It is a kind of to use the primary material of cubic boron nitride monocrystal as initial feed and prepare plycrystalline diamond sintered body
Method
Technical field
The invention belongs to cutter material manufacturing field, specifically a kind of synthesis condition is low, heat-resist, toughness
The high method for using the primary material of cubic boron nitride monocrystal to prepare plycrystalline diamond sintered body as initial feed.
Background technique
Modern mechanical processing technology is just developed rapidly towards high-precision, high efficiency, flexibility and automation direction, numerical control machine
The new techniques such as bed, machining center equipment and the superfine new material application of performance are increasingly extensive, and then want to cutter
Ask higher and higher.As a kind of environmental type high performance structures material, polycrystalline cubic boron nitride (PcBN) is with its super abrasive, resistance to
The excellent properties such as burn into high temperature resistant have fully demonstrated requirement of the modern manufacturing industry to material.PcBN cutter is particularly suitable for various black
The hard turning of non-ferrous metal is realized and is ground with vehicle generation.It not only improves and draws processing efficiency, but also considerably reduce processing cost, it is main
Cut various hardened steels, tool steel, mould steel, bearing steel (HRC45-70), chilled cast iron, rich chromium cast iron, Ni-based and cobalt-based
High temperature alloy, various difficult processing grey cast-irons, other difficult processing black materials etc..Since cubic boron nitride hardness is much higher than ceramics
And hard alloy, the cutter life of preparation are 3-5 times, 5-15 times of hard alloy cutter of sintex.
Currently, difficult-to-machine material is more and more, PcBN cutter uses proportion in total amount in industrially developed country's tool
It is increasing.PcBN its as cutting difficult-to-machine material main cutting tools for cutting material be cutting technology second leap.In China,
60 % of the total cutter of hard alloy cutter dosage Zhan, high-speed steel account for 30-40 %, and PcBN cutter ratio shared at present is considerably less.
In developed country, the potentiality that Digitized Manufacturing Technology is played using efficient cutter have become common recognition.Annual consumption disappears in lathe
Take 50 % or so.And cutter consumption in China's is only the 20-30 % of lathe consumption, this explanation is cheap inefficient in the consumption of China's cutter
Conventional tool still account for mainstream, lathe function gives full play to far away.And currently, PcBN is contour under the overall background of highly-efficient processing
Effect cutter is just widely received simultaneously gradually to substitute conventional tool by market, and therefore, the country, which will exist, uses metal cutting
The great demand of PcBN.
PcBN sintered body is to rely on sintering bonding independent cubic boron nitride particle under high-temperature and high-pressure conditions, makes
Entire cbn layer is sintered into high-intensitive cBN plycrystalline diamond, is a kind of high performance structural material.PcBN material is because of manufacturer
Method and sintering mechanism are different, and synthesis condition and properties of product have apparent difference, in addition, due to Hall-Petch effect
Deng, nanometer cBN monocrystalline with the reduction of its size, some mechanical properties such as hardness will be improved, while broken compared to micron order micro mist
Particle has advantage, will increase substantially the sintering of nanometer PcBN in wearability and toughness, high temperature resistance etc.
Performance and cutting ability.Based on mostly using micron order monocrystalline broken material to synthesize PcBN at present, to further increasing its performance and depth
There is the sin-tering mechanism and practical application for entering to understand PcBN limitation therefore to answer Efforts To Develop sub-micro, the primary material of nanoscale monocrystalline
The development of sintered body.
This is just badly in need of a kind of preparing wearability, toughness and high temperature resistance etc. advantageous plycrystalline diamond nitridation
The method of boron sintered body.
Summary of the invention
The invention aims to provide a kind of strong operability, the high polycrystalline cubic boron nitride of product qualification rate (PcBN)
Preparation method, sintering condition can be greatly lowered, while can be improved the heat resistance, anti-of polycrystalline cubic boron nitride sintered body
The performances such as impact flexibility.
The object of the present invention is achieved like this, method includes the following steps:
1., with Li3N-hBN is system, uses press synthesis sub-micro, nano cubic boron nitride monocrystalline for primary material, thereafter
Progress touching purification, sorting process, cBN degree of purity reach 99.9 wt %, and homogeneity is good, complete crystal form, corner are not damaged, not
Passivation, and monocrystalline with a high refractive index, selected sub-micro, nanoscale cubic boron nitride average grain diameter >=50 nm;
2., by it is above-mentioned 1. in choose cubic boron nitride monocrystal and sintering aid be put into molybdenum cup after evenly mixing and carry out group
Dress, for molybdenum cup as anti-pollution packaging system, wall thickness is 0.08-0.2 mm, can be sintered uniform mixing material enclosed package
Auxiliary agent uses partial size for big metal, ceramics or the metal ceramic powder for being equal to 20 nanometers, the metal or ceramic powder end be Co,
Ni、Ti、Al、Si、TiN、TiC、B4C、La2O3One of or it is several;
3., by the molybdenum cup 2. assembled by pre-molding, vacuum preheating, pyrophyllite composite block cavity assembling, high pressure
The preparation of sintering procedure completion polycrystalline cubic boron nitride.
Beneficial effects of the present invention are as follows:
1, due to it is of the present invention prepare PcBN method be by select crystalline form homogeneity is good, degree of purity is high sub-micro,
It is tough to have had metal concurrently using metal or ceramic material as sintering aid system for raw material for the primary material of nano cubic boron nitride monocrystalline
Property and ceramics the excellent properties such as heat resistance, heat resistance significantly improves and (is greater than 1300 DEG C);
2, method strong operability of the invention, synthesis condition are greatly lowered, and hammer consumption cost into shape with important to reducing
Realistic meaning.Method of the invention will provide a kind of effective approach for the preparation of superhard cutter.
3, the PcBN product stability synthesized is high, can be suitable for the materials such as chilled cast iron, heat-resisting alloy and hardened steel
Roughing and Precision Machining field.
Detailed description of the invention
Fig. 1 is the pyrophyllite composite block cavity assembling sectional view in present invention process.
Mixed raw material 1, insulating trip 2 with molybdenum cup, graphite heating pipe 3, graphite flake 4, copper sheet 5, conductive steel cap 6, pyrophillite
Composite block 7.
Specific embodiment
Plycrystalline diamond boron nitride sintered body of the invention is to study for a long period of time by inventor, and obtain in conjunction with long-term experiment.It should
Method is to use good sub-micro, nanoscale cubic boron nitride monocrystal for primary material, sintering aid is added, using being pressed into advance
Type, vacuum preheating, high pressure sintering processes synthesize the process of plycrystalline diamond boron nitride sintered body.
This synthetic method is further illustrated below with reference to embodiment:
Embodiment 1:
1) with Li3N-hBN is system, uses press synthesizing submicron cubic boron nitride monocrystal for primary material, followed by
Change touching purification, sorting process, it is excellent by equipment such as laser particle size analyzer, microscope and plasma emission spectrometry instrument
CBN degree of purity is selected to reach 99.9 wt %, homogeneity is good, complete crystal form, corner are not damaged, are not passivated, and with a high refractive index
Monocrystalline, selected submicron order cubic boron nitride average grain diameter are 0.5 um.
2) by above-mentioned steps 1) TiN0.7 grams of 1.3 grams of cubic boron nitride monocrystal choosing and sintering aid put after evenly mixing
Enter and assembled in 14.8 mm molybdenum cups, for molybdenum cup as anti-pollution packaging system, wall thickness is 0.08 mm, can be by uniform mixing material
Expect enclosed package, sintering aid partial size is 20 nanometers.
3) the molybdenum cup of step 2 assembling is passed through into 40MPa pre-molding, is put into and adds after 500 DEG C of purification heat treatment 1h of vacuum
In hot graphite-pipe 3, finally component 4-6 is put into together in pyrophyllite composite block 7, pyrophyllite composite block 7 having a size of 32.5 mm ×
The mm of 32.5 mm × 32.5, synthetic cavity diameter are 18 mm, and 3 internal diameter of graphite-pipe is 16 mm, high 17 mm.Pyrophyllite composite block
Carrying out high temperature and pressure synthesis on cubic hinge press, synthesis condition is 4.5 GPa, 1400 DEG C, after 5 min of sintered heat insulating time
Slowly room temperature is cooled to, the PcBN sintered body of Φ 14 mm × 5 mm is obtained after release.
Embodiment 2:
1) with Li3N-hBN is system, uses press synthesis nano cubic boron nitride monocrystalline for primary material, followed by changes
Touching purification, sorting process, by equipment such as laser particle size analyzer, microscope and plasma emission spectrometry instrument, preferably
CBN degree of purity reaches 99.9 wt %, and homogeneity is good, complete crystal form, corner are not damaged, are not passivated, and list with a high refractive index
Crystalline substance, selected nanoscale cubic boron nitride average grain diameter are 250 nm.
2) by above-mentioned steps 1) TiN0.6 grams of 1.3 grams of cubic boron nitride monocrystal choosing and sintering aid put after evenly mixing
Enter and assembled in 14.8 mm molybdenum cups, for molybdenum cup as anti-pollution packaging system, wall thickness is 0.08 mm, can be by uniform mixing material
Expect enclosed package, sintering aid partial size is 20 nanometers.
3) the molybdenum cup of step 2 assembling is passed through into 40 MPa pre-moldings, is put into and adds after 500 DEG C of purification heat treatment 1h of vacuum
In hot graphite-pipe 3, finally component 4-6 is put into together in pyrophyllite composite block 7, pyrophyllite composite block 7 having a size of 32.5 mm ×
The mm of 32.5 mm × 32.5, synthetic cavity diameter are 18 mm, and 3 internal diameter of graphite-pipe is 16 mm, high 17 mm.Pyrophyllite composite block
High temperature and pressure synthesis is carried out on cubic hinge press, synthesis condition is 5 GPa, 1400 DEG C, slow after 5 min of sintered heat insulating time
Room temperature is cooled to, the PcBN sintered body of Φ 14 mm × 5 mm is obtained after release.
Embodiment 3:
1) with Li3N-hBN is system, uses press synthesizing submicron cubic boron nitride monocrystal for primary material, followed by
Change touching purification, sorting process, it is excellent by equipment such as laser particle size analyzer, microscope and plasma emission spectrometry instrument
CBN degree of purity is selected to reach 99.9 wt %, homogeneity is good, complete crystal form, corner are not damaged, are not passivated, and with a high refractive index
Monocrystalline, selected submicron order cubic boron nitride average grain diameter are 1 μm.
2) by above-mentioned steps 1) 1.9 grams of cubic boron nitride monocrystal choosing and 0.06 gram of sintering aid Al, 0.02 gram of Co,
B40.02 gram of C is put into 14.8 mm molybdenum cups after evenly mixing and is assembled, and molybdenum cup is as anti-pollution packaging system, wall thickness
Uniform mixing material enclosed package, sintering aid average grain diameter can be 1 μm by 0.08 mm.
3) the molybdenum cup of step 2 assembling is passed through into 40 MPa pre-moldings, is put into and adds after 500 DEG C of purification heat treatment 1h of vacuum
In hot graphite-pipe 3, finally component 4-6 is put into together in pyrophyllite composite block 7, pyrophyllite composite block 7 having a size of 32.5 mm ×
The mm of 32.5 mm × 32.5, synthetic cavity diameter are 18 mm, and 3 internal diameter of graphite-pipe is 16 mm, high 17 mm.Pyrophyllite composite block
Carrying out high temperature and pressure synthesis on cubic hinge press, synthesis condition is 5.5 GPa, 1450 DEG C, after 5 min of sintered heat insulating time
Slowly room temperature is cooled to, the PcBN sintered body of Φ 14 mm × 5 mm is obtained after release.