CN106116617B - A kind of ultra-fine boron nitride porous fibre toughening WC composite material and preparation method - Google Patents

A kind of ultra-fine boron nitride porous fibre toughening WC composite material and preparation method Download PDF

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CN106116617B
CN106116617B CN201610457523.8A CN201610457523A CN106116617B CN 106116617 B CN106116617 B CN 106116617B CN 201610457523 A CN201610457523 A CN 201610457523A CN 106116617 B CN106116617 B CN 106116617B
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boron nitride
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composite material
porous fibre
nitride porous
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CN106116617A (en
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李小强
曹廷
屈盛官
黄阳
梁良
伍尚华
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South China University of Technology SCUT
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    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
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    • C04B35/5626—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on tungsten carbides
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Abstract

The invention belongs to technical field of alloy material, disclose a kind of ultra-fine boron nitride porous fibre toughening WC composite material and preparation method.By the WC of 99.75~99.99wt.%, the ultra-fine boron nitride porous fibre of 0.01~0.25wt.% and inevitable trace impurity form the composite material.The preparation method is that: WC powder, ultra-fine boron nitride porous fibre and organic solvent are placed in ball mill and carry out wet ball-milling, ball milling slurry is made；It is sieved after ball milling slurry is dried and removed solvent, obtains the composite powder of particle size≤300 μm；Then gained composite powder is placed in sintering curing in mold and shapes, and obtains product.Gained composite material of the invention is a kind of WC composite material without containing any metallic binding phase by ultra-fine boron nitride porous fibre toughening, with very high hardness, wearability, antioxygenic property and preferable toughness, it is suitable as cutter material or mold materials.

Description

A kind of ultra-fine boron nitride porous fibre toughening WC composite material and preparation method
Technical field
The invention belongs to technical field of alloy material, and in particular to a kind of ultra-fine boron nitride porous fibre toughening WC composite wood Material and preparation method thereof.
Background technique
WC-Co hard alloy is a kind of common, important hard alloy type (YG series), is widely used in existing For cutter material, wear-resisting, corrosion-resistant and heat-resisting material field, there is the title of the tooth of modern industry.Pure WC material is difficult to be sintered Densification, even if densified sintering product, sintering temperature also tends to be easy to damage equipment at 2000 DEG C or more, and breaks after being sintered It splits toughness and there was only~4MPam1/2.A kind of Binder Phase when Co is sintered as WC, has extraordinary wetability, while energy to WC WC sintering temperature is set to be reduced to~1400 DEG C, Co becomes liquid phase when sintering, greatly increases WC particle diffusion rate, causes sintering Close, the usual fracture toughness of tungsten carbide composite is in~12MPam after sintering1/2.The distribution of world's Co resource is extremely uneven Weighing apparatus, the sum of the Co reserves of three state of Congo (Congo-Kinshasa), Australia and Cuba just occupy the 68% of world's gross reserves.The Co money of China Source is most deficient, heavy dependence import, so that there is also many unstable factors for the supply of Co raw material.Co is as a kind of viscous simultaneously Agent is tied, the hardness of WC material, corrosion resistance and heat-resisting quantity is reduced, limits WC material under certain extreme Service Environments Using.Therefore, a kind of material of common non-adherent phase from a wealth of sources is found to substitute Co, is got rid of to external dependence, together It is very important for the hardness and high-temperature behavior of Shi Tigao WC series hard alloy.
At present in the research to soap-free emulsion polymeization phase WC material, its fracture toughness is improved frequently with two kinds of means.First is that logical The mode of crystal grain refinement is crossed, the effect for improving hardness and fracture toughness can be played simultaneously；Second is that addition ceramic phase particles/fibre The phase transformation of dimension or ceramic phase improves its fracture toughness.General ceramics addition phase, either particle or fiber/whisker, It is easy to happen the problems such as insufficient with the interfacial bonding property of matrix, while improving toughness, seriously affects hardness performance.Ultra-fine nitrogen Change boron porous fibre, compared to traditional boron nitride nano-tube, due to its porous structure (total pore volume, 0.566cm3/ g) and high-specific surface area (0.515cm2/g)[Jing Lin,Lulu Xu,Yang Huang et al.Ultrafine porous boron nitride nanofibers synthesized via a freeze-drying and pyrolysis process and their adsorption properties.RSC Advances,2016,6, 1253-1259], it is easier to interface cohesion is realized with matrix during the preparation process, improves traditional secondary phase toughening mode, and Micro addition can be effectively improved mechanical property.Grinding using ultra-fine boron nitride porous fibre preparation toughening WC composite material at present Study carefully and not yet has been reported that.
Summary of the invention
In order to solve the disadvantage that the above prior art and shortcoming, the primary purpose of the present invention is that providing a kind of ultra-fine Boron nitride porous fibre toughening WC composite material.
Another object of the present invention is to provide the preparation sides of above-mentioned ultra-fine boron nitride porous fibre toughening WC composite material Method.
The object of the invention is achieved through the following technical solutions:
A kind of ultra-fine boron nitride porous fibre toughening WC composite material, the composite material is by 99.75~99.99wt.% WC, the ultra-fine boron nitride porous fibre of 0.01~0.25wt.% and inevitable trace impurity composition.
The preparation method of above-mentioned ultra-fine boron nitride porous fibre toughening WC composite material, including following preparation step:
(1) WC powder, ultra-fine boron nitride porous fibre and organic solvent are placed in ball mill and carry out wet ball-milling, be made Ball milling slurry；
(2) it is sieved after ball milling slurry being dried and removed solvent, obtains the composite powder of particle size≤300 μm；
(3) composite powder obtained by step (2) is placed in sintering curing in mold to shape, obtains the ultra-fine nitridation of soap-free emulsion polymeization phase Boron porous fibre toughening WC composite material.
Preferably, organic solvent described in step (1) is ethyl alcohol.
Preferably, drying described in step (2) refers to dry to solvent residues quality≤1%.
Preferably, sintering described in step (3) refers to is sintered using discharge plasma sintering technique；Specific sintering Condition is as follows:
Sintering current type is DC pulse current；
Sintering pressure: 30~50MPa；
Sintering atmosphere: low vacuum≤6Pa；
Heating rate: 50~300 DEG C/min；
Sintering temperature: 1650~1850 DEG C；
Soaking time: 0~10min.
Preparation method of the invention and obtained composite material have the following advantages that and the utility model has the advantages that
(1) micro ultra-fine boron nitride porous fibre is added in the present invention in pure WC, and ultra-fine boron nitride porous fibre has height Specific surface area and high void density help preferably to realize interface cohesion with WC matrix during the preparation process, to traditional the Two-phase toughening mode is made that important improvement；
(2) present invention, which uses the thinner WC powder of partial size and adds micro ultra-fine boron nitride porous fibre, is prepared for toughening WC The fiber reinforced mechanism of composite material, the ultra-fine boron nitride porous fibre of tiny WC grain sum is helping to improve basis material While toughness, the high rigidity of basis material itself is kept；
(3) WC composite material prepared by the present invention be it is a kind of by ultra-fine boron nitride porous fibre toughening without containing any gold Belong to the WC composite material of Binder Phase, it has very high hardness, wearability, antioxygenic property and preferable toughness, is suitable for For cutter material or mold materials.
Detailed description of the invention
Fig. 1 is the XRD spectra of 1 gained ultra-fine boron nitride porous fibre toughening WC composite material of embodiment.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited In this.
Embodiment 1
A kind of ultra-fine boron nitride porous fibre toughening WC composite material of the present embodiment, is prepared via a method which:
(1) by 99.95g WC (0.2 μm, purity > 99.9%, Xuzhou victory innovative material Science and Technology Ltd.), 0.05g is super Thin boron nitride porous fibre (outer diameter 20-60nm, Hebei University of Technology's boron nitride material research center) pours into the conjunction of 250ml hard In golden tank, ethyl alcohol is added as solvent (2/3 of the volume of gained mixed slurry no more than ball milling tank volume), obtains mixing slurry Material；Ball grinder equipped with mixed slurry is placed in progress wet ball-milling (revolving speed 180r/min, Ball-milling Time on planetary ball mill For 30h), ball milling slurry is obtained；
(2) ball milling slurry is placed in a vacuum drying oven drying to solvent residues amount≤1%, the powder after taking out drying is ground Broken, sieving, obtains the composite powder of particle size≤300 μm；
(3) 28g composite powder is taken to put into internal diameterAnd outer diameterCylinder-shaped graphite jig in, powder Material, cavity plate and formed punch are separated between any two with graphite paper to demould, also coated outside cavity plate the graphite felt of one layer of 10mm thickness with Reduce heat radiation loss；Graphite jig equipped with composite powder is placed in discharge plasma sintering furnace and is sintered, nothing is obtained Binder Phase CNTs toughening WC composite material.The sintering parameter are as follows: sintering current type is DC pulse current, and sintering atmosphere is Low vacuum (≤6Pa), sintering pressure 30MPa, heating rate are 100 DEG C/min, and thermometric mode is infrared measurement of temperature (>=570 DEG C), sintering temperature is 1700 DEG C, soaking time 0min.
After ultra-fine boron nitride porous fibre toughening WC composite material obtained by the present embodiment is measured the test of its Archimedes method It is 98.1% that relative density, which is calculated,；Using Vickers and set load 10kg power test hardness, hardness HV10 25GPa；According to Vickers hardness impression, fracture toughness 9.3Mpam is calculated using indentation method1/2。
The XRD spectra of ultra-fine boron nitride porous fibre toughening WC composite material obtained by the present embodiment is as shown in Figure 1, institute in figure Diffraction maximum occur is WC phase.
Embodiment 2
A kind of ultra-fine boron nitride porous fibre toughening WC composite material of the present embodiment, is prepared via a method which:
Step (1)~(2) are same as Example 1；
(3) 28g composite powder is taken to put into internal diameterAnd outer diameterCylinder-shaped graphite jig in, powder Material, cavity plate and formed punch are separated between any two with graphite paper to demould, also coated outside cavity plate the graphite felt of one layer of 10mm thickness with Reduce heat radiation loss；Graphite jig equipped with composite powder is placed in discharge plasma sintering furnace and is sintered, is surpassed Thin boron nitride porous fibre toughening WC composite material.The sintering parameter are as follows: sintering current type is DC pulse current, sintering Atmosphere be low vacuum (≤6Pa), sintering pressure 30MPa, heating rate be 100 DEG C/min, thermometric mode be infrared measurement of temperature (>= 570 DEG C), sintering temperature is 1700 DEG C, soaking time 10min.
Through survey calculation, its relative density is ultra-fine boron nitride porous fibre toughening WC composite material obtained by the present embodiment 98.9%, hardness HV1025.6GPa, fracture toughness 9.2Mpam1/2。
Embodiment 3
A kind of ultra-fine boron nitride porous fibre toughening WC composite material of the present embodiment, is prepared via a method which:
Step (1)~(2) are same as Example 1；
(3) 28g composite powder is taken to put into internal diameterAnd outer diameterCylinder-shaped graphite jig in, powder Material, cavity plate and formed punch are separated between any two with graphite paper to demould, also coated outside cavity plate the graphite felt of one layer of 10mm thickness with Reduce heat radiation loss；Graphite jig equipped with composite powder is placed in discharge plasma sintering furnace and is sintered, is surpassed The fiber reinforced WC composite material of thin boron nitride nanometer.The sintering parameter are as follows: sintering current type is DC pulse current, sintering Atmosphere be low vacuum (≤6Pa), sintering pressure 50MPa, heating rate be 300 DEG C/min, thermometric mode be infrared measurement of temperature (>= 570 DEG C), sintering temperature is 1800 DEG C, soaking time 0min.
Through survey calculation, its relative density is ultra-fine boron nitride porous fibre toughening WC composite material obtained by the present embodiment 98.5%, hardness HV1025.8GPa, fracture toughness 9.06Mpam1/2。
Embodiment 4
A kind of ultra-fine boron nitride porous fibre toughening WC composite material of the present embodiment, is prepared via a method which:
Step (1)~(2) are same as Example 1；
(3) 28g composite powder is taken to put into internal diameterAnd outer diameterCylinder-shaped graphite jig in, powder Material, cavity plate and formed punch are separated between any two with graphite paper to demould, also coated outside cavity plate the graphite felt of one layer of 10mm thickness with Reduce heat radiation loss；Graphite jig equipped with composite powder is placed in discharge plasma sintering furnace and is sintered, is surpassed Thin boron nitride porous fibre toughening WC composite material.The sintering parameter are as follows: sintering current type is DC pulse current, sintering Atmosphere be low vacuum (≤6Pa), sintering pressure 30MPa, heating rate be 100 DEG C/min, thermometric mode be infrared measurement of temperature (>= 570 DEG C), thermometric focus point is located at outer mold wall centre bore bottom, and at mould inner wall 7.5mm, sintering temperature is 1800 DEG C, protects Warm time 5min.
Through survey calculation, its relative density is ultra-fine boron nitride porous fibre toughening WC composite material obtained by the present embodiment 98.7%, hardness HV1024.9GPa, fracture toughness 9.15Mpam1/2。
Embodiment 5
A kind of ultra-fine boron nitride porous fibre toughening WC composite material of the present embodiment, is prepared via a method which:
Step (1)~(2) are same as Example 1；
(3) 28g composite powder is taken to put into internal diameterAnd outer diameterCylinder-shaped graphite jig in, powder Material, cavity plate and formed punch are separated between any two with graphite paper to demould, also coated outside cavity plate the graphite felt of one layer of 10mm thickness with Reduce heat radiation loss；Graphite jig equipped with composite powder is placed in discharge plasma sintering furnace and is sintered, is surpassed Thin boron nitride porous fibre toughening WC composite material.The sintering parameter are as follows: sintering current type is DC pulse current, sintering Atmosphere be low vacuum (≤6Pa), sintering pressure 50MPa, heating rate be 100 DEG C/min, thermometric mode be infrared measurement of temperature (>= 570 DEG C), thermometric focus point is located at outer mold wall centre bore bottom, and at mould inner wall 7.5mm, sintering temperature is 1800 DEG C, protects Warm time 0min.
Through survey calculation, its relative density is ultra-fine boron nitride porous fibre toughening WC composite material obtained by the present embodiment 98.5%, hardness HV1024.8GPa, fracture toughness 9.04Mpam1/2。
Embodiment 6
A kind of ultra-fine boron nitride porous fibre toughening WC composite material of the present embodiment, is prepared via a method which:
Step (1)~(2) are same as Example 1；
(3) 28g composite powder is taken to put into internal diameterAnd outer diameterCylinder-shaped graphite jig in, powder Material, cavity plate and formed punch are separated between any two with graphite paper to demould, also coated outside cavity plate the graphite felt of one layer of 10mm thickness with Reduce heat radiation loss；Graphite jig equipped with composite powder is placed in discharge plasma sintering furnace and is sintered, is surpassed Thin boron nitride porous fibre toughening WC composite material.The sintering parameter are as follows: sintering current type is DC pulse current, sintering Atmosphere be low vacuum (≤6Pa), sintering pressure 30MPa, heating rate be 100 DEG C/min, thermometric mode be infrared measurement of temperature (>= 570 DEG C), thermometric focus point is located at outer mold wall centre bore bottom, and at mould inner wall 7.5mm, sintering temperature is 1850 DEG C, protects Warm time 5min.
Through survey calculation, its relative density is ultra-fine boron nitride porous fibre toughening WC composite material obtained by the present embodiment 98.2%, hardness HV1025.9GPa, fracture toughness 9.03Mpam1/2。
Embodiment 7
A kind of ultra-fine boron nitride porous fibre toughening WC composite material of the present embodiment, is prepared via a method which:
Step (1)~(2) are same as Example 1；
(3) 28g composite powder is taken to put into internal diameterAnd outer diameterCylinder-shaped graphite jig in, powder Material, cavity plate and formed punch are separated between any two with graphite paper to demould, also coated outside cavity plate the graphite felt of one layer of 10mm thickness with Reduce heat radiation loss；Graphite jig equipped with composite powder is placed in discharge plasma sintering furnace and is sintered, is surpassed Thin boron nitride porous fibre toughening WC composite material.The sintering parameter are as follows: sintering current type is DC pulse current, sintering Atmosphere be low vacuum (≤6Pa), sintering pressure 50MPa, heating rate be 50 DEG C/min, thermometric mode be infrared measurement of temperature (>= 570 DEG C), thermometric focus point is located at outer mold wall centre bore bottom, and at mould inner wall 7.5mm, sintering temperature is 1850 DEG C, protects Warm time 0min.
Through survey calculation, its relative density is ultra-fine boron nitride porous fibre toughening WC composite material obtained by the present embodiment 98.8%, hardness HV1025.4GPa, fracture toughness 8.99Mpam1/2。
Embodiment 8
A kind of ultra-fine boron nitride porous fibre toughening WC composite material 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 is super Thin boron nitride porous fibre (outer diameter 20-60nm, Hebei University of Technology's boron nitride material research center) pours into the conjunction of 250ml hard In golden tank, ethyl alcohol is added as solvent (2/3 of the volume of gained mixed slurry no more than ball milling tank volume), obtains mixing slurry Material；Ball grinder equipped with mixed slurry is placed in progress wet ball-milling (revolving speed 180r/min, Ball-milling Time on planetary ball mill For 30h), ball milling slurry is obtained；
Step (2)~(3) are same as Example 1.
Through survey calculation, its relative density is ultra-fine boron nitride porous fibre toughening WC composite material obtained by the present embodiment 98.9%, hardness HV1025.5GPa, fracture toughness 8.89Mpam1/2。
Embodiment 9
A kind of ultra-fine boron nitride porous fibre toughening WC composite material 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 is super Thin boron nitride porous fibre (outer diameter 20-60nm, Hebei University of Technology's boron nitride material research center) pours into the conjunction of 250ml hard In golden tank, ethyl alcohol is added as solvent (2/3 of the volume of gained mixed slurry no more than ball milling tank volume), obtains mixing slurry Material；Ball grinder equipped with mixed slurry is placed in progress wet ball-milling (revolving speed 180r/min, Ball-milling Time on planetary ball mill For 30h), ball milling slurry is obtained；
Step (2)~(3) are same as Example 1.
Through survey calculation, its relative density is ultra-fine boron nitride porous fibre toughening WC composite material obtained by the present embodiment 98.8%, hardness HV1024.5GPa, fracture toughness 8.75Mpam1/2。
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention, It should be equivalent substitute mode, be included within the scope of the present invention.

Claims (5)

1. a kind of ultra-fine boron nitride porous fibre toughening WC composite material, it is characterised in that: the composite material by 99.75~ The ultra-fine boron nitride porous fibre of the WC of 99.99wt.%, 0.01~0.25wt.% and inevitable trace impurity composition.
2. a kind of preparation method of ultra-fine boron nitride porous fibre toughening WC composite material described in claim 1, feature exist In including following preparation step:
(1) WC powder, ultra-fine boron nitride porous fibre and organic solvent are placed in ball mill and carry out wet ball-milling, ball milling is made Slurry；
(2) it is sieved after ball milling slurry being dried and removed solvent, obtains the composite powder of particle size≤300 μm；
(3) composite powder obtained by step (2) is placed in sintering curing in mold to shape, the ultra-fine boron nitride for obtaining soap-free emulsion polymeization phase is more The fiber reinforced WC composite material in hole.
3. a kind of preparation method of ultra-fine boron nitride porous fibre toughening WC composite material according to claim 2, special Sign is: organic solvent described in step (1) is ethyl alcohol.
4. a kind of preparation method of ultra-fine boron nitride porous fibre toughening WC composite material according to claim 2, special Sign is: drying described in step (2) refers to dry to solvent residues quality≤1%.
5. a kind of preparation method of ultra-fine boron nitride porous fibre toughening WC composite material according to claim 2, special Sign is: sintering described in step (3) refers to be sintered using discharge plasma sintering technique；Specific sintering condition is such as Under:
Sintering current type is DC pulse current；
Sintering pressure: 30~50MPa；
Sintering atmosphere: low vacuum≤6Pa；
Heating rate: 50~300 DEG C/min；
Sintering temperature: 1650~1850 DEG C；
Soaking time: 0~10min.
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CN103664191A (en) * 2012-09-13 2014-03-26 南京航空航天大学 Preparation method of boron nitride fiber toughened boron nitride and silicon nitride based wave-transparent composite
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