CN105127430B - A kind of superhard material with cubic boron nitride, wurtzite BN and diamond and preparation method thereof - Google Patents
A kind of superhard material with cubic boron nitride, wurtzite BN and diamond and preparation method thereof Download PDFInfo
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- CN105127430B CN105127430B CN201510521165.8A CN201510521165A CN105127430B CN 105127430 B CN105127430 B CN 105127430B CN 201510521165 A CN201510521165 A CN 201510521165A CN 105127430 B CN105127430 B CN 105127430B
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Abstract
The invention discloses a kind of superhard material with cubic boron nitride, wurtzite BN and diamond, including glomerocryst layer and hard alloy layer, glomerocryst layer to be sintered on hard alloy layer, and glomerocryst layer is made up of wurtzite BN, cubic boron nitride and diamond.The invention also discloses the preparation method of the superhard material, and wurtzite BN is changed into cubic boron nitride under high pressure, hot conditions, ultimately forms sintered body.The hardness of gained superhard material is higher than diamond, and various cutting elements, wire drawing tool and milling tool can be made.
Description
Technical field
The invention belongs to superhard material field, and being related to one kind has cubic boron nitride, wurtzite BN and diamond
Superhard material and preparation method thereof.
Background technology
Boron nitride is the crystal being made up of nitrogen-atoms and boron atom, and chemical composition is 43.6% boron and 56.4% nitrogen,
With four kinds of different variants：Hexagonal boron nitride（hBN）, water chestnut side's boron nitride（rBN）, cubic boron nitride（cBN）And wurtzite-type
Boron nitride（wBN）.Wurtzite BN crystal grain is tiny, it is impossible to as cutter body.
With the development of modern technologies, superhard material is widely used, such as cutting tools, grinding tool, brill
Enter instrument and cutting element.Superhard material includes two kinds：Diamond and cubic boron nitride（cBN）.Diamond due to 600 DEG C with
On start to be carbonized, particularly in having material existing for ferro element, with the rise of temperature, its mechanical strength declines rapidly, because
This limits application of the diamond when processing iron series metal product.Cubic boron nitride just overcomes this defect, cube
For boron nitride under the conditions of oxidizing atmosphere, 900 DEG C still ensure that its mechanical strength, therefore in High-Speed Automatic processing machinery field, obtain
To being widely applied.
Traditionally, agglutinant or adhesive are contained in the cubic boron nitride sintered body as cutting element or wear resistant tools,
Such as TiN, TiC and Co.The sintered body be by under 4 ~ 5GPa pressure by cubic boron nitride powder and agglutinant or adhesive
Obtained from sintering.Contain about 10 ~ 40% adhesive in the sintered body, adhesive greatly influences the intensity, heat-resisting of sintered body
Property and heat diffusivity, in high-speed cutting, especially in cutting ferrous metals material, easily occur defect and splitting on the cutting edge
Line, this shortens the life-span of instrument.
In order to extend life tools, the existing cBN without using adhesive sinters manufacturing method.In the method, by six
Square boron nitride and such as Dan Pengization Magnesium etc catalyst are used as raw material, and they are sintered and reacted.According to this method, due to
Without using adhesive, combined strongly between cBN particles, thermal conductivity is up to 6 ~ 7W/cm DEG C.Therefore, cBN sintered bodies are used as radiator
In material or tape-automated bonding instrument.But because partial catalyst is remained in sintered body, and when sintered body is heated
When, due to the thermal dilation difference between cBN and catalyst, hair check is easily produced, so as to as little as 700 DEG C of heat resisting temperature, this is right
It is one very big problem for cutting element.Further, since particle diameter is slightly up to 10 μm or so, although this improves thermal conductivity,
Its intensity is weakened, it can not be born big cutting load.
Although can be in no additive such as metal（Metal can reduce the hardness and service life of final products）Situation
Lower sintered diamond, but sintering needs the pressure more than 10GPa in the case of no additive, and this is pressed for industrial production
Power is too high, can reduce service life of equipment.WBN is the industrial most hard material of energy at present, more than 6GPa and 1400 DEG C
High pressure high temperature under the conditions of can be gradually converted into cBN, fringe time long enough, wBN can be completely reformed into cBN.
The content of the invention
To solve the above problems, there is high rigidity it is an object of the invention to provide one kind, include wurtzite BN
And the superhard material of cubic boron nitride (cBN) and diamond mixed sintering body (wBN).
It is a further object of the present invention to provide the preparation method of the superhard material.
To reach above-mentioned purpose, the present invention uses following technical scheme：
A kind of superhard material with cubic boron nitride, wurtzite BN and diamond, including glomerocryst layer and hard
Alloy-layer, glomerocryst layer are sintered on hard alloy layer, and the main component of hard alloy layer is the content of tungsten carbide and cobalt, wherein cobalt
The 3 ~ 30% of hard alloy gross weight are accounted for, glomerocryst layer also has diamond to form by wurtzite BN and cubic boron nitride.
Further, the cubic boron nitride of the glomerocryst layer is transformed by wurtzite BN.
Further, the cubic boron nitride of the glomerocryst layer by wurtzite BN pressure >=6GPa, temperature >=
Sintering is transformed under conditions of 1400 DEG C.
A kind of method for preparing the above-mentioned superhard material with cubic boron nitride, wurtzite BN and diamond, bag
Include following steps：
（1）Get out wurtzite BN micro mist（Jing Li Chi Cun≤10 μm）And diadust（The μ of Jing Li Chi Cun≤20
m）；
（2）It is encased in and does not melt, in not broken high pressure-temperature container after both are mixed；
（3）Disc-shaped or powdery tungsten carbide are placed on step（2）In container, this disc-shaped or powdery tungsten carbide are pressed in mixing
It is that subsequent tool making is prepared to turn into hard alloy layer above micro mist afterwards, after sintering；
（4）Above-mentioned high temperature and high pressure containers are placed in high-tension apparatus, boost to more than 6GPa, are warming up to more than 1400 DEG C；
（5）Keep step（4）10 ~ 30min of pressure and temperature；
（6）Pressure is reduced, stops heating, device temperature is reached 0 ~ 25 DEG C, pressure reaches standard atmospheric pressure；
（7）Take out container from high-tension apparatus, remove the container of sintered body surface parcel, obtain with cubic boron nitride,
The superhard material of wurtzite BN and diamond.
The beneficial effects of the invention are as follows：
Wurtzite BN is under the conditions of the superhigh-temperature and-pressure more than 6GPa and 1400 DEG C, atom movement and again group
Close, cubic boron nitride can be changed into, conversion ratio depends on the time of HTHP, when time long enough, wurtzite-type nitridation
Boron can be completely converted into cubic boron nitride.The present invention utilizes the principle, and a cube nitridation is converted into all wurtzite BNs
Stop reacting before boron, can obtain the mixed sintering body of wurtzite BN and cubic boron nitride composition, the hardness of the material
Higher than natural diamond, also above the diamond of sintering, what is sintered into has cubic boron nitride, wurtzite BN and Buddha's warrior attendant
The superhard material of stone, performance are better than diamond.It is this that there is high rigidity and rigid boron nitride material various cuttings can be made
Instrument, wire drawing tool and milling tool, modern mechanical industry is met to the higher and higher hardness requirement of cutter.
Embodiment
With reference to specific embodiment, the present invention is described further：
Embodiment 1
1.2g crystallite dimensions is micro- in 2 microns of diamond in 1 micron of wurtzite BN and 0.8g crystallite dimensions
Grain is slightly soaked by toluene, by being stirred, is filled into Φ 12*10mm, in thick 0.5mm zirconium cup.With 20kg/c ㎡ pressure
Pressing, wurtzite BN micro mist thickness is 7mm, is put into Φ 11*3mm tungsten-cobalt alloy disk afterwards.Container is put into height
Press in equipment, synthesized 15 minutes under the conditions of 6.5GPa, 1650 DEG C.After end of synthesis, pressure is reduced to atmospheric pressure, by stopping adding
Hot temperature gradually reduces.Container takes out from high-tension apparatus, the ground removal of zirconium of surface covering.Wurtzite BN and gold
Hard rock is combined closely with tungsten-cobalt alloy part.It is shaped as Φ 11*9mm cylinder.The surface and side of cylinder are all to pass through Buddha's warrior attendant
Stone sand buff polishing.
The surface at wurtzite BN and diamond end passes through X-ray diffraction inspection.It was found that wurtzite BN, vertical
Square boron nitride and diamond peak is present, and the height at wurtzite BN and cubic boron nitride peak is equal.This means fine zinc
Ore deposit type boron nitride is converted into cubic boron nitride, and wurtzite BN is equal with the content of cubic boron nitride, and this change makes
Wurtzite BN, cubic boron nitride and diamond crystalses are combined together to form sintered body.With 500 times of microscope of amplification
Wurtzite BN-cubic boron nitride-diamond surface is observed, stomata is not observed.
The mixed sintering body surface surface hardness of wurtzite BN, cubic boron nitride and diamond：When being loaded as 9.8N,
Micro-vickers hardness is 72GPa.
Embodiment 2
1.2g crystallite dimensions is micro- in 2 microns of diamond in 1 micron of wurtzite BN and 0.8g crystallite dimensions
Grain is slightly soaked by toluene, by being stirred, is filled into Φ 12*10mm, in thick 0.5mm zirconium cup.With 20kg/c ㎡ pressure
Pressing, wurtzite BN micro mist thickness is 7mm, is put into Φ 11*3mm tungsten-cobalt alloy disk afterwards.Container is put into height
Press in equipment, synthesized 11 minutes under the conditions of 6.5GPa, 1650 DEG C.After end of synthesis, pressure is reduced to atmospheric pressure, by stopping adding
Hot temperature gradually reduces.Container takes out from high-tension apparatus, the ground removal of zirconium of surface covering.Wurtzite BN and gold
Hard rock is combined closely with tungsten-cobalt alloy part.It is shaped as Φ 11*9mm cylinder.The surface and side of cylinder are all to pass through Buddha's warrior attendant
Stone sand buff polishing.
The surface at wurtzite BN and diamond end passes through X-ray diffraction inspection.It was found that wurtzite BN, vertical
Square boron nitride and diamond peak is present, and the height at cubic boron nitride peak is the 25% of wurtzite BN.This means fine zinc
Ore deposit type boron nitride is converted into cubic boron nitride, and the content of cubic boron nitride is the 25% of wurtzite BN, and this change makes
Wurtzite BN, cubic boron nitride and diamond crystalses are combined together to form sintered body.With 500 times of microscope of amplification
Wurtzite BN-cubic boron nitride-diamond surface is observed, stomata is not observed.
The mixed sintering body surface surface hardness of wurtzite BN, cubic boron nitride and diamond：When being loaded as 9.8N,
Micro-vickers hardness is 70GPa.
Embodiment 3
1.5g crystallite dimensions is micro- in 2 microns of diamond in 1 micron of wurtzite BN and 0.5g crystallite dimensions
Grain is slightly soaked by toluene, by being stirred, is filled into Φ 12*10mm, in thick 0.5mm zirconium cup.With 20kg/c ㎡ pressure
Pressing, wurtzite BN micro mist thickness is 7mm, is put into Φ 11*3mm tungsten-cobalt alloy disk afterwards.Container is put into height
Press in equipment, synthesized 15 minutes under the conditions of 6.9GPa, 1780 DEG C.After end of synthesis, pressure is reduced to atmospheric pressure, by stopping adding
Hot temperature gradually reduces.Container takes out from high-tension apparatus, the ground removal of zirconium of surface covering.Wurtzite BN and gold
Hard rock is combined closely with tungsten-cobalt alloy part.It is shaped as Φ 11*9mm cylinder.The surface and side of cylinder are all to pass through Buddha's warrior attendant
Stone sand buff polishing.
The surface at wurtzite BN and diamond end passes through X-ray diffraction inspection.It was found that wurtzite BN, vertical
Square boron nitride and diamond peak is present, and the height at cubic boron nitride peak is the 70% of wurtzite BN.This means fine zinc
Ore deposit type boron nitride is converted into cubic boron nitride, and the content of cubic boron nitride is the 70% of wurtzite BN, and this change makes
Wurtzite BN, cubic boron nitride and diamond crystalses are combined together to form sintered body.With 500 times of microscope of amplification
Wurtzite BN-cubic boron nitride-diamond surface is observed, stomata is not observed.
The mixed sintering body surface surface hardness of wurtzite BN, cubic boron nitride and diamond：When being loaded as 9.8N,
Micro-vickers hardness is 73GPa.
Embodiment 4
1.2g crystallite dimensions is micro- in 2 microns of diamond in 1 micron of wurtzite BN and 0.8g crystallite dimensions
Grain is slightly soaked by toluene, by being stirred, is filled into Φ 12*10mm, in thick 0.5mm zirconium cup.With 20kg/c ㎡ pressure
Pressing, wurtzite BN micro mist thickness is 7mm, is put into Φ 11*3mm tungsten-cobalt alloy disk afterwards.Container is put into height
Press in equipment, synthesized 20 minutes under the conditions of 6.5GPa, 1650 DEG C.After end of synthesis, pressure is reduced to atmospheric pressure, by stopping adding
Hot temperature gradually reduces.Container takes out from high-tension apparatus, the ground removal of zirconium of surface covering.Wurtzite BN and gold
Hard rock is combined closely with tungsten-cobalt alloy part.It is shaped as Φ 11*9mm cylinder.The surface and side of cylinder are all to pass through Buddha's warrior attendant
Stone sand buff polishing.
The surface at wurtzite BN and diamond end passes through X-ray diffraction inspection.It was found that wurtzite BN, vertical
Square boron nitride and diamond peak is present, and the height at wurtzite BN and cubic boron nitride peak is equal.This means fine zinc
Ore deposit type boron nitride is converted into cubic boron nitride, and wurtzite BN is equal with the content of cubic boron nitride, and this change makes
Wurtzite BN, cubic boron nitride and diamond crystalses are combined together to form sintered body.With 500 times of microscope of amplification
Wurtzite BN-cubic boron nitride-diamond surface is observed, stomata is not observed.
The mixed sintering body surface surface hardness of wurtzite BN, cubic boron nitride and diamond：When being loaded as 9.8N,
Micro-vickers hardness is 46GPa.
Embodiment 5
1.2g crystallite dimensions is micro- in 2 microns of diamond in 1 micron of wurtzite BN and 0.8g crystallite dimensions
Grain is slightly soaked by toluene, by being stirred, is filled into Φ 12*10mm, in thick 0.5mm zirconium cup.With 20kg/c ㎡ pressure
Pressing, wurtzite BN micro mist thickness is 7mm, is put into Φ 11*3mm tungsten-cobalt alloy disk afterwards.Container is put into height
Press in equipment, synthesized 18 minutes under the conditions of 6.9GPa, 1780 DEG C.After end of synthesis, pressure is reduced to atmospheric pressure, by stopping adding
Hot temperature gradually reduces.Container takes out from high-tension apparatus, the ground removal of zirconium of surface covering.Wurtzite BN and gold
Hard rock is combined closely with tungsten-cobalt alloy part.It is shaped as Φ 11*9mm cylinder.The surface and side of cylinder are all to pass through Buddha's warrior attendant
Stone sand buff polishing.
The surface at wurtzite BN and diamond end passes through X-ray diffraction inspection.It was found that wurtzite BN, vertical
Square boron nitride and diamond peak is present, and the height at wurtzite BN and cubic boron nitride peak is equal.This means fine zinc
Ore deposit type boron nitride is converted into cubic boron nitride, and wurtzite BN is equal with the content of cubic boron nitride, and this change makes
Wurtzite BN, cubic boron nitride and diamond crystalses are combined together to form sintered body.With 500 times of microscope of amplification
Wurtzite BN-cubic boron nitride-diamond surface is observed, stomata is not observed.
The mixed sintering body surface surface hardness of wurtzite BN, cubic boron nitride and diamond：When being loaded as 9.8N,
Micro-vickers hardness is 44GPa.
Embodiment 6
1.2g crystallite dimensions is micro- in 2 microns of diamond in 1 micron of wurtzite BN and 0.8g crystallite dimensions
Grain is slightly soaked by toluene, by being stirred, is filled into Φ 12*10mm, in thick 0.5mm zirconium cup.With 20kg/c ㎡ pressure
Pressing, wurtzite BN micro mist thickness is 7mm, is put into Φ 11*3mm tungsten-cobalt alloy disk afterwards.Container is put into height
Press in equipment, synthesized 25 minutes under the conditions of 6.2GPa, 1580 DEG C.After end of synthesis, pressure is reduced to atmospheric pressure, by stopping adding
Hot temperature gradually reduces.Container takes out from high-tension apparatus, the ground removal of zirconium of surface covering.Wurtzite BN and gold
Hard rock is combined closely with tungsten-cobalt alloy part.It is shaped as Φ 11*9mm cylinder.The surface and side of cylinder are all to pass through Buddha's warrior attendant
Stone sand buff polishing.
The surface at wurtzite BN and diamond end passes through X-ray diffraction inspection.It was found that wurtzite BN, vertical
Square boron nitride and diamond peak is present, and the height at wurtzite BN and cubic boron nitride peak is equal.This means fine zinc
Ore deposit type boron nitride is converted into cubic boron nitride, and wurtzite BN is equal with the content of cubic boron nitride, and this change makes
Wurtzite BN, cubic boron nitride and diamond crystalses are combined together to form sintered body.With 500 times of microscope of amplification
Wurtzite BN-cubic boron nitride-diamond surface is observed, stomata is not observed.
The mixed sintering body surface surface hardness of wurtzite BN, cubic boron nitride and diamond：When being loaded as 9.8N,
Micro-vickers hardness is 46GPa.
Claims (7)
1. a kind of superhard material with cubic boron nitride, wurtzite BN and diamond, it is characterised in that including glomerocryst
Layer and hard alloy layer, glomerocryst layer are sintered on hard alloy layer by HTHP, and the main component of hard alloy layer is carbon
Change tungsten and cobalt, the content of wherein cobalt account for the 3~30% of hard alloy gross weight；The glomerocryst layer includes cubic boron nitride, fibre
Zinc ore type boron nitride and diamond；The cubic boron nitride is by wurtzite BN in pressure >=6GPa, temperature >=1400 DEG C
Under conditions of sinter and be transformed.
A kind of 2. superhard material with cubic boron nitride, wurtzite BN and diamond prepared described in claim 1
Method, it is characterised in that comprise the following steps：
(1) wurtzite BN and the original micro mist of diamond are proportionally weighed；
(2) the original micro mist in blend step (1), addition toluene solution is as lubricant, ball milling 30 minutes so that original micro mist
Mixing evenly, obtains admixed finepowder；
(3) heat drying, toluene is removed；
(4) admixed finepowder is attached in high temperature high voltage resistant container；
(5) disc-shaped or powdery tungsten carbide are placed in step (4) container again, this disc-shaped or powdered tungsten cobalt alloy are pressed in mixed
Close above micro mist, turn into hard alloy layer after sintering；
(6) the high-temperature-resistant high-pressure-resistant container for filling admixed finepowder in step (5) is put into high-temperature high-pressure apparatus, boosted to
More than 6GPa, it is warming up to more than 1400 DEG C；
(7) 10~30min of pressure and temperature of step (6) is kept；
(8) reduce pressure, stop heating, device temperature is reached 0~25 DEG C, pressure reaches standard atmospheric pressure；
(9) container is taken out from high-tension apparatus, the container of sintered body surface parcel is removed, obtains with cubic boron nitride, fine zinc
The superhard material of ore deposit type boron nitride and diamond.
3. the system of the superhard material according to claim 2 with cubic boron nitride, wurtzite BN and diamond
Preparation Method, it is characterised in that diamond in original micro mist before high temperature high pressure process：The mass ratio of wurtzite BN is 1:5
~5:1.
4. the system of the superhard material according to claim 2 with cubic boron nitride, wurtzite BN and diamond
Preparation Method, it is characterised in that crystallite dimension≤10 μm of the wurtzite BN micro mist.
5. the system of the superhard material according to claim 2 with cubic boron nitride, wurtzite BN and diamond
Preparation Method, it is characterised in that crystallite dimension≤20 μm of the diadust.
6. the system of the superhard material according to claim 2 with cubic boron nitride, wurtzite BN and diamond
Preparation Method, it is characterised in that sintered body is made up of cubic boron nitride, wurtzite BN and diamond.
7. the system of the superhard material according to claim 2 with cubic boron nitride, wurtzite BN and diamond
Preparation Method, it is characterised in that the cubic boron nitride in the sintered body：Wurtzite BN passes through X-ray diffraction peak heights
Than for 10:1~1:10.
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| WO2018092195A1 (en) * | 2016-11-15 | 2018-05-24 | 住友電工ハードメタル株式会社 | Cutting tool |
| US11866372B2 (en) | 2020-05-28 | 2024-01-09 | Saudi Arabian Oil Company | Bn) drilling tools made of wurtzite boron nitride (W-BN) |
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| JPH101304A (en) * | 1996-06-17 | 1998-01-06 | Heriosu Hikari Kagaku Kenkyusho:Kk | Photoexcitation production of four coordinate bond bn material |
| US20030162648A1 (en) * | 2002-02-26 | 2003-08-28 | Stewart Middlemiss | Elongate ultra hard particle reinforced ultra hard materials and ceramics, tools and parts incorporating the same, and method of making the same |
| US6852414B1 (en) * | 2002-06-25 | 2005-02-08 | Diamond Innovations, Inc. | Self sharpening polycrystalline diamond compact with high impact resistance |
| CN100374685C (en) * | 2002-07-10 | 2008-03-12 | 戴蒙得创新股份有限公司 | Cutting tools with two-slope profile |
| CN101482016A (en) * | 2009-01-19 | 2009-07-15 | 湖南飞瑞复合材料有限责任公司 | High-performance diamond composite cutter bit |
| EP2942341B1 (en) * | 2011-08-30 | 2020-11-18 | Sumitomo Electric Industries, Ltd. | Cubic boron nitride complex polycrystalline substance, method for manufacturing same, cutting tool, wire-drawing die, and grinding tool |
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Address after: 519160 Longshan No. two East, Doumen Town, Zhuhai City, Guangdong Province, No. 1 Patentee after: Guangdong Ju Xin new material Polytron Technologies Inc Address before: 519160 Longshan No. two East, Doumen Town, Zhuhai City, Guangdong Province, No. 1 Patentee before: ZHUHAI JUXIN TECHNOLOGY DEVELOPMENT CO., LTD. |