CN112323144A - Surface-enhanced polycrystalline diamond compact and preparation method thereof - Google Patents

Surface-enhanced polycrystalline diamond compact and preparation method thereof Download PDF

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CN112323144A
CN112323144A CN202011220069.7A CN202011220069A CN112323144A CN 112323144 A CN112323144 A CN 112323144A CN 202011220069 A CN202011220069 A CN 202011220069A CN 112323144 A CN112323144 A CN 112323144A
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polycrystalline diamond
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temperature
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diamond film
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CN112323144B (en
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吕宪义
范赛飞
张海波
王绍斌
张松
邹广田
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Jilin University
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B28/00—Production of homogeneous polycrystalline material with defined structure
    • C30B28/12—Production of homogeneous polycrystalline material with defined structure directly from the gas state
    • C30B28/14—Production of homogeneous polycrystalline material with defined structure directly from the gas state by chemical reaction of reactive gases
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/04—Diamond

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  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
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  • General Chemical & Material Sciences (AREA)
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  • Crystals, And After-Treatments Of Crystals (AREA)
  • Earth Drilling (AREA)
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Abstract

The invention discloses a surface-enhanced polycrystalline diamond compact and a preparation method thereof, and belongs to the technical field of superhard materials. The surface-enhanced polycrystalline diamond compact comprises a CVD polycrystalline diamond film, a polycrystalline diamond layer and a tungsten carbide-cobalt hard alloy layer, and the preparation method comprises the steps of laser scanning and carving of a prefabricated pattern, integral compaction and forming, high-temperature and high-pressure sintering and the like. According to the invention, a CVD polycrystalline diamond film is sintered on the surface of the PDC in a hot pressing manner, so that the wear resistance of the PDC is improved, the CVD polycrystalline diamond film on the surface is cracked along laser prefabricated lines in the high-temperature and high-pressure sintering process, and a fluid mixture of diamond micro powder, cobalt and tungsten carbide is filled into the cracks to form polycrystals and form firm D-D bond connection with the CVD polycrystalline diamond film. Therefore, the diamond diaphragm is not easy to crack and fall off randomly in the high-temperature high-pressure sintering process and under the high-load working condition, so that the damage to the cutter is avoided.

Description

Surface-enhanced polycrystalline diamond compact and preparation method thereof
Technical Field
The invention belongs to the technical field of superhard materials, and particularly relates to a Polycrystalline Diamond Compact (PDC) with a surface of a hot-pressing sintering Chemical Vapor Deposition (CVD) polycrystalline diamond film applied to industries such as petroleum drilling, geological exploration, coal field drilling and production drill bits, machining tools and the like and a preparation method thereof.
Background
The polycrystalline diamond compact bit has wide application in the aspect of drilling of petroleum and natural gas, along with the gradual reduction of conventional petroleum and natural gas exploitation resources, the rapid development of shale oil and shale gas is a great trend in the future, and the difficult-to-exploit geology such as shale oil and shale gas has higher and higher requirements on the performance of the PDC bit.
The PDC is formed by sintering diamond micro powder and a hard alloy matrix (tungsten carbide-cobalt) at high temperature and high pressure, the diamond micro powder is sintered into a diamond layer, the diamond layer has ultrahigh hardness and wear resistance of diamond, and the hard alloy matrix has sinterability and is convenient to apply to various different working environments.
Cobalt in the hard alloy matrix seeps out of the matrix at high temperature and high pressure and penetrates through the diamond micro powder, the contact parts of diamond grains are melted into the cobalt liquid, and after the temperature is reduced, carbon atoms melted into the cobalt liquid grow into a diamond structure again, so that the diamond grains are firmly combined to form polycrystalline diamond.
The very important performance parameters of a PDC are wear resistance and impact resistance, both of which are very related to the bond strength between the diamond grains. The larger the contact area between the diamond grains, the stronger the diamond grains are bonded.
The traditional method is difficult to further improve the connection strength between diamond grains, and the surface of the PDC is enhanced by adding a superhard coating in order to further improve the wear resistance of the PDC.
Compared with polycrystalline diamond, the crystal grains of the CVD polycrystalline diamond film are combined more firmly and tightly, but the CVD polycrystalline diamond film is easy to crack randomly under the high-temperature and high-pressure environment for preparing the PDC, and the traditional diamond film cutter is easy to crack randomly and fall off under the working condition of ultrahigh load, so that the cutter is damaged.
Disclosure of Invention
The invention provides a brand new formula and a brand new process, wherein a CVD polycrystalline diamond film is sintered on the surface of the traditional PDC at high temperature and high pressure, so that the surface of the polycrystalline diamond film of the PDC is enhanced, and the wear resistance of the PDC is further improved. The CVD polycrystalline diamond film is firstly subjected to laser engraving to prepare grains, the surface CVD polycrystalline diamond film cracks along the laser prepared grains in the sintering process of the PDC under the conditions that the pressure is not less than 5.5GP and the temperature is not less than 1400 ℃, the fluid mixture of the diamond micro powder, the cobalt and the tungsten carbide is filled into the cracks to form polycrystal, and the polycrystal and the CVD polycrystalline diamond film form firm D-D bond connection. Therefore, the CVD polycrystalline diamond film is not easy to crack randomly in a large area in the high-temperature and high-pressure sintering process and under the high-load working condition, so that the cutter is prevented from being damaged.
The technical problem is solved by the following technical scheme:
a surface-enhanced polycrystalline diamond compact comprises a CVD polycrystalline diamond film, a polycrystalline diamond layer and a tungsten carbide-cobalt hard alloy layer, wherein the CVD polycrystalline diamond film is sintered on the polycrystalline diamond layer, and the polycrystalline diamond layer is sintered on the tungsten carbide-cobalt hard alloy layer.
Preferably, the thicknesses of the polycrystalline diamond layer and the tungsten carbide-cobalt hard alloy layer are respectively 2mm and 11 mm.
A method of making a surface enhanced polycrystalline diamond compact, comprising the steps of:
(1) selecting one piece of CVD polycrystalline diamond film with uniform and complete surface and one tungsten carbide-cobalt hard alloy cylindrical blank;
(2) placing the CVD polycrystalline diamond film on a sample table of a laser cutting machine, cutting the CVD polycrystalline diamond film into a wafer with the same diameter as the tungsten carbide-cobalt hard alloy cylindrical blank by using laser, then performing pattern prefabrication on the surface of the wafer, and scanning and engraving by using the laser according to the prefabricated pattern;
(3) sequentially filling the CVD polycrystalline diamond film and the diamond micro powder with the grain size of less than or equal to 50 mu m in the step (2) into a high-temperature-resistant and high-pressure-resistant metal round cup, placing a tungsten carbide-cobalt hard alloy cylindrical blank on the upper layer of the mixed micro powder, and compacting and forming the whole;
(4) putting the CVD polycrystalline diamond film, the diamond micro powder and the tungsten carbide-cobalt hard alloy which are compacted and formed together with the metal round cup into a carbon heating pipe, putting the carbon heating pipe into a pyrophyllite block, putting the pyrophyllite block into high-temperature and high-pressure equipment, boosting the pressure to be more than 5.5GPa, heating to be more than 1400 ℃, and keeping the pressure and the temperature for 300-1000 seconds;
(5) stopping heating, reducing the pressure, and reducing the temperature of the equipment to room temperature and the pressure to the standard atmospheric pressure; and taking out the pyrophyllite blocks from the high-temperature and high-pressure equipment, and removing the pyrophyllite blocks, the carbon heating pipes and the metal round cups outside the sintered body to obtain the surface-enhanced polycrystalline diamond compact.
The CVD polycrystalline diamond film described in step (1) may be prepared by, but not limited to, methods well known in the art, such as a hot filament method, a plasma enhanced hot cathode method, a microwave plasma method, and a microwave plasma torch method.
The thickness of the CVD polycrystalline diamond film in the step (1) is preferably 100 to 1500 μm.
The grain size of the CVD polycrystalline diamond film in the step (1) is preferably 1-100 μm.
The laser prefabricated pattern in the step (2) is preferably formed by a fan-shaped pattern consisting of 2-4 concentric rings with the same width and 3-8 radial line segments with the same included angle.
The laser prefabricated pattern in the step (2) has the grain width of 100-1000 mu m and the depth of 20-80% of the film thickness.
In the step (4), preferably increasing the pressure to a pressure higher than 6.5GPa, and heating to 1450-1600 ℃; keeping the pressure and the temperature for 450-650 seconds.
In the step (5), the surface diamond film of the PDC is cracked along the laser prefabricated lines in the high-temperature high-pressure sintering process, and the fluid diamond micro powder, cobalt and tungsten carbide mixture is filled into the cracks to form polycrystals and form firm D-D bond connection with the CVD polycrystalline diamond film.
Has the advantages that:
1. the wear resistance of the PDC is improved by hot-pressing and sintering a CVD polycrystalline diamond film on the surface of the PDC;
2. the surface CVD polycrystalline diamond film cracks along the laser prefabricated lines in the high-temperature high-pressure sintering process of the PDC, and the fluid diamond micro powder, cobalt and tungsten carbide mixture is filled into the cracks to form polycrystals and form firm D-D bond connection with the CVD polycrystalline diamond film. Therefore, the diamond diaphragm is not easy to crack and fall off randomly in the high-temperature high-pressure sintering process and under the high-load working condition, so that the damage to the cutter is avoided.
Drawings
Fig. 1 is a perspective view of a surface enhanced polycrystalline diamond compact made in accordance with the present invention.
FIG. 2 is a preferred laser pre-texturing of a CVD polycrystalline diamond film.
FIG. 3 is another preferred laser pre-texturing of a CVD polycrystalline diamond film.
FIG. 4 is yet another preferred laser pre-texturing of a CVD polycrystalline diamond film.
Detailed Description
Example 1
The process of the present invention is further described in detail by the following preferred embodiments with reference to the accompanying drawings, but the scope of the invention is not limited thereto, and the examples are only illustrative and not restrictive.
Selecting one piece of CVD polycrystalline diamond film with uniform and complete surface, diameter larger than 20mm, thickness of 800 μm and grain size of 30-70 μm, and one piece of hard alloy (tungsten carbide-cobalt) cylindrical blank phi 16.45 x 12mm with cobalt content of 15% (mass ratio).
Placing the selected CVD polycrystalline diamond film on a sample table of a laser cutting machine, cutting the CVD polycrystalline diamond film into round pieces with the same diameter as that of a hard alloy (tungsten carbide-cobalt) blank by using laser, performing figure prefabrication on the surface of the round pieces, and scanning and engraving by using the laser according to a designed pattern, wherein figures 2-4 are three preferable prefabricated pattern lines. The diameter of the processed CVD polycrystalline diamond film is 16.45mm, the thickness is 800 μm, the grain width is 500 μm, and the depth is 500 μm;
and (3) putting 1.9g of diamond micro powder (with the granularity of 8-15 microns) and the CVD polycrystalline diamond film into absolute ethyl alcohol, carrying out ultrasonic oscillation cleaning for 15 minutes, and then putting into an oven for drying at 80 ℃. Then putting the CVD polycrystalline diamond film and the powder into a zirconium cup with phi 16.50 multiplied by 10mm in sequence, putting the film bottom with the grain surface facing downwards, compacting the powder, and then putting the hard alloy (tungsten carbide-cobalt) cylindrical blank. The metal cup is placed in a carbon heating tube and in a pyrophyllite block, which is then placed in a high temperature and high pressure apparatus. The pressure was gradually increased from atmospheric pressure to 7GPa and the heating temperature was raised to 1500 c for 500 seconds. The surface diamond film of the PDC is cracked along laser prefabricated lines in the high-temperature high-pressure sintering process, and the fluid diamond micro powder, cobalt and tungsten carbide mixture is filled into the cracks to form polycrystals and form firm D-D bond connection with the CVD polycrystalline diamond film.
After the heating, the pressure was reduced to atmospheric pressure and the temperature was reduced to room temperature. Removing pyrophyllite blocks, carbon heating pipes and metal round cups outside the sintered body, and obtaining the PDC with the surface being the CVD polycrystalline diamond film through mechanical processing, wherein the specification is phi 16 multiplied by 13.8mm, the thickness of the polycrystalline diamond layer is 2mm, and the thickness of the hard alloy substrate is 11 mm. The CVD polycrystalline diamond film, the polycrystalline diamond layer and the tungsten carbide-cobalt hard alloy layer are firmly sintered without cracks or delamination, the grain cracks of the prefabricated pattern of the CVD polycrystalline diamond film are filled with polycrystalline diamond, the surface is compact, no pores exist, no edges fall off, no cracks exist, and the structural schematic diagram of the prepared surface-enhanced polycrystalline diamond compact is shown in figure 1.
In the sample prepared by the embodiment, a compact diamond film with the thickness of 800 microns is formed on the surface, so that the wear resistance of the PDC can be improved, and the service life of the PDC during cutting can be prolonged. The traditional PDC polycrystalline diamond layer without surface enhancement has more microscopic pores, poor wear resistance and short service life.
In the sample prepared by the embodiment, the CVD polycrystalline diamond film with the enhanced PDC surface is provided with the laser prefabricated grain structure, so that the delaminated CVD polycrystalline diamond film can be separated according to small blocks divided by laser prefabricated grains under the condition that the CVD polycrystalline diamond film layer is delaminated after being impacted by high load, the large-area random crack is avoided, and the cutter damage and the integral failure of the PDC caused by the large-block separated chips in the cutting work are avoided. And when the surface-enhanced PDC is cut, the CVD polycrystalline diamond film on one side can rotate to another surface which is not fallen for continuous use after falling off according to the small blocks divided by the laser prefabricated grains, and the use cost of the PDC is further reduced. The significance of preventing the CVD polycrystalline diamond film from random cracking and falling off during the work of the PDC by the laser preformed texture and the fluid filling texture in the hot pressing sintering process is shown.

Claims (6)

1. A surface-enhanced polycrystalline diamond compact comprises a CVD polycrystalline diamond film, a polycrystalline diamond layer and a tungsten carbide-cobalt hard alloy layer, wherein the CVD polycrystalline diamond film is sintered on the polycrystalline diamond layer, and the polycrystalline diamond layer is sintered on the tungsten carbide-cobalt hard alloy layer.
2. A surface enhanced polycrystalline diamond compact according to claim 1, in which the thicknesses of the polycrystalline diamond layer and the tungsten carbide-cobalt hard alloy layer are 2mm and 11mm, respectively.
3. A method of making the surface-enhanced polycrystalline diamond compact of claim, comprising the steps of:
(1) selecting one piece of CVD polycrystalline diamond film with uniform and complete surface and one tungsten carbide-cobalt hard alloy cylindrical blank;
(2) placing the CVD polycrystalline diamond film on a sample table of a laser cutting machine, cutting the CVD polycrystalline diamond film into a wafer with the same diameter as the tungsten carbide-cobalt hard alloy cylindrical blank by using laser, then performing pattern prefabrication on the surface of the wafer, and scanning and engraving by using the laser according to the prefabricated pattern;
(3) sequentially filling the CVD polycrystalline diamond film and the diamond micro powder with the grain size of less than or equal to 50 mu m in the step (2) into a high-temperature-resistant and high-pressure-resistant metal round cup, placing a tungsten carbide-cobalt hard alloy cylindrical blank on the upper layer of the mixed micro powder, and compacting and forming the whole;
(4) putting the CVD polycrystalline diamond film, the diamond micro powder and the tungsten carbide-cobalt hard alloy which are compacted and formed together with the metal round cup into a carbon heating pipe, putting the carbon heating pipe into a pyrophyllite block, putting the pyrophyllite block into high-temperature and high-pressure equipment, boosting the pressure to be more than 5.5GPa, heating to be more than 1400 ℃, and keeping the pressure and the temperature for 300-1000 seconds;
(5) stopping heating, reducing the pressure, and reducing the temperature of the equipment to room temperature and the pressure to the standard atmospheric pressure; and taking out the pyrophyllite blocks from the high-temperature and high-pressure equipment, and removing the pyrophyllite blocks, the carbon heating pipes and the metal round cups outside the sintered body to obtain the surface-enhanced polycrystalline diamond compact.
4. A method of making a surface enhanced polycrystalline diamond compact as claimed in claim 3, wherein the CVD polycrystalline diamond film in step (1) has a thickness of 100 μm to 1500 μm and a grain size of 1 μm to 100 μm.
5. The method for preparing a surface-enhanced polycrystalline diamond compact according to claim 3, wherein the laser preformed pattern in the step (2) is a fan-shaped pattern consisting of 2-4 concentric rings with equal width and 3-8 radial line segments with equal included angles, the laser preformed pattern has a line width of 100-1000 μm and a depth of 20-80% of the film thickness.
6. The method of claim 3, wherein in step (4), the pressure is increased to a pressure greater than 6.5GPa, and the temperature is increased to 1450-1600 ℃; keeping the pressure and the temperature for 450-650 seconds.
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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2579910Y (en) * 2002-11-27 2003-10-15 陈继峰 Diamond composite diamond product by chemical gas phase deposition diamond polycrystal
US20040140132A1 (en) * 2003-01-21 2004-07-22 Stewart Middlemiss Polycrystalline diamond with improved abrasion resistance
CN202480460U (en) * 2012-03-29 2012-10-10 成都比拓超硬材料有限公司 Substrate capable of enhancing structure of polycrystalline diamond compact
CN105349965A (en) * 2015-11-03 2016-02-24 富耐克超硬材料股份有限公司 Polycrystalline diamond compact and manufacturing method thereof
CN109128193A (en) * 2017-06-28 2019-01-04 深圳先进技术研究院 Composite polycrystal-diamond and preparation method thereof
CN109128192A (en) * 2017-06-28 2019-01-04 深圳先进技术研究院 Composite polycrystal-diamond and preparation method thereof
CN110253024A (en) * 2019-07-22 2019-09-20 吉林大学 A kind of diamond compact and preparation method thereof containing graphene

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2579910Y (en) * 2002-11-27 2003-10-15 陈继峰 Diamond composite diamond product by chemical gas phase deposition diamond polycrystal
US20040140132A1 (en) * 2003-01-21 2004-07-22 Stewart Middlemiss Polycrystalline diamond with improved abrasion resistance
CN202480460U (en) * 2012-03-29 2012-10-10 成都比拓超硬材料有限公司 Substrate capable of enhancing structure of polycrystalline diamond compact
CN105349965A (en) * 2015-11-03 2016-02-24 富耐克超硬材料股份有限公司 Polycrystalline diamond compact and manufacturing method thereof
CN109128193A (en) * 2017-06-28 2019-01-04 深圳先进技术研究院 Composite polycrystal-diamond and preparation method thereof
CN109128192A (en) * 2017-06-28 2019-01-04 深圳先进技术研究院 Composite polycrystal-diamond and preparation method thereof
CN110253024A (en) * 2019-07-22 2019-09-20 吉林大学 A kind of diamond compact and preparation method thereof containing graphene

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