CN110342943A - The method and its application of binder free plycrystalline diamond boron nitride bulk are synthesized under industrial stresses - Google Patents

The method and its application of binder free plycrystalline diamond boron nitride bulk are synthesized under industrial stresses Download PDF

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CN110342943A
CN110342943A CN201910651003.4A CN201910651003A CN110342943A CN 110342943 A CN110342943 A CN 110342943A CN 201910651003 A CN201910651003 A CN 201910651003A CN 110342943 A CN110342943 A CN 110342943A
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boron nitride
plycrystalline diamond
nitride bulk
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diamond boron
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赵智胜
罗坤
韩俏怡
靳田野
孙磊
刘兵
何巨龙
于栋利
胡文涛
田永君
陈俊云
徐波
柳忠元
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Yanshan University
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Abstract

The invention discloses the method and its application that binder free plycrystalline diamond boron nitride bulk is synthesized under industrial stresses, belong to plycrystalline diamond synthesis of BN field, method mainly includes by any one in cBN, hBN, oBN, pBN or arbitrarily several powder mixing are purified, are prefabricated into column green body after heating in vacuum pretreatment, then processing obtains plycrystalline diamond boron nitride bulk under high temperature and industrial stresses;It is prepared into cutting tool using processing is essentially consisted in, realizes the machining to iron-based material and the contour hard difficult-to-machine material of hard alloy (WC).Synthesis pressure is greatly reduced in the present invention, is suitble to industrialized production.

Description

The method and its application of binder free plycrystalline diamond boron nitride bulk are synthesized under industrial stresses
Technical field
The nitridation of binder free plycrystalline diamond is synthesized the present invention relates to plycrystalline diamond synthesis of BN field, under especially a kind of industrial stresses The methods and applications of boron.
Background technique
Currently, cubic boron nitride (cBN) and diamond are two most widely used class superhard materials.Diamond has superelevation The excellent performances such as hardness (60-120GPa), high-melting-point and high heat conductance, but its thermal stability and chemical inertness are poor, It will be graphitized when being heated to 700 DEG C or more in air.And cBN has high thermal stability and chemical inertness, can be used to Iron series and carbide forming material are cut, but the hardness of cBN is lower than diamond, Vickers hardness theoretical value is only 66GPa, commercial The cBN monocrystalline hardness of synthesis is lower, and only 33-43GPa, in addition the fracture toughness of cBN monocrystalline is very low, only 2.8MPam1/2。 CBN monocrystalline because its synthesis is size-constrained, and there are dissociation face and fracture toughness it is low, seriously limit its answering in the industry With.Develop isotropism, high hard, high-ductility polycrystalline cubic boron nitride (PcBN) bulk becomes science and the main research of industry Target.
Currently, PcBN used in industrial contains binder, wherein the binder mainly used have metal mold (Co, Al etc.), ceramic mould (Si etc.) and ceramic on metal (TiN etc.), the presence of these binders can be effectively reduced synthesis pressure and Temperature, so as to realize production under the conditions of the industrially attainable pressure (≤6GPa) of institute.But metal adhesive is deposited In the thermal stability that can reduce PcBN;And the addition of vitrified bonding can not only be such that the hardness of PcBN reduces, the use longevity of cutter Life shortens, and its thermal-shock resistance can also be deteriorated, and tipping phenomenon is easy to appear in high-speed machining process, it is difficult to competent high speed The service performance requirement of hard state dry cutting.Due to the presence of binder, PcBN hardness, fracture toughness and heat resistance are all undesirable, As hardness is generally 30GPa or so, fracture toughness 3-5MPam1/2, oxidation resistance temperature only has 1000 DEG C, constrains it and answer With.In conclusion addition binder will reduce the hardness and fracture toughness of PcBN bulk, and lead to its wearability and thermostabilization Property reduce, therefore prepare high-performance, binder free PcBN bulk become recent domestic research hot spot.
The preparation method of binder free PcBN bulk mainly utilizes hexagonal boron nitride (hBN), onion structure boron nitride (oBN), cubic boron nitride (cBN), pyrolytic boron nitride (pBN) and their mixed-powder are as raw material, at high temperature under high pressure It is sintered directly into PcBN bulk.Using the every mechanical property for the PcBN that the direct translation method of this binder free can make It is greatly improved.Such as: in 2000, H.Sumiya.S. et al. (document: Mechanical properties of high purity polycrystalline cBN synthesized by direct conversion sintering Method.Journal of Materials Science.35 (2000) 1181-1186) use high-purity hBN for raw material, it is pressing Power 7.7GPa, sintering has synthesized the plycrystalline diamond PcBN bulk of binder free within the scope of 2200-2400 DEG C of temperature, has high Vickers hardness (50-55GPa) and high cross-breaking strength (1.6GPa).In 2007, Natalia Dubrovinskaia et al. (document: Superhard nano-composite of dense polymorphs of boron nitride:Noncarbon material has reached diamond hardness.Applied Physics Letters.2007,90:101912) Using pBN as raw material, nano polycrystal boron nitride composite has been synthesized under conditions of pressure 18GPa, 1600 DEG C of temperature (ABNNCs), crystallite dimension 14nm, hardness reach 85GPa, fracture toughness 15MPam1/2, thermal stability reaches in air 1327℃.In 2009, Kazuhiro Fujisaki et al. (document: Development of ultra-fine-grain binderless cBN tool for precision cutting of ferrous materials.Journal of Materials Processing Technology.2009,209:5646-5652) it is less than the hBN conduct of 100nm using partial size Raw material, is sintered synthesizing nano polycrystal PcBN under conditions of pressure 10GPa, 1800 DEG C of temperature, and the sample that cuts stainless steel obtains Average surface height deviation (Rz) up to 50-100nm, be suitable for Ultra-precision Turning, but raw material is too thin, it is difficult to prepare and Higher cost.In 2013, our seminars (document: Ultrahard nanotwinned cubic boron nitride, Nature, vol.493, no.7432, pp.385-8, Jan.2013) use oBN to be sintered synthesis by martensitic traoformation for raw material The optimal nano twin crystal cBN bulk (nt-cBN) of performance, hardness are up to 108GPa, fracture toughness 12.7MPam at present1 /2, thermal stability reaches 1294 DEG C in air.In 2015, Guoduan Liu et al. people (document: Submicron cubic Boron nitride as hard as diamond.Applied Physics Letters.2015,106:121901) with Asia For micron (0.2-0.5 μm) cBN powder as raw material, the PcBN bulk hardness synthesized at pressure 8GPa, 2000 DEG C of temperature can Up to 75GPa, fracture toughness 13.2MPam1/2, aerial oxidation resistance temperature is 1252 DEG C.In 2017, Teng Liu Et al. (document: Preparation of superhard cubic boron nitride sintered from commercially available submicron powders.Journal of Applied Physics.2017,121: 125902) using sub-micron (0.4-1.0 μm) cBN as raw material, synthesize pure phase PcBN in pressure 8-14GPa, 1750 DEG C of temperature Bulk, wherein the PcBN bulk synthesized under conditions of pressure 11GPa, 1750 DEG C of temperature has best performance, Vickers is hard Degree reaches 72GPa, fracture toughness 12.4MPam1/2, thermal stability reaches 1275 DEG C in air.In 2018, Ming Yang et al. (document: Polycrystalline cubic boron nitride prepared with cubic- hexagonal boron nitride under high pressure and high temperature.Chinese Physics B.2018,27:056105) using cBN the and hBN mixed powder of sub-micron (0.4-1.0 μm) as raw material, in pressure 7.7GPa, 1750 DEG C of temperature synthesize PcBN, bulk Vickers hardness reaches 61.5GPa, and thermal stability reaches in air 1290 DEG C, density reaches 3.46g/cm3
In conclusion the PcBN bulk of binder free has the hardness (> 40GPa) of superelevation, fracture toughness reaches as high as 12- 15MPa·m1/2, high thermal stability (about 1200 DEG C) in air, to present wide application prospect.But current document In patent report, synthesize binder free high-performance PcBN bulk pressure will at least 7.7GPa, this synthesis pressure be higher than industry Press pressure achieved (≤6GPa), it is therefore desirable to which two-stage pressurizing just may be implemented, and cause synthesis cost not only high, synthesize sample Product size is also limited, therefore can not carry out universal commercial introduction and application at present.It is synthesized under industrial pressure condition Binder free, high performance plycrystalline diamond boron nitride bulk are always the dream of scientific circles and industrial circle out, but unfortunately, so far also It is not implemented.
Summary of the invention
The technical problem to be solved by the invention is to provide binder free plycrystalline diamond boron nitride block is synthesized under a kind of industrial stresses The method and its application of material, are greatly reduced synthesis pressure, are suitble to industrialized production.
In order to solve the above technical problems, the technical scheme adopted by the invention is that:
The method that binder free plycrystalline diamond boron nitride bulk is synthesized under industrial stresses, will be any in cBN, hBN, oBN, pBN The mixing of one or any of several powder is purified, is prefabricated into column green body after heating in vacuum pretreatment, then in high temperature and industry Processing obtains plycrystalline diamond boron nitride bulk under pressure.
Technical solution of the present invention further improvement lies in that: specifically includes the following steps:
A, any one or any several powder in cBN, hBN, oBN, pBN are mixed purified, heating in vacuum it is pre- Processing removes the oxygen adsorbed in raw material powder, absorption water and combines water;
Powder pretreated in step a is prefabricated into column green body by b;
Column green body is packed into crucible by c, and crucible is put into high temperature and pressure assembling block;
D will carry out high temperature high pressure process in high temperature and pressure assembling block merging press;
Plycrystalline diamond boron nitride bulk is obtained under e, high temperature and industrial stresses after the completion of processing.
Technical solution of the present invention further improvement lies in that: step d selection is handled in cubic hinge press, is pressed Power range is 1-6GPa, and temperature range is 800-2300 DEG C, and soaking time is 10-400 minutes.
Technical solution of the present invention further improvement lies in that: the cylinder of diameter 3.5mm, high 4mm are prefabricated into the step b Green body.
Technical solution of the present invention further improvement lies in that: the purification of raw material, heating in vacuum pretreatment side in the step a Method are as follows: purified, the raw material powder after purification is inserted in the mold of vacuum hotpressing stove, vacuum using the mode of the molten removal of impurities of acid The vacuum degree of hot pressing furnace is in 4*10-2Hereinafter, temperature is 400-1600 DEG C, pressure 30-50MPa.
The application that binder free plycrystalline diamond boron nitride bulk is synthesized under industrial stresses, carries out processing system for plycrystalline diamond boron nitride bulk For at cutting tool.
The application of plycrystalline diamond boron nitride bulk of the present invention further improvement lies in that: cutting tool is used for including iron-based material And the machining of the hard difficult-to-machine material of height of hard alloy.
By adopting the above-described technical solution, the technological progress achieved by the present invention is:
The plycrystalline diamond boron nitride that the present invention produces is different from the currently commercially material of PcBN containing binder generally used, with Compare, the high-performance plycrystalline diamond boron nitride bulk for the binder free that the present invention prepares, have higher hardness, toughness and heat it is steady It is qualitative.The present invention (≤6GPa) under industrial stresses carries out preparation synthesis simultaneously, is different from super-pressure (>=7.7GPa) synthesis nothing The high-performance PcBN bulk of binder, in contrast, the binder free high-performance plycrystalline diamond boron nitride bulk performance in the present invention is excellent It is different, synthesis pressure is low, can direct industrial production, realize industrialization.
PcBN bulk prepared by the present invention has excellent mechanical property, hardness 40-50GPa, and fracture toughness is 8-10MPa·m1/2, compressive strength 6.5GPa, oxidation resistance temperature is greater than 1200 DEG C in air, may be directly applied to iron series with And the machining of the contour hard difficult-to-machine material of hard alloy (WC), realize the contour hard difficult processing of hardened steel, hard alloy (WC) The ultraprecise mirror-finish cutting of material.
Detailed description of the invention
Fig. 1 shows the X-ray diffractogram for the plycrystalline diamond boron nitride bulk that the embodiment of the present invention 1,2,3,4,5,6 obtains;
Fig. 2 shows the Raman figures for the plycrystalline diamond boron nitride bulk that the embodiment of the present invention 2,4 obtains;
Fig. 3 shows the plycrystalline diamond boron nitride bulk hardness and load mould figure that the embodiment of the present invention 4 obtains;
Fig. 4 shows the transmission electron microscope picture for the plycrystalline diamond boron nitride bulk that the embodiment of the present invention 3 obtains;
Fig. 5 shows the scanning electron microscope (SEM) photograph for the plycrystalline diamond boron nitride bulk that the embodiment of the present invention 4 obtains;
Fig. 6 shows the plycrystalline diamond boron nitride bulk electron energy loss spectroscopy (EELS) that the embodiment of the present invention 1,2,3,5 obtains;
Fig. 7, which shows the plycrystalline diamond boron nitride bulk that the embodiment of the present invention 1,2,3,4,5,6 obtains Tool in Cutting is made, to harden The atomic force microscopy diagram of steel;
Fig. 8 shows the plycrystalline diamond boron nitride bulk that the embodiment of the present invention 1,2,3,4,5,6 obtains and Tool in Cutting hard is made The atomic force microscopy diagram of alloy (WC of the binder containing Co).
Specific embodiment
The present invention is described in further details below with reference to embodiment:
The method that binder free plycrystalline diamond boron nitride bulk is synthesized under industrial stresses, specifically includes the following steps:
A, any one or any several powder in cBN, hBN, oBN, pBN are mixed purified, heating in vacuum it is pre- Processing removes the oxygen adsorbed in raw material powder, absorption water and combines water;
The purification of raw material, heating in vacuum preprocess method are as follows: purified using the mode of the molten removal of impurities of acid, after purification Raw material powder is inserted in the mold of vacuum hotpressing stove, and the vacuum degree of vacuum hotpressing stove is in 4*10-2Hereinafter, temperature is 400-1600 DEG C, pressure 30-50MPa.Wherein the raw material of high-purity can be obtained in sour molten clean, if raw material purity itself is very high, can no longer into This step of row;
Powder pretreated in step a is prefabricated into column green body by b, and the size of column green body is according to press model tune It is whole;
Column green body is packed into crucible by c, and crucible is put into high temperature and pressure assembling block;
D will carry out high temperature high pressure process in high temperature and pressure assembling block merging press;
It specifically may be selected to be handled in cubic hinge press, pressure limit 1-6GPa, temperature range 800- 2300 DEG C, soaking time is 10-400 minutes;
Plycrystalline diamond boron nitride bulk is obtained under e, high temperature and industrial stresses after the completion of processing.
Next it is described in detail with synthetic method of several specific embodiments to plycrystalline diamond boron nitride bulk of the present invention.
Embodiment 1:
The method that binder free plycrystalline diamond boron nitride bulk is synthesized under industrial stresses, specifically includes the following steps:
A, cBN is mixed with any one or any several powder in hBN, oBN, pBN purified, heating in vacuum it is pre- Processing removes the oxygen adsorbed in raw material powder, absorption water and combines the impurity such as water;The specific mode using the molten removal of impurities of acid into Row purification, by the mold of the raw material powder filling vacuum hotpressing stove after purification, the vacuum degree of vacuum hotpressing stove is in 4*10-2With Under, temperature is 400-600 DEG C, pressure 30-50MPa;
Powder pretreated in step a is prefabricated into the cylinder green body of diameter 3.5mm, high 4mm by b;
Column green body is packed into hBN crucible, then crucible is put into high temperature and pressure assembling block by c;
E, by high temperature and pressure assemble it is packaged enter domestic cubic hinge press in handle, pressure be 3~6GPa, temperature It is heated 10-400 minutes under conditions of 1000-2000 DEG C, synthesizes the high-performance plycrystalline diamond boron nitride bulk of binder free.
Obtained bulk is divided using X-ray diffractometer (Bruker D8, Germany) and electron energy loss spectroscopy (EELS) It analyses (as a shown in Figure 6), it can be seen that these samples include cBN and a kind of sp2-sp3Hybridize the BN phase of bonding.Utilize KB-5BVZ The Vickers hardness of microhardness testers measurement is 30-50GPa, fracture toughness 5-10MPam1/2.Show these samples for one kind The high performance plycrystalline diamond boron nitride bulk of binder free.
Embodiment 2:
The method that binder free plycrystalline diamond boron nitride bulk is synthesized under industrial stresses, specifically includes the following steps:
A is purified cBN raw material powder, the pretreatment such as heating in vacuum, and the oxygen adsorbed in raw material powder, absorption water are removed And combine the impurity such as water;The specific mode using the molten removal of impurities of acid is purified, and the raw material powder after purification is inserted vacuum In the mold of hot pressing furnace, the vacuum degree of vacuum hotpressing stove is in 4*10-2Hereinafter, temperature is 400-1600 DEG C, pressure 30-50MPa;
Powder pretreated in step a is prefabricated into the cylinder green body of diameter 3.5mm, high 4mm by b;
Column green body is packed into hBN crucible, then crucible is put into high temperature and pressure assembling block by c;
E, by high temperature and pressure assemble it is packaged enter domestic cubic hinge press in handle, pressure 6GPa, 1400 DEG C of temperature Under conditions of heat 10~40 minutes, synthesize the high-performance plycrystalline diamond boron nitride bulk of binder free.
Using X-ray diffractometer and electron energy loss spectroscopy (EELS), obtained plycrystalline diamond boron nitride bulk is analyzed, can be seen Plycrystalline diamond boron nitride bulk includes cBN and a kind of sp out2-sp3Hybridize the BN phase (as a shown in Figure 6) of bonding;Utilize Raman spectrometer (HORIBA Jobin Yvon) analyzes obtained bulk, as shown in Figure 2, it can be seen that different from pure cBN and pure HBN Raman peak position, shows a kind of sp2-sp3Hybridize the BN phase character of bonding;The dimension measured using KB-5BVZ microhardness testers Family name's hardness is 27GPa.Show that this sample is a kind of high-performance plycrystalline diamond boron nitride bulk of binder free.
Embodiment 3:
The method that binder free plycrystalline diamond boron nitride bulk is synthesized under industrial stresses, specifically includes the following steps:
A is purified cBN raw material powder, the pretreatment such as heating in vacuum, and the oxygen adsorbed in raw material powder, absorption water are removed And combine the impurity such as water;The specific mode using the molten removal of impurities of acid is purified, and the raw material powder after purification is inserted vacuum In the mold of hot pressing furnace, the vacuum degree of vacuum hotpressing stove is in 4*10-2Hereinafter, temperature is 400-1600 DEG C, pressure 30-50MPa;
Powder pretreated in step a is prefabricated into the cylinder green body of diameter 3.5mm, high 4mm by b;
Column green body is packed into hBN crucible, then crucible is put into high temperature and pressure assembling block by c;
E, by high temperature and pressure assemble it is packaged enter domestic cubic hinge press in handle, pressure 6GPa, 1800 DEG C of temperature Under conditions of heat 10~40 minutes, synthesize the high-performance plycrystalline diamond boron nitride bulk of binder free.
Using X-ray diffractometer and electron energy loss spectroscopy (EELS), obtained plycrystalline diamond boron nitride bulk is analyzed, as Fig. 1, Shown in 6, it can be seen that plycrystalline diamond boron nitride bulk includes cBN and a kind of sp2-sp3Hybridize the BN phase of bonding;Utilize Raman spectrometer Obtained bulk is analyzed, Raman peak position is similar with 1400 DEG C of peak position in Fig. 2, shows a kind of sp2-sp3It is miscellaneous Hand over the BN phase character of bonding;Vickers hardness using the measurement of KB-5BVZ microhardness testers is 36GPa, fracture toughness 7MPa m1/2.As shown in figure 4, the figure is the high-resolution picture of plycrystalline diamond boron nitride bulk, as can be seen from the figure sp2-sp3Hybridize bonding The juncture area of BN phase and cBN phase.Show that this sample is a kind of high-performance plycrystalline diamond boron nitride bulk of binder free.
Embodiment 4:
The method that binder free plycrystalline diamond boron nitride bulk is synthesized under industrial stresses, specifically includes the following steps:
A is purified cBN raw material powder, the pretreatment such as heating in vacuum, and the oxygen adsorbed in raw material powder, absorption water are removed And combine the impurity such as water;The specific mode using the molten removal of impurities of acid is purified, and the raw material powder after purification is inserted vacuum In the mold of hot pressing furnace, the vacuum degree of vacuum hotpressing stove is in 4*10-2Hereinafter, temperature is 400-1600 DEG C, pressure 30-50MPa;
Powder pretreated in step a is prefabricated into the cylinder green body of diameter 3.5mm, high 4mm by b;
Column green body is packed into hBN crucible, then crucible is put into high temperature and pressure assembling block by c;
E, by high temperature and pressure assemble it is packaged enter domestic cubic hinge press in handle, pressure 6GPa, 1700 DEG C of temperature Under conditions of heat 10~40 minutes, synthesize the high-performance plycrystalline diamond boron nitride bulk of binder free.
It is analyzed using X-ray diffractometer bulk is obtained, as shown in Figure 1, it can be seen that its phase composition is cube nitrogen Change boron;Obtained bulk is analyzed using Raman spectrometer, as shown in Fig. 2, there is the feature peak position of cubic boron nitride (1057 and 1305);Using the Vickers hardness result of KB-5BVZ microhardness testers measurement as shown in figure 3, asymptote hardness is 45GPa, maximum hardness is up to 50GPa.Load mould figure shown in Fig. 3 is respectively Vickers hardness load mould and 0.8Kg under 5Kg load Knoop hardness load mould under load, by measuring the crack length of load mould, the fracture toughness that PcBN is calculated is 8-10MPa m1/2.Fig. 5 is the SEM picture of PcBN bulk, it can be seen that is be sintered between crystal grain is fine.We also measured were the PcBN bulk Compressive strength, compressive strength 6.5GPa.Show that this sample is a kind of high-performance PcBN bulk of binder free.
Embodiment 5:
The method that binder free plycrystalline diamond boron nitride bulk is synthesized under industrial stresses, specifically includes the following steps:
A is purified cBN raw material powder, the pretreatment such as heating in vacuum, and the oxygen adsorbed in raw material powder, absorption water are removed And combine the impurity such as water;The specific mode using the molten removal of impurities of acid is purified, and the raw material powder after purification is inserted vacuum In the mold of hot pressing furnace, the vacuum degree of vacuum hotpressing stove is in 4*10-2Hereinafter, temperature is 400-1600 DEG C, pressure 30-50MPa;
Powder pretreated in step a is prefabricated into the cylinder green body of diameter 3.5mm, high 4mm by b;
Column green body is packed into hBN crucible, then crucible is put into high temperature and pressure assembling block by c;
E, by high temperature and pressure assemble it is packaged enter domestic cubic hinge press in handle, pressure 6GPa, 1200 DEG C of temperature Under conditions of heat 10~40 minutes, synthesize the high-performance plycrystalline diamond boron nitride bulk of binder free.
Using X-ray diffractometer and electron energy loss spectroscopy (EELS) (as a shown in Figure 6), to obtained plycrystalline diamond boron nitride bulk into Row analysis, it can be seen that plycrystalline diamond boron nitride bulk includes cBN and a kind of sp2-sp3Hybridize the BN phase of bonding;Utilize Raman spectrometer Obtained bulk is analyzed, Raman peak position is similar with 1400 DEG C of peak position in Fig. 2, shows a kind of sp2-sp3Hybridization The BN phase character of bonding;Vickers hardness using the measurement of KB-5BVZ microhardness testers is 18GPa.Show that this sample is a kind of nothing The high-performance plycrystalline diamond boron nitride bulk of binder.
Embodiment 6:
The method that binder free plycrystalline diamond boron nitride bulk is synthesized under industrial stresses, specifically includes the following steps:
A is purified cBN raw material powder, the pretreatment such as heating in vacuum, and the oxygen adsorbed in raw material powder, absorption water are removed And combine the impurity such as water;The specific mode using the molten removal of impurities of acid is purified, and the raw material powder after purification is inserted vacuum In the mold of hot pressing furnace, the vacuum degree of vacuum hotpressing stove is in 4*10-2Hereinafter, temperature is 400-1600 DEG C, pressure 30-50MPa;
Powder pretreated in step a is prefabricated into the cylinder green body of diameter 3.5mm, high 4mm by b;
Column green body is packed into hBN crucible, then crucible is put into high temperature and pressure assembling block by c;
E, by high temperature and pressure assemble it is packaged enter domestic cubic hinge press in handle, pressure 6GPa, 900 DEG C of temperature Under the conditions of heat 20~40 minutes, synthesize the high-performance plycrystalline diamond boron nitride bulk of binder free.
It is analyzed using X-ray diffractometer bulk is obtained, as shown in Figure 1, it can be seen that plycrystalline diamond boron nitride bulk phase Group becomes cBN and hBN.Vickers hardness using the measurement of KB-5BVZ microhardness testers is 10GPa.Show that this sample is not also complete It sinters.
The application of plycrystalline diamond boron nitride bulk:
It is prepared into cutter after being processed using the binder free plycrystalline diamond boron nitride bulk that above-described embodiment synthesizes, cutter Specific preparation process includes being ground and being polished on mechanical grinding device.Abrasive parameters: revolving speed 1500rpm (rev/min), Grinding pressure 3.6N, 1 μm of abrasive grains size.
The cutter of preparation carrys out cutting of hardened steel, and (4140 mould steel of hardened steel model AISI, diameter 20mm are put down after quenching The test value of equal Vickers hardness is Hv 494, is about 4.8GPa after conversion) and WC hard alloy (diameter 11mm, hardness containing Co For 13-18GPa, fracture toughness 8-12MPam1/2).Wherein machined parameters of cutting of hardened steel: revolving speed 5000rpm, cutting 3 μm of depth, feed speed 10mm/min (being 2 μm/rev (micron/turn) after being converted according to revolving speed);Cut the processing of hard alloy Parameter: revolving speed 5000rpm, 2 μm of cutting depth, feed speed 3mm/min (after being converted according to revolving speed for 0.6 μm/rev (micron/ Turn)).WC hard alloy containing Co and hardened steel surface both after machining are in mirror effect.Also make after machining Surface roughness detection (the Dimension Icon of AFM, Bruker company production is carried out with atomic force microscope and scanning electron microscope Model;The Scios model of SEM, ThermoFisher company production).Testing result is as shown in Figure 7 and Figure 8, and Fig. 7 is hardened steel AFM testing result, Fig. 8 is the AFM testing result of hard alloy, wherein RaFor the arithmetic mean of instantaneous value of surface height deviation.It quenches Testing result after hard steel mirror-finish cutting: RaFor 24.80nm;Testing result after hard alloy mirror-finish cutting: RaFor 8.66nm.It is comprehensive Upper described, the binder free plycrystalline diamond boron nitride bulk of this patent research and development can be used to prepare high-performance lathe tool, and iron series, carbon may be implemented The super-precision mirror surface grinding of the difficult-to-machine materials such as compound forming material and high rigidity hard alloy.

Claims (7)

1. synthesizing the method for binder free plycrystalline diamond boron nitride bulk under industrial stresses, it is characterised in that: by cBN, hBN, oBN, pBN In any one or any several powder mixing purified, be prefabricated into column green body after heating in vacuum pretreatment, then in height Processing obtains plycrystalline diamond boron nitride bulk under mild industrial stresses.
2. the method for synthesizing binder free plycrystalline diamond boron nitride bulk under industrial stresses according to claim 1, feature exist In specifically includes the following steps:
A, by any one in cBN, hBN, oBN, pBN or arbitrarily several powder mixing are purified, heating in vacuum pre-processes, It removes the oxygen adsorbed in raw material powder, absorption water and combines water;
Powder pretreated in step a is prefabricated into column green body by b;
Column green body is packed into crucible by c, and crucible is put into high temperature and pressure assembling block;
D will carry out high temperature high pressure process in high temperature and pressure assembling block merging press;
Plycrystalline diamond boron nitride bulk is obtained under e, high temperature and industrial stresses after the completion of processing.
3. the method for synthesizing binder free plycrystalline diamond boron nitride bulk under industrial stresses according to claim 2, feature exist In: the step d selection is handled in cubic hinge press, and pressure limit 1-6GPa, temperature range is 800-2300 DEG C, Soaking time is 10-400 minutes.
4. the method for synthesizing binder free plycrystalline diamond boron nitride bulk under industrial stresses according to claim 2, feature exist In: the cylinder green body of diameter 3.5mm, high 4mm are prefabricated into the step b.
5. the method for synthesizing binder free plycrystalline diamond boron nitride bulk under industrial stresses according to claim 2, feature exist In: the purification of raw material, heating in vacuum preprocess method in the step a are as follows: purified, will be mentioned using the mode of the molten removal of impurities of acid In the mold of raw material powder filling vacuum hotpressing stove after pure, the vacuum degree of vacuum hotpressing stove is in 4*10-2Hereinafter, temperature is 400- 1600 DEG C, pressure 30-50MPa.
6. the application of binder free plycrystalline diamond boron nitride bulk is synthesized under described in any item industrial stresses according to claim 1~5, It is characterized by: plycrystalline diamond boron nitride bulk, which is carried out processing, is prepared into cutting tool.
7. synthesizing the application of binder free plycrystalline diamond boron nitride bulk under industrial stresses according to claim 6, feature exists In: cutting tool is used for the machining to the hard difficult-to-machine material of the height comprising iron-based material and hard alloy.
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