CN106694887B - A kind of preparation method and composite polycrystal-diamond of composite polycrystal-diamond - Google Patents

A kind of preparation method and composite polycrystal-diamond of composite polycrystal-diamond Download PDF

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CN106694887B
CN106694887B CN201611248423.0A CN201611248423A CN106694887B CN 106694887 B CN106694887 B CN 106694887B CN 201611248423 A CN201611248423 A CN 201611248423A CN 106694887 B CN106694887 B CN 106694887B
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diamond
composite polycrystal
preparation
pressure
bortz powder
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CN106694887A (en
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解亚军
黄红卫
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Funik Ultrahard Material Co Ltd
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Funik Ultrahard Material Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention discloses a kind of preparation method of composite polycrystal-diamond and composite polycrystal-diamonds, belong to technical field of superhard material.The preparation method of composite polycrystal-diamond of the invention is assembled bortz powder and matrix using hard alloy as matrix, and compression moulding obtains blank；Then by blank at a temperature of 4~5.5GPa pressure, 1100 DEG C~1600 DEG C 10~180s of heat-insulation pressure keeping；Then increase pressure to 5~8GPa, increase temperature to 1400 DEG C~2000 DEG C, 5~40min of heat-insulation pressure keeping to get.Preparation method of the invention combines to avoid the breakage of raw material diamond, improve the consistency of the bed of material with double sintering by of short duration heat-insulation pressure keeping for the first time.The prepared composite polycrystal-diamond bed of material is fine and close, is composite polycrystal-diamond with high performance.

Description

A kind of preparation method and composite polycrystal-diamond of composite polycrystal-diamond
Technical field
The present invention relates to a kind of preparation method of composite polycrystal-diamond and composite polycrystal-diamonds, belong to superhard material Expect technical field.
Background technique
Composite polycrystal-diamond (polycrystalline diamond compact, PDC) belongs to new function material Material is to be sintered under ultra high pressure and high temperature conditions using diadust with cemented carbide substrate, both with the height of diamond Hardness, high-wearing feature and thermal conductivity, and intensity and toughness with hard alloy are manufacture cutting tool, drilling well brill The ideal material of head and other wear resistant tools.
Diamond compact has the high wearability of dimond synneusis and the high impact-resistant of hard alloy, and diamond concurrently Layer can remain sharp-cutting edge, thus soft to medium ground use in petroleum and geological drilling, and effect is very good. But raw material diamond is easy breakage in current composite polycrystal-diamond preparation process, the consistency deficiency of the bed of material leads to it Service life reduces.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of composite polycrystal-diamond, can be avoided raw material diamond Consistency that is damaged, improving the bed of material.
In order to achieve the goal above, the technical scheme adopted by the invention is that:
A kind of preparation method of composite polycrystal-diamond, includes the following steps:
1) bortz powder and matrix are assembled as matrix using hard alloy, compression moulding obtains blank；
2) synthesize: by blank at a temperature of 4~5.5GPa pressure, 1100 DEG C~1600 DEG C 10~180s of heat-insulation pressure keeping；So Increase afterwards pressure to 5~8GPa, increase temperature to 1400 DEG C~2000 DEG C, 5~40min of heat-insulation pressure keeping to get.
The preparation method of composite polycrystal-diamond of the invention passes through the available micro- graphite of of short duration heat-insulation pressure keeping for the first time The diamond of change improves its bulk density on the one hand to the rearrangement conducive to mixing, on the other hand weakens pressure to diamond The damage of grain.
1 × 10 after the bortz powder and matrix assembling-4~1 × 10-5Pa pressure, vacuum at a temperature of 700 ~ 1400 DEG C Dry 1~10h.
The bortz powder is cleaned before assembling, and the cleaning is cleaned using acid, alkali or acetone；The acid For one of the concentrated sulfuric acid, concentrated hydrochloric acid, concentrated nitric acid, hypochlorous acid or a variety of；The alkali is concentrated ammonia liquor, sodium hydroxide solution, dioxygen One of water is a variety of.It is described to clean the surface impurity that can remove bortz powder, purify diamond surface.
The partial size of the bortz powder is 0.1~40 μm.
The assembling is that matrix and bortz powder are assembled can, the diameter and hard of the diamond layer of the can Alloy diameter ratio is 1:1~1.1:1.
The hard alloy is containing cobalt hard alloy, and the mass content of cobalt is 13%~20%.
A kind of composite polycrystal-diamond, using the preparation method of composite polycrystal-diamond as described in claim 1 It is made.
It is compound mainly to improve synthesis polycrystalline diamond in terms of two for the preparation method of composite polycrystal-diamond of the invention Piece: 1. change the pre-molding structure of composite polycrystal-diamond by improving the transverse pressure of the bed of material in synthesis process；2. adjusting It is integrated into technique, is combined by of short duration heat-insulation pressure keeping for the first time with double sintering to avoid the breakage of raw material diamond, improve material The consistency of layer.
The composite polycrystal-diamond bed of material prepared using above-mentioned preparation method is fine and close, is plycrystalline diamond Buddha's warrior attendant with high performance Stone composite sheet.
Specific embodiment
The present invention is further illustrated With reference to embodiment.
Embodiment 1
The preparation method of the composite polycrystal-diamond of the present embodiment, includes the following steps:
1) diamond particles are washed with the concentrated sulfuric acid, it is dry, obtain pure bortz powder；The partial size of the bortz powder is 1 μm~30 μm；2) using cobalt content is 13% hard alloy as matrix, is assembled into pure bortz powder obtained by step 1) Can；
3) can is placed in high vacuum furnace, 8 × 10-5Pa pressure, the dry 5h of heat-insulation pressure keeping at a temperature of 700 DEG C, pressure Can processed；Buddha's warrior attendant stone layer diameter/hard alloy diameter ratio is 1.05:1 in can after compacting；
4) synthesize: by pressed can at a temperature of 4Gpa pressure, 1100 DEG C heat-insulation pressure keeping 180s, then increase pressure Power is to 5.5GPa, raising temperature to 1400 DEG C of heat-insulation pressure keeping 40min to get high-performance composite polycrystal-diamond.
The composite polycrystal-diamond of the present embodiment is made of above-mentioned preparation method.
Embodiment 2
The preparation method of the composite polycrystal-diamond of the present embodiment, includes the following steps:
1) diamond particles are washed with sodium hydroxide solution, it is dry, obtain pure bortz powder；The bortz powder Partial size is 0.1 μm~5 μm；
2) using cobalt content is 15% hard alloy as matrix, is assembled into gold with pure bortz powder obtained by step 1) Belong to box；
3) can is placed in high vacuum furnace, 1 × 10-5Pa pressure, the dry 1h of heat-insulation pressure keeping at a temperature of 1000 DEG C, pressure Can processed；Buddha's warrior attendant stone layer diameter/hard alloy diameter ratio is 1:1 in can after compacting；
4) synthesize: by pressed can at a temperature of 5Gpa pressure, 1300 DEG C heat-insulation pressure keeping 10s, then increase pressure Power is to 5.5GPa, raising temperature to 1700 DEG C of heat-insulation pressure keeping 20min to get high-performance composite polycrystal-diamond.
The composite polycrystal-diamond of the present embodiment is made of above-mentioned preparation method.
Embodiment 3
The preparation method of the composite polycrystal-diamond of the present embodiment, includes the following steps:
1) dry by diamond particles acetone washing, obtain pure bortz powder；The partial size of the bortz powder is 20 ~40 μm；
2) using cobalt content is 20% hard alloy as matrix, is assembled into gold with pure bortz powder obtained by step 1) Belong to box；
3) can is placed in high vacuum furnace, 1 × 10-4Pa pressure, the dry 1h of heat-insulation pressure keeping at a temperature of 1400 DEG C, pressure Can processed；Buddha's warrior attendant stone layer diameter/hard alloy diameter ratio is 1.1:1 in can after compacting；
4) synthesize: by pressed can at a temperature of 4Gpa pressure, 1600 DEG C heat-insulation pressure keeping 10s, then increase pressure Power is to 5GPa, raising temperature to 2000 DEG C of heat-insulation pressure keeping 5min to get high-performance composite polycrystal-diamond.
The composite polycrystal-diamond of the present embodiment is made of above-mentioned preparation method.
Embodiment 4
The preparation method of the composite polycrystal-diamond of the present embodiment, includes the following steps:
1) diamond particles are washed with concentrated hydrochloric acid, it is dry, obtain pure bortz powder；The partial size of the bortz powder is 0.1~1 μm；
2) using cobalt content is 15% hard alloy as matrix, is assembled into gold with pure bortz powder obtained by step 1) Belong to box；
3) can is placed in high vacuum furnace, 8 × 10-5Pa pressure, the dry 5h of heat-insulation pressure keeping at a temperature of 1000 DEG C；Pressure Can processed；Buddha's warrior attendant stone layer diameter/hard alloy diameter ratio is 1.1:1 in can after compacting；
4) synthesize: by pressed can at a temperature of 4Gpa pressure, 1100 DEG C heat-insulation pressure keeping 180s, then increase pressure Power is to 5GPa, raising temperature to 1400 DEG C of heat-insulation pressure keeping 40min to get high-performance composite polycrystal-diamond.
The composite polycrystal-diamond of the present embodiment is made of above-mentioned preparation method.
Embodiment 5
The preparation method of the composite polycrystal-diamond of the present embodiment, includes the following steps:
1) diamond particles are washed with hypochlorous acid, it is dry, obtain pure bortz powder；The partial size of the bortz powder is 15μm；
2) using cobalt content is 13% hard alloy as matrix, is assembled into gold with pure bortz powder obtained by step 1) Belong to box；
3) can is placed in high vacuum furnace, 8 × 10-5Pa pressure, the dry 5h of heat-insulation pressure keeping at a temperature of 1000 DEG C；Pressure Can processed；Buddha's warrior attendant stone layer diameter/hard alloy diameter ratio is 1.1:1 in can after compacting；
4) synthesize: by pressed can at a temperature of 5.5Gpa pressure, 1100 DEG C heat-insulation pressure keeping 180s, then increase Pressure is to 8GPa, raising temperature to 1400 DEG C of heat-insulation pressure keeping 10min to get high-performance composite polycrystal-diamond.
The composite polycrystal-diamond of the present embodiment is made of above-mentioned preparation method.
Embodiment 6
The preparation method of the composite polycrystal-diamond of the present embodiment, includes the following steps:
1) diamond particles are washed with concentrated ammonia liquor, it is dry, obtain pure bortz powder；The partial size of the bortz powder is 40μm；
2) using cobalt content is 13% hard alloy as matrix, is assembled into gold with pure bortz powder obtained by step 1) Belong to box；
3) can is placed in high vacuum furnace, 8 × 10-5Pa pressure, the dry 5h of heat-insulation pressure keeping at a temperature of 1000 DEG C, pressure Can processed；Buddha's warrior attendant stone layer diameter/hard alloy diameter ratio is 1.1:1 in can after compacting；
4) synthesize: by pressed can at a temperature of 5.5Gpa pressure, 1100 DEG C heat-insulation pressure keeping 180s, then increase Pressure is to 8GPa, raising temperature to 1400 DEG C of heat-insulation pressure keeping 10min to get high-performance composite polycrystal-diamond.
The composite polycrystal-diamond of the present embodiment is made of above-mentioned preparation method.

Claims (4)

1. a kind of preparation method of composite polycrystal-diamond, characterized by the following steps:
1) bortz powder and matrix are assembled as matrix using hard alloy, compression moulding obtains blank；
2) synthesize: by blank at a temperature of 4~5.5GPa pressure, 1100 DEG C~1600 DEG C 10~180s of heat-insulation pressure keeping；Then it rises High pressure to 5~8GPa, increase temperature to 1400 DEG C~2000 DEG C, 5~40min of heat-insulation pressure keeping to get；
1 × 10 after the bortz powder and matrix assembling-4~1 × 10-5Pa pressure is dried in vacuo 1 at a temperature of 700 ~ 1400 DEG C ~10h；
The hard alloy is containing cobalt hard alloy, and the mass content of cobalt is 13%~20%；
The assembling is that matrix and bortz powder are assembled can, the diameter and hard alloy of the diamond layer of the can Diameter ratio is 1.05:1~1.1:1.
2. the preparation method of composite polycrystal-diamond according to claim 1, it is characterised in that: the bortz powder exists It is cleaned before assembling, the cleaning is cleaned using acid, alkali or acetone；The acid is the concentrated sulfuric acid, concentrated hydrochloric acid, dense nitre One of acid, hypochlorous acid are a variety of；The alkali is one of concentrated ammonia liquor, sodium hydroxide solution, hydrogen peroxide or a variety of.
3. the preparation method of composite polycrystal-diamond according to claim 1, it is characterised in that: the bortz powder Partial size is 0.1~40 μm.
4. a kind of composite polycrystal-diamond, it is characterised in that: using composite polycrystal-diamond as described in claim 1 Preparation method is made.
CN201611248423.0A 2016-12-29 2016-12-29 A kind of preparation method and composite polycrystal-diamond of composite polycrystal-diamond Active CN106694887B (en)

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CN110500039A (en) * 2019-07-10 2019-11-26 河南四方达超硬材料股份有限公司 With the composite polycrystal-diamond extended

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US9068410B2 (en) * 2006-10-26 2015-06-30 Schlumberger Technology Corporation Dense diamond body
GB0810184D0 (en) * 2008-06-04 2008-07-09 Element Six Production Pty Ltd Method for producing a compact
US8728382B2 (en) * 2011-03-29 2014-05-20 David R. Hall Forming a polycrystalline ceramic in multiple sintering phases
CN104563889A (en) * 2013-11-25 2015-04-29 莱州市原野科技有限公司 Pre-graphitized polycrystalline diamond compact
CN105798312B (en) * 2016-03-16 2018-02-13 郑州新亚复合超硬材料有限公司 A kind of oil bit diamond compact sintering process
CN105840104B (en) * 2016-03-25 2018-07-17 河南四方达超硬材料股份有限公司 A kind of thermostable type high impact-resistant composite polycrystal-diamond and manufacturing method
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