CN105859300A - Preparation method of diamond-cubic boron nitride-boron carbide composite material - Google Patents
Preparation method of diamond-cubic boron nitride-boron carbide composite material Download PDFInfo
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Abstract
The invention relates to a preparation method of a diamond-cubic boron nitride-boron carbide composite material. With a high-temperature high-pressure sintering technology, the method comprises the following specific step: under high-temperature high-pressure conditions (HPHT, 5-6 GPa and 1,350-1,500 DEG C), preparing the diamond-cubic boron nitride-boron carbide composite material by adopting high-purity powder (Co, Ti, Al, Si and the like) with a particle size of 20nm-20mu m as a sintering binder and the powder of diamond, cubic boron nitride and boron carbide (B4C) different in content proportion as raw materials. In the method for preparing a high-performance structural material, provided by the invention, through the sintering combination technology of the diamond, cBN and B4C and the binder, the sintered phases such as diamond, boron nitride, alloy solid solution and metal ceramic are formed in the composite material; and the sintered body has a uniform and dense structure and relatively high heat resistance. The method has high operability; and the synthesized product has high stability, can fill in the blank between the diamond and the boron nitride composite material, and provides a novel composite material suitable for the cutting of hard materials.
Description
Technical field
The invention belongs to cutting tool superhard material and manufacture field, a kind of diamond, cubic boron nitride, carbon
Change the preparation method of gem grade diamond-cubic boron nitride-boron carbide composite material that Boron contents is controlled, heat stability is high.
Background technology
Modern mechanical process technology just develops rapidly towards high accuracy, high efficiency, flexibility and automation direction, novel skill
Art equipment and the most excellent new material application of Digit Control Machine Tool, machining center and performance are increasingly extensive, particularly to cutter material
The requirement of material is more and more higher.Superhard material diamond, cubic boron nitride (cBN) and boron carbide (B4And composite (Buddha's warrior attendant C)
Stone, polycrystalline cubic boron nitride and composite sheet, boron carbide-based ceramic metal etc.) play in modern manufacturing industry with the performance of its excellence
Important effect, is widely used in the fields such as oil, geology, aviation, machining, metallurgy, electronics, superhard material industry
As one of national seven great strategy new industries, it is thus achieved that policy is supported energetically.
It has been generally acknowledged that preferable superhard material system should meet following key element, i.e. high rigidity, high-fracture toughness, height
Heat stability, high chemical stability.In known superhard material, diamond, cBN and B4C is most widely used at present, but
It is that they there is also self deficiency and restriction.Diamond has the hardness (60-120 GPa) of superelevation, but its heat stability and
Chemical inertness is poor, is at high temperature oxidized easily (680 DEG C), produces chemical reaction with iron containing alloy and makes it at ferrous material
Processing is very restricted.Cubic boron nitride has outstanding thermostability (1100 DEG C) and a chemical inertness, and its hardness
(50-72 GPa) only has 1/2nd of diamond.There is the B of diamond structure4C, hardness is only second to diamond and cBN(Mohs
Hardness 9.36, microhardness 55-67 GPa), have and be bordering on constant high temperature hardness (> 30 GPa), but, B4C fracture toughness
Relatively low (2.5 MPa m1/2), oxidation resistance poor (in atmosphere 600 DEG C time aoxidize, 900 DEG C of rapid oxidation), to gold
The less stable (easy and metal reaction generates metal boride) belonged to, constrains its actual application.Buddha's warrior attendant of the prior art
Stone and cubic boron nitride alloy or solid solution composite material have certain advantage in terms of hardness, the general relatively Buddha's warrior attendant of its thermostability
Stone is high (800 DEG C), but these performance indications are relatively low, and as main application indexes, preparation has the compound of high-fire resistance
Superhard material has great realistic meaning.
Thus, combination property can make up diamond, cBN and B4C limits, and can realize obtaining high efficiency, high stability, height
Precision, long-life novel superhard material is an important development direction of superhard material manufacturing.
Summary of the invention
It is an object of the invention to provide a kind of workable, that heat stability is high diamond-cubic boron nitride-carbonization
The preparation method of boron composite, by effectively regulating diamond, boron nitride, boron carbide and the content proportioning of binding agent, changes
Kind Composite Sintering soma structure and compactness, can be effectively improved the heat stability of material simultaneously, being combined of preparation
Material through cut, can weld and sharpen and be fabricated to the cutter of the different angles trade mark according to tool demands.
The object of the present invention is achieved like this:
The preparation method of this diamond-cubic boron nitride-boron carbide composite material, comprises the following steps:
1., diamond, cubic boron nitride, boron carbide powder are chosen as raw material,
2., by above-mentioned 1. in the mixed-powder chosen uniformly mix after put in molybdenum cup and be packaged,
3., the molybdenum cup that 2. assembles is assembled through pre-molding, vacuum preheating, pyrophyllite composite block cavity, high-pressure sinter
Program completes the preparation of composite；
This composite material and preparation method thereof step 1. in also include binder material.
Beneficial effects of the present invention is as follows:
1, the method that the present invention uses can be by regulation diamond, cBN, B4C and the proportioning of binding agent, it is thus achieved that a kind of novel multiple
Condensation material, synthesizes reproducible, workable.Combination property can make up diamond, cBN and B4C limits, and can realize obtaining
High efficiency, high stability, in high precision, long-life novel superhard material.
2, of the present invention preparing super-hard compound material method, product stability of its synthesis is high, shape in composite
Becoming the sintering phases such as diamond, boron nitride, Alloy solid solution, ceramic metal, its tissue of sintered body even structure is fine and close, has higher
Thermostability (1400 DEG C).It is applicable to the machining field of the materials such as chilled cast iron, heat-resisting alloy and hardened steel.
Accompanying drawing explanation
Fig. 1 is that the pyrophyllite composite block cavity in the present invention assembles sectional view.
Label in Fig. 1: mixed-powder 1, molybdenum cup 2, heating graphite-pipe 3, insulating trip 4, insulation graphite flake 5, conductive metal sheet
6, conductive steel cap 7, pyrophyllite composite block 8.
Detailed description of the invention
The application provides the preparation method of a kind of diamond-cubic boron nitride-boron carbide composite material, this composite energy
Enough make up diamond, cBN and B4The restriction of tri-kinds of material properties of C, can realize obtaining high efficiency, high stability, in high precision, long-lived
The novel superhard material of life.
Composite material and preparation method thereof comprises the following steps:
1. diamond, cubic boron nitride, boron carbide powder, are chosen as raw material；Diamond, cubic boron nitride, boron carbide powder
End requires that purified treatment falls impurity, mean diameter 20 nm-20 μm, and diamond dust weight portion is 10-80 part, cubic boron nitride
Powder weight part is 20-80 part, and boron carbide powder weight portion is 5-20 part.Also include binder material, described binding agent powder
End need to be compound or simple substance according to actual processing object, Co, Ti, Al, Si, SiC therein one or more, particle diameter is 20
Nm-20 μm, adhesive powder weight portion is 0-50 part.
2., by above-mentioned 1. in the mixed-powder chosen uniformly mix after put in molybdenum cup and be packaged；
3., the molybdenum cup that 2. assembles is assembled through pre-molding, vacuum preheating, pyrophyllite composite block cavity, high-pressure sinter
Program completes the preparation of composite.Pre-molding, vacuum preheating, pyrophyllite composite block cavity assemble, high-pressure sinter mistake
Journey is that after 5-20MPa pre-molding, 500 DEG C of heat treatment 0.5-1h of vacuum, the molybdenum cup 2. assembled is put into graphite heating pipe box
All parts are finally put in pyrophyllite composite block and are assembled, carry out High Temperature High Pressure synthesis on cubic hinge press by part in the lump, close
One-tenth condition is 5～6GPa, 1350～1500 DEG C, and the sintered heat insulating time is 3-10min.
Embodiment 1
As shown in Figure 1: choose the diamond dust of particle diameter 0.5 μm, 0.25 μm cBN powder, the B of 3 μm4C, the Si powder of 1 μm is made
For raw and auxiliary material, weight portion is respectively as follows: 15 parts, 70 parts, 10 parts, 5 parts.By powder mixing 2h to uniformly, by 1g mixed-powder 1 warp
After crossing 5MPa pre-molding, putting in the molybdenum cup 2 of internal diameter 14.8mm, 500 DEG C of vacuum purifies heat treatment 0.5h, is then placed in heating
In graphite-pipe 3, finally by assembling parts insulating trip 4, insulation graphite flake 5, conductive metal sheet 6, that leaf put in the lump by conductive steel cap 7 is cured
In stone composite block 8, pyrophyllite composite block a size of 32.5mm × 32.5mm × 32.5mm, a diameter of 18mm of synthetic cavity, graphite
Pipe 7 internal diameter is 16mm, high 17mm.At cubic hinge press (CS-, 6 × 14000 KN) on carry out High Temperature High Pressure synthesis, synthesize bar
Part is 5 GPa, 1400 DEG C, cools to room temperature slowly after sintered heat insulating time 3min, obtains the superhard of Φ 14mm × 3mm after release
Composite.
Embodiment 2
As shown in Figure 1: choose the diamond dust of particle diameter 0.5 μm, 0.25 μm cBN powder, the B of 3 μm4C micropowder is as former material
Material, weight portion is respectively as follows: 60,20,20.By powder mixing 2h to uniformly, put in the molybdenum cup 2 of internal diameter 14.8mm, 2g is mixed
Powder 1, after 5MPa pre-molding, is put in heating graphite-pipe 3, finally by assembling parts after 500 DEG C of heat treatment 0.5h of vacuum
Insulating trip 4, insulation graphite flake 5, conductive metal sheet 6, conductive steel cap 7 are put in pyrophyllite composite block 8 in the lump, pyrophyllite composite block
A size of 32.5mm × 32.5mm × 32.5mm, a diameter of 18mm of synthetic cavity, graphite-pipe 7 internal diameter is 16mm, high 17mm.Six
Face high pressure apparatus (CS-, 6 × 14000 KN) on carry out High Temperature High Pressure synthesis, synthesis condition is 5 GPa, 1400 DEG C, sintering protect
Slowly cool to room temperature after temperature time 5min, after release, obtain the composite of Φ 14mm × 5.5mm.
Claims (6)
1. the preparation method of diamond-cubic boron nitride-boron carbide composite material, it is characterised in that: this composite system
Preparation Method comprises the following steps:
1. diamond, cubic boron nitride, boron carbide powder, are chosen as raw material；
2., by above-mentioned 1. in the mixed-powder chosen uniformly mix after put in molybdenum cup and be packaged；
3., the molybdenum cup that 2. assembles is assembled through pre-molding, vacuum preheating, pyrophyllite composite block cavity, high-pressure sinter
Program completes the preparation of composite.
The preparation method of a kind of diamond-cubic boron nitride-boron carbide composite material the most according to claim 1, it is special
Levy and be: this composite material and preparation method thereof step 1. in also include binder material.
The preparation method of a kind of diamond-cubic boron nitride-boron carbide composite material the most according to claim 1, it is special
Levy and be: described diamond, cubic boron nitride, boron carbide powder require that purified treatment falls impurity, mean diameter 20 nm-20 μ
M, diamond dust weight portion is 10-80 part, and cubic boron nitride powder weight portion is 20-80 part, and boron carbide powder weight portion is
5-20 part.
The preparation method of a kind of diamond-cubic boron nitride-boron carbide composite material the most according to claim 2, it is special
Levy and be: described binding agent be Co, Ti, Al, Si, SiC therein one or more, particle diameter is 20 nm-20 μm, binding agent
Powder weight part is 0-50 part.
5. according to the preparation side of a kind of diamond-cubic boron nitride-boron carbide composite material described in claim 1 or 3 or 4
Method, it is characterised in that: this composite material and preparation method thereof step 3. pre-molding, vacuum preheating, pyrophyllite composite block cavity
Assemble, high pressure sintering processes be by the molybdenum cup that 2. assembles after 5-20MPa pre-molding, 500 DEG C of heat treatment 0.5-1h of vacuum
Put into graphite heating pipe box part, finally all parts are put in the lump in pyrophyllite composite block and assemble, enterprising at cubic hinge press
Row High Temperature High Pressure synthesizes, and synthesis condition is 5～6GPa, 1350～1500 DEG C, and the sintered heat insulating time is 3-10min.
The preparation method of a kind of diamond-cubic boron nitride-boron carbide composite material the most according to claim 5, it is special
Levy and be: choose the diamond dust 15 parts of particle diameter 0.5 μm, 0.25 70 parts of μm cBN powder, the B of 3 μm4C10 part, 1 μm
5 parts of Si powder is as raw and auxiliary material；By powder mixing 2h to uniformly, 1g mixed-powder (1) is put into the molybdenum cup of internal diameter 14.8mm
(2) in, mixed-powder (1) is after 5MPa pre-molding, and 500 DEG C of vacuum purifies heat treatment 0.5h, is then placed in heating graphite
In pipe (3), finally by assembling parts insulating trip (4), insulation graphite flake (5), conductive metal sheet (6), conductive steel cap (7), in the lump
Putting in pyrophyllite composite block (8), pyrophyllite composite block a size of 32.5mm × 32.5mm × 32.5mm, synthetic cavity is a diameter of
18mm, graphite-pipe 7 internal diameter is 16mm, high 17mm；At cubic hinge press (CS-, 6 × 14000 KN) on carry out High Temperature High Pressure conjunction
Become, synthesis condition is 5 GPa, 1400 DEG C, cools to room temperature slowly after sintered heat insulating time 3min, obtain after release Φ 14mm ×
The super-hard compound material of 3mm.
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Cited By (10)
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| CN106699190A (en) * | 2017-01-03 | 2017-05-24 | 吉林师范大学 | Method for preparing polycrystalline sintered body by using cubic boron nitride single crystal bioblast as initial raw material |
| CN107602123A (en) * | 2017-08-16 | 2018-01-19 | 河南四方达超硬材料股份有限公司 | A kind of polycrystalline diamond superhard material and preparation method thereof |
| CN109079145A (en) * | 2018-08-30 | 2018-12-25 | 中南钻石有限公司 | A kind of composite polycrystal-diamond Synthetic block and its method for synthesizing composite polycrystal-diamond |
| CN110785504A (en) * | 2017-08-24 | 2020-02-11 | 住友电气工业株式会社 | Composite sintered body |
| CN111592356A (en) * | 2020-06-09 | 2020-08-28 | 欧阳晓平 | Polycrystal SiC-B4C-diamond three-layer composite material and preparation method thereof |
| CN111592360A (en) * | 2020-06-09 | 2020-08-28 | 欧阳晓平 | Polycrystal B4C-diamond double-layer composite material and preparation method thereof |
| CN111960811A (en) * | 2020-08-27 | 2020-11-20 | 广东工业大学 | DLP (digital light processing) forming method for diamond/cubic boron nitride-ceramic composite material |
| CN112159231A (en) * | 2020-10-09 | 2021-01-01 | 武汉理工大学 | Rapid preparation method of super-hard light diamond-B4C-SiC ternary composite ceramic |
| CN113200748A (en) * | 2021-04-19 | 2021-08-03 | 郑州博特硬质材料有限公司 | Boron nitride-diamond-zirconia hybrid composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106180733A (en) * | 2016-08-31 | 2016-12-07 | 开封贝斯科超硬材料有限公司 | A kind of processing method of superhard material knurling tool |
| CN106180733B (en) * | 2016-08-31 | 2017-11-17 | 开封贝斯科超硬材料有限公司 | A kind of processing method of superhard material knurling tool |
| CN106699190A (en) * | 2017-01-03 | 2017-05-24 | 吉林师范大学 | Method for preparing polycrystalline sintered body by using cubic boron nitride single crystal bioblast as initial raw material |
| CN107602123A (en) * | 2017-08-16 | 2018-01-19 | 河南四方达超硬材料股份有限公司 | A kind of polycrystalline diamond superhard material and preparation method thereof |
| CN110785504A (en) * | 2017-08-24 | 2020-02-11 | 住友电气工业株式会社 | Composite sintered body |
| CN109079145A (en) * | 2018-08-30 | 2018-12-25 | 中南钻石有限公司 | A kind of composite polycrystal-diamond Synthetic block and its method for synthesizing composite polycrystal-diamond |
| CN111592356A (en) * | 2020-06-09 | 2020-08-28 | 欧阳晓平 | Polycrystal SiC-B4C-diamond three-layer composite material and preparation method thereof |
| CN111592360A (en) * | 2020-06-09 | 2020-08-28 | 欧阳晓平 | Polycrystal B4C-diamond double-layer composite material and preparation method thereof |
| CN111592356B (en) * | 2020-06-09 | 2021-12-31 | 欧阳晓平 | Polycrystal SiC-B4C-diamond three-layer composite material and preparation method thereof |
| CN111960811A (en) * | 2020-08-27 | 2020-11-20 | 广东工业大学 | DLP (digital light processing) forming method for diamond/cubic boron nitride-ceramic composite material |
| CN112159231A (en) * | 2020-10-09 | 2021-01-01 | 武汉理工大学 | Rapid preparation method of super-hard light diamond-B4C-SiC ternary composite ceramic |
| CN113200748A (en) * | 2021-04-19 | 2021-08-03 | 郑州博特硬质材料有限公司 | Boron nitride-diamond-zirconia hybrid composite material and preparation method thereof |
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