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CN106622032B - A kind of synthesis technology of composite superhard material - Google Patents

A kind of synthesis technology of composite superhard material Download PDF

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Publication number
CN106622032B
CN106622032B CN201611245382.XA CN201611245382A CN106622032B CN 106622032 B CN106622032 B CN 106622032B CN 201611245382 A CN201611245382 A CN 201611245382A CN 106622032 B CN106622032 B CN 106622032B
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China
Prior art keywords
superhard material
synthesis technology
hammer
technology according
warming
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Expired - Fee Related
Application number
CN201611245382.XA
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Chinese (zh)
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CN106622032A (en
Inventor
蒋向上
蒋孟瑶
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Hunan Taiding New Material LLC
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Hunan Taiding New Material LLC
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Priority to CN201611245382.XA priority Critical patent/CN106622032B/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/06Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
    • B01J3/062Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies characterised by the composition of the materials to be processed
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2203/00Processes utilising sub- or super atmospheric pressure
    • B01J2203/06High pressure synthesis
    • B01J2203/0605Composition of the material to be processed
    • B01J2203/062Diamond
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2203/00Processes utilising sub- or super atmospheric pressure
    • B01J2203/06High pressure synthesis
    • B01J2203/0605Composition of the material to be processed
    • B01J2203/0645Boronitrides

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Cutting Tools, Boring Holders, And Turrets (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a kind of synthesis technologies of composite superhard material, 1) hard alloy of assembling and superhard material the following steps are included: be placed in pyrophillite body by the synthesis technology, it is added in cubic hydraulic press, is forced into 8~10MPa, and be warming up to 700 DEG C~800 DEG C;2) it is further forced into 90~100MPa, is warming up to 1400 DEG C~1700 DEG C.The present invention can reduce the dialysis of hard alloy element during synthesis composite superhard material, reduce the tenor in superhard material, improve the yield rate and thermal stability of composite superhard material, and improve wear resistance ratio.

Description

A kind of synthesis technology of composite superhard material
Technical field
The invention belongs to composite superhard material manufacturing fields, and in particular to a kind of synthesis technology of composite superhard material.
Background technique
In the composite superhard material manufacturing in China, usually with hard alloy and superhard material (diamond or cube Boron nitride etc.) on cubic hydraulic press, a kind of completely new composite superhard material product is synthesized by high temperature and pressure.It is all at present It is all almost the same for manufacturing the production technology of composite superhard material product, it may be assumed that by assembled composite superhard material pyrophillite Synthesis of cubic body is placed among six top hammers of cubic hydraulic press, after press system pressure is risen to 50~90MPa, just Power on, directly to composite superhard material pyrophillite cube heat temperature raising;When synthesis pressure reaches rated pressure (90~ 100MPa) heat temperature raising still continues for some time, and when heat temperature raising finishes, composite sheet superhard material cube is taken out after release Body breaks pyrophillite, and taking-up has synthesized the composite superhard material product finished, and the synthesis technology of a round trip terminates.This mesh The synthesis technology in forward position has a fewer defects, most important one be in hard alloy metallic atom in the effect of high temperature and pressure Under, the largely dialysis into superhard material;And product type seeps although completely the same to superhard material in each round trip technique The amount of analysis be it is inconsistent, this also causes the tenor in superhard material to be 9~20% to differ, and the metal in superhard material The inconsistent single product quality that will cause in whole batch products of content is uneven, unstable.
In addition, by inspection and practical application, the thermal stability for the composite superhard material product that prior art is prepared It is low, wear resistance ratio decline.Moreover, the yield rate of products obtained therefrom is low, and generally below 85%.
Summary of the invention
The purpose of the present invention is to provide hard alloy element dialysis during a kind of reduction synthesis composite superhard material, drops Tenor in low superhard material, improves the yield rate and thermal stability of composite superhard material, and improves the compound super of wear resistance ratio The synthesis technology of hard material.
Technical program of the present invention lies in providing a kind of synthesis technology of composite superhard material, the synthesis technology include with Lower step:
1) hard alloy of assembling and superhard material are placed in pyrophillite body, are added in cubic hydraulic press, are forced into 8-10MPa, and it is warming up to 700 DEG C~800 DEG C;
2) it is further forced into 90~100MPa, is warming up to 1400 DEG C~1700 DEG C.
The present inventor has found in production practice, metal contained in the superhard material of composite superhard material product It is a key index for influencing product quality.How much metalliferous institute is in superhard material in composite superhard material product, directly Determine two physical properties of product most critical, a thermal stability, two are wear resistance ratios.Thermal stability refers to product through height Temperature welding after physical properties parameter with before high-temperature soldering compared with the case where, reduction the smaller proof thermal stability of amplitude It is good, (traditional handicraft reduces amplitude up to 10%~40%).And tenor is directly proportional to wear resistance ratio decline, i.e., tenor is got over Height, generated wear resistance ratio drop-out value are bigger.Even if the superhard material of composite superhard material product is added without metal in proportion, But in high temperature and pressure synthesis, metal in hard alloy is to superhard material dialysis, and metal increases in superhard material, causes hot steady Qualitative variation, wear resistance ratio reduce.
In this regard, inventor has carried out a large amount of trial and test, it is desirable to be able to improve to above situation.And then it proposes Technical solution of the present invention.
Specifically, in the synthesis process, being first forced into 5-10MPa, then make the heating hammer flat side of a hammer and leading in pyrophillite body Electric steel ring is in close contact, and power transmission heat temperature raising, when being warming up to 700 DEG C~800 DEG C, diamond or boron nitride are at 700 DEG C~800 DEG C In the temperature of (unprotect gas), the compound working lining of diamond or boron nitride approaches and reaches theoretical density, and surface can be light It is micro- nitridation and metallic atom can not jump the traces power at these temperatures.It is further forced into 90~100MPa, is warming up to 1400 At DEG C -1700 DEG C, the combination between finish button and key, make the powder body being made of numerous fine particle become one it is firm It is whole.The speed for reducing the metal dialysis in superhard material achievees the purpose that reduce tenor in superhard material.
The present invention further comprises following preferred technical solution:
Preferred scheme further comprises step 3) on the basis of step 1), step 2): by cubic hydraulic press two The pressure increase 10%~40% of a heating hammer flat side of a hammer, remaining four surface pressure are constant.
It is pressurizeed by third time, the pressure that two heating hammer flat side of a hammers are born is continued to increase, is higher than the non-heated hammer flat side of a hammer Pressure 3%~40%, and in vertical state by the hard alloy of control assembling and superhard material and two heating hammers, Ke Yiyou The retardance metallic atom movement velocity of effect, to achieve the purpose that further decrease the tenor in superhard material, to improve The thermal stability and wear resistance ratio of super-hard compound material provide effective guarantee.
Preferred scheme, on the basis of step 2), further by the pressure of the cubic hydraulic press two heating hammer flat side of a hammers Increase by 3%~40%, remaining four surface pressure is constant.
Preferred scheme, in step 3), by the pressure increase 10%~20% of the cubic hydraulic press two heating hammer flat side of a hammers.
Preferred scheme in step 1), keeps 30s-50s after being warming up to 700 DEG C~800 DEG C.
Preferred scheme in step 2), keeps 100s-1000s after being warming up to 1400 DEG C~1700 DEG C.
Preferred scheme in step 3), keeps 1-5min after pressurization.
Preferred scheme in step 1), after being first forced into 5-10MPa, then heats up.
Preferred scheme in step 2), after being first forced into 90~100MPa, then heats up.
Preferred scheme, in step 3), two heating hammers and the hard alloy assembled are vertical with superhard material.
Preferred scheme, the superhard material are diamond and/or cubic boron nitride.
Beneficial effects of the present invention:
1) in Superhard composite film product, the metal dialysis amount of hard alloy is continued to use synthesis technology compared to tradition and is greatly reduced.
2) yield rate of the invention reaches 95% or so.
3) technical solution of the present invention products obtained therefrom before welding after thermostabilization parameter be not much different, thermal stability is good.
4) wear resistance ratio of technical solution of the present invention products obtained therefrom has a more substantial increase.
Detailed description of the invention
Fig. 1 is the phasor for continuing to use the superhard material that traditional handicraft is prepared, and white portion is metal.Tenor is 11.3%.
Fig. 2 is the phasor for the superhard material that present invention process is prepared, and white portion is metal.Tenor is 2.01%.
Specific embodiment
Embodiment 1
The hard alloy of assembling and diamond are placed in pyrophillite body, be placed in cubic hydraulic press six top hammers it In, it is first forced into 10MPa, 700 DEG C~800 DEG C are heated to heating hammer power transmission, heating time is 30 seconds, is forced into 90MPa is warming up to 1400 DEG C~1700 DEG C, reaches (5~15 minutes) after the made quota of synthesis technology is fixed time, and stops heating, And pressure is down to zero, take out the product that synthesis finishes.
Tenor is 9%~20% in superhard material in traditional handicraft product;
In the product that above-mentioned technique obtains, the tenor in superhard material is 1.05%~5.06%.
And products obtained therefrom thermal stability increases, the difference of the thermostabilization parameter before and after Product jointing is 6%.
Embodiment 2
The hard alloy of assembling and diamond are placed in pyrophillite body, be placed in cubic hydraulic press six top hammers it In, when being first forced into 10MPa, 700 DEG C~800 DEG C are heated to heating hammer power transmission, heating time is 30 seconds, is forced into 90MPa is warming up to 1400 DEG C~1700 DEG C, reaches (5~15 minutes) after the made quota of synthesis technology is fixed time, and heats at two The hammer flat side of a hammer further presses, and the pressure for bearing its hammer flat side of a hammer more non-heated than four is high by 11%, reaches synthesis technology and is formulated Time rating after (3~5 minutes), stop heating, and pressure is down to zero, take out the product that synthesis finishes.
Superhard material tenor in traditional handicraft product is 9%~20%;
The tenor of superhard material is only 3.14% in above-mentioned technique products obtained therefrom.
The difference of thermostabilization parameter before and after Product jointing is 4.31%.
Embodiment 3
The hard alloy of assembling and diamond are placed in pyrophillite body, be placed in cubic hydraulic press six top hammers it In, when being first forced into 10MPa, 700 DEG C~800 DEG C are warming up to, heating time is 30 seconds, is forced into 90MPa, is warming up to 1400 DEG C ~1700 DEG C, reaches after the made quota of synthesis technology fixes time, further press in two heating hammer flat side of a hammers, keep it more non-than four The pressure born of the heating hammer flat side of a hammer is high by 19%, after reaching synthesis technology prepared time rating, stops heating, and by pressure It is down to zero, takes out the product that synthesis finishes.
Compound working lining tenor in traditional handicraft product is 9%~20%;
Tenor in above-mentioned technique products obtained therefrom in superhard material is only 2.01%.
The difference of thermostabilization parameter before and after Product jointing is 2.33%.

Claims (9)

1. a kind of synthesis technology of composite superhard material, which is characterized in that the synthesis technology the following steps are included:
1) hard alloy of assembling and superhard material are placed in pyrophillite body, are added in cubic hydraulic press, it is forced into 8 ~ 10MPa, and 700 DEG C ~ 800 DEG C are warming up to, then keep 30s-50s;
2) it is further forced into 90 ~ 100MPa, is warming up to 1400 DEG C ~ 1700 DEG C.
2. synthesis technology according to claim 1, which is characterized in that on the basis of step 1), step 2, further wrap Include step 3): by the pressure increase 3% ~ 40% of the cubic hydraulic press two heating hammer flat side of a hammers, remaining four non-heated hammer flat side of a hammer pressures Power is constant.
3. synthesis technology according to claim 2, which is characterized in that two heating hammer the flat side of a hammers and assembling hard alloy with Superhard material is vertical.
4. synthesis technology according to claim 2, which is characterized in that in step 3), cubic hydraulic press two are heated Hammer the pressure increase 10% ~ 20% of the flat side of a hammer into shape.
5. synthesis technology according to claim 1, which is characterized in that in step 2, protected after being warming up to 1400 DEG C ~ 1700 DEG C Hold 100s-1000s.
6. synthesis technology according to claim 2, which is characterized in that in step 3), 1-5min is kept after pressurization.
7. synthesis technology according to claim 1, which is characterized in that in step 1), after being first forced into 8-10MPa, then rise Temperature.
8. synthesis technology according to claim 1 or 5, which is characterized in that in step 2, carry out synchronous with heating of pressurizeing.
9. synthesis technology according to claim 1 or 2, which is characterized in that the superhard material be diamond and/or cube Boron nitride.
CN201611245382.XA 2016-12-29 2016-12-29 A kind of synthesis technology of composite superhard material Expired - Fee Related CN106622032B (en)

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CN107338470A (en) * 2017-06-01 2017-11-10 成都贝施美生物科技有限公司 A kind of porcelain block epitaxis technique

Citations (4)

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Publication number Priority date Publication date Assignee Title
CN103009270A (en) * 2012-12-03 2013-04-03 北京工业大学 Online self-sharpening metallic bond and super-hard abrasive precision grinding pellet and preparation method thereof
CN103623747A (en) * 2013-12-03 2014-03-12 深圳市海明润实业有限公司 PDC with high thermal conductivity and preparation method thereof
CN104313459A (en) * 2014-01-16 2015-01-28 郑州大学 Ni coated SiC compound powder enhanced iron-based composite material, and preparation method thereof
CN105289417A (en) * 2015-10-27 2016-02-03 蒋向上 Production technology of synthetic composite material

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US7575425B2 (en) * 2006-08-31 2009-08-18 Hall David R Assembly for HPHT processing

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
CN103009270A (en) * 2012-12-03 2013-04-03 北京工业大学 Online self-sharpening metallic bond and super-hard abrasive precision grinding pellet and preparation method thereof
CN103623747A (en) * 2013-12-03 2014-03-12 深圳市海明润实业有限公司 PDC with high thermal conductivity and preparation method thereof
CN104313459A (en) * 2014-01-16 2015-01-28 郑州大学 Ni coated SiC compound powder enhanced iron-based composite material, and preparation method thereof
CN105289417A (en) * 2015-10-27 2016-02-03 蒋向上 Production technology of synthetic composite material

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Title
金刚石—立方氮化硼—硬质合金复合柱齿的研究;马保松等;《地质与勘探》;20000331;第36卷(第2期);第71-73页

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Denomination of invention: A synthetic process of composite superhard material

Effective date of registration: 20220218

Granted publication date: 20190129

Pledgee: Hunan Chaoji Testing Technology Co.,Ltd.

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