CN110090963B - High-toughness conductive polycrystalline diamond compact and preparation method thereof - Google Patents

High-toughness conductive polycrystalline diamond compact and preparation method thereof Download PDF

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CN110090963B
CN110090963B CN201910445130.9A CN201910445130A CN110090963B CN 110090963 B CN110090963 B CN 110090963B CN 201910445130 A CN201910445130 A CN 201910445130A CN 110090963 B CN110090963 B CN 110090963B
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temperature
powder
sintering
micro powder
pressure
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CN110090963A (en
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刘宝昌
陈朝然
朱艺清
石佳鑫
曹鑫
戴文昊
王姝婧
朱月
李思奇
韩哲
赵新哲
张帅
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Jilin University
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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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B22F1/142—Thermal or thermo-mechanical treatment
    • 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
    • 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
    • B22F3/10—Sintering only
    • B22F3/1017—Multiple heating or additional steps
    • 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
    • B22F3/24—After-treatment of workpieces or articles
    • 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
    • B22F7/02—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 layers
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
    • C22C47/14—Making alloys containing metallic or non-metallic fibres or filaments by powder metallurgy, i.e. by processing mixtures of metal powder and fibres or filaments
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
    • C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
    • 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
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/247—Removing material: carving, cleaning, grinding, hobbing, honing, lapping, polishing, milling, shaving, skiving, turning the surface

Abstract

The invention discloses a high-toughness conductive polycrystalline diamond compact and a preparation method thereof, belonging to the field of materials science, wherein the polycrystalline diamond compact is prepared by sintering silicon-plated diamond micro powder, carbon fiber, diamond micro powder and iron-nickel alloy powder as mixed powder with a hard alloy by using a traditional cubic-top large-cavity press under the conditions of the pressure of 5.5-6.0 GPa and the temperature of 1500-1700 ℃; according to the invention, the carbon fiber and the iron-nickel alloy powder are used as additives to prepare the high-impact-toughness composite sheet for the drilling field, and the comprehensive performance of the PDC composite sheet is improved. Further improving the strength, fracture toughness and impact toughness of the composite material to deal with various complex formation drilling.

Description

High-toughness conductive polycrystalline diamond compact and preparation method thereof
Technical Field
The invention relates to a polycrystalline diamond compact, in particular to a high-toughness conductive polycrystalline diamond compact and a preparation method thereof, belonging to the field of materials science.
Background
Polycrystalline Diamond of artificial Diamond (PCD for short) is formed by sintering Diamond micropowder under high pressure, and PCD, a novel superhard material, is widely applied to the fields of cutters, geological core drilling, oil exploitation drilling and the like, is also the key point of continuous research and breakthrough in the fields of oil and gas drilling, geological engineering exploration and the like, but has an unsatisfactory application effect under certain extreme working environment conditions.
Most PDC compacts are composite superhard materials formed by sintering diamond micro powder, cobalt powder and a hard alloy substrate under the conditions of high temperature and high pressure, and because the thermal expansion coefficients of diamond, cobalt and hard alloy are different greatly, the residual metal cobalt binder in the polycrystalline diamond has adverse effect on the performance of the polycrystalline diamond. Therefore, researchers at home and abroad have developed researches on preparing polycrystalline diamond by sintering a novel binder and removing metallic cobalt in the polycrystalline diamond.
The carbon fiber is brittle fiber with carbon content of more than 90% and is formed by converting organic fiber through a series of heat treatments, and has the advantages of high electric conductivity, high specific strength, high heat conductivity, small thermal expansion coefficient, good size stability, high temperature resistance, corrosion resistance and the like. At present, carbon fibers are mainly used for reinforcing silicon carbide ceramic matrix and other composite materials, and research on polycrystalline diamond compacts is less. Chinese patent document CN103880460B discloses a method for preparing polycrystalline diamond sintered body, which refers to polycrystalline diamond and chopped carbon fiber, but adopts a microwave thermal sintering method, and uses sol to wrap the material, and then microwave heating sintering is performed. Polycrystalline diamond is not obtained by the method, and effective bonding cannot be formed between the diamond and the diamond. At present, in the domestic synthesis of polycrystalline diamond, diamond particles are in a compressed state after high-temperature and high-pressure sintering, and are in contact with each other, and under the action of a binder, the diamond-diamond direct bonding (D-D bond) is promoted to be a sintered body.
Unlike PDC (polycrystalline diamond compact) compacts used in the field of cutters, compacts used in the field of drilling are considered to be drilled into hard rock under various extreme environmental conditions, and PDC compacts used in the field of drilling are considered to be comprehensive in hardness, heat resistance, wear resistance, and impact toughness. The PDC composite sheet sintered by the diamond micro powder with small granularity has good wear resistance, but poor impact resistance, the practical application effect in the drilling field is comprehensively considered, the comprehensive performance of the diamond micro powder is optimal when the diamond micro powder is 30-50 um, the micro powder with single granularity is small in stacking density, large in pores in the sintered polycrystal and low in wear resistance, the larger the specific gravity occupied by the micro powder with coarse granularity is, the more obvious the result is, so that different granularity ratios need to be researched to realize the comprehensive performance of the PDC composite sheet.
Disclosure of Invention
The invention aims to provide a high-toughness conductive polycrystalline diamond compact and a preparation method thereof, wherein silicon-plated diamond micro powder with the particle size of 30-50 um is used as the main particle size, and from the aspect of optimal bulk density and optimal proportion, a traditional domestic cubic-top large-cavity press is used for preparing the high-impact-toughness compact for the drilling field by using carbon fiber and iron-nickel alloy powder as additives under the conditions of pressure of 5.5-6.0 GPa and temperature of 1500-1700 ℃, so that the comprehensive performance of the PDC compact is improved.
In order to achieve the purpose, the invention provides a high-toughness conductive polycrystalline diamond compact, which is characterized in that the high-toughness conductive polycrystalline diamond compact is prepared by sintering silicon-plated diamond micro powder, carbon fiber, diamond micro powder and iron-nickel alloy powder serving as mixed powder with a cubic apparatus large-cavity press and hard alloy under the conditions that the pressure is 5.5 GPa-6.0 GPa and the temperature is 1500-1700 ℃; wherein, the dosage of the silicon-plated diamond micro powder, the carbon fiber, the diamond micro powder and the iron-nickel alloy powder is as follows according to the weight percentage: 80-95 wt% of silicon-plated diamond micro powder, 0.1-2 wt% of carbon fiber, 1-10 wt% of diamond micro powder and 1-10 wt% of iron-nickel alloy powder;
the grain diameter of the silicon-plated diamond micro powder is 30-50 mu m;
the particle size of the carbon fiber is 1 nm-100 mu m;
the grain size of the diamond micro powder is 0.1-12 mu m;
the particle size of the iron-nickel alloy powder is 1 nm-8 mu m.
The fracture toughness reaches 9.4 (+ -0.3) MPa-m 1/2, and the impact crushing energy is 30 (+ -2) J.
The mass ratio of iron to nickel in the iron-nickel alloy powder is 5: 5.
The hard alloy is made of tungsten-cobalt alloy, and the cobalt content of the hard alloy is 15-16%.
The diameter of the hard alloy is 10 mm-30 mm, and the thickness of the hard alloy is 4 mm-8 mm.
The invention also provides a method for preparing the high-toughness conductive polycrystalline diamond compact, which is characterized by comprising the following steps of:
step 1, preparing raw materials:
firstly, carrying out acid treatment on the surface of the diamond micro powder to remove residual metal impurities on the surface of the diamond micro powder, washing the diamond micro powder to be neutral by distilled water, and placing the diamond micro powder into a drying container for later use after drying;
hard alloy purification treatment: performing ultrasonic extraction under the condition of absolute ethyl alcohol to remove impurities on the surface of the hard alloy;
③ the usage amount of the silicon-plated diamond micro powder, the carbon fiber, the diamond micro powder and the iron-nickel alloy powder is that 80wt% -95 wt% of the silicon-plated diamond micro powder, 0.1wt% -2 wt% of the carbon fiber, 1wt% -10 wt% of the diamond micro powder and 1wt% -10 wt% of the iron-nickel alloy powder are weighed respectively, the components are evenly mixed under a ball mill, the ball-milling adopts a ball-to-material ratio of 1:1, the mixed powder is put into a graphite cup, then the graphite cup with the powder is put into a vacuum furnace for vacuum heat treatment, the highest temperature in the vacuum furnace is 650 ℃, and the vacuum degree is 3 × 10-3Pa, obtaining mixed powder, putting the obtained mixed powder and the purified hard alloy into a metal container, and tabletting to obtain a composite material;
step 2, a high-temperature high-pressure assembly sintering process:
placing the composite material subjected to impurity removal and cold pressing in a zirconium oxide wrapping container along with a metal container wrapped outside the composite material, placing the composite material in a cubic apparatus large-cavity press, sintering at high temperature and high pressure, and keeping the temperature for a preset time in the sintering process to obtain a polycrystalline diamond compact;
in the high-temperature high-pressure sintering process, the range of the sintering pressure P is 5.5GPa < P <6.0GPa, the range of the sintering temperature T is 1500 ℃ < T <1700 ℃, and the range of the sintering duration T is 5min < T <20 min;
step 3, grinding and polishing the polycrystalline diamond compact obtained in the step 2 to obtain the high-toughness conductive polycrystalline diamond compact;
further, in the step 2, during sintering, the pressure is increased to the sintering pressure at the pressure increasing rate of 0.5 GPa/min-1 GPa/min, the temperature is increased to the sintering temperature at the temperature increasing rate of 20 ℃/s-40 ℃/s for high-temperature sintering, the temperature is increased to the sintering temperature within 30s after the temperature is maintained at 1400 ℃ for 60s, the temperature is reduced to 600 ℃ at the temperature decreasing rate of 15 ℃/s-30 ℃/s after the sintering is finished, the temperature is reduced to the room temperature after the temperature is maintained for 3 min-5 min, and the pressure is reduced to the normal pressure at the pressure reducing rate of 0.1 GPa/min-0.8 GPa/min.
Through the design scheme, the invention can bring the following beneficial effects: the invention provides a high-toughness conductive polycrystalline diamond compact and a preparation method thereof, wherein silicon-plated diamond micro powder with the particle size of 30-50 mu m is used as the main particle size, and from the aspect of optimal bulk density and optimal proportion, a traditional domestic cubic-top large-cavity press is utilized, under the conditions of the pressure of 5.5-6.0 GPa and the temperature of 1500-1700 ℃, carbon fiber and iron-nickel alloy powder are used as additives, so that the high-impact-toughness compact used in the drilling field is researched, and the comprehensive performance of the PDC compact is improved. Further improving the strength, fracture toughness and impact toughness of the composite material to deal with various complex formation drilling.
The method is adopted to prepare the polycrystalline diamond compact under the conditions of high temperature and high pressure by adding a certain proportion of carbon fibers, the microhardness reaches 68 (+/-2.1) GPa, and the fracture toughness reaches 9.4 (+/-0.3) MPa.m1/2Compared with the polycrystalline diamond compact without carbon fibers, the impact breaking energy of 30 (+/-2) J is increased by 55% in hardness, 43.5% in fracture toughness and 86% in impact toughness. The addition of carbon fiber in a certain proportion can play a good toughening role among diamond particles, and after the PDC composite sheet is cooled down from high temperature, the fiber has the functions of tensile stress and matrix compressive stress. The strength of the high performance fiber is advantageously developed when the fiber is subjected to a small tensile stress, and the matrix is subjected to a compressive stress, so that cracks on the surface of the matrix are healed. And the fracture toughness and the impact toughness of the polycrystalline diamond compact are improved.
Raman spectrum analysis of samples before and after high-temperature and high-pressure treatment on the carbon fiber shows that: the synthesized product has no diamond single crystal, and the Raman spectrum shows the property of the carbon fiber. The uniformly dispersed carbon fibers enable the polycrystalline diamond compact prepared by the invention to have good electric and heat conducting properties besides good mechanical properties. Wherein the heat-conducting property of the polycrystalline diamond prepared by carbon fiber reinforcement is improved by 32 percent. The diamond is not conductive, the polycrystalline diamond prepared by carbon fiber reinforcement can form a three-dimensional conductive network in the material, the resistivity of the polycrystalline diamond compact prepared by adding no carbon fiber is 412.16 +/-15 omega.m measured by adopting a four-probe method, and the resistivity of the polycrystalline diamond compact prepared by carbon fiber reinforcement is 18.048 +/-0.6 omega.m. The resistivity is inversely proportional to the conductivity, so that the conductivity of the carbon fiber reinforced polycrystalline diamond composite sheet is improved by about 23 times, the PDC composite sheet belongs to a superhard material, the conventional processing means cannot cut the PDC composite sheet, laser cutting is mostly adopted, and the laser processing needs a material with good conductivity, so that the prepared PDC composite sheet has excellent conductivity and is more beneficial to the subsequent processing and treatment of the polycrystalline diamond composite sheet.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention to the right, and in which:
FIG. 1 is a schematic distribution diagram of silicon-plated diamonds with different particle sizes and diamond mixing;
FIG. 2 is a schematic view of a zirconia coated container;
fig. 3 is an electron microscope image of the carbon fiber-toughened polycrystalline diamond compact.
In the figure: i is silicon-plated diamond micro powder, II is diamond micro powder, III is iron-nickel alloy powder, IV is carbon fiber, 1 is a zirconium oxide packaging container, 2 is a heat preservation sheet, and 3 is a composite material.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below with reference to preferred embodiments and the accompanying drawings. As will be appreciated by those skilled in the art. The following detailed description is illustrative rather than limiting in nature and is not intended to limit the scope of the invention.
The high-toughness conductive polycrystalline diamond compact provided by the invention is prepared by sintering silicon-plated diamond micro powder, carbon fiber, diamond micro powder and iron-nickel alloy powder serving as mixed powder with a conventional cubic apparatus large-cavity press under the conditions that the pressure is 5.5-6.0 GPa and the temperature is 1500-1700 ℃;
according to the weight percentage, the dosage of the silicon-plated diamond micro powder, the carbon fiber, the diamond micro powder and the iron-nickel alloy powder is as follows: 80-95 wt% of silicon-plated diamond micro powder, 0.1-2 wt% of carbon fiber, 1-10 wt% of diamond micro powder and 1-10 wt% of iron-nickel alloy powder.
Wherein the grain diameter of the silicon-plated diamond micro powder is 30-50 mu m.
Wherein the particle size of the carbon fiber is 1 nm-100 mu m.
Wherein the grain diameter of the diamond micro powder is 0.1-12 μm.
Wherein the particle size of the iron-nickel alloy powder is 1 nm-8 μm, and the mass ratio of iron to nickel in the iron-nickel alloy powder is 5: 5.
Wherein the hard alloy is tungsten-cobalt alloy, the cobalt content of the hard alloy is 15-16%, the diameter of the hard alloy is 10-30 mm, and the thickness of the hard alloy is 4-8 mm.
The high-toughness conductive polycrystalline diamond compact provided by the invention adopts silicon-plated diamond micro powder with the particle size of 30-50 microns as the main particle size, and uses a traditional domestic cubic-top large-cavity press as well as carbon fiber and iron-nickel alloy powder as additives under the conditions of 5.5-6.0 GPa and 1500-1700 ℃ from the aspect of optimal bulk density and optimal proportion, so that the high-impact-toughness compact used in the drilling field is researched, and the comprehensive performance of the PDC compact is improved. Further improving the strength, fracture toughness and impact toughness of the composite material to deal with various complex formation drilling.
The carbon fiber is used for toughening the PDC composite sheet, and is characterized in that when cracks are expanded, the cracks meet the carbon fiber with specific orientation and distribution, the cracks are difficult to deflect and can only continue to expand along the original expansion path, the interface of the carbon fiber and the composite sheet matrix is well combined, the fibers are subjected to debonding, pulling-out and breaking to form broken fiber bridging, the breaking energy is consumed, the driving force for continuing expansion of the cracks is increased, and the expansion of the cracks is effectively hindered.
The silicon-plated diamond micro powder with the particle size of 30-50 mu m is adopted as the main particle size and is mixed with the diamond micro powder, and the iron-nickel alloy powder is used as the binder, so that the problem that the thermal stress is generated on a diamond interface due to large difference of thermal expansion coefficients of diamond and Co in the preparation of the composite sheet by using cobalt and Co as the binder can be effectively solved. The Si on the surface of the silicon-plated diamond is firmly combined with the diamond at high temperature and high pressure to form a SiC ceramic phase, the expansion coefficient of the SiC ceramic phase is similar to that of the diamond, and the thermal residual stress of the PDC composite sheet caused by the difference of the thermal expansion coefficients is effectively reduced.
FIG. 1 is a schematic distribution diagram of silicon-plated diamonds with different particle sizes and diamond mixing; FIG. 2 is a schematic view of a zirconia coated container 1; FIG. 3 is an electron microscope image of a carbon fiber-toughened polycrystalline diamond compact; in the figure, I is silicon-plated diamond micro powder, II is diamond micro powder, III is iron-nickel alloy powder, IV is carbon fiber, 1 is a zirconium oxide packaging container, 2 is a heat preservation sheet, and 3 is a composite material, wherein the heat preservation sheet 2 is a sodium chloride heat preservation sheet or a magnesium oxide heat preservation sheet.
The structure for assembling the cavity of the cubic apparatus large cavity press adopts a double-layer heat preservation design that a pyrophyllite sheet and a carbon column are used as sealing pressure transmission media, and a MgO tube and a graphite tube are sleeved outside a composite material 3 obtained by tabletting mixed powder and purified hard alloy, so that the cavity of the cubic apparatus large cavity press is assembled to realize higher temperature gradient, and the accurate temperature of the cavity during reaction is ensured, thereby realizing better experimental effect. Zirconia parcel container 1's size design is diameter 30mm, height 30mm, zirconia parcel container 1 processes into 0 ~ 3 through holes, wraps up required corresponding size composite piece, and zirconia parcel container 1 middle is arranged in to heat preservation piece 2, as the wall and the heat preservation effect between the corresponding composite piece. The sintered compact can be any size below 30mm in diameter, the compact with the diameter of 10mm can be sintered for 6-9 times according to the adjustment of the thickness of the hard alloy, the compact with the diameter of 13-15 mm can be sintered for 4-6 times according to the adjustment of the thickness of the hard alloy, the synthesized compact with the diameter of 15-30 mm can be cut into the compact with any size according to the needs of laser, the needs of quantitative production are met, and the high impact toughness conductive type polycrystalline diamond compact applicable to the drilling field can be synthesized in large batch.
The preparation method of the high-toughness conductive polycrystalline diamond compact provided by the invention comprises the following steps:
step 1, preparing raw materials:
firstly, surface treatment of diamond micro powder: the method comprises the steps of heating and boiling away residual metal impurities on the surface of the diamond micro powder by aqua regia or other acid, washing the diamond micro powder to be neutral by distilled water, drying the diamond micro powder, putting the diamond micro powder into a drying container for later use, carrying out surface treatment on the diamond micro powder, and then carrying out high-temperature and high-pressure sintering on the diamond micro powder, wherein the obtained material has high strength and wear resistance.
Hard alloy purification treatment: performing ultrasonic treatment for 30min under the condition of absolute ethyl alcohol to remove impurities such as oil stains on the surface of the hard alloy;
③ the usage amount of the silicon-plated diamond micro powder, the carbon fiber, the diamond micro powder and the iron-nickel alloy powder is that 80wt% -95 wt% of the silicon-plated diamond micro powder, 0.1wt% -2 wt% of the carbon fiber, 1wt% -10 wt% of the diamond micro powder and 1wt% -10 wt% of the iron-nickel alloy powder are weighed respectively, and the components are evenly mixed under a ball mill, the ball-milling adopts a ball-to-material ratio of 1:1, wherein the total amount of the silicon-plated diamond micro powder, the carbon fiber, the diamond micro powder and the iron-nickel alloy powder is 1 g-6 g, the ball-milling medium is no silicon diamond micro powderThe method comprises the following steps of using 10mL of absolute ethyl alcohol, enabling the rotation speed of a ball mill to be 600r/min, enabling the diameter of steel balls in the ball mill to be 2mm, adding a part of absolute ethyl alcohol every 2 hours in the ball milling process, stopping ball milling after ball milling for 48 hours, opening the ball mill, after the absolute ethyl alcohol is evaporated, filling mixed powder into a graphite cup, then placing the graphite cup filled with the powder into a vacuum furnace for vacuum heat treatment, removing oxygen, water vapor and the like adsorbed on the surface of the powder, enabling the surface of the powder to have good reaction activity, obtaining mixed powder, and enabling the maximum temperature in the vacuum furnace to be 650 ℃ and the vacuum degree to be 3 × 10 during heating-3Pa; and putting the obtained mixed powder and the purified hard alloy into a metal container, and performing tabletting treatment by using a material pressing machine to obtain the composite material 3, wherein the metal container is a metal molybdenum container or a metal tantalum container.
Step 2, a high-temperature high-pressure assembly sintering process:
placing the composite material 3 subjected to impurity removal and cold pressing in a zirconium oxide wrapping container 1 along with a metal container wrapped outside the composite material, placing the composite material in a cubic apparatus large-cavity press, sintering at high temperature and high pressure, and preserving heat for a period of time after sintering to obtain a polycrystalline diamond compact;
in the high-temperature high-pressure sintering process, the range of the sintering pressure P is 5.5GPa < P <6.0GPa, the range of the sintering temperature T is 1500 ℃ < T <1700 ℃, and the range of the sintering duration T is 5min < T <20 min;
during sintering, the pressure is increased to the sintering pressure at the rate of 0.5 GPa/min-1 GPa/min, the temperature is rapidly increased to the sintering temperature at the rate of 20 ℃/s-40 ℃/s for high-temperature sintering, the temperature is reduced to 600 ℃ at the rate of 15 ℃/s-30 ℃/s after sintering, the temperature is reduced to room temperature after 3 min-5 min of heat preservation, and the pressure is reduced to normal pressure at the rate of 0.1 GPa/min-0.8 GPa/min; in the sintering process, after the temperature is kept at 1400 ℃ for 60s, the temperature is increased to the sintering temperature within 30s, because Si on the surface of the silicon-plated diamond reacts with the diamond when the sintering temperature is increased to 1400 ℃, a wear-resistant and high-temperature-resistant metal ceramic phase is formed, and meanwhile, the temperature is quickly increased within a short time, so that the cobalt liquid of the hard alloy substrate can sweep towards the diamond layer along the gaps of diamond particles.
Example 1
The preparation method of the high-toughness conductive polycrystalline diamond compact in this embodiment is as follows:
step 1, preparing raw materials:
according to the weight percentage, 80wt% of silicon-plated diamond micro powder with the grain diameter of 30-50 mu m, 2wt% of carbon fiber with the grain diameter of 1-10 mu m, 12wt% of diamond micro powder with the grain diameter of 4-8 mu m and 6wt% of iron-nickel alloy powder with the grain diameter of 2-8 nm are respectively weighed and evenly mixed under a ball mill, the ball mill adopts the ball-to-material ratio of 1:1, the mass of a mixed material consisting of the silicon-plated diamond micro powder, the carbon fiber, the diamond micro powder and the iron-nickel alloy powder is 1-6 g, the ball milling medium is absolute ethyl alcohol, the dosage is 10mL, the rotating speed of the ball mill is 600r/min, the diameter of a steel ball in the ball mill is 2mm, a part of absolute ethyl alcohol is added every 2h in the ball milling process, the ball milling is stopped after 48 hours, the ball mill is opened, the absolute ethyl alcohol is evaporated to dryness, the mixed diamond powder mixed with a binder is firstly put into a graphite cup, then the graphite cup filled with the material is put into a vacuum furnace for vacuum heat treatment, oxygen, water vapor and the surface of the powder is enabled to have the highest temperature of 3 × 10 ℃ and react well, and the vacuum degree of the graphite cup is-3Pa; weighing 1-6 g of mixed powder subjected to vacuum heat treatment and hard alloy, putting the mixed powder and the hard alloy into a metal molybdenum container, and putting the metal molybdenum container into a mold for prepressing molding, wherein the prepressing pressure is 10MPa, and the pressure maintaining time is 60s, so as to obtain a composite material;
and 2, high-temperature high-pressure sintering:
placing the composite material 3 subjected to impurity removal and cold pressing in a zirconium oxide wrapping container 1 along with a metal molybdenum container wrapped outside the composite material 3, placing in a six-side top large-cavity press with the volume ratio of 6 x 40MN, increasing the pressure to the sintering pressure of 5.5GPa at the pressure increasing rate of 0.6GPa/min, rapidly increasing the temperature at the temperature increasing rate of 40 ℃/s to 1400 ℃, preserving the temperature for 60s, rapidly increasing the temperature to 1600 ℃ within 30s after preserving the temperature, preserving the temperature for 1000s, reducing the temperature to 600 ℃ at the temperature reducing rate of 25 ℃/min after sintering, reducing the temperature to room temperature after preserving the temperature for 3min, and reducing the pressure to normal pressure at the pressure reducing rate of 0.5 GPa/. Removing the metal molybdenum container wrapped outside the sample of the composite sheet from the sand blasting machine to obtain the polycrystalline diamond composite sheet, and performing primary observation on the polycrystalline diamond composite sheet by using a body microscope to ensure that the surface of a sintered body is uniformly sintered without defects such as pits, cracks and the like;
step 3, grinding and polishing the polycrystalline diamond compact obtained in the step 2 to obtain the high-toughness conductive polycrystalline diamond compact;
the Si of the silicon-plated diamond is completely participated in forming new phases or bonding, and new phases of SiC ceramic exist. Si has the same lattice structure and lattice constant as diamond and thus wets the diamond surface well. The expansion coefficient of SiC is similar to that of diamond, so that the thermal residual stress of the PDC due to the difference of the thermal expansion coefficients is effectively reduced, and the impact toughness and the high temperature resistance of the PDC are improved. During an impact resistance test, the uniformly dispersed carbon fibers have fiber bridging and crack deflection effects, when the cracks meet fibers in a specific orientation and distribution, the cracks are difficult to deflect and can only continue to expand along the original expansion path, because the elastic coefficient of the fibers is slightly larger than that of a base material, the fibers at the tip of the cracks are not broken and are arranged at the two ends of the cracks, and the carbon fibers effectively counteract the action of external tensile stress, so that the cracks do not have power for continuing expansion, and the toughening effect is achieved. The polycrystalline diamond compact prepared by carbon fiber reinforcement can form a three-dimensional conductive network in the material. The initial oxidation temperature of the composite sheet prepared by the embodiment is 968 ℃, the initial oxidation temperature is increased by about 208 ℃, and the impact toughness is increased by 52%. The conductivity is improved by 19 times.
Example 2
The preparation method of the high-toughness conductive polycrystalline diamond compact in this embodiment is as follows:
step 1, preparing raw materials:
according to the weight percentage, 85wt% of silicon-plated diamond micro powder with the grain diameter of 30-50 mu m, 0.5wt% of carbon fiber with the grain diameter of 10-20 nm, 10wt% of diamond micro powder with the grain diameter of 8-12 mu m and 4.5wt% of iron-nickel alloy powder with the grain diameter of 2-8 nm are respectively weighed and evenly mixed under a ball mill, the ball mill adopts a ball-to-material ratio of 1:1, the mass of a mixed material consisting of the silicon-plated diamond micro powder, the carbon fiber, the diamond micro powder and the iron-nickel alloy powder is 1-6 g, the ball milling medium is absolute ethyl alcohol, and the dosage is 10mLThe rotation speed of the ball mill is 600r/min, the diameter of a steel ball in the ball mill is 2mm, a part of absolute ethyl alcohol is added every 2h in the ball milling process, the ball milling is stopped after 48 h, after the ball mill is opened, the absolute ethyl alcohol is evaporated to be dry, the mixed diamond powder mixed with the binder is firstly filled into a graphite cup, then the graphite cup filled with the material is placed in a vacuum furnace for vacuum heat treatment, oxygen, water vapor and the like adsorbed on the surface of the powder are removed, the surface of the powder has better reaction activity, mixed powder is obtained, and during the heating period, the highest temperature in the vacuum furnace is 650 ℃, and the vacuum degree is 3 × 10-3Pa; weighing 1-6 g of mixed powder subjected to vacuum heat treatment and hard alloy, putting the mixed powder and the hard alloy into a metal molybdenum container, and putting the metal molybdenum container into a mold for prepressing molding, wherein the prepressing pressure is 10MPa, and the pressure maintaining time is 60s, so as to obtain a composite material;
and 2, high-temperature high-pressure sintering:
placing the composite material 3 subjected to impurity removal and cold pressing in a zirconium oxide wrapping container 1 along with a metal molybdenum container wrapped outside the composite material 3, placing in a six-side top large-cavity press with the volume ratio of 6 x 40MN, increasing the pressure to the sintering pressure of 5.8GPa at the pressure increasing rate of 0.6GPa/min, rapidly increasing the temperature at the temperature increasing rate of 40 ℃/s to 1400 ℃, preserving the temperature for 60s, rapidly increasing the temperature to 1500 ℃ within 30s after preserving the temperature, preserving the temperature for 800s, reducing the temperature to 600 ℃ at the temperature reducing rate of 25 ℃/min after sintering, reducing the temperature to room temperature after preserving the temperature for 3min, and reducing the pressure to normal pressure at the pressure reducing rate of 0.5 GPa/. Removing the metal molybdenum container wrapped outside the sample of the composite sheet from the sand blasting machine to obtain the polycrystalline diamond composite sheet, and performing primary observation on the polycrystalline diamond composite sheet by using a body microscope to ensure that the surface of a sintered body is uniformly sintered without defects such as pits, cracks and the like;
step 3, grinding and polishing the polycrystalline diamond compact obtained in the step 2 to obtain the high-toughness conductive polycrystalline diamond compact;
the Si of the silicon-plated diamond is completely participated in forming new phases or bonding, and new phases of SiC ceramic exist. Si has the same lattice structure and lattice constant as diamond and thus wets the diamond surface well. The expansion coefficient of SiC is similar to that of diamond, so that the thermal residual stress of the PDC due to the difference of the thermal expansion coefficients is effectively reduced, and the impact toughness and the high temperature resistance of the PDC are improved. During an impact resistance test, the uniformly dispersed carbon fibers have fiber bridging and crack deflection effects, when the cracks meet fibers in a specific orientation and distribution, the cracks are difficult to deflect and can only continue to expand along the original expansion path, because the elastic coefficient of the fibers is slightly larger than that of a base material, the fibers at the tip of the cracks are not broken and are arranged at the two ends of the cracks, and the carbon fibers effectively counteract the action of external tensile stress, so that the cracks do not have power for continuing expansion, and the toughening effect is achieved. The polycrystalline diamond compact prepared by carbon fiber reinforcement can form a three-dimensional conductive network in the material. The initial oxidation temperature of the composite sheet prepared by the embodiment is 950 ℃, the initial oxidation temperature is increased by about 190 ℃, and the impact toughness is increased by 56%. The conductivity is improved by 20 times.
Example 3
The preparation method of the high-toughness conductive polycrystalline diamond compact in this embodiment is as follows:
step 1, preparing raw materials:
weighing 86wt% of silicon-plated diamond micro powder with the grain size of 30-50 microns, 1wt% of carbon fiber with the grain size of 1-10 microns, 9wt% of diamond micro powder with the grain size of 4-8 microns and 4wt% of iron-nickel alloy powder with the grain size of 2-8 nm respectively, uniformly mixing under a ball mill, wherein the ball mill adopts a ball-to-material ratio of 1:1, the mass of a mixed material consisting of the silicon-plated diamond micro powder, the carbon fiber, the diamond micro powder and the iron-nickel alloy powder is 1-6 g, the ball milling medium is absolute ethyl alcohol with the dosage of 10mL, the rotating speed of the ball mill is 600r/min, the diameter of a steel ball in the ball mill is 2mm, a part of absolute ethyl alcohol is added every 2h in the ball milling process, the ball mill is stopped after 48 hours of ball milling, the ball mill is opened, the absolute ethyl alcohol is evaporated to dryness, the mixed diamond powder mixed with a binder is firstly put into a graphite cup, then the graphite cup filled with the material is put into a vacuum furnace for vacuum heat treatment, oxygen, water vapor and the surface of the powder is well reacted with the highest temperature of 3 × 10 ℃ and the vacuum degree of the mixed powder is obtained, the vacuum furnace, the vacuum degree is-3Pa; weighing 1-6 g of mixed powder subjected to vacuum heat treatment and hard alloy, putting the mixed powder and the hard alloy into a metal molybdenum container, and putting the metal molybdenum container into a dieCarrying out pre-pressing molding in the mold, wherein the pre-pressing pressure is 10MPa, and the pressure maintaining time is 60s, so as to obtain a composite material;
and 2, high-temperature high-pressure sintering:
placing the composite material 3 subjected to impurity removal and cold pressing in a zirconium oxide wrapping container 1 along with a metal molybdenum container wrapped outside the composite material 3, placing in a six-side top large-cavity press with the volume ratio of 6 x 40MN, increasing the pressure to the sintering pressure of 6.0GPa at the pressure increasing rate of 0.6GPa/min, rapidly increasing the temperature at the temperature increasing rate of 40 ℃/s to 1400 ℃, preserving the temperature for 60s, rapidly increasing the temperature to 1700 ℃ within 30s after heat preservation, preserving the temperature for 900s, reducing the temperature to 600 ℃ at the temperature reducing rate of 25 ℃/min after sintering, preserving the temperature for 3min, reducing the temperature to room temperature, and reducing the pressure to normal pressure at the pressure reducing rate of 0.5 GPa/min. Removing the metal molybdenum container wrapped outside the sample of the composite sheet from the sand blasting machine to obtain the polycrystalline diamond composite sheet, and performing primary observation on the polycrystalline diamond composite sheet by using a body microscope to ensure that the surface of a sintered body is uniformly sintered without defects such as pits, cracks and the like;
step 3, grinding and polishing the polycrystalline diamond compact obtained in the step 2 to obtain the high-toughness conductive polycrystalline diamond compact;
the Si of the silicon-plated diamond is completely participated in forming new phases or bonding, and new phases of SiC ceramic exist. Si has the same lattice structure and lattice constant as diamond and thus wets the diamond surface well. The expansion coefficient of SiC is similar to that of diamond, so that the thermal residual stress of the PDC due to the difference of the thermal expansion coefficients is effectively reduced, and the impact toughness and the high temperature resistance of the PDC are improved. During an impact resistance test, the uniformly dispersed carbon fibers have fiber bridging and crack deflection effects, when the cracks meet fibers in a specific orientation and distribution, the cracks are difficult to deflect and can only continue to expand along the original expansion path, because the elastic coefficient of the fibers is slightly larger than that of a base material, the fibers at the tip of the cracks are not broken and are arranged at the two ends of the cracks, and the carbon fibers effectively counteract the action of external tensile stress, so that the cracks do not have power for continuing expansion, and the toughening effect is achieved. The polycrystalline diamond compact prepared by carbon fiber reinforcement can form a three-dimensional conductive network in the material. The initial oxidation temperature of the composite sheet prepared by the embodiment is 988 ℃, the initial oxidation temperature is improved by about 228 ℃, and the impact toughness is improved by 62%. The conductivity is improved by 21 times.
Example 4
The preparation method of the high-toughness conductive polycrystalline diamond compact in this embodiment is as follows:
step 1, preparing raw materials:
according to the weight percentage, 85wt% of silicon-plated diamond micro powder with the grain size of 30-50 mu m, 0.5wt% of carbon fiber with the grain size of 10-20 nm, 5wt% of diamond micro powder with the grain size of 4-8 mu m, 5wt% of diamond micro powder with the grain size of 8-12 mu m and 4.5wt% of iron-nickel alloy powder with the grain size of 2-8 nm are respectively weighed and uniformly mixed under a ball mill, the ball mill adopts a ball-material ratio of 1:1, the mass of a mixed material consisting of the silicon-plated diamond micro powder, the carbon fiber, the diamond micro powder and the iron-nickel alloy powder is 1-6 g, a ball milling medium is absolute ethyl alcohol with the dosage of 10mL, the rotating speed of the ball mill is 600r/min, the diameter of a steel ball in the ball mill is 2mm, a part of the absolute ethyl alcohol is added every 2h in the ball milling process, the ball mill is stopped after 48 h, the ball mill is opened, the absolute ethyl alcohol is evaporated to dryness, the mixed diamond powder is firstly put into a graphite cup to be placed in a vacuum adsorption furnace to be subjected to heat treatment, the surface of the graphite cup, the graphite cup is heated to obtain the mixed powder with the highest temperature of 353 and the vacuum reaction temperature of the vacuum reaction is equal to obtain the active vapor-3Pa; weighing 1-6 g of mixed powder subjected to vacuum heat treatment and hard alloy, putting the mixed powder and the hard alloy into a metal molybdenum container, and putting the metal molybdenum container into a mold for prepressing molding, wherein the prepressing pressure is 10MPa, and the pressure maintaining time is 60s, so as to obtain a composite material;
and 2, high-temperature high-pressure sintering:
placing the composite material 3 subjected to impurity removal and cold pressing in a zirconium oxide wrapping container 1 along with a metal molybdenum container wrapped outside the composite material 3, placing in a six-side top large-cavity press with the volume ratio of 6 x 40MN, increasing the pressure to the sintering pressure of 6.0GPa at the pressure increasing rate of 0.6GPa/min, rapidly increasing the temperature at the temperature increasing rate of 40 ℃/s to 1400 ℃, preserving the temperature for 60s, rapidly increasing the temperature to 1700 ℃ within 30s after heat preservation, preserving the temperature for 900s, reducing the temperature to 600 ℃ at the temperature reducing rate of 25 ℃/min after sintering, preserving the temperature for 3min, reducing the temperature to room temperature, and reducing the pressure to normal pressure at the pressure reducing rate of 0.5 GPa/min. Removing the metal molybdenum container wrapped outside the sample of the composite sheet from the sand blasting machine to obtain the polycrystalline diamond composite sheet, and performing primary observation on the polycrystalline diamond composite sheet by using a body microscope to ensure that the surface of a sintered body is uniformly sintered without defects such as pits, cracks and the like;
step 3, grinding and polishing the polycrystalline diamond compact obtained in the step 2 to obtain the high-toughness conductive polycrystalline diamond compact;
the Si of the silicon-plated diamond is completely participated in forming new phases or bonding, and new phases of SiC ceramic exist. Si has the same lattice structure and lattice constant as diamond and thus wets the diamond surface well. The expansion coefficient of SiC is similar to that of diamond, so that the thermal residual stress of the PDC due to the difference of the thermal expansion coefficients is effectively reduced, and the impact toughness and the high temperature resistance of the PDC are improved. During an impact resistance test, the uniformly dispersed carbon fibers have fiber bridging and crack deflection effects, when the cracks meet fibers in a specific orientation and distribution, the cracks are difficult to deflect and can only continue to expand along the original expansion path, because the elastic coefficient of the fibers is slightly larger than that of a base material, the fibers at the tip of the cracks are not broken and are arranged at the two ends of the cracks, and the carbon fibers effectively counteract the action of external tensile stress, so that the cracks do not have power for continuing expansion, and the toughening effect is achieved. The polycrystalline diamond compact prepared by carbon fiber reinforcement can form a three-dimensional conductive network in the material. The initial oxidation temperature of the composite sheet prepared by the embodiment is 1050 ℃, the initial oxidation temperature is increased by about 290 ℃, and the impact toughness is increased by 66%. The conductivity is improved by 23 times.

Claims (5)

1. A high-toughness conductive polycrystalline diamond compact is characterized in that the high-toughness conductive polycrystalline diamond compact is prepared by sintering silicon-plated diamond micro powder, carbon fiber, diamond micro powder and iron-nickel alloy powder serving as mixed powder with a cubic apparatus large-cavity press and a hard alloy under the conditions that the pressure is 5.5 GPa-6.0 GPa and the temperature is 1500-1700 ℃; wherein, the dosage of the silicon-plated diamond micro powder, the carbon fiber, the diamond micro powder and the iron-nickel alloy powder is as follows according to the weight percentage: 80-95 wt% of silicon-plated diamond micro powder, 0.1-2 wt% of carbon fiber, 1-10 wt% of diamond micro powder and 1-10 wt% of iron-nickel alloy powder;
the grain diameter of the silicon-plated diamond micro powder is 30-50 mu m;
the particle size of the carbon fiber is 1 nm-100 mu m;
the grain size of the diamond micro powder is 0.1-12 mu m;
the particle size of the iron-nickel alloy powder is 1 nm-8 mu m;
the fracture toughness reaches 9.4 (+/-0.3) MPa.m1/2Impact crush energy 30 (+ -2) J.
2. The high-toughness conductive polycrystalline diamond compact according to claim 1, wherein the mass ratio of iron to nickel in the iron-nickel alloy powder is 5: 5.
3. The high toughness conductive polycrystalline diamond compact of claim 1, wherein the hard alloy is a tungsten-cobalt alloy, and the cobalt content of the hard alloy is 15-16%.
4. A high toughness conductive polycrystalline diamond compact according to claim 3, wherein the diameter of the cemented carbide is 10mm to 30mm, and the thickness is 4mm to 8 mm.
5. A method of making the high toughness, electrically conductive polycrystalline diamond compact of claim 1, comprising the steps of:
step 1, preparing raw materials:
firstly, carrying out acid treatment on the surface of the diamond micro powder to remove residual metal impurities on the surface of the diamond micro powder, washing the diamond micro powder to be neutral by distilled water, and placing the diamond micro powder into a drying container for later use after drying;
hard alloy purification treatment: performing ultrasonic extraction under the condition of absolute ethyl alcohol to remove impurities on the surface of the hard alloy;
③ the dosage of the silicon-plated diamond micro powder 80, the carbon fiber, the diamond micro powder and the iron-nickel alloy powder in percentage by weightRespectively weighing the components by weight percent to 95 percent, the carbon fiber by weight percent to 0.1 percent to 2 percent, the diamond micro powder by weight percent to 1 percent and the iron-nickel alloy powder by weight percent to 1 percent, uniformly mixing the components in a ball mill, putting the mixed powder into a graphite cup by ball-to-material ratio of 1:1, and then putting the graphite cup filled with the powder into a vacuum furnace for vacuum heat treatment, wherein the maximum temperature in the vacuum furnace is 650 ℃, and the vacuum degree is 3 × 10-3Pa, obtaining mixed powder, putting the obtained mixed powder and the purified hard alloy into a metal container, and tabletting to obtain a composite material;
step 2, a high-temperature high-pressure assembly sintering process:
placing the composite material subjected to impurity removal and cold pressing in a zirconium oxide wrapping container along with a metal container wrapped outside the composite material, placing the composite material in a cubic apparatus large-cavity press, sintering at high temperature and high pressure, and keeping the temperature for a preset time in the sintering process to obtain a polycrystalline diamond compact;
in the high-temperature high-pressure sintering process, the range of the sintering pressure P is 5.5GPa < P <6.0GPa, the range of the sintering temperature T is 1500 ℃ < T <1700 ℃, and the range of the sintering duration T is 5min < T <20 min;
step 3, grinding and polishing the polycrystalline diamond compact obtained in the step 2 to obtain the high-toughness conductive polycrystalline diamond compact;
in the step 2, during sintering, the pressure is increased to the sintering pressure at the pressure increasing rate of 0.5 GPa/min-1 GPa/min, the temperature is increased to the sintering temperature at the temperature increasing rate of 20 ℃/s-40 ℃/s for high-temperature sintering, the temperature is maintained at 1400 ℃ for 60s, the temperature is increased to the sintering temperature within 30s, the temperature is reduced to 600 ℃ at the temperature decreasing rate of 15 ℃/s-30 ℃/s after sintering, the temperature is reduced to the room temperature after 3 min-5 min, and the pressure is reduced to the normal pressure at the pressure reducing rate of 0.1 GPa/min-0.8 GPa/min.
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