CN107602123A - A kind of polycrystalline diamond superhard material and preparation method thereof - Google Patents
A kind of polycrystalline diamond superhard material and preparation method thereof Download PDFInfo
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- CN107602123A CN107602123A CN201710703496.2A CN201710703496A CN107602123A CN 107602123 A CN107602123 A CN 107602123A CN 201710703496 A CN201710703496 A CN 201710703496A CN 107602123 A CN107602123 A CN 107602123A
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Abstract
It is more particularly to a kind of using polycrystalline cubic boron nitride as polycrystalline diamond superhard material of bonding agent and preparation method thereof the invention belongs to technical field of superhard material.The superhard material is combined into by the cubic monocrystalline boron nitride crystal grain and single-crystal diamond crystal grain of submicron order, and wherein cubic monocrystalline boron nitride crystal grain forms polycrystalline cubic boron nitride in sintering process, and diamond particles are bonded together as bonding agent.A kind of polycrystalline diamond superhard material using polycrystalline cubic boron nitride as bonding agent of the invention, has the inertia of diamond high rigidity and cubic boron nitride to iron family element concurrently；Its preparation method is simple, and the temperature and pressure scope of demand is more slightly higher than the product of routine, is reached by suitably adjusting assembling scheme can, is adapted to industrialized production.
Description
Technical field
The invention belongs to technical field of superhard material, more particularly to a kind of glomerocryst using polycrystalline cubic boron nitride as bonding agent
Diamond superhard material and preparation method thereof.
Background technology
Polycrystalline diamond material is a kind of superhard material for having good wearability and hardness, in commercial Application generally
By as cutting element and wear resistant tools, and applied in underground mining and DRILLING APPLICATION.
In order to synthesize polycrystalline diamond material, it is necessary to which diamond particles are sintered under high-temperature and high-pressure conditions, with
Obtain the material of superhard synneusis texture.Need catalyst material being added to the mixture of diamond particles before sintering
In, to promote to form polycrystalline diamond structure when HTHP sinters.The selection of catalyst is usually the periodic table of elements
VIII in metal, including iron, cobalt, nickel or their alloy, commonly referred to as metallic catalyst.
In some applications, polycrystalline diamond material is such as needed to have improved heat steady in for abrasion or cutting operation
It is qualitative.And the polycrystalline diamond material being conventionally synthesized exist one it is known that the problem of, they are easy under the high temperature conditions
Thermal degradation.This is due to thermal expansion systems different between the Metal catalyst materials in polycrystalline diamond material and diamond crystalses
Caused by number.This different thermal coefficient of expansion when relatively low temperature is such as 400 DEG C if it is existing, and thermal stress can be induced, entered
And the intergranular for destroying diamond combines, and crack is ultimately resulted in, destroyed polycrystalline diamond material.In addition, with temperature
Continuous rise, metallic catalyst can also cause diamond that bad phase transformation occurs（Carbon monoxide, carbon dioxide can be such as converted into
Or graphite）So as to influence the heat endurance of polycrystalline diamond material so that the use of polycrystalline diamond material in actual applications
Temperature limiting is at about 750 DEG C.
The content of the invention
It is an object of the invention to provide it is a kind of using polycrystalline cubic boron nitride as the polycrystalline diamond superhard material of bonding agent and
Its preparation method.
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows：
A kind of polycrystalline diamond superhard material, the superhard material are golden by the cubic monocrystalline boron nitride crystal grain and monocrystalline of submicron order
Hard rock crystal grain is combined into, and wherein cubic monocrystalline boron nitride crystal grain forms polycrystalline cubic boron nitride, and conduct in sintering process
Diamond particles are bonded together by bonding agent.
The mass ratio of polycrystalline cubic boron nitride not higher than 50% and is not zero in the polycrystalline diamond superhard material, its
Remaining is diamond.
The polycrystalline diamond superhard material is preferably prepared in accordance with the following methods：Only with cubic boron nitride monocrystal powder and gold
Hard rock monocrystal is raw material, be sufficiently mixed simultaneously pre-molding by the two, carries out heat treatment removal of impurities afterwards, carried out after removal of impurities
Sintering, processing, produce the polycrystalline diamond superhard material；Wherein, cubic boron nitride monocrystal powder and diamond single crystal powder
Mass ratio be 0-50:100-50, wherein, cubic boron nitride monocrystal content of powder is not 0, and cubic boron nitride monocrystal powder
It is not more than 1 micron with the particle diameter of diamond single crystal powder.
Raw material be sufficiently mixed and is placed into pre-molding in canister, described canister be zirconium, niobium, molybdenum,
Tantalum or its alloy are made.
The temperature range of the heat treatment removal of impurities is 600 DEG C~1200 DEG C.
Sintering is through superhigh temperature ultra-high pressure sintering and to keep the powder stock after removal of impurities the regular hour after removal of impurities, is sintered
Pressure limit is 6~15GPa, and sintering temperature is 1500 DEG C~2300 DEG C, and the heat-insulation pressure keeping time is 180s~1200s.
During sintering, sintering pressure, then the heating with 15 DEG C~30 DEG C/s are first boosted to speed 0.1GPa~1GPa/min
Speed is rapidly heated carries out high temperature sintering to sintering temperature, and with 10 DEG C~30 DEG C/s rate of temperature fall room temperature is down to after to be sintered,
Normal pressure is down to from high pressure with 0.1GPa~0.5GPa/min rate of pressure reduction.
Can according to be actually needed adjustment wherein as bonding agent cubic boron nitride ratio, be selectively achieved with this
Have the high rigidity or cubic boron nitride heat endurance and the inertia with iron family element of diamond concurrently.Compacting can be adjusted as needed
Pressure and sintering temperature adjust its hardness and toughness.
Specifically, the preparation method of the polycrystalline diamond superhard material, step are as follows：
1）Raw material prepares：Using the cubic boron nitride monocrystal powder and diamond single crystal powder of submicron order as raw material, the two is pressed
It is sufficiently mixed, dried, is fitted into canister according to ratio, and pre-molding is carried out via mould；
2）Removal of impurities：The powder stock of pre-molding is heat-treated to remove impurity contained in powder stock；
3）Hyperpressure hyperthermal sinters：Powder stock after thermally treated removal of impurities through superhigh temperature ultra-high pressure sintering and is kept certain
Time, then removed through decrease temperature and pressure can obtain after coated thing outside it bulk using polycrystalline cubic boron nitride as combination
The sintered body of the polycrystalline diamond superhard material of agent；
4）By 3）Obtained block sintered body is ground, polished and the polycrystalline diamond superhard material is produced after cleaning.
Wherein, the bulk material obtained（Diameter is more than 10mm）Various required products can be processed into according to being actually needed.
The present invention relates to a kind of using polycrystalline cubic boron nitride as the polycrystalline diamond superhard material of bonding agent and its preparation side
Method.Using the mixture of the cubic boron nitride of submicron order and diamond particles as raw material, cube nitridation under high-temperature and high-pressure conditions
Boron crystal grain combines to form polycrystalline cubic boron nitride, while with the formation of polycrystalline cubic boron nitride, using polycrystalline cubic boron nitride as
Bonding agent promotes also to be formed to be bonded between diamond crystalses and crystal grain to be closely combined together, and synthesizes and is nitrogenized with polycrystalline cubic
Boron is the polycrystalline diamond superhard material of bonding agent.The polycrystalline diamond is stood with the glomerocryst formed in HTHP sintering process
Square boron nitride is bonding agent, the polycrystalline diamond superhard material without any other metal or non-metallic catalyst.
The polycrystalline diamond superhard material using polycrystalline cubic boron nitride as bonding agent that the present invention obtains, wherein diamond with
The performance complement of cubic boron nitride, have the inertia of diamond high rigidity and cubic boron nitride to iron family element concurrently.
The present invention compared with prior art, has the following advantages that：
A kind of polycrystalline diamond superhard material using polycrystalline cubic boron nitride as bonding agent of the invention, have concurrently diamond high rigidity and
Inertia of the cubic boron nitride to iron family element；Its preparation method is simple, and the temperature and pressure scope of demand is omited than the product of routine
Height, reached by suitably adjusting assembling scheme can, be adapted to industrialized production.
Brief description of the drawings
Fig. 1 is the polycrystalline diamond superhard material pictorial diagram that embodiment 1 is prepared；
Fig. 2 is the surface scan electron microscope for the polycrystalline diamond superhard material that embodiment 1 is prepared；
Fig. 3 is the profile scanning electron microscope for the polycrystalline diamond superhard material that embodiment 1 is prepared；
Fig. 4 is the surface scan electron microscope for the polycrystalline diamond superhard material that embodiment 2 is prepared；
Fig. 5 is the profile scanning electron microscope for the polycrystalline diamond superhard material that embodiment 2 is prepared；
Fig. 6 is the surface scan electron microscope for the polycrystalline diamond superhard material that embodiment 3 is prepared；
Fig. 7 is the profile scanning electron microscope for the polycrystalline diamond superhard material that embodiment 3 is prepared；
Fig. 8 is the scanning electron microscope (SEM) photograph on the polycrystalline diamond surface without bonding agent addition sintering；
Fig. 9 is the scanning electron microscope (SEM) photograph on the polycrystalline cubic boron nitride surface without bonding agent addition sintering.
Embodiment
Technical scheme, but protection scope of the present invention not limited to this are illustrated with specific embodiment below：
6 × 25MN of model of cubic hinge press described in following examples；Described cubic boron nitride monocrystal powder purity>
99.9%, described diamond single crystal powder purity>99.9%.
Embodiment 1
A kind of polycrystalline diamond superhard material, technique acquisition is prepared by the following procedure：
（1）Raw material prepares
By the cubic boron nitride monocrystal powder and diamond single crystal powder that average grain diameter is 1 micron, it is according to mass ratio by the two
10：90 ratio is mixed, and being subject to suitable alcohols with grinding rod in mortar is lightly ground mixing, after mixing about 4 hours
Powder is dried after alcohol volatilization, mixed raw material 1g is weighed, load weighted material powder is fitted into metal molybdenum cup, so
Metal molybdenum cup is put into mould afterwards and pre-molding is carried out on powder compressing machine, pressure applied 8MPa, during pressurize
Between be 300s, the molybdenum cup size after precompressed is Φ 13*5.0/mm；
（2）Removal of impurities
Will（1）In the metal molybdenum cup equipped with powder stock of pre-molding be heat-treated at 900 DEG C, to remove powder stock
In contained impurity；
（3）Hyperpressure hyperthermal sinters
The metal molybdenum cup equipped with powder stock after thermally treated removal of impurities is positioned on 6 × 25MN cubic hinge press, with
Pressure is risen to 10GPa by 0.2GPa/min speed, then pressurize, while temperature is risen into 1900 DEG C with 15 DEG C/s speed,
And 1200s is incubated, and after terminating, room temperature is cooled the temperature to 10 DEG C/s speed respectively, will with 0.1GPa/min speed
Pressure is down to normal pressure.Then remove sample outside coated thing after i.e. can obtain bulk using polycrystalline cubic boron nitride as bonding agent
Polycrystalline diamond superhard material sintered body, sintered body surface sintering is uniform, no hole point, crackle, falls the open defects such as side.
（4）Will（3）Obtained sintered body is ground, polished and the polycrystalline diamond superhard material is produced after cleaning.
Fig. 1 is the pictorial diagram for the composite polycrystal-diamond that the present embodiment is prepared；Fig. 2 and Fig. 3 is respectively glomerocryst Buddha's warrior attendant
The scanning electron microscope (SEM) photograph of stone surface of ultra-hard material and section, multiplication factor be 10000 times, as can be seen from the figure diamond particles with
Bonding is formed between cubic boron nitride particle.
Embodiment 2
（1）Raw material prepares
By the cubic boron nitride monocrystal powder and diamond single crystal powder that average grain diameter is 0.5 micron, the two is incited somebody to action according to mass ratio
For 20：80 ratio is mixed, and being subject to suitable alcohols with grinding rod in mortar is lightly ground mixing, mixing about 4 hours it
After powder dried after alcohol volatilization, weigh mixed raw material 1g, load weighted material powder be fitted into metal molybdenum cup,
Then metal molybdenum cup is put into mould and pre-molding, pressure applied 8MPa, pressurize is carried out on powder compressing machine
Time is 300s, and the molybdenum cup size after precompressed is Φ 13*5.0/mm；
（2）Removal of impurities
Will（1）In the metal molybdenum cup equipped with powder stock of pre-molding be heat-treated at 1000 DEG C, to remove powder original
Contained impurity in material；
（3）Hyperpressure hyperthermal sinters
The metal molybdenum cup equipped with powder stock after thermally treated removal of impurities is positioned on 6 × 25MN cubic hinge press, with
Pressure is risen to 10GPa by 0.2GPa/min speed, then pressurize, while temperature is risen into 2000 DEG C with 15 DEG C/s speed,
And 1000s is incubated, and after terminating, room temperature is cooled the temperature to 10 DEG C/s speed respectively, will with 0.1GPa/min speed
Pressure is down to normal pressure.Then remove sample outside coated thing after i.e. can obtain bulk using polycrystalline cubic boron nitride as bonding agent
Polycrystalline diamond superhard material sintered body, sintered body surface sintering is uniform, no hole point, crackle, falls the open defects such as side.
（4）Will（3）Obtained sintered body is ground, polished and the polycrystalline diamond superhard material is produced after cleaning.
Fig. 4 and Fig. 5 is respectively the scanning of the polycrystalline diamond composite superhard material surface that the present embodiment is prepared and section
Electron microscope, multiplication factor are 10000 times, and key is as can be seen from the figure formed between diamond particles and cubic boron nitride particle
Close.
Embodiment 3
（1）Raw material prepares
By the cubic boron nitride monocrystal powder that average grain diameter is 1 micron and the diamond single crystal powder that average grain diameter is 0.5 micron,
The two is 40 according to mass ratio：60 ratio is mixed, and being subject to suitable alcohols with grinding rod in mortar is lightly ground mixing,
Mixing dried powder after alcohol volatilization after about 4 hours, weighs mixed raw material 1g, load weighted material powder is filled
Enter in metal molybdenum cup, then metal molybdenum cup is put into mould and pre-molding, the pressure applied are carried out on powder compressing machine
Power is 8MPa, dwell time 300s, and the molybdenum cup size after precompressed is Φ 13*5.0/mm；
（2）Removal of impurities
Will（1）In the metal molybdenum cup equipped with powder stock of pre-molding be heat-treated at 1000 DEG C, to remove powder original
Contained impurity in material；
（3）Hyperpressure hyperthermal sinters
The metal molybdenum cup equipped with powder stock after thermally treated removal of impurities is positioned on 6 × 25MN cubic hinge press, with
Pressure is risen to 10GPa by 0.2GPa/min speed, then pressurize, while temperature is risen into 2200 DEG C with 15 DEG C/s speed,
And 1000s is incubated, and after terminating, room temperature is cooled the temperature to 10 DEG C/s speed respectively, will with 0.1GPa/min speed
Pressure is down to normal pressure.Then remove sample outside coated thing after i.e. can obtain bulk using polycrystalline cubic boron nitride as bonding agent
Polycrystalline diamond superhard material sintered body, sintered body surface sintering is uniform, no hole point, crackle, falls the open defects such as side.
（4）Will（3）Obtained sintered body is ground, polished and the polycrystalline diamond superhard material is produced after cleaning.
Fig. 6 and Fig. 7 is respectively the surface of polycrystalline diamond composite superhard material and sweeping for section that the present embodiment is prepared
Electron microscope is retouched, multiplication factor is 10000 times, and key is as can be seen from the figure formed between diamond particles and cubic boron nitride particle
Close, diamond crystalses are closely combined together using the polycrystalline cubic boron nitride after sintering as bonding agent.
Comparative example
Because the presence of bonding agent can influence the property of polycrystalline diamond and polycrystalline cubic boron nitride, same as Example 1
Under reaction condition, the polycrystalline diamond and polycrystalline cubic boron nitride of no bonding agent addition, all complete nothing of the slice, thin piece synthesized are synthesized
Open defect.
Wherein, Fig. 8 is the scanning electron microscope (SEM) photograph on the polycrystalline diamond surface of the pure submicron order without bonding agent addition, from figure
As can be seen that simply pressing together by machinery, crystal grain are not combined together between diamond crystalses；
Fig. 9 is the scanning electron microscope (SEM) photograph on the polycrystalline cubic boron nitride surface of the pure submicron order without bonding agent addition, can be with from figure
Find out, be closely combined together between cubic boron nitride crystal grain and crystal grain, bonding is formed between crystal grain.
Claims (8)
1. a kind of polycrystalline diamond superhard material, it is characterised in that the superhard material is nitrogenized by the cubic monocrystalline of submicron order
Boron crystal grain and single-crystal diamond crystal grain are combined into, and wherein cubic monocrystalline boron nitride crystal grain forms polycrystalline cubic in sintering process
Boron nitride, and diamond particles are bonded together as bonding agent.
2. polycrystalline diamond superhard material as claimed in claim 1, it is characterised in that in the polycrystalline diamond superhard material
The mass ratio of polycrystalline cubic boron nitride is not higher than 50% and is not zero, and remaining is diamond.
3. the preparation method of polycrystalline diamond superhard material as claimed in claim 1 or 2, it is characterised in that only nitrogenized with cube
Boron single crystal powder and diamond single crystal powder are raw material, be sufficiently mixed simultaneously pre-molding by the two, are heat-treated afterwards
Removal of impurities, is sintered after removal of impurities, handles, produce the polycrystalline diamond superhard material；Wherein, cubic boron nitride monocrystal powder with
The mass ratio of diamond single crystal powder is 0-50:100-50, wherein, cubic boron nitride monocrystal content of powder is not 0, and cube
The particle diameter of boron nitride single crystal powder and diamond single crystal powder is not more than 1 micron.
4. the preparation method of polycrystalline diamond superhard material as claimed in claim 3, it is characterised in that after removal of impurities sintering be by
Powder stock after removal of impurities through superhigh temperature ultra-high pressure sintering and is kept for the regular hour, and sintering pressure scope is 6~15GPa, is burnt
Junction temperature is 1500 DEG C~2300 DEG C, and the heat-insulation pressure keeping time is 180s~1200s.
5. the preparation method of polycrystalline diamond superhard material as claimed in claim 4, it is characterised in that during sintering, first with speed
Rate 0.1GPa~1GPa/min boosts to sintering pressure, then is rapidly heated with 15 DEG C~30 DEG C/s heating rate to sintering temperature
High temperature sintering is carried out, normal temperature is down to 10 DEG C~30 DEG C/s rate of temperature fall after to be sintered, with 0.1GPa~0.5GPa/min's
Rate of pressure reduction is down to normal pressure from high pressure.
6. the preparation method of polycrystalline diamond superhard material as claimed in claim 3, it is characterised in that the heat treatment removal of impurities
Temperature range be 600 DEG C~1200 DEG C.
7. the preparation method of polycrystalline diamond superhard material as claimed in claim 3, it is characterised in that carry out raw material abundant
Mixing is placed into pre-molding in canister, and described canister is made up of zirconium, niobium, molybdenum, tantalum or its alloy.
8. the preparation method of any polycrystalline diamond superhard materials of claim 3-7, it is characterised in that step is as follows：
1）Raw material prepares：Using the cubic boron nitride monocrystal powder and diamond single crystal powder of submicron order as raw material, the two is pressed
It is sufficiently mixed, dried, is fitted into canister according to ratio, and pre-molding is carried out via mould；
2）Removal of impurities：The powder stock of pre-molding is heat-treated to remove impurity contained in powder stock；
3）Hyperpressure hyperthermal sinters：Powder stock after thermally treated removal of impurities through superhigh temperature ultra-high pressure sintering and is kept certain
Time, then removed through decrease temperature and pressure can obtain after coated thing outside it bulk using polycrystalline cubic boron nitride as combination
The sintered body of the polycrystalline diamond superhard material of agent；
4）By 3）Obtained block sintered body is ground, polished and the polycrystalline diamond superhard material is produced after cleaning.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109016197A (en) * | 2018-07-18 | 2018-12-18 | 郑州磨料磨具磨削研究所有限公司 | A kind of novel electroplating diamond fretsaw |
| CN111185858A (en) * | 2020-02-28 | 2020-05-22 | 北京道天技术研发有限公司 | Method for processing high-precision superhard abrasive material integral cutting grinding wheel |
| CN111635231A (en) * | 2020-06-05 | 2020-09-08 | 四川大学 | Preparation method of polycrystalline diamond transparent ceramic |
| CN112678817A (en) * | 2021-01-08 | 2021-04-20 | 南方科技大学 | Preparation method of millimeter polycrystalline diamond |
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| CN111635231A (en) * | 2020-06-05 | 2020-09-08 | 四川大学 | Preparation method of polycrystalline diamond transparent ceramic |
| CN111635231B (en) * | 2020-06-05 | 2021-12-17 | 四川大学 | Preparation method of polycrystalline diamond transparent ceramic |
| CN112678817A (en) * | 2021-01-08 | 2021-04-20 | 南方科技大学 | Preparation method of millimeter polycrystalline diamond |
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