CN105127429A - Boron nitride super-hard material and preparation method thereof - Google Patents
Boron nitride super-hard material and preparation method thereof Download PDFInfo
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- CN105127429A CN105127429A CN201510520848.1A CN201510520848A CN105127429A CN 105127429 A CN105127429 A CN 105127429A CN 201510520848 A CN201510520848 A CN 201510520848A CN 105127429 A CN105127429 A CN 105127429A
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- boron nitride
- wurtzite
- superhard material
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- 229910052582 BN Inorganic materials 0.000 title claims abstract description 65
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 239000000463 material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 229910052984 zinc sulfide Inorganic materials 0.000 claims abstract description 25
- 239000000956 alloy Substances 0.000 claims abstract description 11
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 11
- 239000003595 mist Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 abstract description 10
- 238000000227 grinding Methods 0.000 abstract description 3
- 238000005491 wire drawing Methods 0.000 abstract description 2
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 230000009466 transformation Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 229910003460 diamond Inorganic materials 0.000 description 5
- 239000010432 diamond Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 235000003283 Pachira macrocarpa Nutrition 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 241001083492 Trapa Species 0.000 description 1
- 235000014364 Trapa natans Nutrition 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000010339 dilation Effects 0.000 description 1
- -1 ferrous metals Chemical class 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 235000009165 saligot Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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- Ceramic Products (AREA)
- Cutting Tools, Boring Holders, And Turrets (AREA)
Abstract
The invention discloses a boron nitride super-hard material. The boron nitride super-hard material comprises a polycrystalline layer and a hard alloy layer. The polycrystalline layer is sintered on the hard alloy layer and composed of wurtzite type boron nitride and cubic boron nitride. The invention further discloses a preparation method of the boron nitride super-hard material. The wurtzite type boron nitride is partially converted into the cubic boron nitride under the high-temperature and high-pressure conditions, and finally a sintered body is formed. The obtained boron nitride material is high in rigidity and can be manufactured into various cutting tools, wire drawing tools and grinding tools.
Description
Technical field
The invention belongs to superhard material field, relate to a kind of boron nitride 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.
Summary of the invention
For solving the problem, the object of this invention is to provide a kind of boron nitride superhard material that there is high rigidity, comprise wBN and cBN mixed sintering body.
Another object of the present invention is to provide the preparation method of this boron nitride superhard material.
For achieving the above object, the present invention by the following technical solutions:
A kind of boron nitride superhard material, comprise glomerocryst layer and hard alloy layer, glomerocryst layer is sintered in hard alloy layer, and glomerocryst layer is made up of wurtzite BN and cubic boron nitride.
The ratio of glomerocryst layer and hard alloy layer does not have particular requirement, can need to decide according to client.
Further, the volume ratio of described wurtzite BN and cubic boron nitride is 10:1 ~ 1:10.
Further, described cubic boron nitride is transformed by wurtzite BN.
Further, described cubic boron nitride is sintered by wurtzite BN and is transformed under the condition of pressure >=6GPa, temperature >=1400 DEG C.
Further, the particle diameter of described cubic boron nitride is 1 ~ 100 μm.
Further, described hard alloy layer is diamondite.
Prepare a method for boron nitride superhard material according to claim 1, comprise the following steps:
(1) wurtzite BN micro mist is loaded in container;
(2) carbide alloy is placed on above wurtzite BN micro mist;
(3) container is placed in high-tension apparatus, boosts to more than 6GPa, be warming up to more than 1400 DEG C;
(4) the pressure and temperature 10 ~ 30min of step (3) is kept;
(5) reduce pressure, stop heating, treat that normal pressure and temperature is down to by container;
(6) take out container, remove the container of sintered body surface parcel, obtain boron nitride superhard material.
Further, crystallite dimension≤20 μm of described wurtzite BN micro mist.
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, can obtain wurtzite BN and cubic boron nitride composition mixed sintering body, the hardness of this material higher than cubic boron nitride, also higher than general 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
Boron nitride superhard material is produced according to following steps
(1) the wBN toluene of 2g crystallite dimension at 0 ~ 20 μm slightly being soaked, by being uniformly mixed, being filled in the high temperature high voltage resistant container of Φ 12*10mm, thick 0.5mm, with 20kg/cm
2pressure presses, and wBN micro mist thickness is 7mm;
(2) the diamondite disk of Φ 11*3mm is put in a reservoir above wurtzite BN micro mist;
(3) container filling wBN micro mist is placed in high-tension apparatus, boosts to 6.5GPa, be warming up to 1650 DEG C;
(4) above-mentioned pressure and temperature 15min is kept;
(5) after end of synthesis, reduce pressure, stop heating, treat that normal pressure and temperature is down to by container;
(6) container is taken out from high-tension apparatus, removed the container of sintered body surface coverage by grinding, obtain boron nitride superhard material, boron nitride is combined with diamondite moieties into close, shape is the cylinder of Φ 11*9mm, and the surface of cylinder and side are by boart boart buff polishing.
Check mixed sintering body by X-ray diffraction, find that wBN, cBN peak exists, the wBN that X-ray diffraction shows 50% is converted into cBN, and this means that wBN is converted into cBN, wBN and cBN crystal grain is combined together to form sintered body.
Detect the mixed sintering surface hardness of wBN and cBN: when being loaded as 19.8N, micro-vickers hardness is 78GPa.
embodiment 2
Produce boron nitride superhard material according to the step identical with embodiment 1, but the transformation time of step (4) is reduced to 11min.The sintered body obtained combines firmly.After surface finish, the wBN that X-ray diffraction shows 25% is converted into cBN.Detect the mixed sintering surface hardness of wBN and cBN: when being loaded as 19.8N, micro-vickers hardness is 76GPa.
embodiment 3
Produce boron nitride superhard material according to the step identical with embodiment 1, but the pressure of step (3) is 6.9GPa, temperature is 1780 DEG C.The sintered body obtained combines firmly.After surface finish, the wBN that X-ray diffraction shows 70% is converted into cBN.Detect the mixed sintering surface hardness of wBN and cBN: when being loaded as 19.8N, micro-vickers hardness is 70GPa.
comparative example 1
Produce boron nitride material according to the step identical with embodiment 1, but the transformation time of step (4) is increased to 20min.The sintered body obtained combines firmly.After surface finish, X-ray diffraction display wBN is all converted into cBN.Detect sintered body case hardness: when being loaded as 19.8N, micro-vickers hardness is 46GPa.
comparative example 2
Produce boron nitride material according to the step identical with embodiment 1, but the pressure of step (3) is 6.9GPa, temperature is 1780 DEG C, and the transformation time of step (4) is increased to 18min.The sintered body obtained combines firmly.After surface finish, X-ray diffraction display wBN is all converted into cBN.Detect sintered body case hardness: when being loaded as 19.8N, micro-vickers hardness is 44GPa.
comparative example 3
Produce boron nitride material according to the step identical with embodiment 1, but the pressure of step (3) is 6.2GPa, temperature is 1580 DEG C, and the transformation time of step (4) is increased to 25min.The sintered body obtained combines firmly.After surface finish, X-ray diffraction display wBN is all converted into cBN.Detect sintered body case hardness: when being loaded as 19.8N, micro-vickers hardness is 46GPa.
From embodiment 1 ~ 3 and comparative example 1 ~ 3, the temperature of reaction, pressure and time can affect the conversion ratio of wBN, the temperature that the present invention is reacted by control, pressure and time, obtain the sintered body be made up of wBN and cBN, the hardness (>=70GPa) of this boron nitride superhard material higher than the cubic boron nitride material (about 45GPa) of comparative example 1 ~ 3, also higher than general diamond (60 ~ 70GPa).
embodiment 4
Produce boron nitride superhard material according to the step identical with embodiment 1, but the pressure of step (3) is 6.2GPa, temperature is 1450 DEG C, and the transformation time of step (4) is 30min.The sintered body obtained combines firmly, and the volume ratio of wurtzite BN and cubic boron nitride is 1:10.
embodiment 5
Produce boron nitride superhard material according to the step identical with embodiment 1, but the pressure of step (3) is 6.3GPa, temperature is 1410 DEG C, and the transformation time of step (4) is 10min.The sintered body obtained combines firmly, and the volume ratio of wurtzite BN and cubic boron nitride is 10:1.
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, anyly belongs to those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (8)
1. a boron nitride superhard material, is characterized in that, comprises glomerocryst layer and hard alloy layer, and glomerocryst layer is sintered in hard alloy layer, and glomerocryst layer is made up of wurtzite BN and cubic boron nitride.
2. boron nitride superhard material according to claim 1, is characterized in that, the volume ratio of described wurtzite BN and cubic boron nitride is 10:1 ~ 1:10.
3. boron nitride superhard material according to claim 1, is characterized in that, described cubic boron nitride is transformed by wurtzite BN.
4. boron nitride superhard material according to claim 1, is characterized in that, described cubic boron nitride is sintered by wurtzite BN and is transformed under the condition of pressure >=6GPa, temperature >=1400 DEG C.
5. boron nitride superhard material according to claim 1, is characterized in that, the particle diameter of described cubic boron nitride is 1 ~ 100 μm.
6. boron nitride superhard material according to claim 1, is characterized in that, described hard alloy layer is diamondite.
7. prepare a method for boron nitride superhard material according to claim 1, it is characterized in that, comprise the following steps:
(1) wurtzite BN micro mist is loaded in container;
(2) carbide alloy is placed on above wurtzite BN micro mist;
(3) container is placed in high-tension apparatus, boosts to more than 6GPa, be warming up to more than 1400 DEG C;
(4) the pressure and temperature 10 ~ 30min of step (3) is kept;
(5) reduce pressure, stop heating, treat that normal pressure and temperature is down to by container;
(6) take out container, remove the container of sintered body surface parcel, obtain boron nitride superhard material.
8. the preparation method of boron nitride superhard material according to claim 7, is characterized in that, crystallite dimension≤20 μm of described wurtzite BN micro mist.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510520848.1A CN105127429A (en) | 2015-08-24 | 2015-08-24 | Boron nitride super-hard material and preparation method thereof |
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| CN201510520848.1A CN105127429A (en) | 2015-08-24 | 2015-08-24 | Boron nitride super-hard material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108002353A (en) * | 2017-10-23 | 2018-05-08 | 富耐克超硬材料股份有限公司 | Water white transparency polycrystalline cubic boron nitride, preparation method and applications, the cutter for including the water white transparency polycrystalline cubic boron nitride |
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| US4188194A (en) * | 1976-10-29 | 1980-02-12 | General Electric Company | Direct conversion process for making cubic boron nitride from pyrolytic boron nitride |
| CN86108847A (en) * | 1986-01-14 | 1987-08-05 | 通用电气公司 | The polycrystalline compacts of band supporting |
| CN103157797A (en) * | 2013-03-19 | 2013-06-19 | 河南富耐克超硬材料股份有限公司 | Tool bit blank and synthetic process thereof and synthetic mold thereof and tool bit production method |
| CN103537699A (en) * | 2012-07-11 | 2014-01-29 | 吉林师范大学 | Preparation method of polycrystalline cubic boron nitride composite sheet |
-
2015
- 2015-08-24 CN CN201510520848.1A patent/CN105127429A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4188194A (en) * | 1976-10-29 | 1980-02-12 | General Electric Company | Direct conversion process for making cubic boron nitride from pyrolytic boron nitride |
| CN86108847A (en) * | 1986-01-14 | 1987-08-05 | 通用电气公司 | The polycrystalline compacts of band supporting |
| CN103537699A (en) * | 2012-07-11 | 2014-01-29 | 吉林师范大学 | Preparation method of polycrystalline cubic boron nitride composite sheet |
| CN103157797A (en) * | 2013-03-19 | 2013-06-19 | 河南富耐克超硬材料股份有限公司 | Tool bit blank and synthetic process thereof and synthetic mold thereof and tool bit production method |
Non-Patent Citations (2)
| Title |
|---|
| S.K.BHAUMIK ETAL: "Machining Ti-6Al-4V alloy with a wBN-cBN composite tool", 《MATERIALS & DESIGN》 * |
| 刘波: "纤锌矿型氮化硼与硬质合金在高温高压下的烧结", 《吉林大学硕士论文》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108002353A (en) * | 2017-10-23 | 2018-05-08 | 富耐克超硬材料股份有限公司 | Water white transparency polycrystalline cubic boron nitride, preparation method and applications, the cutter for including the water white transparency polycrystalline cubic boron nitride |
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