CN106116617A - A kind of ultra-fine boron nitride porous fibre toughness reinforcing WC composite and preparation method thereof - Google Patents

A kind of ultra-fine boron nitride porous fibre toughness reinforcing WC composite and preparation method thereof Download PDF

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CN106116617A
CN106116617A CN201610457523.8A CN201610457523A CN106116617A CN 106116617 A CN106116617 A CN 106116617A CN 201610457523 A CN201610457523 A CN 201610457523A CN 106116617 A CN106116617 A CN 106116617A
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boron nitride
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porous fibre
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CN106116617B (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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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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 toughness reinforcing WC composite and preparation method thereof.Described composite by 99.75～99.99wt.% WC, the ultra-fine boron nitride porous fibre of 0.01～0.25wt.% and inevitably trace impurity composition.Described preparation method is: WC powder body, ultra-fine boron nitride porous fibre 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 gained composite powder is placed in sintering curing shaping in mould, obtains product.Gained composite of the present invention is a kind of WC composite of not containing any metallic binding phase toughness reinforcing by ultra-fine boron nitride porous fibre, there is the highest hardness, wearability, antioxygenic property and preferable toughness, be suitable as cutter material or mold materials.

Description

A kind of ultra-fine boron nitride porous fibre toughness reinforcing WC composite and preparation method thereof
Technical field
The invention belongs to technical field of alloy material, be specifically related to a kind of ultra-fine boron nitride porous fibre toughness reinforcing WC composite wood Material 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, it is easy to cause damage equipment, and disconnected after sintering Split toughness to only have～4MPa m1/2.A kind of Binder Phase when Co sinters as WC, has extraordinary wettability, simultaneously energy to WC Making WC sintering temperature be reduced to～1400 DEG C, during sintering, Co becomes liquid phase, is greatly increased WC particle diffusion rate, makes sintering cause Close, after sintering the usual fracture toughness of tungsten carbide composite～12MPa m1/2.World's Co distribution of resource is extremely uneven Weighing apparatus, the Co reserves sum of Congo (Congo-Kinshasa), Australia and state of Cuba three just occupies the 68% of world's gross reserves.The Co money of China Source is most deficient, heavy dependence import so that the supply of Co raw material there is also a lot of unstable factor.Co glues as one simultaneously Knot agent, reduces the hardness of WC material, corrosion resistance and heat-resisting quantity, limits WC material under some extreme Service Environment Application.Therefore, find the material of non-adherent phase of a kind of common wide material sources to substitute Co, break away from external dependence, with The hardness of Shi Tigao WC series hard alloy and high-temperature behavior just seem 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.General pottery adds phase, either granule or fiber/whisker, all It is susceptible to the problems such as the interfacial bonding property with matrix is not enough, while improving toughness, has a strong impact on hardness performance.Ultra-fine nitrogen Change boron porous fibre, compare traditional boron nitride nano-tube, due to its loose 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 in preparation process, realize interface cohesion with matrix, improve traditional secondary phase toughening mode, and Trace adds can be effectively improved mechanical property.Ultra-fine boron nitride porous fibre is used to prepare grinding of toughness reinforcing WC composite at present Study carefully and not yet have been reported that.
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 ultra-fine Boron nitride porous fibre toughness reinforcing WC composite.
Another object of the present invention is to provide the preparation side of above-mentioned ultra-fine boron nitride porous fibre toughness reinforcing WC composite Method.
The object of the invention is achieved through the following technical solutions:
A kind of ultra-fine boron nitride porous fibre toughness reinforcing WC composite, described composite is by 99.75～99.99wt.% WC, the ultra-fine boron nitride porous fibre of 0.01～0.25wt.% and inevitably trace impurity composition.
The preparation method of above-mentioned ultra-fine boron nitride porous fibre toughness reinforcing WC composite, including following preparation process:
(1) WC powder body, ultra-fine boron nitride porous fibre 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 is placed in sintering curing in mould shape, obtains the ultra-fine nitridation of soap-free emulsion polymeization phase Boron porous fibre 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 obtained composite of the present invention have the advantage that and beneficial effect:
(1) present invention adds trace ultra-fine boron nitride porous fibre in pure WC, and ultra-fine boron nitride porous fibre has height Specific surface area and high void density, contribute in preparation process preferably and WC matrix realize interface cohesion, to traditional the The toughness reinforcing mode of two-phase is made that important improvement；
(2) present invention uses WC powder body that particle diameter is thinner and adds trace ultra-fine boron nitride porous fibre and be prepared for toughness reinforcing WC Composite, the fiber reinforced mechanism of the ultra-fine boron nitride porous fibre of tiny WC grain sum is being favorably improved matrix material While toughness, keep the high rigidity of matrix material itself；
(3) the WC composite that prepared by the present invention be a kind of by ultra-fine boron nitride porous fibre toughness reinforcing do not contain any gold Belonging to the WC composite of Binder Phase, it has the highest hardness, wearability, antioxygenic property and preferable toughness, is suitable as For cutter material or mold materials.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of embodiment 1 gained ultra-fine boron nitride porous fibre 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 ultra-fine boron nitride porous fibre toughness reinforcing WC composite 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 surpasses Thin boron nitride porous fibre (external diameter 20-60nm, Hebei University of Technology's boron nitride material research center), pours 250ml hard into and closes In gold tank, add ethanol as solvent the 2/3 of ball grinder volume (volume of gained mixed slurry less than), obtain mixing slurry Material；Will be equipped with the ball grinder of mixed slurry to be placed on planetary ball mill and carry out wet ball-milling (rotating speed 180r/min, Ball-milling Time For 30h), obtain ball milling slurry；
(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 CNTs 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 ultra-fine boron nitride porous fibre toughness reinforcing WC composite is after measuring the test of its Archimedes method Being calculated relative density is 98.1%；Using Vickers and set load 10kg power test hardness, hardness is HV10 25GPa；According to Vickers hardness impression, indentation method is used to be calculated fracture toughness 9.3Mpa m1/2。
The XRD spectra of the present embodiment gained ultra-fine boron nitride porous fibre toughness reinforcing WC composite is as it is shown in figure 1, institute in figure Occur that diffraction maximum is WC phase.
Embodiment 2
A kind of ultra-fine boron nitride porous fibre 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, surpassed Thin boron nitride porous fibre toughness reinforcing WC composite.Described sintering parameter is: sintering current type is DC pulse current, sintering Atmosphere is coarse vacuum (≤6Pa), and sintering pressure is 30MPa, and heating rate is 100 DEG C/min, thermometric mode be infrared measurement of temperature (>= 570 DEG C), sintering temperature is 1700 DEG C, temperature retention time 10min.
The present embodiment gained ultra-fine boron nitride porous fibre toughness reinforcing WC composite through its relative density of survey calculation is 98.9%, hardness is HV1025.6GPa, fracture toughness 9.2Mpa m1/2。
Embodiment 3
A kind of ultra-fine boron nitride porous fibre 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, surpassed Thin boron nitride nanometer fiber reinforced WC composite.Described sintering parameter is: sintering current type is DC pulse current, sintering Atmosphere is coarse vacuum (≤6Pa), and sintering pressure is 50MPa, and heating rate is 300 DEG C/min, thermometric mode be infrared measurement of temperature (>= 570 DEG C), sintering temperature is 1800 DEG C, temperature retention time 0min.
The present embodiment gained ultra-fine boron nitride porous fibre toughness reinforcing WC composite through its relative density of survey calculation is 98.5%, hardness is HV1025.8GPa, fracture toughness 9.06Mpa m1/2。
Embodiment 4
A kind of ultra-fine boron nitride porous fibre 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, surpassed Thin boron nitride porous fibre toughness reinforcing WC composite.Described sintering parameter is: sintering current type is DC pulse current, sintering Atmosphere is coarse vacuum (≤6Pa), and sintering pressure is 30MPa, and heating rate is 100 DEG C/min, thermometric mode be 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, protects Temperature time 5min.
The present embodiment gained ultra-fine boron nitride porous fibre toughness reinforcing WC composite through its relative density of survey calculation is 98.7%, hardness is HV1024.9GPa, fracture toughness 9.15Mpa m1/2。
Embodiment 5
A kind of ultra-fine boron nitride porous fibre 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, surpassed Thin boron nitride porous fibre toughness reinforcing WC composite.Described sintering parameter is: sintering current type is DC pulse current, sintering Atmosphere is coarse vacuum (≤6Pa), and sintering pressure is 50MPa, and heating rate is 100 DEG C/min, thermometric mode be 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, protects Temperature time 0min.
The present embodiment gained ultra-fine boron nitride porous fibre toughness reinforcing WC composite through its relative density of survey calculation is 98.5%, hardness is HV1024.8GPa, fracture toughness 9.04Mpa m1/2。
Embodiment 6
A kind of ultra-fine boron nitride porous fibre 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, surpassed Thin boron nitride porous fibre toughness reinforcing WC composite.Described sintering parameter is: sintering current type is DC pulse current, sintering Atmosphere is coarse vacuum (≤6Pa), and sintering pressure is 30MPa, and heating rate is 100 DEG C/min, thermometric mode be 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, protects Temperature time 5min.
The present embodiment gained ultra-fine boron nitride porous fibre toughness reinforcing WC composite through its relative density of survey calculation is 98.2%, hardness is HV1025.9GPa, fracture toughness 9.03Mpa m1/2。
Embodiment 7
A kind of ultra-fine boron nitride porous fibre 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, surpassed Thin boron nitride porous fibre toughness reinforcing WC composite.Described sintering parameter is: sintering current type is DC pulse current, sintering Atmosphere is coarse vacuum (≤6Pa), and sintering pressure is 50MPa, and heating rate is 50 DEG C/min, thermometric mode be 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, protects Temperature time 0min.
The present embodiment gained ultra-fine boron nitride porous fibre toughness reinforcing WC composite through its relative density of survey calculation is 98.8%, hardness is HV1025.4GPa, fracture toughness 8.99Mpa m1/2。
Embodiment 8
A kind of ultra-fine boron nitride porous fibre 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 surpasses Thin boron nitride porous fibre (external diameter 20-60nm, Hebei University of Technology's boron nitride material research center), pours 250ml hard into and closes In gold tank, add ethanol as solvent the 2/3 of ball grinder volume (volume of gained mixed slurry less than), obtain mixing slurry Material；Will be equipped with the ball grinder of mixed slurry to be placed on planetary ball mill and carry out wet ball-milling (rotating speed 180r/min, Ball-milling Time For 30h), obtain ball milling slurry；
Step (2)～(3) are same as in Example 1.
The present embodiment gained ultra-fine boron nitride porous fibre toughness reinforcing WC composite through its relative density of survey calculation is 98.9%, hardness is HV1025.5GPa, fracture toughness 8.89Mpa m1/2。
Embodiment 9
A kind of ultra-fine boron nitride porous fibre 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 surpasses Thin boron nitride porous fibre (external diameter 20-60nm, Hebei University of Technology's boron nitride material research center), pours 250ml hard into and closes In gold tank, add ethanol as solvent the 2/3 of ball grinder volume (volume of gained mixed slurry less than), obtain mixing slurry Material；Will be equipped with the ball grinder of mixed slurry to be placed on planetary ball mill and carry out wet ball-milling (rotating speed 180r/min, Ball-milling Time For 30h), obtain ball milling slurry；
Step (2)～(3) are same as in Example 1.
The present embodiment gained ultra-fine boron nitride porous fibre toughness reinforcing WC composite through its relative density of survey calculation is 98.8%, hardness is HV1024.5GPa, fracture toughness 8.75Mpa 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 ultra-fine boron nitride porous fibre toughness reinforcing WC composite, it is characterised in that: described composite by 99.75～ The WC of 99.99wt.%, the ultra-fine boron nitride porous fibre of 0.01～0.25wt.% and inevitable trace impurity composition.
2. the preparation method of a kind of ultra-fine boron nitride porous fibre toughness reinforcing WC composite described in claim 1, its feature exists In including following preparation process:
(1) WC powder body, ultra-fine boron nitride porous fibre 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 ultra-fine boron nitride obtaining soap-free emulsion polymeization phase is many Hole fiber reinforced WC composite.
The preparation method of a kind of ultra-fine boron nitride porous fibre the most according to claim 2 toughness reinforcing WC composite, it is special Levy and be: the organic solvent described in step (1) is ethanol.
The preparation method of a kind of ultra-fine boron nitride porous fibre the most according to claim 2 toughness reinforcing WC composite, it is special Levy and be: dry the referring to described in step (2) is dried to solvent residues quality≤1%.
The preparation method of a kind of ultra-fine boron nitride porous fibre the most according to claim 2 toughness reinforcing WC composite, it is special Levy and be: the sintering described in step (3) refers to use discharge plasma sintering technique to be sintered；Concrete sintering condition is such as Under:
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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