CN110578128B - Preparation method of dome-shaped polycrystalline diamond compact - Google Patents

Preparation method of dome-shaped polycrystalline diamond compact Download PDF

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CN110578128B
CN110578128B CN201910790693.1A CN201910790693A CN110578128B CN 110578128 B CN110578128 B CN 110578128B CN 201910790693 A CN201910790693 A CN 201910790693A CN 110578128 B CN110578128 B CN 110578128B
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hard alloy
pressure
polycrystalline diamond
diamond
diamond compact
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张涛
卢灿华
宋子衡
朱培
邱林
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Zhongnan Diamond Co Ltd
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    • 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
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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Abstract

The invention discloses a preparation method of a circular arch polycrystalline diamond compact, which comprises the following steps: 1) purifying the hard alloy matrix; 2) depositing a transition layer on the surface of the hard alloy substrate; 3) ion implantation into diamond; 4) mixing materials; 5) assembling the complex; 6) purifying the complex; 7) and (4) sintering at high temperature and high pressure. The invention utilizes ion beam implantation technology to implant N on the surface of diamond+And B+The chemical vapor deposition technology is utilized to sequentially deposit the silicon carbide layer and the silicon carbide-diamond gradient composite layer on the hard alloy surface, so that the stress between the polycrystalline diamond layer and the hard alloy matrix is reduced, and the bonding strength of the polycrystalline diamond and the hard alloy matrix is improved.

Description

Preparation method of dome-shaped polycrystalline diamond compact
Technical Field
The invention belongs to the technical field of superhard materials, and particularly relates to a circular arch polycrystalline diamond compact and a preparation method thereof.
Background
The polycrystalline diamond compact is a superhard composite material consisting of a polycrystalline diamond layer and a hard alloy substrate, and the polycrystalline diamond compact integrates the advantages of two materials, namely the polycrystalline diamond and the hard alloy, and the polycrystalline diamond layer can always keep a sharp cutting edge, so that the polycrystalline diamond compact is widely applied to geological and oil drilling and obtains a very good use effect in soft to medium hard rock layers.
Although the advantages of the polycrystalline diamond layer and the hard alloy matrix can be combined into a single product by connecting the two materials together, due to the inherent difference in properties of the two materials, the interface of the two materials becomes the weakest area of the product, and in the high-temperature and high-pressure sintering process, the thermal expansion coefficient, the elastic modulus and other physical performance parameters of the polycrystalline diamond layer and the hard alloy matrix are greatly different, so that serious thermal residual stress inevitably exists at the interface, the adhesion between the polycrystalline diamond and the hard alloy matrix is not strong, the impact resistance is poor, interface cracks are easily formed, and the polycrystalline diamond layer is easy to fall off and break during working, so that the drill bit fails. At present, traditional flat tooth and special-shaped tooth diamond composite sheets (such as shallow concave surface PDC, tapered PDC, ridge-shaped PDC and the like) on the market are weak when applied to deep complicated hard rock stratums, and the development of a drilling technology is seriously influenced by the frequently occurring tooth breakage and the lower drilling efficiency.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the dome-shaped polycrystalline diamond compact and the preparation method thereof, so that the wear resistance, the heat resistance and the impact resistance of the dome-shaped polycrystalline diamond compact are improved, the service life of the dome-shaped polycrystalline diamond compact is further prolonged, and the continuous working efficiency is improved.
To achieve the above object, the present invention prepares a dome-shaped polycrystalline diamond compact using a method comprising the steps of:
step 1) hard alloy matrix purification treatment: purifying the hard alloy matrix to obtain a purified hard alloy matrix; the selected hard alloy matrix consists of the following raw materials in percentage by weight: 5-8% of cobalt, 2-3% of tantalum-niobium solid solution (TaC: NbC = 6: 4), 89.5-91% of tungsten carbide and 0.5-1% of samarium oxide, wherein the hardness of the hard alloy is greater than 93HRA, and the bending strength is greater than 2500N/mm;
step 2) depositing a transition layer on the surface of the hard alloy substrate: sequentially depositing a silicon carbide layer and a silicon carbide-diamond gradient composite layer on the surface of the purified hard alloy substrate by adopting a chemical vapor deposition method to serve as a transition layer, so as to obtain the hard alloy substrate with the transition layer deposited on the surface;
step 3), ion implantation of diamond: sequentially injecting N into the surface of the diamond micropowder by ion injection equipment+And B+To obtain a compound containing N+And B+The diamond micro powder;
step 4), mixing materials: the said N is contained+And B+The diamond micro powder and the bonding agent are poured into a ball milling tank and are placed in a ball mill for ball milling and mixing to obtain mixed powder, wherein the material proportion of the bonding agent in the mixed powder is 5-10% (weight percentage);
step 5) assembling a complex: pouring the mixed powder into a metal vessel to be scraped, putting the transition layer of the hard alloy substrate with the transition layer deposited on the surface into the metal vessel with the transition layer facing downwards, and then performing prepressing molding through a mold to obtain a composite assembly;
step 6) complex purification: placing the composite assembly in a vacuum sintering furnace, and vacuumizing and heating to obtain a purified composite assembly;
step 7), high-temperature high-pressure sintering: and placing the purified composite body assembly in a synthesis assembly block, and performing high-temperature and high-pressure sintering by using a cubic press to prepare the circular arch polycrystalline diamond compact.
Further, in step 1), the cemented carbide substrate cleaning treatment: firstly, immersing a hard alloy substrate into deionized water and potassium hydroxide according to a mass ratio of 1: boiling in alkali liquor prepared by 0.1-0.2 for 2-5 min, and then soaking the hard alloy matrix in sulfuric acid with the mass fraction of 98% and deionized water according to the volume ratio of 1: 4-5 ultrasonic vibration cleaning in sulfuric acid solution for 2-5 min, then immersing in acetone or absolute ethyl alcohol for ultrasonic vibration cleaning for 5-10 min, finally placing the hard alloy substrate in a vacuum sintering furnace, wherein the air pressure in the furnace is not more than 4 multiplied by 10-4Pa, at a temperature of 500-600 DEG CAnd introducing carbon monoxide reducing gas until the pressure in the furnace is 15-20 Mbar, and carrying out vacuum treatment on the hard alloy matrix for 1-2 hours.
Further, in step 2), the depositing the transition layer includes the following steps: firstly, hot wire chemical vapor deposition equipment is adopted, hydrogen and tetramethylsilane are used as reaction gases, tetramethylsilane accounts for 0.01-1% of the total gas volume, a silicon carbide layer with the thickness of 4-6 mu m is deposited on the surface of a hard alloy substrate, then hydrogen, methane and tetramethylsilane are used as the reaction gases, the flow of methane is controlled in the reaction process, so that the proportion of methane in the total gas volume is gradually increased from 0.4% to 3%, meanwhile, the proportion of tetramethylsilane in the total gas volume is gradually reduced from 0.3% to 0.01%, and a silicon carbide-diamond gradient composite layer with the thickness of 30-40 mu m is formed on the surface of the silicon carbide layer through deposition.
In the deposition process, the vacuum chamber air pressure of the hot wire chemical vapor deposition equipment is 3-10 kPa, the filament temperature is 1500-2600 ℃, and the temperature of the hard alloy substrate is 700-900 ℃.
Further, in step 3), the specific operation of ion implanting the diamond is as follows: placing diamond micropowder with the particle size of 5-35 mu m in a vacuum working cavity of an ion implanter, separating ions supplied by an ion source into monovalent nitrogen ions by a mass spectrometer, accelerating the monovalent nitrogen ions by an electric field, and carrying out particle size reduction on the monovalent nitrogen ions by 4 x 1014～4×1016 N+/cm2Is implanted into the surface of the diamond with an energy of 50 to 80keV, and then ions supplied from an ion source are separated into monovalent boron ions which are accelerated by an electric field and are 4 x 1014～4×1016 B+/cm2The ion density and the energy of 50-100 keV are implanted into the surface of the diamond.
Further, in the step 4), the binder is composed of the following raw materials in percentage by weight: 2-4% of titanium, 1.5-2% of tungsten, 1.5-2% of zirconium, 1-1.5% of chromium, 0.25-1% of inorganic nonmetal whisker, 0.25-0.5% of rare earth oxide and the balance of cobalt.
The inorganic non-metal whisker is one or two of alumina, zirconia, silicon carbide and boron fiber, the length of the whisker is in the range of 100 nanometers to 20 micrometers, and the diameter of the whisker is not more than 100 nanometers.
The rare earth oxide is one or two of thulium oxide, samarium oxide, europium oxide, praseodymium oxide, ytterbium oxide, dysprosium oxide, holmium oxide, moment oxide and scandium oxide.
Further, in the step 4), the mixing operation is as follows: firstly, according to the mass ratio of the ball grinding body to the binding agent (4-8): 1, placing the bonding agent in a ball milling tank of a ball mill for ball milling for 5-10 h; and then, according to the mass ratio of the ball grinding body to the diamond micropowder of (8-12): 1, placing the diamond micro powder in a ball milling tank of a ball mill to be ball milled for 12-24 hours together with the bonding agent, wherein the specific ball milling mode is as follows: firstly, rotating at a speed of 30-40 r/min for two minutes in clockwise operation, then rotating at a speed of 20-30 r/min for two minutes in anticlockwise operation, and performing ball milling and mixing in such an alternate operation manner; the ball milling body and the ball milling tank are made of zirconia materials.
Further, in step 5), the metal vessel is made of zirconium, niobium, molybdenum, tantalum or an alloy thereof.
Further, in step 6), the evacuating and heating include: roughly vacuumizing the furnace until the pressure in the furnace reaches 8 x 10-2Heating to 180-230 ℃ below Pa, preserving heat for 0.5-1 h, then continuously vacuumizing and heating to 500-600 ℃ until the pressure in the furnace is stabilized at 3 x 10-3Pa below, stopping vacuumizing, charging carbon monoxide gas into the vacuum heating furnace at 500-600 ℃ until the pressure in the furnace is 60-80 Mbar, reducing the composite assembly for 2-3 h under the condition, and vacuumizing until the pressure in the furnace is 4 multiplied by 10-4Pa below, heating to 900-1000 deg.C, and continuously vacuumizing until the furnace pressure is stabilized at 3 × 10-3And (4) performing vacuum treatment on the composite assembly for 1-2 hours under the condition of Pa or less.
Further, in step 7), the specific operation of the high-temperature high-pressure sintering is as follows: during sintering, the pressure is increased to 6-7 GPa at the pressure increasing rate of 0.1-1 GPa/min, then the temperature is increased to the sintering temperature of 1450-1550 ℃ at the temperature increasing rate of 15-30 ℃/min for sintering, after the sintering is carried out for 150-800 s, the temperature is reduced to the normal temperature at the temperature reducing rate of 10-30 ℃/min, and the pressure is reduced to the normal pressure at the pressure reducing rate of 0.1-0.5 GPa/min.
The dome-shaped polycrystalline diamond compact obtained by the preparation method comprises the following steps: the polycrystalline diamond hard alloy comprises a hard alloy substrate, and a transition layer and a polycrystalline diamond layer which are arranged on the surface of the hard alloy substrate, wherein the upper surface of the polycrystalline diamond layer is in a circular arch shape; the lower part of the hard alloy matrix is a cylinder, the upper part of the hard alloy matrix is a hemisphere, and the hemisphere and the cylinder are integrally formed.
The invention has the following beneficial effects:
(1) according to the invention, the silicon carbide layer and the silicon carbide-diamond gradient composite layer are sequentially deposited on the surface of the hard alloy substrate by adopting a chemical vapor deposition method, so that the diffusion of cobalt element of the hard alloy substrate to the polycrystalline diamond layer can be effectively inhibited, the excellent performance is ensured, the bonding strength between the hard alloy substrate and the polycrystalline diamond layer is greatly enhanced, and the service life of the polycrystalline diamond layer is greatly prolonged. Further, the silicon carbide has an expansion coefficient of (1.8X 10)-3K) between the cemented carbide (4.8 x 10)-3K) and polycrystalline diamond (1.5X 10)-3K), thereby effectively improving the problem of overlarge residual stress caused by large difference of thermal expansion coefficients.
(2) The invention adopts an ion beam implantation method to implant N on the surface of the diamond+And B+The structural defect on the surface of the common diamond particle is made up, and the thermal stability of the polycrystalline diamond compact is improved: the reason is that: the lattice constant close to that of the diamond enables nitrogen atoms to enter the lattice of the diamond, so that the effects of substituting and supplementing vacancies are achieved, the structure of the diamond is more complete, and the thermal stability of the diamond is improved; boron differs in its mechanism of action, being concentrated mainly on the surface, with B being formed when heated2O3，B2O3Has a low melting point, is easily melted and reacts with a metal oxide to form a stable borate, thus slowing down the oxidation rate of diamond carbon (C) and improving the thermal stability of diamond.
(3) The test performance indexes of the dome-shaped polycrystalline diamond compact obtained by the method are as follows: the abrasion ratio is 38-42 ten thousand, the impact toughness is 1200-1300 joules, and the performance indexes of the traditional flat-tooth diamond composite sheet are obviously improved.
(4) The circular arch polycrystalline diamond compact obtained by the method can be applied to a deep layer complex hard rock stratum, compared with the traditional flat-tooth diamond compact, the service life of the circular arch polycrystalline diamond compact is prolonged by more than 35%, the cost is saved, the time is saved, and the drilling efficiency can be greatly improved.
Drawings
Fig. 1 is a schematic cross-sectional view of a dome-shaped polycrystalline diamond compact of the present disclosure at a central axis of symmetry;
in the figure: 1. a cemented carbide substrate; 2. a silicon carbide layer; 3. a silicon carbide-diamond transition layer; 4. a polycrystalline diamond layer.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention.
Example 1
A preparation method of a circular arch polycrystalline diamond compact comprises the following steps:
step 1) matrix purification treatment: the hard alloy matrix consists of the following raw materials in percentage by weight: 5% of cobalt, 3% of tantalum-niobium solid solution (TaC: NbC = 6: 4), 91% of tungsten carbide and 1% of samarium oxide, wherein the hardness of the hard alloy is 93.5HRA, and the bending strength is 2550N/mm; firstly, immersing a hard alloy substrate into deionized water and potassium hydroxide according to a mass ratio of 1: boiling in 0.1 prepared alkali liquor for 2min, and then immersing the hard alloy matrix into sulfuric acid with the mass fraction of 98% and deionized water in a volume ratio of 1: 4 ultrasonic vibration cleaning in sulfuric acid solution prepared by 4 for 2min, then immersing in acetone solution for ultrasonic vibration cleaning for 5min, then placing the hard alloy substrate in a vacuum sintering furnace, wherein the air pressure in the furnace is not more than 4 multiplied by 10-4Pa, the temperature is 500 ℃, carbon monoxide reducing gas is filled to the pressure of 15Mbar in the furnace, and the hard alloy matrix is vacuumizedTreating for 1 h;
step 2) depositing a transition layer on the surface of the hard alloy substrate: adopting hot filament chemical vapor deposition equipment, setting the air pressure of a vacuum chamber to be 3kPa, the filament temperature to be 1500 ℃, the temperature of a hard alloy substrate to be 700 ℃, hydrogen and tetramethylsilane are used as reaction gases, tetramethylsilane accounts for 0.01 percent of the total gas volume (volume ratio, the same applies below), depositing a silicon carbide layer with the thickness of 4 mu m on the surface of the hard alloy substrate, then introducing methane into the hot wire chemical vapor deposition equipment, namely, hydrogen, methane and tetramethylsilane are used as reaction gases, the methane accounts for 0.4 percent of the total gas volume (volume ratio, the same below), the tetramethylsilane accounts for 0.3 percent of the total gas volume (volume ratio, the same below), and depositing on the surface of the silicon carbide to form a silicon carbide-diamond transition composite layer with the thickness of 30 mu m, and gradually increasing the flow of methane to 3% and simultaneously gradually reducing the flow of tetramethylsilane from 0.3% to 0.01% in the reaction process.
Step 3), ion implantation of diamond: placing diamond micropowder with the particle size of 5-35 mu m in a vacuum working cavity of an ion implanter, separating ions supplied by an ion source into monovalent nitrogen ions by a mass spectrometer, accelerating the monovalent nitrogen ions by an electric field, and carrying out particle size reduction on the monovalent nitrogen ions by 4 x 1014 N+/cm2Is implanted into the surface of the diamond at an energy of 50keV, and then the ions supplied from the ion source are separated into monovalent boron ions which are accelerated by an electric field at 4 x 1014 B+/cm2And an energy of 50keV into the surface of the diamond;
step 4), mixing materials: the said N is contained+And B+The diamond micro powder and the bonding agent are respectively weighed according to the weight percentage of 90 percent and 10 percent, and the mass ratio of the ball grinding body to the bonding agent is 4: 1, placing the bonding agent in a ball milling tank of a ball mill for ball milling for 5 hours; then, according to the mass ratio of the ball grinding body to the diamond micropowder of 8: 1, putting the diamond micro powder into a ball milling tank of a ball mill, and carrying out ball milling for 12 hours together with the bonding agent; the specific ball milling process is as follows: running for 2min at 30 r/min clockwise, then running for 2min at 20 r/min anticlockwise, and performing ball milling to obtain mixed powder;
wherein the ball milling body and the ball milling tank are made of zirconia materials; the binding agent is composed of the following raw materials in percentage by weight: 89% of cobalt, 4% of titanium, 2% of tungsten, 2% of zirconium, 1.5% of chromium, 1% of aluminum oxide whisker and 0.5% of samarium oxide.
Step 5) assembling a complex: pouring the mixed powder into a tantalum cup, leveling the mixed powder, placing the hard alloy substrate transition layer with the transition layer deposited on the surface downwards into the tantalum cup, and then performing prepressing molding through a mold to obtain a composite assembly;
step 6) complex purification: placing the composite assembly in a vacuum sintering furnace, and vacuumizing and heating to obtain a purified composite assembly; wherein, the specific operations of vacuumizing and heating are as follows: roughly vacuumizing the furnace until the pressure in the furnace reaches 8 x 10-2Heating to 180 deg.C below Pa, maintaining for 0.5h, vacuumizing, heating to 500 deg.C, and stabilizing furnace pressure at 3 × 10-3Pa below, stopping vacuumizing, introducing carbon monoxide gas with gas pressure of 60Mbar into the vacuum heating furnace at 500 deg.C to reduce the complex assembly for 2 hr, and vacuumizing to 4 × 10-4Continuously vacuumizing and heating to 900 deg.C below Pa until furnace pressure is stabilized at 3 × 10-3And (4) performing vacuum treatment on the composite assembly for 1h under Pa.
Step 7), high-temperature high-pressure sintering: placing the purified composite assembly in a synthesis assembly block, and sintering at high temperature and high pressure by using a cubic press to prepare a circular arch polycrystalline diamond compact; the high-temperature high-pressure sintering operation comprises the following specific steps: during sintering, the pressure is increased to 6GPa at the rate of 0.1GPa/min, then the temperature is rapidly increased to 1450 ℃ at the rate of 15 ℃/min for sintering, the temperature is reduced to normal temperature at the rate of 10 ℃/min after sintering for 150s, and the pressure is reduced from high pressure to normal pressure at the rate of 0.1 GPa/min.
As shown in fig. 1, the dome-shaped polycrystalline diamond compact obtained by the preparation method sequentially comprises a hard alloy substrate, a transition layer and a polycrystalline diamond layer from bottom to top on the surface of the hard alloy substrate, wherein the upper surface of the polycrystalline diamond layer is in a dome shape; the lower part of the hard alloy matrix is a cylinder, the upper part of the hard alloy matrix is a hemisphere, and the hemisphere and the cylinder are integrally formed;
A. and (3) performance testing:
respectively carrying out performance tests on the dome-shaped polycrystalline diamond compact obtained by the method and the traditional flat-tooth diamond compact with the same specification, wherein the test results are as follows: the abrasion ratio of the dome-shaped polycrystalline diamond compact is 40 ten thousand, the impact toughness is 1210 joules, the test standard of the abrasion ratio is JB/T3235-2013 'method for measuring the abrasion ratio of an artificial diamond sintered body', and the impact toughness is tested by adopting a drop hammer impact method (namely, the dome-shaped polycrystalline diamond compact is fixed on a punch head of a hammer dropping frame of an impact machine and is impacted by energy of 20 and 30J in sequence, the impact times corresponding to each impact energy are 20 and 30 in sequence, and under the condition that a diamond polycrystalline layer does not crack or fall off, the sum of the obtained energy is used as the impact toughness value of a sample). The abrasion ratio of the traditional flat-tooth diamond composite sheet is 30 ten thousand, the impact toughness is 800 joules, compared with the traditional flat-tooth diamond composite sheet, the abrasion resistance is improved by 33 percent, the impact toughness is improved by 51 percent, and the performance of the circular arch polycrystalline diamond composite sheet is obviously improved.
B. Drilling test
The circular arch polycrystalline diamond composite sheet obtained by the method and the traditional flat-tooth diamond composite sheet with the same specification are manufactured into 1 standard drill bit respectively, the same drilling parameters (the bit pressure is 60 KN, the rotating speed is 75r/min, the discharge capacity is 38L/S, and the mechanical drilling speed is 45 m/h) are adopted, after the circular arch polycrystalline diamond composite sheet drill bit is drilled into a gravel-containing interlayer stratum by 2000m, the traditional flat-tooth diamond composite sheet drill bit is seriously damaged, the circular arch polycrystalline diamond composite sheet drill bit can still be used, the phenomena of breakage, cracks and layering are avoided, compared with the traditional flat-tooth diamond composite sheet drill bit, the service life is prolonged by 38%, and the drilling efficiency is obviously improved.
Example 2
A preparation method of a circular arch polycrystalline diamond compact comprises the following steps:
step 1) hard alloy matrix purification treatment: the hard alloy matrix consists of the following raw materials in percentage by weight: 8% of cobalt, 2% of tantalum-niobium solid solution (TaC: NbC = 6: 4), 89.5% of tungsten carbide and 0.5% of samarium oxide, wherein the hardness of the hard alloy is 94HRA, and the bending strength is 2530N/mm; firstly, immersing a hard alloy substrate into deionized water and potassium hydroxide according to a mass ratio of 1: boiling in 0.2 prepared alkali liquor for 5min, and then immersing the hard alloy matrix into sulfuric acid with the mass fraction of 98% and deionized water according to the volume ratio of 1: 5 ultrasonic vibration cleaning for 5min in the prepared sulfuric acid solution, and then soaking in absolute ethyl alcohol for ultrasonic vibration cleaning for 10 min. Then the hard alloy substrate is placed in a vacuum sintering furnace, and the pressure in the furnace is not more than 4 multiplied by 10-4Pa, the temperature is 600 ℃, carbon monoxide reducing gas with the pressure of 20Mbar in the furnace is filled in to carry out vacuum treatment on the hard alloy matrix for 2 hours.
Step 2) depositing a transition layer on the surface of the hard alloy substrate: adopting hot-wire chemical vapor deposition equipment, setting the air pressure of a vacuum chamber to be 0kPa, the filament temperature to be 2600 ℃, and the matrix temperature to be 900 ℃; controlling tetramethylsilane to account for 1% of the total gas volume by taking hydrogen and tetramethylsilane as reaction gases, depositing a silicon carbide layer with the thickness of 6 microns on the surface of a hard alloy substrate, then introducing methane into the hot wire chemical vapor deposition equipment, namely, controlling methane to account for 0.4% (volume ratio, the same below) of the total gas volume by taking hydrogen, methane and tetramethylsilane as reaction gases, depositing and forming a silicon carbide-diamond transition composite layer with the thickness of 40 microns on the surface of the silicon carbide, gradually increasing the methane flow to 3% in the reaction process, and gradually reducing the tetramethylsilane flow from 0.3% to 0.01%.
Step 3), ion implantation of diamond: placing diamond micropowder with the particle size of 5-35 mu m in a vacuum working cavity of an ion implanter, separating ions supplied by an ion source into monovalent nitrogen ions by a mass spectrometer, accelerating the monovalent nitrogen ions by an electric field, and carrying out particle size reduction on the monovalent nitrogen ions by 4 x 1016 N+/cm2Is implanted into the surface of the diamond at an energy of 100keV, and then the ions supplied from the ion source are separated into monovalent boron ions which are accelerated by an electric field at 4 x 1016 B+/cm2And an energy of 80keV into the surface of the diamond.
Step 4), mixing materials: the said N is contained+And B+The diamond micro powder and the bonding agent are respectively weighed according to the weight percentage of 95 percent and 5 percent, and the mass ratio of the ball grinding body to the bonding agent is 8: 1, placing the bonding agent in a ball milling tank of a ball mill for ball milling for 10 hours; then, according to the mass ratio of the ball grinding body to the diamond micropowder of 12: 1, putting the diamond micro powder into a ball milling tank of a ball mill, and carrying out ball milling for 24 hours together with the bonding agent; the specific ball milling process is as follows: running for 2min at 40 r/min clockwise and running for 2min at 30 r/min anticlockwise, and performing ball milling to obtain mixed powder;
wherein the ball milling body and the ball milling tank are made of zirconia materials; the binding agent is composed of the following raw materials in percentage by weight: 93.5 percent of cobalt, 2 percent of titanium, 1.5 percent of tungsten, 1.5 percent of zirconium, 1 percent of chromium, 0.25 percent of silicon carbide whisker and 0.25 percent of europium oxide
Step 5) assembling a complex: firstly, pouring the diamond mixed powder into a molybdenum cup to be stricken off, then putting the hard alloy matrix transition layer containing the transition layer downwards into the molybdenum cup, and then carrying out prepressing molding through a mold to obtain a composite assembly;
step 6) complex purification: placing the composite assembly in a vacuum sintering furnace, and vacuumizing and heating to obtain a purified composite assembly; wherein, the specific operations of vacuumizing and heating are as follows: firstly, the furnace is vacuumized until the air pressure in the furnace reaches 8 multiplied by 10-2Heating to 230 deg.C under Pa, maintaining for 1 hr, vacuumizing and heating to 600 deg.C until the pressure in the furnace is stabilized at 3 × 10-3Stopping vacuumizing below Pa, introducing carbon monoxide gas with an internal gas pressure of 80Mbar into a vacuum heating furnace at 600 deg.C to reduce the complex assembly for 3h, and vacuumizing to an internal gas pressure of 4 × 10-4Below Pa, vacuumizing while heating to 1000 deg.C until the furnace pressure is stabilized at 3 × 10-3And (4) performing vacuum treatment on the composite assembly for 2h under Pa.
Step 7), high-temperature high-pressure sintering: placing the purified composite assembly in a synthesis assembly block, and sintering at high temperature and high pressure by using a cubic press to prepare a circular arch polycrystalline diamond compact; the high-temperature high-pressure sintering operation comprises the following specific steps: during sintering, the pressure is increased to 7GPa at the rate of 1GPa/min, then the temperature is rapidly increased to 1550 ℃ at the rate of 30 ℃/min for sintering, and after sintering for 800s, the temperature is reduced to normal temperature at the rate of 30 ℃/min, and the pressure is reduced from high pressure to normal pressure at the rate of 0.5 GPa/min.
The structure of the dome-shaped polycrystalline diamond compact obtained by the preparation method is the same as that of example 1;
A. performance testing
Respectively carrying out the circular arch polycrystalline diamond compact obtained by the method and the traditional flat-tooth diamond compact with the same specification
Performance test, test result: the abrasion ratio of the circular arch polycrystalline diamond compact is 38 thousands, the impact toughness is 1250 joules, the abrasion ratio of the traditional flat-tooth diamond compact is 29 thousands, the impact toughness is 830 joules, compared with the traditional flat-tooth diamond compact, the abrasion resistance is improved by 31 percent, the impact toughness is improved by 50 percent, and the performance of the circular arch polycrystalline diamond compact is obviously improved.
B. Drilling test
The circular arch polycrystalline diamond compact obtained by the method and the traditional flat-tooth diamond compact with the same specification are manufactured into 1 standard drill bit respectively, and the same drilling parameters (the bit pressure is 60 KN, the rotating speed is 75r/min, the discharge capacity is 38L/S, and the mechanical drilling speed is 45 m/h) are adopted. In the stratum containing the gravel interlayer, after 2000m is drilled, the conventional conical diamond compact drill bit is seriously damaged, the circular arch-shaped polycrystalline diamond compact drill bit can still be used, the phenomena of damage, cracks and layering are avoided, compared with the conventional conical diamond compact drill bit, the service life is prolonged by 36%, and the drilling efficiency is obviously improved.
Example 3
A preparation method of a circular arch polycrystalline diamond compact comprises the following steps:
step 1) hard alloy matrix purification treatment: the hard alloy matrix consists of the following raw materials in percentage by weight: 6.5% cobalt, 2.5% tantalum-niobium solid solution (TaC: NbC = 6: 4), 90.25% tungsten carbide andsamarium oxide 0.75%, the hardness of the hard alloy is more than 93.8HRA, and the bending strength is 2510N/mm; firstly, immersing a hard alloy substrate into deionized water and potassium hydroxide according to a mass ratio of 1: boiling in 0.15 prepared alkali liquor for 2.5min, and then immersing the hard alloy matrix into sulfuric acid with the mass fraction of 98% and deionized water according to the volume ratio of 1: 4.5 ultrasonic vibration cleaning for 2.5min in the prepared sulfuric acid solution, and then immersing in acetone for ultrasonic vibration cleaning for 7.5 min. Then the hard alloy substrate is placed in a vacuum sintering furnace, and the pressure in the furnace is not more than 4 multiplied by 10-4Pa, the temperature is 550 ℃, and carbon monoxide reducing gas with the pressure of 17.5Mbar in the furnace is filled in to carry out vacuum treatment on the hard alloy matrix for 1.5 h.
Step 2) depositing a transition layer on the surface of the hard alloy substrate: adopting hot wire chemical vapor deposition equipment, setting the air pressure of a vacuum chamber to be 6.5kPa, the filament temperature to be 2050 ℃ and the temperature of a hard alloy matrix to be 800 ℃; hydrogen and tetramethylsilane are used as reaction gases, tetramethylsilane accounts for 0.55 percent of the total gas volume, a silicon carbide layer with the thickness of 5 mu m is deposited on the surface of a hard alloy substrate, then methane is introduced into the hot wire chemical vapor deposition equipment, namely, hydrogen, methane and tetramethylsilane are used as the reaction gases, methane accounts for 0.4 percent (volume ratio, the same applies below) of the total gas volume, tetramethylsilane accounts for 0.3 percent (volume ratio, the same applies below) of the total gas volume, a silicon carbide-diamond transition composite layer with the thickness of 35 mu m is deposited on the surface of the silicon carbide, the flow of methane is gradually increased to 3 percent in the reaction process, and the flow of tetramethylsilane is gradually reduced from 0.3 percent to 0.01 percent.
Step 3), ion implantation of diamond: placing common diamond micropowder in vacuum working chamber of ion implanter, separating ions supplied from ion source into monovalent nitrogen ions by mass spectrometer, accelerating with electric field to 4 × 1015N+/cm2Is implanted into the surface of the diamond at an energy of 75keV, and then the ions supplied from the ion source are separated into monovalent boron ions which are accelerated by an electric field to 4 x 1015B+/cm2The ion density and the energy of 65keV are injected into the surface of the diamond, and the granularity of the diamond is 5-35 mu m.
Step 4), mixing materials: the said N is contained+And B+The diamond micro powder and the bonding agent are respectively weighed according to the weight percentage of 92.5 percent and 7.5 percent, and the mass ratio of the ball grinding body to the bonding agent is 6: 1, placing the bonding agent in a ball milling tank of a ball mill for ball milling for 7.5 hours; then, according to the mass ratio of the ball grinding body to the diamond micropowder of 10: 1, putting the diamond micro powder into a ball milling tank of a ball mill, and carrying out ball milling for 13 hours together with the bonding agent; the concrete operation of the mixing is as follows: running for 2min at 35 r/min clockwise and 2min at 25 r/min anticlockwise, and alternately carrying out the steps;
wherein, the bonding agent is composed of the following raw materials by weight percentage: 91.25% of cobalt, 3% of titanium, 1.75% of tungsten, 1.75% of zirconium, 1.25% of chromium, 0.625% of boron fiber whisker and 0.375% of dysprosium oxide; the ball milling body and the ball milling tank are made of zirconia materials.
Step 5) assembling a complex: pouring the mixed powder into a niobium cup and scraping, putting the hard alloy matrix transition layer containing the transition layer downwards into the niobium cup, and then performing prepressing molding through a mold to obtain a composite assembly;
step 6) complex purification: placing the composite assembly in a vacuum sintering furnace, and vacuumizing and heating to obtain a purified composite assembly; wherein, the specific operations of vacuumizing and heating are as follows: firstly, the furnace is vacuumized until the air pressure in the furnace reaches 8 multiplied by 10-2Heating to 205 deg.C below Pa, maintaining for 0.75 hr, vacuumizing while heating to 550 deg.C until the pressure in the furnace is stabilized at 3 × 10-3Pa below, stopping vacuumizing, introducing carbon monoxide gas with an internal gas pressure of 70Mbar into the vacuum heating furnace at 550 deg.C to reduce the complex assembly for 2.5 hr, and vacuumizing to an internal gas pressure of 4 × 10-4Pa below, then continuously vacuumizing and heating to 950 ℃ at the same time until the furnace pressure is stabilized at 3 x 10-3And (4) carrying out vacuum treatment on the composite assembly for 1.2h under Pa.
Step 7), high-temperature high-pressure sintering: placing the purified composite assembly in a synthesis assembly block, and sintering at high temperature and high pressure by using a cubic press to prepare a circular arch polycrystalline diamond compact; the high-temperature high-pressure sintering operation comprises the following specific steps: during sintering, the pressure is increased to 6.5GPa at the rate of 0.55GPa/min, then the temperature is rapidly increased to 1500 ℃ at the rate of 22.5 ℃/min for sintering, after 475s of sintering, the temperature is reduced to normal temperature at the rate of 15 ℃/min, and the pressure is reduced from high pressure to normal pressure at the rate of 0.3 GPa/min.
The structure of the dome-shaped polycrystalline diamond compact obtained by the preparation method is the same as that of example 1;
A. performance testing
Respectively carrying out the circular arch polycrystalline diamond compact obtained by the method and the traditional flat-tooth diamond compact with the same specification
Performance test, test result: the abrasion ratio of the circular arch polycrystalline diamond compact is 41 thousands, the impact toughness is 1280 joules, the abrasion ratio of the traditional flat-tooth diamond compact is 30 thousands, the impact toughness is 850 joules, and compared with the traditional flat-tooth diamond compact, the abrasion resistance is improved by 36%, and the impact toughness is improved by 50%, which indicates that the performance of the circular arch polycrystalline diamond compact is obviously improved.
B. Drilling test
The circular arch polycrystalline diamond compact and the traditional flat-tooth diamond compact with the same specification obtained by the method are manufactured into 1 standard drill bit respectively, and the same drilling parameters (the bit pressure is 60 KN, the rotating speed is 75r/min, the discharge capacity is 38L/S, and the mechanical drilling speed is 45 m/h) are adopted. In the deep position contains gravel intermediate layer stratum, after drilling 2000m, the collapse of traditional flat tooth diamond compact drill bit is serious, and dome shape polycrystalline diamond compact drill bit still can use, and no collapse is decreased, crackle, layering phenomenon appear, compares with traditional flat tooth diamond compact drill bit, and life has improved 36%, and drilling efficiency promotes obviously.
Comparative example 1
The difference from the embodiment 3 is that:
in the step 2), hot wire chemical vapor deposition equipment is adopted, the air pressure of a vacuum chamber is set to be 6.5kPa, the filament temperature is 2050 ℃, and the temperature of a hard alloy substrate is 800 ℃; hydrogen and tetramethylsilane are used as reaction gases, tetramethylsilane accounts for 0.55 percent of the total gas volume, and a silicon carbide layer with the thickness of 40 mu m is deposited on the surface of the hard alloy substrate.
A. Performance testing
Respectively carrying out performance measurement on the dome-shaped polycrystalline diamond compact obtained by the method and the traditional flat-tooth diamond compact
Test, test results: the abrasion ratio of the circular arch polycrystalline diamond compact is 32 ten thousand, the impact toughness is 880 joules, while the abrasion ratio of the traditional flat-tooth diamond compact is 30 thousand, the impact toughness is 850 joules, and compared with the traditional flat-tooth diamond compact, the abrasion ratio is not obviously improved.
B. Drilling test
The circular arch polycrystalline diamond composite sheet and the traditional flat-tooth diamond composite sheet obtained by the method are manufactured into 1 standard drill bit respectively, the same drilling parameters (the bit pressure is 60 KN, the rotating speed is 75r/min, the discharge capacity is 38L/S, and the mechanical drilling speed is 45 m/h) are adopted, after 2000m is drilled in a gravel-contained interlayer stratum, 2 drill bits cannot be used again, the composite sheet is seriously broken, and cracks appear. Compared with the traditional flat-tooth diamond compact bit, the circular arch-shaped polycrystalline diamond compact bit only has the service life prolonged by 2 percent, and the drilling efficiency is not obviously improved.
Comparative example 2
The difference from the embodiment 3 is that:
step 3) boron ion implantation into diamond: placing common diamond micropowder in vacuum working chamber of ion implanter, separating ions supplied from ion source into monovalent boron ions, accelerating with electric field at 4 × 1015B+/cm2And an energy of 65keV into the surface of the diamond.
A. Performance testing
Respectively carrying out performance measurement on the dome-shaped polycrystalline diamond compact obtained by the method and the traditional flat-tooth diamond compact
Test, test results: the abrasion ratio of the circular arch polycrystalline diamond compact is 31 ten thousand, the impact toughness is 870 joules, while the abrasion ratio of the traditional flat-tooth diamond compact is 29 ten thousand, the impact toughness is 840 joules, and the abrasion ratio is not obviously improved compared with the traditional flat-tooth diamond compact.
B. Drilling test
The circular arch polycrystalline diamond compact and the traditional flat-tooth diamond compact obtained by the method are manufactured into standard drill bits
1 bit, 2 bits can not be reused after drilling 2000m in a gravel-containing interlayer stratum by adopting the same drilling parameters (bit pressure of 60 KN, rotation speed of 75r/min, discharge capacity of 38L/S and mechanical drilling speed of 45 m/h), and the composite sheet has cracks and is layered
Such as a mouse. Compared with the traditional flat-tooth diamond compact bit, the circular arch-shaped polycrystalline diamond compact bit only has the service life prolonged by 3 percent, and the drilling efficiency is not obviously improved.
Obviously, the dome-shaped polycrystalline diamond compact prepared in the embodiments 1 to 3 can be used in a deep layer complex hard rock layer
Compared with the traditional flat-tooth diamond composite sheet, the application of the diamond composite sheet has the advantages that the service life is prolonged by more than 35%, the cost is saved, the time is saved, and the drilling efficiency can be greatly improved.
Finally, it should be noted that: the above embodiments are merely illustrative and not restrictive of the technical solutions of the present invention, and any equivalent substitutions and modifications or partial substitutions made without departing from the spirit and scope of the present invention should be included in the scope of the claims of the present invention.

Claims (8)

1. The preparation method of the circular arch-shaped polycrystalline diamond compact is characterized in that the polycrystalline diamond compact sequentially comprises a hard alloy substrate, a transition layer on the surface of the hard alloy substrate and a polycrystalline diamond layer from bottom to top, wherein the upper surface of the polycrystalline diamond layer is in a circular arch shape; the lower part of the hard alloy matrix is a cylinder, and the upper part of the hard alloy matrix is a hemisphere;
the preparation method comprises the following steps:
step 1) hard alloy matrix purification treatment: purifying the hard alloy matrix to obtain a purified hard alloy matrix;
step 2) depositing a transition layer on the surface of the hard alloy substrate: depositing a silicon carbide layer and a silicon carbide-diamond gradient composite layer as a transition layer on the surface of the hard alloy substrate purified in the step 1) in sequence by adopting a chemical vapor deposition method to obtain the hard alloy substrate with the transition layer deposited on the surface;
step 3), ion implantation of diamond: sequentially injecting N into the surface of the diamond micropowder by ion injection equipment+And B+To obtain a compound containing N+And B+The diamond micro powder;
step 4), mixing materials: the said N is contained+And B+Performing ball milling and mixing on the diamond micro powder and a binding agent to obtain mixed powder, wherein the binding agent accounts for 5-10 wt% of the mixed powder;
step 5) assembling a complex: flatly placing the hard alloy substrate with the transition layer deposited on the surface, which is obtained in the step 2), on the mixed powder in a mode that the transition layer is downward, and then performing prepressing molding through a mold to obtain a composite assembly;
step 6) complex purification: placing the composite assembly in a vacuum sintering furnace, and vacuumizing and heating to obtain a purified composite assembly;
step 7), high-temperature high-pressure sintering: placing the purified composite assembly in a synthesis assembly block, and sintering at high temperature and high pressure by using a cubic press to prepare a circular arch polycrystalline diamond compact;
in the step 4), the binding agent is composed of the following raw materials in percentage by weight: 2-4% of titanium, 1.5-2% of tungsten, 1.5-2% of zirconium, 1-1.5% of chromium, 0.25-1% of inorganic nonmetal whisker, 0.25-0.5% of rare earth oxide and the balance of cobalt.
2. The method for preparing the dome-shaped polycrystalline diamond compact according to claim 1, wherein in the step 1), the specific operation of the hard alloy matrix purification treatment is as follows: firstly, immersing a hard alloy substrate into deionized water and potassium hydroxide according to a mass ratio of 1: boiling in alkali liquor prepared by 0.1-0.2 for 2-5 min, and then soaking the hard alloy substrate into sulfuric acid with the mass fraction of 98% and deionized water in a volume ratio of 1: 4-5 in sulfuric acid solutionUltrasonic oscillation cleaning for 2-5 min, then immersing in acetone or absolute ethyl alcohol solution for ultrasonic oscillation cleaning for 5-10 min, finally placing the hard alloy substrate in a vacuum sintering furnace, wherein the air pressure in the furnace is not more than 4 multiplied by 10-4Pa, at the temperature of 500-600 ℃, introducing carbon monoxide gas until the pressure in the furnace is 15-20 Mbar, and carrying out vacuum treatment on the hard alloy matrix for 1-2 h.
3. The method of preparing a dome-shaped polycrystalline diamond compact according to claim 1, wherein in step 2), the operation of depositing the transition layer is as follows: hydrogen and tetramethylsilane are used as reaction gases, the proportion of tetramethylsilane to the total gas volume is controlled to be 0.01-1%, a hot wire chemical vapor deposition device is adopted to deposit a silicon carbide layer with the thickness of 4-6 mu m on the surface of a hard alloy substrate, then hydrogen, methane and tetramethylsilane are used as the reaction gases, the flow rate of methane is controlled in the reaction process, so that the proportion of methane to the total gas volume is gradually increased from 0.4% to 3%, and meanwhile, the proportion of tetramethylsilane to the total gas volume is gradually reduced from 0.3% to 0.01%, and a silicon carbide-diamond gradient composite layer with the thickness of 30-40 mu m is formed on the surface of the silicon carbide layer by deposition.
4. The method for preparing the dome-shaped polycrystalline diamond compact according to claim 3, wherein in the chemical vapor deposition process, the vacuum chamber pressure of the hot wire chemical vapor deposition equipment is 3-10 kPa, the filament temperature is 1500-2600 ℃, and the temperature of the hard alloy substrate is 700-900 ℃.
5. The method of making a dome-shaped polycrystalline diamond compact of claim 1, wherein in step 3), the ion implantation of diamond is performed as follows: placing diamond micropowder with the particle size of 5-35 mu m in a vacuum working cavity of an ion implanter, separating ions supplied by an ion source into monovalent nitrogen ions by a mass spectrometer, accelerating the monovalent nitrogen ions by an electric field, and carrying out particle size reduction on the monovalent nitrogen ions by 4 x 1014～4×1016 N+/cm2Is implanted into the surface of the diamond with an energy of 50 to 80keV, and then ions supplied from an ion source are separated into monovalent boron ions which are accelerated by an electric field and are 4 x 1014～4×1016 B+/cm2The ion density and the energy of 50-100 keV are implanted into the surface of the diamond.
6. The method of making a dome shaped polycrystalline diamond compact of claim 1, wherein the inorganic non-metallic whiskers are one or two of alumina, zirconia, silicon carbide, and boron fibers, the whiskers have a length in a range of 100 nanometers to 20 micrometers, and a whisker diameter of no more than 100 nanometers; the rare earth oxide is one or two of thulium oxide, samarium oxide, europium oxide, praseodymium oxide, ytterbium oxide, dysprosium oxide, holmium oxide, moment oxide and scandium oxide.
7. The method of manufacturing a dome-shaped polycrystalline diamond compact according to claim 1, wherein in step 6), the specific operations of evacuating and heating are: in the vacuum sintering furnace, firstly, the vacuum is pumped to the pressure in the furnace reaching 8 multiplied by 10-2Heating to 180-230 ℃ below Pa, preserving heat for 0.5-1 h, and then continuously vacuumizing until the pressure in the furnace is stabilized at 3 x 10- 3Heating to 500-600 ℃ below Pa, stopping vacuumizing, filling carbon monoxide gas into the vacuum sintering furnace at 500-600 ℃ until the pressure in the furnace is 60-80 Mbar, reducing the composite assembly for 2-3 h under the condition, and vacuumizing to 4 x 10-4Pa below, heating to 900-1000 deg.C, and continuously vacuumizing while heating until the furnace pressure is stabilized at 3 × 10-3And Pa or less, and performing vacuum treatment on the composite assembly for 1-2 h under the condition.
8. The method for preparing the dome-shaped polycrystalline diamond compact according to claim 1, wherein in the step 7), the specific operation of the high-temperature high-pressure sintering is as follows: during sintering, the pressure is increased to 6-7 GPa at the pressure increasing rate of 0.1-1 GPa/min, then the temperature is increased to 1450-1550 ℃ at the temperature increasing rate of 15-30 ℃/min, and after sintering is carried out for 150-800 s under the condition, the temperature is reduced to the normal temperature at the temperature decreasing rate of 10-30 ℃/min, and the pressure is reduced to the normal pressure at the pressure reducing rate of 0.1-0.5 GPa/min.
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