CN105127430A - Ultra-hard material containing cubic boron nitride, wurtzite type boron nitride and diamond and preparation method of ultra-hard material - Google Patents
Ultra-hard material containing cubic boron nitride, wurtzite type boron nitride and diamond and preparation method of ultra-hard material Download PDFInfo
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Abstract
The invention discloses an ultra-hard material containing cubic boron nitride, wurtzite type boron nitride and diamond. The ultra-hard material comprises a crystal combination layer and a hard alloy layer. The crystal combination layer is sintered on the hard alloy layer and is composed of wurtzite type boron nitride, cubic boron nitride and diamond. The invention further discloses a preparation method of the ultra-hard material. Wurtzite type boron nitride is converted into cubic boron nitride under the high-pressure and high-temperature condition, and finally a sintered body is formed. The hardness of the ultra-hard material is higher than that of diamond, and therefore the ultra-hard material can be manufactured into all types of cutting tools, wire-drawing tools and grinding tools.
Description
Technical field
The invention belongs to superhard material field, relate to one and there is cubic boron nitride, wurtzite BN and adamantine superhard material and preparation method thereof.
Background technology
Boron nitride is the crystal be made up of nitrogen-atoms and boron atom, chemical composition is the boron of 43.6% and the nitrogen of 56.4%, has four kinds of different variants: hexagonal boron nitride (hBN), water chestnut side's boron nitride (rBN), cubic boron nitride (cBN) and wurtzite BN (wBN).Wurtzite BN crystal grain is tiny, can not as cutter body.
Along with the development of modern technologies, superhard material is widely used, such as cutting tools, grinding tool, boring means and cutting element.Superhard material comprises two kinds: diamond and cubic boron nitride (cBN).Diamond owing to starting carbonization more than 600 DEG C, and particularly in the material having ferro element to exist, along with the rising of temperature, its mechanical strength declines rapidly, because which limit the application of diamond when processing iron series metal goods.Cubic boron nitride just in time overcomes this defect, and cubic boron nitride is under oxidizing atmosphere condition, and 900 DEG C still can ensure its mechanical strength, therefore in High-Speed Automatic processing equipment field, is widely used.
Traditionally, as in the cubic boron nitride sintered body of cutting element or wear resistant tools containing agglutinant or adhesive, as TiN, TiC and Co.This sintered body obtains by cubic boron nitride powder and agglutinant or adhesive being sintered under the pressure of 4 ~ 5GPa.In this sintered body containing have an appointment 10 ~ 40% adhesive, adhesive greatly affects the intensity of sintered body, heat resistance and heat diffusivity, high-speed cutting, especially at cutting ferrous metals material time, easily there is defect and crackle on the cutting edge, which reduce the life-span of instrument.
In order to extend life tools, the existing cBN sintered body manufacture method not using adhesive.In the method, the catalyst of hexagonal boron nitride and such as Dan Pengization Magnesium and so on is used as raw material, they is sintered and reacts.According to the method, owing to not using adhesive, strongly combine between cBN particle, thermal conductivity is up to 6 ~ 7W/cm DEG C.Therefore, cBN sintered body is used as in radiator material or the automatic combination tool of winding.But because partially catalyzed agent remains in sintered body, and when sintered body is heated, due to the thermal dilation difference between cBN and catalyst, easily produce hair check, thus heat resisting temperature is low to moderate 700 DEG C, this is a very large problem for cutting element.In addition, because particle diameter slightly reaches about 10 μm, although this improves thermal conductivity, weaken its intensity, make it cannot bear large cutting load.
Although can when there is no additive as sintered diamond metal (metal can reduce hardness and the service life of final products), but sintering needs the pressure more than 10GPa when additive, this, for hypertonia industrial production, can reduce service life of equipment.WBN is current energy the hardest industrial material, and can change cBN into gradually under the high pressure high temperature condition more than 6GPa and 1400 DEG C, fringe time long enough, wBN all can change cBN into.
Summary of the invention
For solving the problem, the object of this invention is to provide one there is high rigidity, the superhard material of comprise wurtzite BN (wBN) and cubic boron nitride (cBN) and diamond mixed sintering body.
Another object of the present invention is to provide the preparation method of this superhard material.
For achieving the above object, the present invention by the following technical solutions:
One has cubic boron nitride, wurtzite BN and adamantine superhard material, comprise glomerocryst layer and hard alloy layer, glomerocryst layer sintering is on hard alloy layer, the main component of hard alloy layer is tungsten carbide and cobalt, wherein the content of cobalt accounts for 3 ~ 30% of carbide alloy gross weight, and glomerocryst layer also has diamond to form by wurtzite BN and cubic boron nitride.
Further, the cubic boron nitride of described glomerocryst layer is transformed by wurtzite BN.
Further, the cubic boron nitride of described glomerocryst layer is sintered by wurtzite BN and is transformed under the condition of pressure >=6GPa, temperature >=1400 DEG C.
Prepare an above-mentioned method with cubic boron nitride, wurtzite BN and adamantine superhard material, comprise the following steps:
(1) wurtzite BN micro mist (Jing Li Chi Cun≤10 μm) and diadust (Jing Li Chi Cun≤20 μm) is got out;
(2) be encased in not melting, not broken high pressure-temperature container after both being mixed;
(3) be placed in step (2) container by disc-shaped or powdery tungsten carbide, this disc-shaped or powdery tungsten carbide are pressed in above mixed micro mist, and becoming hard alloy layer after sintering is that subsequent tool making is prepared;
(4) above-mentioned high temperature and high pressure containers is placed in high-tension apparatus, boosts to more than 6GPa, be warming up to more than 1400 DEG C;
(5) the pressure and temperature 10 ~ 30min of step (4) is kept;
(6) reduce pressure, stop heating, make device temperature reach 0 ~ 25 DEG C, pressure reaches standard atmospheric pressure;
(7) from high-tension apparatus, take out container, remove the container of sintered body surface parcel, obtain that there is cubic boron nitride, wurtzite BN and adamantine superhard material.
The invention has the beneficial effects as follows:
Wurtzite BN is under the superhigh-temperature and-pressure condition more than 6GPa and 1400 DEG C, atom moves and reconfigures, and can change cubic boron nitride into, and conversion ratio depends on the time of HTHP, when time long enough, wurtzite BN all can be converted into cubic boron nitride.The present invention utilizes this principle, reaction was stopped before all wurtzite BNs are converted into cubic boron nitride, the mixed sintering body of wurtzite BN and cubic boron nitride composition can be obtained, the hardness of this material is higher than natural diamond, also higher than the diamond of sintering, what sinter into has cubic boron nitride, wurtzite BN and adamantine superhard material, and performance is better than diamond.This boron nitride material with high rigidity and rigidity can make various cutting element, wire drawing tool and milling tool, meets the hardness requirement that modern mechanical industry is more and more higher to cutter.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described further:
embodiment 1
1.2g crystallite dimension slightly being soaked by toluene at the wurtzite BN of 1 micron and the 0.8g crystallite dimension diamond particle at 2 microns, by being uniformly mixed, being filled into Φ 12*10mm, in the zirconium cup of thick 0.5mm.With the pressing of 20kg/c ㎡ pressure, wurtzite BN micro mist thickness is 7mm, puts into the tungsten-cobalt alloy disk of Φ 11*3mm afterwards.Container is put into high-tension apparatus, synthesizes 15 minutes under 6.5GPa, 1650 DEG C of conditions.After end of synthesis, pressure reduces to atmospheric pressure, is reduced gradually by heating stop temperature.Container takes out from high-tension apparatus, and the zirconium of surface coverage is removed through grinding.Wurtzite BN and diamond are combined with tungsten-cobalt alloy moieties into close.Shape is the cylinder of Φ 11*9mm.The surface of cylinder and side are all by boart boart buff polishing.
The surface of wurtzite BN and diamond end is checked by X-ray diffraction.Find that wurtzite BN, cubic boron nitride and diamond peak exist, and the height at wurtzite BN and cubic boron nitride peak is equal.This means that wurtzite BN is converted into cubic boron nitride, wurtzite BN is equal with the content of cubic boron nitride, and this change makes wurtzite BN, cubic boron nitride and diamond crystals be combined together to form sintered body.With the microscopic examination wurtzite BN-cubic boron nitride-diamond surface of amplification 500 times, do not observe pore.
Wurtzite BN, cubic boron nitride and adamantine mixed sintering surface hardness: when being loaded as 9.8N, micro-vickers hardness is 72GPa.
embodiment 2
1.2g crystallite dimension slightly being soaked by toluene at the wurtzite BN of 1 micron and the 0.8g crystallite dimension diamond particle at 2 microns, by being uniformly mixed, being filled into Φ 12*10mm, in the zirconium cup of thick 0.5mm.With the pressing of 20kg/c ㎡ pressure, wurtzite BN micro mist thickness is 7mm, puts into the tungsten-cobalt alloy disk of Φ 11*3mm afterwards.Container is put into high-tension apparatus, synthesizes 11 minutes under 6.5GPa, 1650 DEG C of conditions.After end of synthesis, pressure reduces to atmospheric pressure, is reduced gradually by heating stop temperature.Container takes out from high-tension apparatus, and the zirconium of surface coverage is removed through grinding.Wurtzite BN and diamond are combined with tungsten-cobalt alloy moieties into close.Shape is the cylinder of Φ 11*9mm.The surface of cylinder and side are all by boart boart buff polishing.
The surface of wurtzite BN and diamond end is checked by X-ray diffraction.Find that wurtzite BN, cubic boron nitride and diamond peak exist, and the height at cubic boron nitride peak is 25% of wurtzite BN.This means that wurtzite BN is converted into cubic boron nitride, the content of cubic boron nitride is 25% of wurtzite BN, and this change makes wurtzite BN, cubic boron nitride and diamond crystals be combined together to form sintered body.With the microscopic examination wurtzite BN-cubic boron nitride-diamond surface of amplification 500 times, do not observe pore.
Wurtzite BN, cubic boron nitride and adamantine mixed sintering surface hardness: when being loaded as 9.8N, micro-vickers hardness is 70GPa.
embodiment 3
1.5g crystallite dimension slightly being soaked by toluene at the wurtzite BN of 1 micron and the 0.5g crystallite dimension diamond particle at 2 microns, by being uniformly mixed, being filled into Φ 12*10mm, in the zirconium cup of thick 0.5mm.With the pressing of 20kg/c ㎡ pressure, wurtzite BN micro mist thickness is 7mm, puts into the tungsten-cobalt alloy disk of Φ 11*3mm afterwards.Container is put into high-tension apparatus, synthesizes 15 minutes under 6.9GPa, 1780 DEG C of conditions.After end of synthesis, pressure reduces to atmospheric pressure, is reduced gradually by heating stop temperature.Container takes out from high-tension apparatus, and the zirconium of surface coverage is removed through grinding.Wurtzite BN and diamond are combined with tungsten-cobalt alloy moieties into close.Shape is the cylinder of Φ 11*9mm.The surface of cylinder and side are all by boart boart buff polishing.
The surface of wurtzite BN and diamond end is checked by X-ray diffraction.Find that wurtzite BN, cubic boron nitride and diamond peak exist, and the height at cubic boron nitride peak is 70% of wurtzite BN.This means that wurtzite BN is converted into cubic boron nitride, the content of cubic boron nitride is 70% of wurtzite BN, and this change makes wurtzite BN, cubic boron nitride and diamond crystals be combined together to form sintered body.With the microscopic examination wurtzite BN-cubic boron nitride-diamond surface of amplification 500 times, do not observe pore.
Wurtzite BN, cubic boron nitride and adamantine mixed sintering surface hardness: when being loaded as 9.8N, micro-vickers hardness is 73GPa.
embodiment 4
1.2g crystallite dimension slightly being soaked by toluene at the wurtzite BN of 1 micron and the 0.8g crystallite dimension diamond particle at 2 microns, by being uniformly mixed, being filled into Φ 12*10mm, in the zirconium cup of thick 0.5mm.With the pressing of 20kg/c ㎡ pressure, wurtzite BN micro mist thickness is 7mm, puts into the tungsten-cobalt alloy disk of Φ 11*3mm afterwards.Container is put into high-tension apparatus, synthesizes 20 minutes under 6.5GPa, 1650 DEG C of conditions.After end of synthesis, pressure reduces to atmospheric pressure, is reduced gradually by heating stop temperature.Container takes out from high-tension apparatus, and the zirconium of surface coverage is removed through grinding.Wurtzite BN and diamond are combined with tungsten-cobalt alloy moieties into close.Shape is the cylinder of Φ 11*9mm.The surface of cylinder and side are all by boart boart buff polishing.
The surface of wurtzite BN and diamond end is checked by X-ray diffraction.Find that wurtzite BN, cubic boron nitride and diamond peak exist, and the height at wurtzite BN and cubic boron nitride peak is equal.This means that wurtzite BN is converted into cubic boron nitride, wurtzite BN is equal with the content of cubic boron nitride, and this change makes wurtzite BN, cubic boron nitride and diamond crystals be combined together to form sintered body.With the microscopic examination wurtzite BN-cubic boron nitride-diamond surface of amplification 500 times, do not observe pore.
Wurtzite BN, cubic boron nitride and adamantine mixed sintering surface hardness: when being loaded as 9.8N, micro-vickers hardness is 46GPa.
embodiment 5
1.2g crystallite dimension slightly being soaked by toluene at the wurtzite BN of 1 micron and the 0.8g crystallite dimension diamond particle at 2 microns, by being uniformly mixed, being filled into Φ 12*10mm, in the zirconium cup of thick 0.5mm.With the pressing of 20kg/c ㎡ pressure, wurtzite BN micro mist thickness is 7mm, puts into the tungsten-cobalt alloy disk of Φ 11*3mm afterwards.Container is put into high-tension apparatus, synthesizes 18 minutes under 6.9GPa, 1780 DEG C of conditions.After end of synthesis, pressure reduces to atmospheric pressure, is reduced gradually by heating stop temperature.Container takes out from high-tension apparatus, and the zirconium of surface coverage is removed through grinding.Wurtzite BN and diamond are combined with tungsten-cobalt alloy moieties into close.Shape is the cylinder of Φ 11*9mm.The surface of cylinder and side are all by boart boart buff polishing.
The surface of wurtzite BN and diamond end is checked by X-ray diffraction.Find that wurtzite BN, cubic boron nitride and diamond peak exist, and the height at wurtzite BN and cubic boron nitride peak is equal.This means that wurtzite BN is converted into cubic boron nitride, wurtzite BN is equal with the content of cubic boron nitride, and this change makes wurtzite BN, cubic boron nitride and diamond crystals be combined together to form sintered body.With the microscopic examination wurtzite BN-cubic boron nitride-diamond surface of amplification 500 times, do not observe pore.
Wurtzite BN, cubic boron nitride and adamantine mixed sintering surface hardness: when being loaded as 9.8N, micro-vickers hardness is 44GPa.
embodiment 6
1.2g crystallite dimension slightly being soaked by toluene at the wurtzite BN of 1 micron and the 0.8g crystallite dimension diamond particle at 2 microns, by being uniformly mixed, being filled into Φ 12*10mm, in the zirconium cup of thick 0.5mm.With the pressing of 20kg/c ㎡ pressure, wurtzite BN micro mist thickness is 7mm, puts into the tungsten-cobalt alloy disk of Φ 11*3mm afterwards.Container is put into high-tension apparatus, synthesizes 25 minutes under 6.2GPa, 1580 DEG C of conditions.After end of synthesis, pressure reduces to atmospheric pressure, is reduced gradually by heating stop temperature.Container takes out from high-tension apparatus, and the zirconium of surface coverage is removed through grinding.Wurtzite BN and diamond are combined with tungsten-cobalt alloy moieties into close.Shape is the cylinder of Φ 11*9mm.The surface of cylinder and side are all by boart boart buff polishing.
The surface of wurtzite BN and diamond end is checked by X-ray diffraction.Find that wurtzite BN, cubic boron nitride and diamond peak exist, and the height at wurtzite BN and cubic boron nitride peak is equal.This means that wurtzite BN is converted into cubic boron nitride, wurtzite BN is equal with the content of cubic boron nitride, and this change makes wurtzite BN, cubic boron nitride and diamond crystals be combined together to form sintered body.With the microscopic examination wurtzite BN-cubic boron nitride-diamond surface of amplification 500 times, do not observe pore.
Wurtzite BN, cubic boron nitride and adamantine mixed sintering surface hardness: when being loaded as 9.8N, micro-vickers hardness is 46GPa.
Claims (10)
1. one kind has cubic boron nitride, wurtzite BN and adamantine superhard material, it is characterized in that, comprise glomerocryst layer and hard alloy layer, glomerocryst layer is sintered on hard alloy layer by HTHP, the main component of hard alloy layer is tungsten carbide and cobalt, and wherein the content of cobalt accounts for 3 ~ 30% of carbide alloy gross weight.
2. one according to claim 1 has cubic boron nitride, wurtzite BN and adamantine superhard material, it is characterized in that, described glomerocryst layer includes cubic boron nitride, wurtzite BN and diamond.
3. one according to claim 1 has cubic boron nitride, wurtzite BN and adamantine superhard material, it is characterized in that, the cubic boron nitride of described glomerocryst layer is transformed by wurtzite BN.
4. one according to claim 1 has cubic boron nitride, wurtzite BN and adamantine superhard material, it is characterized in that, the cubic boron nitride of described glomerocryst layer is sintered by wurtzite BN and is transformed under the condition of pressure >=6GPa, temperature >=1400 DEG C.
5. prepare a method with cubic boron nitride, wurtzite BN and adamantine superhard material according to claim 1, it is characterized in that, comprise the following steps:
(1) wurtzite BN and the original micro mist of diamond is proportionally taken;
(2) the original micro mist in blend step (1), ball milling 30 minutes, make original micro mist mix evenly, obtain admixed finepowder, add toluene solution as lubricant;
(3) heat drying, removing toluene;
(4) admixed finepowder is installed in high temperature high voltage resistant container;
(5) be placed in step (4) container by disc-shaped or powdery tungsten carbide again, this disc-shaped or powdery tungsten carbide are pressed in above admixed finepowder, become hard alloy layer after sintering;
(6) the high-temperature-resistant high-pressure-resistant container filling admixed finepowder in step (5) is put into high-temperature high-pressure apparatus, boost to more than 6GPa, be warming up to more than 1400 DEG C;
(7) the pressure and temperature 10 ~ 30min of step (6) is kept;
(8) reduce pressure, stop heating, make device temperature reach 0 ~ 25 DEG C, pressure reaches standard atmospheric pressure;
(9) from high-tension apparatus, take out container, remove the container of sintered body surface parcel, obtain that there is cubic boron nitride, wurtzite BN and adamantine superhard material.
6. the preparation method with cubic boron nitride, wurtzite BN and adamantine superhard material according to claim 5, it is characterized in that, diamond in original micro mist before high temperature high pressure process: the mass ratio of (cubic boron nitride+wurtzite BN) is 1:5 ~ 5:1.
7. the preparation method with cubic boron nitride, wurtzite BN and adamantine superhard material according to claim 5, is characterized in that, crystallite dimension≤10 μm of described wurtzite BN micro mist.
8. the preparation method with cubic boron nitride, wurtzite BN and adamantine superhard material according to claim 5, is characterized in that, crystallite dimension≤20 μm of described diadust.
9. the preparation method with cubic boron nitride, wurtzite BN and adamantine superhard material according to claim 5, it is characterized in that, sintered body is made up of cubic boron nitride, wurtzite BN and diamond.
10. the preparation method with cubic boron nitride, wurtzite BN and adamantine superhard material according to claim 5, it is characterized in that, the cubic boron nitride in described sintered body: wurtzite BN is 10:1 ~ 1:10 by X-ray diffraction peak heights ratio.
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