CN111906319B - Preparation method of diamond compact - Google Patents

Preparation method of diamond compact Download PDF

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Publication number
CN111906319B
CN111906319B CN202010731910.2A CN202010731910A CN111906319B CN 111906319 B CN111906319 B CN 111906319B CN 202010731910 A CN202010731910 A CN 202010731910A CN 111906319 B CN111906319 B CN 111906319B
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diamond
micro powder
hard alloy
alloy base
temperature
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CN111906319A (en
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江雨明
张彩琴
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Suzhou Sibolier Industrial Technology Co ltd
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Suzhou Sibolier Industrial Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00Manufacture 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
    • B22F7/06Manufacture 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
    • B22F7/062Manufacture 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 involving the connection or repairing of preformed parts
    • B22F7/064Manufacture 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 involving the connection or repairing of preformed parts using an intermediate powder layer
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00Manufacture 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
    • B22F7/06Manufacture 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
    • B22F7/08Manufacture 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 with one or more parts not made from powder

Abstract

The invention relates to a preparation method of a diamond compact, firstly taking diamond micro powder, and carrying out surface purification treatment on the diamond micro powder; cleaning the surface of the hard alloy base, and plating metal cobalt on the combined surface of the hard alloy base and the diamond micro powder; packaging a hard alloy base plated with metal cobalt and diamond micro powder in a high-temperature resistant metal cup, and paving the diamond micro powder on a joint surface; and (2) placing the high-temperature-resistant metal cup in a high-pressure cavity, sintering for 10-20 min at the temperature of 1450-1500 ℃ and under the pressure of 5.5-8.0 GPa, melting metal cobalt, penetrating into the diamond micropowder layer under the drive of high pressure, filling gaps among the micropowder particles to form a bonding agent in the polycrystalline diamond layer, sintering the diamond micropowder into the polycrystalline diamond layer, and sintering the polycrystalline diamond layer and the hard alloy base into a whole to obtain the diamond compact blank. The diamond is uniformly distributed, the local aggregation phenomenon of the bonding agent is avoided, and the wear resistance is improved by more than 20%.

Description

Preparation method of diamond compact
Technical Field
The invention relates to a preparation method of a diamond compact, belonging to the technical field of manufacturing of superhard materials.
Background
At present, a material mixing process is adopted for preparing the diamond composite sheet, the problems of uneven distribution of a binding agent, easy aggregation and agglomeration, surface oxidation of cobalt powder and the like caused by material mixing are caused, the defects of uneven material mixing, surface oxidation of metal cobalt powder in the material mixing process and the like are caused, and the quality of the sintered diamond composite sheet is seriously influenced by the defects.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a diamond compact.
The purpose of the invention is realized by the following technical scheme:
the preparation method of the diamond compact is characterized in that: the method comprises the following steps:
1) Taking diamond micro powder, and carrying out surface purification treatment on the diamond micro powder;
2) Cleaning the surface of the hard alloy base, and plating metal cobalt on the combined surface of the hard alloy base and the diamond micro powder;
3) Packaging a hard alloy base plated with metal cobalt and diamond micro powder in a high-temperature resistant metal cup, and paving the diamond micro powder on a joint surface;
4) And (2) placing the high-temperature-resistant metal cup in a high-pressure cavity, sintering for 10-20 min at the temperature of 1450-1500 ℃ and under the pressure of 5.5-8.0 GPa, melting metal cobalt, penetrating into the diamond micropowder layer under the drive of high pressure, filling gaps among the micropowder particles to form a bonding agent in the polycrystalline diamond layer, sintering the diamond micropowder into the polycrystalline diamond layer, and sintering the polycrystalline diamond layer and the hard alloy base into a whole to obtain the diamond compact blank.
Further, in the preparation method of the diamond compact, in the step 1), the diamond micro powder is soaked in acid and alkali to remove surface impurities, and then is repeatedly cleaned by high-purity water, and the surface of the diamond micro powder is purified.
Further, in the preparation method of the diamond compact, step 2), the surface of the hard alloy base is subjected to sand blasting cleaning treatment.
Further, in the above method for producing a diamond compact, in step 2), the metallic cobalt is plated on the bonding surface of the cemented carbide base to which the diamond fine powder is bonded by a CVD plating method or a PVD plating method.
Further, in the preparation method of the diamond compact, the material of the high-temperature resistant metal cup is Ti, zr, mo or Ta.
Further, in the method for manufacturing the diamond compact, the bonding surface is planar or non-planar.
Further, in the preparation method of the diamond compact, in the step 4), the high-temperature resistant metal cup is tightly adhered to the diamond compact blank after being sintered, and is removed by a diamond grinding wheel grinding method.
Compared with the prior art, the invention has obvious advantages and beneficial effects, which are embodied in the following aspects:
the invention is different from the traditional method for mixing and processing the bonding agent of the polycrystalline diamond layer and the diamond micro powder, but adopts CVD or PVD technology to evenly coat the metal cobalt on the bonding surface of the hard alloy, when the diamond composite sheet is sintered under high temperature and high pressure, the metal cobalt is melted and permeates into the diamond micro powder layer under the driving of high pressure and fills the gaps among the micro powder particles, the diamond micro powder is sintered into the polycrystalline diamond layer, and simultaneously the polycrystalline diamond layer and the hard alloy base are sintered into a whole to prepare the diamond composite sheet. The mixing process is avoided, two defects of uneven mixing and surface oxidation of the metal cobalt powder in the mixing process are avoided, and the problems of uneven distribution of the binding agent, easy aggregation and agglomeration, surface oxidation of the cobalt powder and the like are solved. Compared with the traditional process, the diamond distribution of the polycrystalline diamond layer is uniform, the local aggregation phenomenon of the bonding agent is avoided, the wear resistance of the prepared diamond compact is improved by more than 20%, and the impact resistance is improved by more than 12%.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims thereof.
Drawings
FIG. 1: a schematic view of the layered cross-sectional structure of the material before sintering;
FIG. 2: the layered cross-sectional structure of the sintered material is shown schematically.
Detailed Description
In order to more clearly understand the technical features, objects, and effects of the present invention, specific embodiments will now be described in detail.
Uniformly plating metal cobalt on the bonding surface of the hard alloy base by adopting a CVD or PVD technology, sintering at high temperature and high pressure, melting the metal cobalt plated on the bonding surface of the hard alloy base and permeating diamond micro powder, and filling gaps among diamond micro powder particles to form a polycrystalline diamond layer to obtain the diamond composite sheet.
Example 1
Soaking the diamond micro powder with acid and alkali to remove surface impurities, repeatedly cleaning the diamond micro powder with high-purity water, and purifying the surface of the diamond micro powder;
performing sand blasting cleaning treatment on the surface of a hard alloy base 1, as shown in figure 1, plating metal cobalt 2 on a bonding surface 4 formed by bonding the hard alloy base and diamond micro powder by adopting a CVD (chemical vapor deposition) plating method, wherein the bonding surface 4 is planar; the thickness of the metal cobalt plating is 0.1mm;
a hard alloy base 1 plated with metal cobalt 2 and diamond micro powder 3 are packaged in a high-temperature resistant metal cup, the diamond micro powder 3 is paved on a joint surface 4, and the high-temperature resistant metal cup is made of Ti;
placing the high-temperature-resistant metal cup in a high-pressure cavity, sintering for 10min at 1450-1480 ℃ and under the pressure of 5.5-6.0 GPa, melting metal cobalt 2, and allowing the metal cobalt to penetrate into a diamond micropowder layer under the drive of high pressure and fill gaps among micropowder particles to form a bonding agent in the polycrystalline diamond layer, sintering the diamond micropowder into a polycrystalline diamond layer 5, and sintering the polycrystalline diamond layer 5 and the hard alloy base 1 into a whole to obtain a diamond compact blank as shown in figure 2;
the high-temperature resistant metal cup is tightly adhered to the diamond compact blank after being sintered, and is removed by a diamond grinding wheel grinding method.
Example 2
Removing surface impurities of the diamond micro powder by acid and alkali soaking, repeatedly cleaning with high-purity water, and performing surface purification treatment on the diamond micro powder;
carrying out sand blasting cleaning treatment on the surface of the hard alloy base, plating metal cobalt on a bonding surface which is bonded with the diamond micropowder on the hard alloy base by adopting a PVD (physical vapor deposition) plating method, wherein the bonding surface is non-planar, and the plating thickness of the metal cobalt is 0.4mm;
packaging a hard alloy base plated with metal cobalt and diamond micro powder in a high-temperature resistant metal cup, wherein the diamond micro powder is laid on a bonding surface, and the high-temperature resistant metal cup is made of Zr;
placing the high-temperature-resistant metal cup in a high-pressure cavity, sintering for 15min at the temperature of 1480-1500 ℃ and under the pressure of 5.5-6.5 GPa, melting metal cobalt, and penetrating a diamond micropowder layer under the drive of high pressure and filling gaps among micropowder particles to form a bonding agent in the polycrystalline diamond layer, sintering the diamond micropowder into the polycrystalline diamond layer, and sintering the polycrystalline diamond layer and the hard alloy base into a whole to obtain a diamond compact blank;
the high-temperature resistant metal cup is tightly adhered to the diamond compact blank after being sintered and removed by a diamond grinding wheel grinding method.
Example 3
Removing surface impurities of the diamond micro powder by acid and alkali soaking, repeatedly cleaning with high-purity water, and performing surface purification treatment on the diamond micro powder;
carrying out sand blasting cleaning treatment on the surface of the hard alloy base, plating metal cobalt on a bonding surface which is bonded with the diamond micro powder on the hard alloy base by adopting a CVD (chemical vapor deposition) plating method, wherein the bonding surface is planar, and the plating thickness of the metal cobalt is 0.8mm;
packaging a hard alloy base plated with metal cobalt and diamond micro powder in a high-temperature resistant metal cup, paving the diamond micro powder on a joint surface, and making the high-temperature resistant metal cup made of Mo;
placing the high-temperature-resistant metal cup in a high-pressure cavity, sintering for 20min at the temperature of 1450-1480 ℃ and under the pressure of 6.0-8.0 GPa, melting metal cobalt, and penetrating a diamond micropowder layer under the drive of high pressure to fill gaps among micropowder particles to form a bonding agent in the polycrystalline diamond layer, sintering the diamond micropowder into the polycrystalline diamond layer, and sintering the polycrystalline diamond layer and the hard alloy base into a whole to obtain a diamond compact blank;
the high-temperature resistant metal cup is tightly adhered to the diamond compact blank after being sintered and removed by a diamond grinding wheel grinding method.
Example 4
Soaking the diamond micro powder with acid and alkali to remove surface impurities, repeatedly cleaning the diamond micro powder with high-purity water, and purifying the surface of the diamond micro powder;
carrying out sand blasting cleaning treatment on the surface of the hard alloy base, plating metal cobalt on a bonding surface which is bonded with the diamond micro powder on the hard alloy base by adopting a PVD (physical vapor deposition) plating method, wherein the bonding surface is non-planar, and the plating thickness of the metal cobalt is 1.0mm;
packaging a hard alloy base plated with metal cobalt and diamond micro powder in a high-temperature resistant metal cup, wherein the diamond micro powder is laid on a bonding surface, and the high-temperature resistant metal cup is made of Ta;
placing the high-temperature-resistant metal cup in a high-pressure cavity, sintering for 16min at 1470-1500 ℃ and under the pressure of 5.5-6.0 GPa, melting metal cobalt, driving the metal cobalt to penetrate into a diamond micropowder layer under high pressure and fill gaps among micropowder particles to form a bonding agent in the polycrystalline diamond layer, sintering the diamond micropowder into a polycrystalline diamond layer, and sintering the polycrystalline diamond layer and the hard alloy base into a whole to obtain a diamond compact blank;
the high-temperature resistant metal cup is tightly adhered to the diamond compact blank after being sintered and removed by a diamond grinding wheel grinding method.
Comparative example
Uniformly mixing the diamond bonding agent powder and the diamond micro powder in a mixing mode such as premixing, three-dimensional mixing and the like;
putting the diamond mixed powder into a high-temperature vacuum furnace, heating to 600-900 ℃ in a vacuum state, preserving heat for 3-6 h, and purifying;
placing the diamond mixed micro powder on a hard alloy base, then placing the base in a high-temperature-resistant metal cup, and covering the cup with a cover, wherein the high-temperature-resistant metal cup is made of Ta;
the high-temperature resistant metal cup loaded with the diamond micro powder, the bonding agent powder and the hard alloy base is placed in a high-pressure cavity and sintered for 10-20 min under the conditions of the temperature of 1400-1500 ℃ and the pressure of 5.5-8.0 GPa, so that the diamond cutting tooth is obtained.
The diamond compact blanks prepared in the above examples 1 to 4 and comparative examples were tested for wear resistance and impact resistance, and the test results were as follows:
example 1 Example 2 Example 3 Example 4 Comparative example
Abrasion resistance/wear resistance 746 596 503 468 344
Impact resistance/J 80 70 65 55 39
In summary, the invention is different from the traditional method of mixing the polycrystalline diamond layer binding agent and the diamond micro powder, the CVD or PVD technology is adopted to uniformly coat the metal cobalt on the hard alloy binding surface, when the diamond composite sheet is sintered under high temperature and high pressure, the metal cobalt is melted and permeates the diamond micro powder layer under the driving of high pressure and fills gaps among micro powder particles, the diamond micro powder is sintered into the polycrystalline diamond layer, and simultaneously the polycrystalline diamond layer and the hard alloy base are sintered into a whole to prepare the diamond composite sheet. The mixing process is avoided, two defects of uneven mixing and surface oxidation of the metal cobalt powder in the mixing process are avoided, and the problems of uneven distribution of the binding agent, easy aggregation and agglomeration, surface oxidation of the cobalt powder and the like are solved. Compared with the traditional process, the diamond distribution of the polycrystalline diamond layer is uniform, the local aggregation phenomenon of the bonding agent is avoided, the wear resistance of the prepared diamond compact is improved by more than 20%, and the impact resistance is improved by more than 12%.
It should be noted that: the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention; while the foregoing description will be apparent to those skilled in the relevant art and it is intended to cover in the appended claims all such modifications and changes as fall within the true spirit of the invention.

Claims (6)

1. The preparation method of the diamond compact is characterized by comprising the following steps: the method comprises the following steps:
1) Taking diamond micro powder, and carrying out surface purification treatment on the diamond micro powder;
2) Cleaning the surface of the hard alloy base, and plating metal cobalt on a bonding surface of the hard alloy base and the diamond micro powder by adopting a CVD plating method or a PVD plating method;
3) Packaging a hard alloy base plated with metal cobalt and diamond micro powder in a high-temperature resistant metal cup, and paving the diamond micro powder on a joint surface;
4) And (2) placing the high-temperature-resistant metal cup in a high-pressure cavity, sintering for 10-20 min at the temperature of 1450-1500 ℃ and under the pressure of 5.5-8.0 GPa, melting metal cobalt, penetrating into the diamond micropowder layer under the drive of high pressure, filling gaps among the micropowder particles to form a bonding agent in the polycrystalline diamond layer, sintering the diamond micropowder into the polycrystalline diamond layer, and sintering the polycrystalline diamond layer and the hard alloy base into a whole to obtain the diamond compact blank.
2. The method of making a diamond compact of claim 1, wherein: step 1), soaking the diamond micro powder by acid and alkali to remove surface impurities, repeatedly cleaning the diamond micro powder by high-purity water, and carrying out surface purification treatment on the diamond micro powder.
3. The method of making a diamond compact of claim 1, wherein: and 2), carrying out sand blasting cleaning treatment on the surface of the hard alloy base.
4. The method of making a diamond compact of claim 1, wherein: the material of the high-temperature resistant metal cup is Ti, zr, mo or Ta.
5. The method of making a diamond compact of claim 1, wherein: the bonding surface is planar or non-planar.
6. The method of making a diamond compact of claim 1, wherein: and 4) sintering the high-temperature-resistant metal cup, then tightly adhering the sintered high-temperature-resistant metal cup to the diamond compact blank, and removing the high-temperature-resistant metal cup by using a diamond grinding wheel grinding method.
CN202010731910.2A 2020-07-27 2020-07-27 Preparation method of diamond compact Active CN111906319B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8297382B2 (en) * 2008-10-03 2012-10-30 Us Synthetic Corporation Polycrystalline diamond compacts, method of fabricating same, and various applications
CN107912051A (en) * 2015-08-17 2018-04-13 哈利伯顿能源服务公司 Polycrystalline diamond table is attached to substrate to form PCD cutter using reaction/exothermic process
CN110029942B (en) * 2019-05-27 2020-11-24 吉林大学 Thermal-stable polycrystalline diamond compact suitable for drilling and preparation method thereof
CN110578128B (en) * 2019-08-26 2021-08-20 中南钻石有限公司 Preparation method of dome-shaped polycrystalline diamond compact
CN111283205B (en) * 2020-03-26 2022-03-01 成都比拓超硬材料有限公司 Super-thick polycrystalline diamond composite material, preparation method and application thereof

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