017-03-13 | 2017-07-14 | 华南理工大学 | A kind of B4C toughness reinforcing WC composites and preparation method thereof |
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Application publication date: 20161109 |