CN107098704A - A kind of preparation method of polycrystalline cubic boron nitride sintered material - Google Patents

A kind of preparation method of polycrystalline cubic boron nitride sintered material Download PDF

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CN107098704A
CN107098704A CN201710316198.8A CN201710316198A CN107098704A CN 107098704 A CN107098704 A CN 107098704A CN 201710316198 A CN201710316198 A CN 201710316198A CN 107098704 A CN107098704 A CN 107098704A
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boron nitride
cubic boron
polycrystalline cubic
preparation
sintered material
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李启泉
李新奇
张旺玺
刘磊
赵豆豆
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Zhongyuan University of Technology
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Zhongyuan University of Technology
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Abstract

The invention provides a kind of preparation method of polycrystalline cubic boron nitride sintered material, new combined binder is prepared first with metal powder, carbide and/or nitride；Afterwards by cubic boron nitride micro mist and combined binder mixing and ball milling, the compressing preceding micro-nano mixed powder by the way that cubic boron nitride to be broken for 07 microns under protective atmosphere；It is last compressing.The present invention causes the counterdiffusion of component phase, infiltration, solid solution in bonding agent to form the combined binder of homogeneous by high melt, and combined binder can reduce polycrystalline cubic boron nitride（PcBN）The temperature and pressure needed during synthesis, can also improve polycrystalline cubic boron nitride（PcBN）Combination property；Deng measure, cubic boron nitride is destroyed（CBN）The fine and close oxidation layer film of single-crystal surface obtains the polycrystalline cubic boron nitride of high intensity in favor of being bonded between CBN and CBN（PcBN）；A large amount of CBN surfaces for being free of oxide-film are produced simultaneously.

Description

A kind of preparation method of polycrystalline cubic boron nitride sintered material
Technical field
The invention provides a kind of polycrystalline cubic boron nitride（PcBN）The preparation method of sintered material, is related to cutting and milling Cut preparing technical field of the processing using super-hard compound material cutter, and in particular to a kind of polycrystalline cubic boron nitride（PcBN）Sintering The preparation method of body material.
Background technology
Diamond is known most hard material, cubic boron nitride in the world（CBN）Similar diamond lattic structure, its hardness is only secondary In diamond, diamond and cubic boron nitride（It is referred to as superhard material）.Superhard material is widely used in cutting tools, grinding work Tool, boring means and cutting tool.
Diamond high temperature is easily aoxidized, particularly good with iron series element compatibility, is not suitable for iron series element black gold Category processing.Cubic boron nitride（CBN）Heat endurance is better than diamond, remains to keep sufficiently high mechanical property at high temperature And hardness, with good red hardness；Cubic boron nitride（CBN）Stability Analysis of Structures, with high oxidation resistance, chemical stability It is good, compared with diamond, cubic boron nitride（CBN）Also chemistry is not played at a temperature of up to 1100-1300 DEG C with iron family element Reaction, therefore cubic boron nitride is particularly suitable for processing ferrous material.Due to cubic boron nitride（CBN）Three high property：It is high Hardness, high heat endurance and the high inertia with iron family element, in industrially developed country as in raising processing industry Benefit（Energy-conservation, efficient, accurate, automation）Important precise materials developed, especially space flight, military project, spraying weldering plus It is more prominent in work industry.And the cubic boron nitride of monocrystalline（CBN）Granularity is small, and can not in the presence of " cleavage surface " easily cleaved It is directly used in manufacture cutting tool, and polycrystalline cubic boron nitride（PcBN）It is made up of countless tiny cubic boron nitride monocrystals, Because of polycrystalline cubic boron nitride（PcBN）The non-directional influence that can make splitting is greatly reduced, and with the abrasion of working angles cutter New crystal, therefore industrially cutter material --- the polycrystalline cubic boron nitride as processing ferrous metal iron can continuously be spilt （PcBN）Have a wide range of applications.
But, there are one layer of fine and close oxide films on cubic boron nitride monocrystal surface, and this layer film hinders a cube nitridation Between boron (CBN) crystal directly in conjunction with so being difficult to obtain cubic boron nitride (CBN) and cubic boron nitride（CBN）Directly in conjunction with High intensity polycrystalline cubic boron nitride, thus add a variety of bonding agents in the course of the polymerization process to strengthen cubic boron nitride（CBN）It is brilliant The connection of intergranular.
Polycrystalline cubic boron nitride（PcBN）Cutter material can be divided into polycrystalline cubic boron nitride by its composition and manufacture method and burn Knot body（PcBN sintered bodies）With composite polycrystalline cubic boron nitride（PcBN composite blades）.Polycrystalline cubic boron nitride also has following spy Different performance：(1) high rigidity；(2) high-wearing feature；(3) high chemical inertness；(4) high temperature red hardness；Polycrystalline cubic boron nitride （PcBN）Heat resistance can reach 1400 DEG C, it is more much higher than diamond cutter (700-800 DEG C), through using prove 1100 DEG C More than cutting temperature remain to maintain high sharp cutting ability, be suitable for doing, wet type cutting.(5) high-termal conductivity；(6) it is low Coefficient of friction and；(7) high-speed cutting characteristic and high manufacturing accuracy.Just because of polycrystalline cubic boron nitride（PcBN）With height Hardness, high-wearing feature, high heat transfer efficiency and excellent high-temperature behavior etc., it is believed that polycrystalline CBN cutting tool is Preferred cutting element at a high speed, efficiently, accurate can most be met in the world so far.
It is usually used in polycrystalline cubic boron nitride both at home and abroad at present（PcBN）Bonding agent have three basic forms of it：（1）Metal knot Mixture：The metallic bond being made up of metal and its alloy, such bonding agent can soften as liquid phase, bonding at a lower temperature CBN particles, make sintered body, are commonly used in the PcBN of high content, to improve its toughness.Though under wearability and red hardness Drop, but prepared cutter is less prone to the phenomenon of tipping at work, improves cutting-tool's used life, it is adaptable to cast iron class Processing；（2）Vitrified bond：It is made up of nitride, carbide, boride, silicide, oxide and nitrogen carbide, it is common There are aluminium nitride, carborundum, aluminum oxide and titanium carbide etc..Because this kind of PcBN has higher wearability and thermally-stabilised at high temperature Property, though its poor thermal conductivity, but still it is used for preparing the cutter of the low cBN contents of cutting of hardened steel；（3）Metal or cermet knot Mixture, is made up of, the characteristics of having metal and vitrified bond concurrently ceramics and metal.
Current polycrystalline cubic boron nitride（PcBN）Preparation method mainly prepared using the hot pressing sintering method under HTHP, The method of existing manufacture polycrystalline cubic boron nitride is that shaping is carried out simultaneously with sintering, can only use a class bonding agent, not only Pressure required for shaping is very big（6-10GP）, sintering temperature is higher（1200℃-2800℃）, and setting needed for preparation technology Standby complicated, cost is high, so limiting polycrystalline cubic boron nitride to a certain extent（PcBN）Use.
Chinese patent 201010615047.0 discloses a kind of powdered bonding agent of polycrystalline cubic boron nitride compound sheets, Include TiN, AlN, Si3N4, Co and SiO2, the shock resistance of composite sheet can be strengthened.
Patent WO2004040029 disclosed in Element Six companies of Britain, using the mixed of various carbide and nitride Compound forms a kind of complicated core and is scattered in matrix, and superhard material cubic boron nitride and diamond, Yi Jijie are surrounded by matrix Mixture, has a kind of polycrystalline cubic boron nitride of alveolate texture through high pressure-temperature synthesis, tough with excellent intensity and fracture Property.
Above patent is single angle from enhancing toughness, does not take into full account that polycrystalline cubic boron nitride sintered body is mixed Material, prepare the problems such as cost and quality control that difficult and superhigh-temperature and-pressure is brought.
The content of the invention
For problem above, the invention discloses a kind of polycrystalline cubic boron nitride sintered material and preparation method thereof, adopt New process is taken to reduce synthesis polycrystalline cubic boron nitride（PcBN）Required temperature and pressure during synthesis, is improved poly- Brilliant cubic boron nitride（PcBN）Combination property.Meanwhile, new process makes the polycrystalline cubic boron nitride of synthesis（PcBN）No Only performance has homogeneity, and with foresight and controllability.
Realize the technical scheme is that：A kind of preparation method of polycrystalline cubic boron nitride sintered material, step is such as Under：
（1）Raw material cubic boron nitride micro mist, metal powder, carbide and/or nitride are handled through chemical acid alkali respectively, physics it is true After the reason of vacancy, oxygen, water and the impurity in raw material are removed；
（2）By step（1）After metal powder, carbide after processing and/or nitride mixing at 1000-1300 DEG C high temperature melting Refining, melting matter is crushed, is classified, obtain combined binder afterwards；
（3）By step（1）Cubic boron nitride micro mist and step after processing（2）Ball milling, ball after obtained combined binder mixing Ratio of grinding media to material 4 during mill:1, rotating speed is 300-800r/min, and the time is 3-15h；
（4）By step（3）Material after middle ball milling is crushed under protective atmosphere argon gas, obtains mixed powder；
（5）By step（4）Obtained mixed powder cold moudling, cold moudling makes blank forming using distribution pressurization, first exists Base substrate is pressed under low pressure 10-20MPa, 20-100MPa is then pressurized to and obtains block；
（6）By step（5）Obtained block loads in graphite jig, is then charged into pyrophillite cavity, then successively conducting steel ring Load pyrophillite cavity with sheet metal, be assembled into Synthetic block and be put into 100 DEG C of baking ovens dry 30min, HTHP is sintered afterwards Polycrystalline cubic boron nitride sintered material is made.
The step（1）In metal powder at least one of for aluminium powder, titanium valve, cobalt powder, the purity of metal powder is all higher than 99.9%, particle diameter is 0.1-5 microns.
The step（1）Middle nitride is at least one of titanium nitride, silicon nitride, aluminium nitride；Carbide be titanium carbide, At least one of tungsten carbide, chromium carbide, TiCN.
The step（2）The mass fraction of carbide and/or nitride is 10-90% in middle combined binder.
The purity of the carbide and/or nitride is both greater than 98%, 0.1-5 microns of particle diameter.
The step（3）The particle diameter of material after ball milling is 5-30 microns.
The step（4）The particle diameter of mixed powder after broken is 0.1-4 microns.
The step（6）The condition of HTHP sintering is synthesized using cubic pressure machine equipment, and pressure is 3.3- 4.5GPa, 1000-1600 DEG C of temperature, generated time 2-35min.
The step（2）Particle diameter≤2 micron of middle combined binder.
The step（3）The mass ratio of cubic boron nitride micro mist and combined binder is（5-9.5）：（0.5-5）.
The beneficial effects of the invention are as follows：（1）Manufacturing process is different compared with traditional method, using " two-step method ".First New combined binder is prepared, by high melt so that the counterdiffusion of component phase, infiltration, solid solution in bonding agent form homogeneous Combined binder, combined binder can reduce polycrystalline cubic boron nitride（PcBN）The temperature and pressure needed during synthesis, may be used also To improve polycrystalline cubic boron nitride（PcBN）Combination property；Because combined binder has foresight and controllability, greatly The homogeneity and yield rate of polycrystalline cubic boron nitride sintered body are improved, manufacturing cost is reduced indirectly, polycrystalline cubic is nitrogenized Boron sintered body can obtain more preferable popularization and application；Simultaneously combined binder constituent element can be used together with heavy and lightweight without Cause produces lamination in the mixing of material, transportation, improves the quality of sintered body；
（2）Secondly, mixed before compressing by the way that cubic boron nitride is broken for into 0-7 micron micro-nano under protective atmosphere The measures such as powder are closed, cubic boron nitride is destroyed（CBN）The fine and close oxidation layer film of single-crystal surface is in favor of between CBN and CBN Bonding, obtains the polycrystalline cubic boron nitride of high intensity（PcBN）；A large amount of CBN surfaces for being free of oxide-film are produced simultaneously；
（3）The polycrystalline cubic boron nitride prepared using the present invention（PcBN）Sintered material performance is homogeneous, with preferably resistance to The characteristics such as mill property, heat endurance and low machinery part surface processing roughness.Chemically and physically purify, melt with powder body material The technologies such as refining, high-energy ball milling, the first base of cold-press moulding, the nitridation of fine granularity polycrystalline cubic is prepared for using hexahedron top press high-pressure sintering Boron sintered material, the material has excellent combination property and long life.Knife is processed suitable for cast iron class, hardened steel etc. Has material.
Brief description of the drawings
Fig. 1 is the process chart of traditional preparation methods；
Fig. 2 is the process chart of preparation method of the present invention；
Fig. 3 is the mass spectral analysis figure of PcBN sintered materials prepared by embodiment 1；
Fig. 4 is the mass spectral analysis figure of PcBN sintered materials prepared by embodiment 2.
Embodiment
Embodiment 1
The preparation method of the present embodiment polycrystalline cubic boron nitride sintered material is as follows：
The mass fraction ratio that selection cementing metal powder and titanium carbide, tungsten carbide, titanium nitride account for raw material micro mist is 40%, wherein carbon The mass ratio of compound or nitride is 9.5:1, the content of cobalt powder is not more than the 4% of total mass fraction, and the content of aluminium powder is not more than always Mass fraction obtains 6%, and the particle diameter of metal powder is at 0.1-3 microns；The cubic boron nitride micro mist of 35 microns of particle diameter is broken for particle diameter 0-7 The particle of micron is raw material, and the mass fraction ratio that cubic boron nitride micro mist accounts for raw material micro mist is 60%.Above-mentioned raw materials micro mist is passed through respectively Cross after chemical acid alkali processing, physical vacuum processing, remove oxygen, water and the other impurity of raw material.
Above-mentioned cementing metal powder and titanium carbide, tungsten carbide, titanium nitride micro mist are evenly mixed in high temperature melting at 1200 DEG C Refining, obtained mixture is crushed, is classified, combined binder is made.Then it is combined binder is micro- with cubic boron nitride Powder is mixed by setting ratio in high energy ball mill, and drum's speed of rotation 400r/min, incorporation time is set as 9h, measures powder The particle mean size of body material is 2.2 microns.Then 400 mesh sieves were granulated, the test block of set shape is pressed into.
Obtained test block is loaded in pre-designed graphite jig, be then charged into pyrophillite cavity, conducting steel ring, gold Category piece is assembled into Synthetic block, is put into baking oven and dries, then is sintered together by HTHP, and polycrystalline cubic boron nitride is made （PcBN）Sintered material.The actual conditions of sintering is synthesized using cubic pressure machine equipment, and pressure is 4.0GPa, temperature 1300 DEG C, generated time 8 minutes.
The polycrystalline CBN cutting tool material microhardness that the above method is prepared is HV3250, and bending strength is 863MPa, cutter average life span improves 18%.It is mainly used in the processing of hardened steel.Fig. 1 is the mass spectral analysis figure of the material.In figure It was found that there is C3N4、Al2OC and a small amount of SiO2The appearance of novel substance, illustrates to be chemically reacted in sintering process and thing The complicated material transport essence such as matter solid solution.Wherein C3N4It is the material that a kind of hardness is only second to diamond and hexagonal boron nitride, reason Even to exceed diamond and hexagonal boron nitride by the hardness of the above material, therefore the generation of the material is conducive to strengthening bonding agent Partial wearability, so as to reach the effect of the bonding agent part abrasion synchronous with CBN particulates in working angles；Al2OC is one Metastable material is planted, illustrates that metal Al can slough oxygen and carbon dioxide micro in sintered body in addition to being reacted with CBN, Al2OC generation is probably a kind of gas-solid reaction, so as to advantageously reduce micro- stomata in sintered body, makes material fine and close；SiO2's Generation should be that the trace impurity Si in material reacts caused with oxygen, and Si is conducive to cleaning the surface of reactant, acceleration of sintering Progress, while SiO2It is also hard material.
Embodiment 2
The preparation method of the present embodiment polycrystalline cubic boron nitride sintered material is as follows：
The mass fraction ratio that selection cementing metal powder and tungsten carbide, titanium carbide, TiCN account for raw material micro mist is 20%, wherein Tungsten carbide, titanium carbide, the mass ratio of TiCN are 2:2:1, the content of titanium valve is not more than the 3% of gross mass, the content of aluminium powder No more than total mass fraction obtains 7%, and the particle diameter of metal powder is at 0.1~3.5 micron；The cubic boron nitride micro mist of 35 microns of particle diameter is broken Broken is that the particle of 0~7 micron of particle diameter is raw material, and the mass fraction ratio that cubic boron nitride micro mist accounts for raw material micro mist is 80%.Pass through respectively Cross oxygen, water and other impurity that the methods such as chemical acid alkali processing, physical vacuum processing remove raw material.
Above-mentioned cementing metal powder and tungsten carbide, titanium carbide, TiCN micro mist are evenly mixed in high temperature at 1200 DEG C Melting, obtained mixture is crushed, is classified, combined binder is made.Then combined binder and cubic boron nitride Micro mist is mixed by setting ratio in high energy ball mill, and drum's speed of rotation 400r/min, incorporation time is set as 20h, is surveyed The particle mean size for obtaining powder body material is 2.7 microns.Then 400 mesh sieves were granulated, the test block of set shape is pressed into.
Obtained test block is loaded in pre-designed graphite jig, be then charged into pyrophillite cavity, conducting steel ring, sheet metal Synthetic block is assembled into, is put into baking oven and dries, then is sintered together by HTHP, polycrystalline cubic boron nitride is made（PcBN） Sintered material.The actual conditions of sintering is synthesized using cubic pressure machine equipment, and pressure is 3.8GPa, temperature 1300 DEG C, generated time 7 minutes.
The polycrystalline CBN cutting tool material microhardness that the above method is prepared is HV3805, and bending strength is 890MPa, cutter average life span improves 36% compared with product prepared by original technique.It is mainly used in the process tool of cast iron class. Fig. 2 is the mass spectral analysis figure of the material.As can be seen from the figure metallic titanium powder generates TiN and TiB with CBN2, TiN and TiB2 They are all hard materials, and the toughness of sintered body can also be improved in addition to firmly CBN particles are held；Equally, C3N4Generation be conducive to Strengthen the wearability of bonding agent part, so as to reach the effect of the bonding agent part abrasion synchronous with CBN particulates in working angles； Ti3Al solid solution alloys can be greatly enhanced the toughness of sintered body.
Embodiment 3
The preparation method of the present embodiment polycrystalline cubic boron nitride sintered material is as follows：
（1）Raw material cubic boron nitride micro mist, aluminium powder, silicon nitride and titanium carbide are handled through chemical acid alkali respectively, at physical vacuum After reason, oxygen, water and the impurity in raw material are removed；
（2）By step（1）Aluminium powder, silicon nitride after processing mixed with titanium carbide after at 1000 DEG C high melt, afterwards will be molten Refine thing to crush, be classified, obtain combined binder；The mass fraction of silicon nitride and titanium carbide is 10%, silicon nitride in combined binder Mass ratio with titanium carbide is 5:1；
（3）By step（1）Cubic boron nitride micro mist and step after processing（2）Ball milling after obtained combined binder mixing, stands The mass ratio of square boron nitride micro mist and combined binder is 5：5, the particle diameter of the material after ball milling is 5 microns, ratio of grinding media to material during ball milling 4:1, rotating speed is 300r/min, and the time is 15h；
（4）By step（3）Material after middle ball milling is crushed under protective atmosphere argon gas, obtains mixed powder, after crushing The particle diameter of mixed powder is 0-7 microns；
（5）By step（4）Obtained mixed powder cold moudling, cold moudling makes blank forming using distribution pressurization, first exists Base substrate is pressed under low pressure 10MPa, 20MPa is then pressurized to and obtains block；
（6）By step（5）Obtained block loads in graphite jig, is then charged into pyrophillite cavity, then successively conducting steel ring Load pyrophillite cavity with sheet metal, be assembled into Synthetic block and be put into 100 DEG C of baking ovens dry 30min, HTHP is sintered afterwards Polycrystalline cubic boron nitride sintered material is made.The condition of HTHP sintering is synthesized using cubic pressure machine equipment, Pressure is 3.3GPa, 1000 DEG C of temperature, generated time 35min.
Embodiment 4
The preparation method of the present embodiment polycrystalline cubic boron nitride sintered material is as follows：
（1）Raw material cubic boron nitride micro mist, cobalt powder, silicon nitride, tungsten carbide, TiCN are handled through chemical acid alkali respectively, thing Manage after application of vacuum, remove oxygen, water and the impurity in raw material；
（2）By step（1）Cobalt powder, silicon nitride, tungsten carbide after processing, after TiCN mixing at 1100 DEG C high melt, Melting matter is crushed afterwards, is classified, combined binder is obtained；Silicon nitride in combined binder, tungsten carbide and TiCN it is total Mass fraction be 30%, the mass ratio of silicon nitride, tungsten carbide and TiCN is 3:1:1；
（3）By step（1）Cubic boron nitride micro mist and step after processing（2）Ball milling after obtained combined binder mixing, stands The mass ratio of square boron nitride micro mist and combined binder is 7：3, the particle diameter of the material after ball milling is 15 microns, ratio of grinding media to material during ball milling 4:1, rotating speed is 500r/min, and the time is 8h；
（4）By step（3）Material after middle ball milling is crushed under protective atmosphere argon gas, obtains mixed powder, after crushing The particle diameter of mixed powder is 0-7 microns；
（5）By step（4）Obtained mixed powder cold moudling, cold moudling makes blank forming using distribution pressurization, first exists Base substrate is pressed under low pressure 15MPa, 50MPa is then pressurized to and obtains block；
（6）By step（5）Obtained block loads in graphite jig, is then charged into pyrophillite cavity, then successively conducting steel ring Load pyrophillite cavity with sheet metal, be assembled into Synthetic block and be put into 100 DEG C of baking ovens dry 30min, HTHP is sintered afterwards Polycrystalline cubic boron nitride sintered material is made.The condition of HTHP sintering is synthesized using cubic pressure machine equipment, Pressure is 4.0GPa, 1300 DEG C of temperature, generated time 20min.
Embodiment 5
The preparation method of the present embodiment polycrystalline cubic boron nitride sintered material is as follows：
（1）Raw material cubic boron nitride micro mist, titanium valve, aluminium nitride and chromium carbide are handled through chemical acid alkali respectively, at physical vacuum After reason, oxygen, water and the impurity in raw material are removed；
（2）By step（1）Titanium valve, aluminium nitride after processing mixed with chromium carbide after at 1300 DEG C high melt, afterwards will be molten Refine thing to crush, be classified, obtain combined binder；The mass fraction of aluminium nitride and chromium carbide is 90%, aluminium nitride in combined binder Mass ratio with chromium carbide is 7:2；
（3）By step（1）Cubic boron nitride micro mist and step after processing（2）Ball milling after obtained combined binder mixing, stands The mass ratio of square boron nitride micro mist and combined binder is 9.5：0.5, the particle diameter of the material after ball milling is 30 microns, ball during ball milling Material compares 4:1, rotating speed is 800r/min, and the time is 3h；
（4）By step（3）Material after middle ball milling is crushed under protective atmosphere argon gas, obtains mixed powder, after crushing The particle diameter of mixed powder is 0-7 microns；
（5）By step（4）Obtained mixed powder cold moudling, cold moudling makes blank forming using distribution pressurization, first exists Base substrate is pressed under low pressure 20MPa, 100MPa is then pressurized to and obtains block；
（6）By step（5）Obtained block loads in graphite jig, is then charged into pyrophillite cavity, then successively conducting steel ring Load pyrophillite cavity with sheet metal, be assembled into Synthetic block and be put into 100 DEG C of baking ovens dry 30min, HTHP is sintered afterwards Polycrystalline cubic boron nitride sintered material is made.The condition of HTHP sintering is synthesized using cubic pressure machine equipment, Pressure is 4.5GPa, 1600 DEG C of temperature, generated time 2min.
Embodiment 6
The preparation method of the present embodiment polycrystalline cubic boron nitride sintered material is as follows：
（1）Raw material cubic boron nitride micro mist, titanium valve, aluminium nitride are handled through chemical acid alkali respectively, physical vacuum processing after, remove Oxygen, water and impurity in raw material；
（2）By step（1）Titanium valve after processing, after aluminium nitride mixing at 1300 DEG C high melt, afterwards by melting matter it is broken, Classification, obtains combined binder；The mass fraction of aluminium nitride is 50% in combined binder, and the mass ratio of aluminium nitride is 7:2；
（3）By step（1）Cubic boron nitride micro mist and step after processing（2）Ball milling after obtained combined binder mixing, stands The mass ratio of square boron nitride micro mist and combined binder is 9.5：0.5, the particle diameter of the material after ball milling is 30 microns, ball during ball milling Material compares 4:1, rotating speed is 800r/min, and the time is 3h；
（4）By step（3）Material after middle ball milling is crushed under protective atmosphere argon gas, obtains mixed powder, after crushing The particle diameter of mixed powder is 0-7 microns；
（5）By step（4）Obtained mixed powder cold moudling, cold moudling makes blank forming using distribution pressurization, first exists Base substrate is pressed under low pressure 20MPa, 100MPa is then pressurized to and obtains block；
（6）By step（5）Obtained block loads in graphite jig, is then charged into pyrophillite cavity, then successively conducting steel ring Load pyrophillite cavity with sheet metal, be assembled into Synthetic block and be put into 100 DEG C of baking ovens dry 30min, HTHP is sintered afterwards Polycrystalline cubic boron nitride sintered material is made.The condition of HTHP sintering is synthesized using cubic pressure machine equipment, Pressure is 4.5GPa, 1600 DEG C of temperature, generated time 2min.
Embodiment 7
The preparation method of the present embodiment polycrystalline cubic boron nitride sintered material is as follows：
（1）Raw material cubic boron nitride micro mist, titanium valve, chromium carbide are handled through chemical acid alkali respectively, physical vacuum processing after, remove Oxygen, water and impurity in raw material；
（2）By step（1）Titanium valve after processing, after chromium carbide mixing at 1300 DEG C high melt, afterwards by melting matter it is broken, Classification, obtains combined binder；The mass fraction of chromium carbide is 20% in combined binder, and the mass ratio of chromium carbide is 7:2；
（3）By step（1）Cubic boron nitride micro mist and step after processing（2）Ball milling after obtained combined binder mixing, stands The mass ratio of square boron nitride micro mist and combined binder is 9.5：0.5, the particle diameter of the material after ball milling is 30 microns, ball during ball milling Material compares 4:1, rotating speed is 800r/min, and the time is 3h；
（4）By step（3）Material after middle ball milling is crushed under protective atmosphere argon gas, obtains mixed powder, after crushing The particle diameter of mixed powder is 0-7 microns；
（5）By step（4）Obtained mixed powder cold moudling, cold moudling makes blank forming using distribution pressurization, first exists Base substrate is pressed under low pressure 20MPa, 100MPa is then pressurized to and obtains block；
（6）By step（5）Obtained block loads in graphite jig, is then charged into pyrophillite cavity, then successively conducting steel ring Load pyrophillite cavity with sheet metal, be assembled into Synthetic block and be put into 100 DEG C of baking ovens dry 30min, HTHP is sintered afterwards Polycrystalline cubic boron nitride sintered material is made.The condition of HTHP sintering is synthesized using cubic pressure machine equipment, Pressure is 4.5GPa, 1600 DEG C of temperature, generated time 2min.

Claims (10)

1. a kind of preparation method of polycrystalline cubic boron nitride sintered material, it is characterised in that step is as follows：
（1）Raw material cubic boron nitride micro mist, metal powder, carbide and/or nitride are handled through chemical acid alkali respectively, physics it is true After the reason of vacancy, oxygen, water and the impurity in raw material are removed；
（2）By step（1）After metal powder, carbide after processing and/or nitride mixing at 1000-1300 DEG C high temperature melting Refining, melting matter is crushed, is classified, obtain combined binder afterwards；
（3）By step（1）Cubic boron nitride micro mist and step after processing（2）Ball milling, ball after obtained combined binder mixing Ratio of grinding media to material 4 during mill:1, rotating speed is 300-800r/min, and the time is 3-15h；
（4）By step（3）Material after middle ball milling is crushed under protective atmosphere argon gas, obtains mixed powder；
（5）By step（4）Obtained mixed powder cold moudling, cold moudling makes blank forming using distribution pressurization, first exists Base substrate is pressed under low pressure 10-20MPa, 20-100MPa is then pressurized to and obtains block；
（6）By step（5）Obtained block loads in graphite jig, is then charged into pyrophillite cavity, then successively conducting steel ring Load pyrophillite cavity with sheet metal, be assembled into Synthetic block and be put into 100 DEG C of baking ovens dry 30min, HTHP is sintered afterwards Polycrystalline cubic boron nitride sintered material is made.
2. the preparation method of polycrystalline cubic boron nitride sintered material according to claim 1, it is characterised in that：The step Suddenly（1）In metal powder at least one of for aluminium powder, titanium valve, cobalt powder, the purity of metal powder is all higher than 99.9%, and particle diameter is 0.1-5 microns.
3. the preparation method of polycrystalline cubic boron nitride sintered material according to claim 1, it is characterised in that：The step Suddenly（1）Middle nitride is at least one of titanium nitride, silicon nitride, aluminium nitride；Carbide be titanium carbide, tungsten carbide, chromium carbide, At least one of TiCN.
4. the preparation method of polycrystalline cubic boron nitride sintered material according to claim 1, it is characterised in that：It is described
Step（2）The mass fraction of carbide and/or nitride is 10-90% in middle combined binder.
5. the preparation method of polycrystalline cubic boron nitride sintered material according to claim 4, it is characterised in that：The nitrogen Compound or the purity of carbide are both greater than 98%, 0.1-5 microns of particle diameter.
6. the preparation method of polycrystalline cubic boron nitride sintered material according to claim 1, it is characterised in that：The step Suddenly（3）The particle diameter of material after ball milling is 5-30 microns.
7. the preparation method of polycrystalline cubic boron nitride sintered material according to claim 1, it is characterised in that：The step Suddenly（4）The particle diameter of mixed powder after broken is 0.1-4 microns.
8. the preparation method of polycrystalline cubic boron nitride sintered material according to claim 1, it is characterised in that：The step Suddenly（6）The condition of HTHP sintering is synthesized using cubic pressure machine equipment, and pressure is 3.3-4.5GPa, temperature 1000-1600 DEG C, generated time 2-35min.
9. the preparation method of polycrystalline cubic boron nitride sintered material according to claim 1, it is characterised in that：The step Suddenly（2）Particle diameter≤2 micron of middle combined binder.
10. the preparation method of polycrystalline cubic boron nitride sintered material according to claim 1, it is characterised in that：It is described Step（3）The mass ratio of cubic boron nitride micro mist and combined binder is（5-9.5）：（0.5-5）.
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