CN117921231A - Transparent diamond drill tooth, preparation method and application thereof - Google Patents
Transparent diamond drill tooth, preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a transparent diamond drilling tooth, a preparation method and application thereof, and belongs to the field of oil and gas drilling teeth. The preparation method comprises the following steps: putting a matrix into a metal material, paving a scaling powder on the surface of the matrix, putting the transparent polycrystalline diamond after impurity removal on the surface of the scaling powder, and tightly wrapping the transparent polycrystalline diamond with the metal material; and (3) wrapping the whole polycrystalline diamond drill tooth at the pressure of 1.5 GPa-10 GPa and the temperature of 300 ℃ to 2000 ℃ for welding for 20 s-6000 s to obtain the transparent polycrystalline diamond drill tooth. According to the preparation method of the transparent diamond drill tooth, the transparent polycrystalline diamond and the matrix are combined to manufacture the drill tooth in a split mode, welding is needed to be conducted under the high-temperature and high-pressure condition through welding materials, and the combination of the transparent polycrystalline diamond and the matrix with high quality and high strength can greatly enhance the mechanical performance of the whole drill tooth.
Description
Technical Field
The invention relates to the field of oil and gas drilling teeth, in particular to a transparent diamond drilling tooth, a preparation method and application.
Background
Diamond, the hardest known natural material for the earth, has excellent properties such as high wear resistance, wide band gap, high thermal conductivity, low thermal expansion coefficient and the like, and is widely applied to the fields of mineral products, oil and gas drilling, machining, semiconductors and the like. Since each crystal face of the diamond single crystal has anisotropy and different physical properties, polycrystalline diamond (Polycrystalline Diamond, PCD) sintered at high temperature and high pressure is mostly used in industry to eliminate the anisotropy of the diamond single crystal. The most representative application of polycrystalline diamond is polycrystalline diamond teeth (Polycrystalline Diamond Cutter, PDC), which are widely used in the field of oil and gas drilling, so the performance of PDC largely determines the depth and efficiency of drilling. At present, the exploitation difficulty of oil and gas resources is continuously increased, the deepest drilling depth of a domestic drilling platform is over 8000 meters, and the deepest drilling depth of a foreign drilling platform is over 12000 meters, so that higher requirements are provided for the performance of drilling teeth used for oil and gas drilling. 20-60 PDCs are typically embedded in each bit to improve drilling efficiency, and the PDC with the worst performance in the bit can affect or even determine overall performance according to the barrel effect. The PDC drill bit failure causes the process of replacing the drill bit, the workload is large, the cost is high, and safety risks such as blowout exist, so that the guarantee of uniformity of physical properties of each PDC is a key for guaranteeing good operation of the drill bit.
The PDC currently used for oil and gas drilling uses several types of materials: 1) The whole body is sintered polycrystalline diamond without binder; 2) The whole is sintered polycrystalline diamond with a binder; 3) The sintered polycrystalline diamond without the binder is formed by connecting a matrix in a split way; 4) The sintered polycrystalline diamond is formed by connecting a binder with a matrix in a split manner. Wherein the component of the matrix part can be one or more of tungsten carbide, cobalt, titanium carbide, silicon carbide and chromium carbide. In general, the binder-sintered diamond requires more than 1wt% of a binder containing a non-carbon component during sintering, and the binder includes a metal material such as iron group elements or a non-metal material such as silicon carbide, boron carbide and titanium carbide. The addition of the binder may promote bonding between diamond particles, but this may lead to heat and stress generated in actual drilling to break the bond between the binder and the diamond, reducing the service life of the PDC due to the difference in physical properties between the binder and the diamond. On the other hand, the addition of the binder reduces isotropy of optical conduction between diamond grain boundaries, thereby creating extinction factors; while impurities and voids between the polycrystalline diamond may absorb and scatter visible light, the bonded polycrystalline diamond is generally non-transparent. The binderless polycrystalline diamond is required to be sintered under extremely high temperature and pressure conditions due to the lack of a binder to promote bonding between the diamonds, and isotropy between grain boundaries is well preserved during this process; and meanwhile, pores in the sample can be well eliminated under the higher temperature and pressure condition, so that the transparent polycrystalline diamond block is sintered. Because the temperature and pressure conditions required by sintering the binder-free transparent polycrystalline diamond by adopting the diamond micro powder are extremely harsh, the hardness and toughness of the sintered transparent polycrystalline diamond are far superior to those of the transparent polycrystalline diamond of the same type. In particular, since the diamond working layers of PDCs commonly used in the market are all opaque, the method for detecting defects inside PDCs is generally only able to detect by ultrasound, but ultrasound is limited to the wavelength of ultrasound, and cannot detect minute defects, and the resolution of defects is generally less than 0.1mm, so that uniformity of performance of PDCs applied to each drill bit cannot be ensured.
PDC teeth used in oil and gas drilling bits in industry are generally non-transparent polycrystalline diamond teeth, but the existing teeth have the following disadvantages that severely restrict drilling efficiency and service life of the bit:
(1) In the polycrystalline diamond sintered by adding the binder, the binder is uniformly dispersed in each diamond crystal grain. When drilling with the diamond teeth made of polycrystalline diamond of this type, the heat generated by friction between the diamond teeth and the rock causes the binder to expand and squeeze the inner diamond grains, causing cracks and shortening the service life of the PDC due to the difference in thermal expansion coefficient and elastic coefficient between the diamond and the binder, thereby reducing the service life of the entire drill bit.
(2) Both opaque binder-sintered polycrystalline diamond and opaque non-binder-sintered polycrystalline diamond lack nondestructive testing means to detect defects and microcracks within them. In particular, defects and microcracks distributed inside the diamond layer and at the interface between the diamond layer and the substrate, even those of the order of microns, can have a serious impact on the performance of the PDC. The only ultrasonic means at present is limited by the fact that the wavelength and the frequency cannot detect the defects of microcracks and the like in the polycrystalline diamond and at the joint interface of the diamond layer and the matrix. Therefore, when the drill teeth made of the opaque polycrystalline diamond are applied to a drill bit, uniformity of performance of each drill tooth cannot be guaranteed, and the stability of the drill bit in use is seriously reduced.
(3) In actual use, polycrystalline diamond is typically combined with a substrate to form a single bit. Generally, polycrystalline diamond is bonded to a substrate by several methods: high temperature high pressure sintering, vacuum welding, laser welding, microwave welding, high frequency induction welding or mechanical fixing. In the welding process of using opaque polycrystalline diamond and a matrix, tiny defects of a welding part cannot be observed in a nondestructive detection mode such as ultrasonic. This also results in a variation in the uniformity of each tooth, reducing the overall bit life and efficiency.
Disclosure of Invention
The invention aims to provide a transparent diamond drill tooth, a preparation method and application thereof, and solves the problems of long service life and low efficiency of the drill tooth formed by combining polycrystalline diamond and a matrix.
The invention is realized by the following technical scheme:
the invention provides a preparation method of a transparent diamond drill tooth, which comprises the following steps:
Putting a matrix into a metal material, paving a scaling powder on the surface of the matrix, putting the transparent polycrystalline diamond after impurity removal on the surface of the scaling powder, and tightly wrapping the transparent polycrystalline diamond with the metal material;
And (3) wrapping the whole polycrystalline diamond drill tooth at the pressure of 1.5 GPa-10 GPa and the temperature of 300 ℃ to 2000 ℃ for welding for 20 s-6000 s to obtain the transparent polycrystalline diamond drill tooth.
Further, in a preferred embodiment of the present invention, the substrate is a high hardness ceramic material, comprising: one or more of tungsten carbide, aluminum oxide, silicon nitride, titanium carbide, silicon carbide and chromium carbide.
Further, in a preferred embodiment of the invention, the substrate is a sinter formed block or unsintered powder.
Further, in a preferred embodiment of the present invention, the metal material includes: one or more of tantalum, rhenium, molybdenum, niobium and platinum.
Further, in a preferred embodiment of the present invention, the flux includes: one or more of iron, chromium, nickel, silicon carbide, boron carbide and titanium carbide.
Further, in a preferred embodiment of the present invention, the flux is added in an amount of 3wt% of the base.
Further, in a preferred embodiment of the present invention, the preparation of the transparent polycrystalline diamond comprises: under the heating condition, cleaning the diamond micro powder with hydrofluoric acid and hydrochloric acid in sequence to remove impurities;
The diamond micro powder after impurity removal is treated for 8 hours under the condition that the vacuum degree is 5 multiplied by 10 -3 Pa and the temperature is 800 ℃;
placing the treated diamond powder into a metal wrapping material, and pre-pressing and forming under the pressure of 400 MPa;
and (3) wrapping the pre-pressed and molded transparent polycrystalline diamond with the pressure of 15GPa and the temperature of 2200 ℃ for sintering for 5min, reducing the pressure and cooling to normal pressure and room temperature, removing the wrapping material, and polishing to obtain the transparent polycrystalline diamond.
Further, in a preferred embodiment of the present invention, the welding conditions are: 5GPa, and welding at 1200 ℃ for 300s.
The invention also provides the transparent diamond drill tooth prepared by the preparation method of the transparent diamond drill tooth.
The invention also provides application of the transparent diamond drilling tooth in oil and gas drilling.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. According to the preparation method of the transparent diamond drill tooth, the transparent polycrystalline diamond and the matrix are combined to manufacture the drill tooth in a split mode, welding is needed to be conducted under the high-temperature and high-pressure condition through welding materials, and the combination of the transparent polycrystalline diamond and the matrix with high quality and high strength can greatly enhance the mechanical performance of the whole drill tooth. The matrix material is usually non-transparent, and defects and microcracks at the bonding interface of the diamond and the matrix and welding conditions of the defects and microcracks can be observed through the transparent polycrystalline diamond part, so that the uniformity of the performance of each application to the teeth in the drill bit is ensured.
2. The invention is used for detecting the defects of the diamond part in the transparent polycrystalline diamond drill tooth by using an optical microscope, the current optical microscope can distinguish the defects with the minimum 200nm, the resolution capability is far greater than the resolution capability of ultrasound (usually less than 0.1 mm), and meanwhile, the optical detection is convenient and quick, and the time cost is saved.
3. The transparent polycrystalline diamond drill tooth prepared by the invention is tested by a numerical control lathe through an abrasion resistance cutting test, wherein the cutting linear speed is 100m/min, and the cutting depth is 0.5mm. The cutting experiment shows that the wear resistance of the transparent polycrystalline diamond drill tooth is better than that of the non-transparent polycrystalline diamond drill tooth, and the service life of the transparent polycrystalline diamond drill tooth is prolonged by more than 2.5 times than that of the polycrystalline diamond drill tooth added with the binder in the synthesis process.
Drawings
In order to more clearly illustrate the technical solutions of the exemplary embodiments of the present invention, the drawings that are needed in the examples will be briefly described below, it being understood that the following drawings only illustrate some examples of the present invention and therefore should not be considered as limiting the scope, and that other related drawings may be obtained from these drawings without inventive effort for a person skilled in the art. In the drawings:
FIG. 1 is an optical photograph of a drill bit for oil and gas drilling;
Fig. 2 is a high temperature high pressure sintered binderless transparent polycrystalline diamond of example 1 of the present invention;
Fig. 3 is a block diagram of a transparent polycrystalline diamond without binder for use in a tooth according to example 1 of the present invention;
fig. 4 is a drawing showing the numbers and corresponding parts names of the drill tooth with transparent polycrystalline diamond end after high temperature and high pressure welding in example 2:
1-transparent polycrystalline diamond, 2-welding layer and 3-matrix.
Detailed Description
For the purpose of making apparent the objects, technical solutions and advantages of the present invention, the present invention will be further described in detail with reference to the following examples and the accompanying drawings, wherein the exemplary embodiments of the present invention and the descriptions thereof are for illustrating the present invention only and are not to be construed as limiting the present invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The technical scheme of the invention is as follows:
a method of preparing a transparent diamond drill tooth comprising:
(1) Putting the substrate into a metal material, paving a soldering flux on the surface of the substrate, putting the transparent polycrystalline diamond after impurity removal on the surface of the soldering flux, and tightly wrapping the transparent polycrystalline diamond with the metal material.
The matrix is a high-hardness ceramic material and comprises: one or more of tungsten carbide, aluminum oxide, silicon nitride, titanium carbide, silicon carbide and chromium carbide.
The matrix is a sintered shaped block or unsintered powder. The powder can be fully contacted with the surface of the diamond under high pressure by adopting a powder matrix welding mode, the bonding strength is better through a high-temperature welding interface, the defects of the bonding position are fewer, and meanwhile, the generation of microcracks in the diamond can be reduced.
The metal material includes: one or more of tantalum, rhenium, molybdenum, niobium and platinum.
The soldering flux comprises: one or more of iron, chromium, nickel, silicon carbide, boron carbide and titanium carbide.
The addition amount of the soldering flux is 2-15wt% of the matrix.
The preparation of the transparent polycrystalline diamond comprises the following steps: under the heating condition, cleaning the diamond micro powder with hydrofluoric acid and hydrochloric acid in sequence to remove impurities;
The diamond micro powder after impurity removal is treated for 8 hours under the condition that the vacuum degree is 5 multiplied by 10 -3 Pa and the temperature is 800 ℃;
placing the treated diamond powder into a metal wrapping material, and pre-pressing and forming under the pressure of 400 MPa;
and (3) wrapping the pre-pressed and molded transparent polycrystalline diamond with the pressure of 15GPa and the temperature of 2200 ℃ for sintering for 5min, reducing the pressure and cooling to normal pressure and room temperature, removing the wrapping material, and polishing to obtain the transparent polycrystalline diamond.
Wherein, the impurity removing step in the step (1) comprises the following steps: and (3) treating impurities on the surface of the transparent polycrystalline diamond subjected to high-temperature high-pressure sintering by acid or alkali to obtain the pure transparent polycrystalline diamond. Wherein, acid treatment: mixing one or more of nitric acid, hydrofluoric acid, hydrochloric acid and sulfuric acid, and dissolving impurities on the surface of polycrystalline diamond at the temperature of 5-200 ℃; and then washing with deionized water, separating and drying.
(2) And (3) placing the whole package in a high-pressure assembly of a large-cavity static high-pressure device, and welding for 20 s-6000 s at the temperature of 300-2000 ℃ under the pressure of 1.5-10 GPa to obtain the transparent polycrystalline diamond drill tooth.
Further, the welding conditions are as follows: 5.5GPa, and welding at 1200 ℃ for 300s.
The transparent polycrystalline diamond drill tooth provided by the invention has the advantages that the ultra-high hardness and toughness are ensured, and meanwhile, the transparent polycrystalline diamond drill tooth has high light transmittance, so that the transparent polycrystalline diamond drill tooth has the unique advantages (optical detection) in the aspect of detecting microcracks and defects in the diamond. Because the sintered polycrystalline diamond needs to adopt a high-temperature and high-pressure environment, the sintered sample in the high-temperature and high-pressure environment may generate microcracks in the sample due to stress, or the microcracks in the sample may be generated by polishing, grinding and other processes introduced in the process of drilling teeth. If the sample is opaque, the most intuitive optical detection method cannot be used to detect defects inside the sample. Therefore, the transparent polycrystalline diamond capable of nondestructively detecting internal defects by using an optical microscope (the defect of 200nm can be distinguished at minimum) can ensure the uniformity of the diamond layer in each manufactured drill tooth.
The transparent polycrystalline diamond provided by the invention is a binder-free sintered transparent polycrystalline diamond, and compared with the traditional binder-free opaque polycrystalline diamond, the transparent polycrystalline diamond has the same hardness and wear resistance as the binder-free sintered diamond while having visible light transmittance. On the basis, the transparent diamond drill tooth obtained by welding the transparent polycrystalline diamond and the matrix has the following advantages: 1. after welding, the optical microscope can be used for directly observing whether the defects such as microcracks and the like appear in the drill teeth after welding, and meanwhile, the situation that whether the welding layers have poor welding such as cold welding and the like can be directly observed. Therefore, each drill tooth applied to the drill bit can have uniform performance, the defect density inside the drill tooth is ensured to be uniform, and the situation that the whole drill bit needs to be replaced because one drill tooth is damaged is prevented. 2. The welding degree of the transparent polycrystalline diamond and the matrix can be intuitively known, if the non-transparent diamond is used for welding the matrix, the degree of the welding of the transparent polycrystalline diamond and the matrix cannot be observed from the diamond side (namely, whether the diamond part and the matrix part are completely combined under the action of the soldering flux or not, and the diamond teeth with air holes at the combined part are eliminated). In the past, the welding strength of the test diamond and the matrix is measured by shearing the bonding layer by an instrument, but the instrument measurement is only macroscopic observation, and the detail of the welding bonding layer cannot be checked in microscopic aspect. 3. The binding strength is different for different substrates because of the different affinities with the diamond layer. The failure reason and the maximum use failure time (the maximum time which cannot be used) of the matrix and the diamond bonding part can be observed by adopting the transparent diamond, so that the drill bit can be utilized to the greatest extent; meanwhile, the failure cause is directly observed, the welding process can be modified in reverse, and better welding flux is selected to weld the drill teeth with stronger bonding capability and longer failure time.
The preparation method of the transparent diamond drill tooth further comprises the following steps:
(3) And taking out the polycrystalline diamond drill teeth for high-pressure assembly, removing the outer layer package to obtain transparent polycrystalline diamond drill teeth, and obtaining the final PDC drill teeth through grinding, polishing and other processes.
And placing the transparent polycrystalline diamond drill teeth on a high-power optical microscope to observe internal defects and microcracks, and ensuring the uniformity of each drill tooth.
For further explanation of the present invention, the method for preparing a transparent diamond drill tooth according to the present invention will be described with reference to examples, but it should be understood that these examples are implemented on the premise of the technical solution of the present invention, and detailed embodiments and specific operation procedures are given only for further explanation of the features and advantages of the present invention, and not for limitation of the claims of the present invention, and the scope of protection of the present invention is not limited to the examples described below.
Example 1:
a method of preparing transparent polycrystalline diamond, comprising:
Seed crystal: diamond micropowder synthesized by static high pressure method is yellow, irregular in morphology and 10um in granularity. Heating hydrofluoric acid with concentration of 30% according to a mass ratio of 1:4 for 48 hours in an acid washing process at 60 ℃; placing the diamond powder into hydrochloric acid with the concentration of 25%, adding the diamond powder and the hydrochloric acid with the weight ratio of 1:3 into a purification kettle, stirring and heating to 60 ℃ in a water bath, treating for 48 hours, pouring out liquid after the powder subsides, washing to be neutral by deionized water, repeating the acid dissolving and impurity removing steps for 2 times, drying the diamond powder, washing to be neutral by deionized water and drying, and treating the diamond powder for 8 hours under the conditions that the vacuum degree is 5 multiplied by 10 -3 Pa and the temperature is 800 ℃ to remove oxygen, nitrogen, water vapor and other impurities adsorbed on the surface of the diamond.
And (5) placing the treated diamond powder into a package for prepressing forming, wherein the prepressing pressure is 400MPa. Placing the pre-pressed and molded package into a static high-pressure large-cavity press, sintering for 5min under the conditions of 15GPa pressure and 2200 ℃ temperature, reducing the pressure and cooling to normal pressure and room temperature, then placing the sample with the package into mixed acid of 10ml of 30% hydrofluoric acid and 10ml of 40% nitric acid to remove the tantalum as a package material, and polishing the sample to be bright by using a polishing disc to obtain the transparent polycrystalline diamond without the binder, wherein the size of the transparent polycrystalline diamond is phi 10mm multiplied by 5mm in the second figure.
In order to eliminate pores, microcracks and stresses in the sample, and thus prepare transparent polycrystalline diamond, the temperature and pressure sintering paths of the experiment are as follows: after the sample assembly is put into a press, cold pressing is carried out to 10GPa, at the moment, the sample assembly is heated, the temperature of a sample cavity is heated to 1600 ℃ by adopting a heating temperature gradient between 50 ℃ and 300 ℃/min, at the moment, the temperature is kept unchanged and continuously increased to 15GPa (the step is that certain yield can be generated on crystal grains of the diamond at high temperature and high pressure, certain creep can be generated on the diamond after the continuous pressurization, pores among crystal boundaries can be eliminated by the creep crystal grains, so that the sample becomes transparent), and then the temperature is increased to 2200 ℃ under the pressure of 15GPa and the temperature is kept. And cooling operation is performed after heat preservation is completed, and in order to reduce microcracks and release stress, a mode of pressure relief with temperature is adopted in experiments, and the specific method is that when the temperature of the cavity is reduced to 1200 ℃, pressure relief is started to be synchronous until normal temperature and normal pressure are achieved.
After polishing treatment, the sintered sample is detected by a spectrophotometer, and the visible light (wavelength 400-800 nm) transmittance of the sample is found to be 61-73%, so that the transmittance is good. The hardness of the sample is detected to be more than 126GPa, and the fracture toughness is more than 18.7 MPa.m 1/2.
And (3) detecting the wear resistance of the sample, wherein the cutting target is granite, comparing the sample of the non-binder polycrystalline diamond with the experimental sample, and simultaneously cutting 6000m granite (cutting conditions: wet cutting; cutting speed: 100m/min, feeding amount 0.4mm, and cutting depth: 0.2 mm).
Cutting comparison shows that the matrix loss volume of the transparent polycrystalline diamond prepared in the embodiment is 0.046mm 3 after 6000m cutting, and the abrasion volume of a commercial binderless polycrystalline diamond sample is 0.173mm 3 after 6000m cutting, and the abrasion amount is 3.7 times that of the transparent polycrystalline diamond sample.
The sample is processed into a required size, and whether microcracks or other types of defects exist in the sample is observed under an optical microscope, and the transparent polycrystalline diamond can be integrally embedded on a drill bit as a drilling tooth (figure three). After a plurality of drill teeth are inspected, the drill teeth are inlaid on a drill bit to form a drill bit (figure I) with a plurality of transparent polycrystalline diamond drill teeth. The hardness of each drilling tooth of the transparent polycrystalline diamond is about 120GPa, the service life of the transparent polycrystalline diamond in oil and gas drilling is prolonged by more than 3 times compared with that of the polycrystalline diamond drilling tooth added with the binder in the synthesis process, and the transparent polycrystalline diamond can drill into underground strata at one time by more than 4000 meters.
Example 2:
Diamond micropowder synthesized by static high pressure method is yellow, irregular in morphology and 10um in granularity; heating hydrofluoric acid with concentration of 30% according to a mass ratio of 1:4 for 48 hours in an acid washing process at 60 ℃; placing the diamond powder into hydrochloric acid with the concentration of 25%, adding the diamond powder and the hydrochloric acid with the weight ratio of 1:3 into a purification kettle, stirring and heating to 60 ℃ in a water bath, treating for 48 hours, pouring out liquid after the powder subsides, washing to be neutral by deionized water, repeating the acid dissolving and impurity removing steps for 2 times, drying the diamond powder, washing to be neutral by deionized water and drying, and treating the diamond powder for 8 hours under the conditions that the vacuum degree is 5 multiplied by 10 -3 Pa and the temperature is 800 ℃ to remove oxygen, nitrogen, water vapor and other impurities adsorbed on the surface of the diamond.
And (5) placing the treated diamond powder into a package for prepressing forming, wherein the prepressing pressure is 400MPa. And (3) placing the pre-pressed and molded package into a static high-pressure large-cavity press, sintering for 5min under the conditions of 15GPa and 2200 ℃ in pressure, reducing the pressure and cooling to normal pressure and room temperature, then placing the sample with the package into mixed acid of 10ml of 30% hydrofluoric acid and 10ml of 40% nitric acid to remove the tantalum as a package material, and polishing the sample with a polishing disc until the sample is bright to obtain the transparent polycrystalline diamond without the binder, wherein the size of the transparent polycrystalline diamond is phi 10mm multiplied by 5 mm.
The transparent polycrystalline diamond without adhesive with the size of phi 10mm multiplied by 5mm is cut into two diamond pieces with the size of phi 10mm multiplied by 2mm by means of cutting and the like, and polished to a mirror surface. In order to process a binderless transparent polycrystalline diamond sheet with the size of phi 10mm multiplied by 2mm into a highly suitable drill tooth, the diamond and the matrix are bonded by adopting a high-temperature and high-pressure welding mode. The solder used for welding the transparent polycrystalline diamond layer and the hard alloy matrix needs to be soaked in diamond and hard alloy simultaneously during high-temperature welding, and has chemical affinity (solder silicon, nickel, silver, copper simple substance or alloys of the above) for the diamond and the hard alloy simultaneously so as to obtain high welding bonding strength; however, in general, the melting point of the solder is usually higher than 600 ℃ under normal pressure, and this temperature is higher than the oxidation temperature of diamond under normal pressure, so that high-pressure welding is used to inhibit graphitization of diamond (the oxidation temperature and graphitization temperature of diamond are raised by pressure) and improve the strength of the welded part.
Placing the processed hard alloy block (YG 10: phi 10mm multiplied by 7 mm) into a tantalum package, then placing 0.2g of nickel-based soldering flux (BNi-2: ni > 82%) on the upper surface of the hard alloy, then placing the processed block polycrystalline diamond thereon, and finally pre-pressing (100-200 MPa) the packaged package together for molding. The inclusion after pre-pressing forming is placed into a large-cavity static high-pressure device, and sintered under the conditions of high temperature and high pressure (temperature and pressure conditions: 2-5.5GPa,600-1300 ℃ and sintering time 600 s) to obtain the drilling tooth blank with high bonding strength, wherein the sintering temperature and the sintering pressure are matched to avoid graphitization of diamond, as shown in figure four.
Taking out the sintered diamond blank after high-temperature and high-pressure welding, grinding to remove the tantalum metal package outside, and polishing the front end surface of the diamond to a mirror surface to obtain the diamond with the transparent polycrystalline diamond end.
The hardness of the sample is about 115GPa, and the fracture toughness exceeds 19 MPa.m 1/2. And (3) detecting the wear resistance of the sample, wherein the cutting target is granite, comparing the sample of the non-binder polycrystalline diamond with the experimental sample, and simultaneously cutting 6000m granite (cutting conditions: wet cutting; cutting speed: 100m/min, feeding amount 0.4mm, and cutting depth: 0.2 mm).
Cutting comparison shows that the matrix loss volume of the transparent polycrystalline diamond prepared in the embodiment is 0.054mm 3 after 6000m cutting, and the abrasion volume of a commercial binderless polycrystalline diamond sample is 0.176mm 3 after 6000m cutting, and the abrasion amount is 3.3 times that of the transparent polycrystalline diamond sample.
And observing whether microcracks or other types of defects exist in each drilling tooth under an optical microscope, and observing the welding condition of a high-temperature high-pressure welding part of the diamond and the matrix at the same time to ensure that the performance of each drilling tooth is kept uniform. And then embedding the inspected drilling teeth on the drill bit to form the drill bit with a plurality of transparent polycrystalline diamond end drilling teeth. The hardness of each drill tooth of the transparent polycrystalline diamond is about 110GPa, and meanwhile, the error of defect density in each drill tooth is within 5% because the transparent polycrystalline diamond is detectable. The practical drilling shows that the service life of the polycrystalline diamond tooth with the binder added in the oil and gas drilling is prolonged by more than 2.5 times compared with that of the polycrystalline diamond tooth with the binder added in the synthesis process, and the service life of the polycrystalline diamond tooth can reach more than 3000 m when drilling underground strata once.
Example 3:
The transparent polycrystalline diamond obtained by sintering in example 1 was cut according to the processing method in example 2 to obtain two transparent polycrystalline diamond pieces having a size Φ10mm×2mm.
Then placing a commercially available silicon carbide block (phi 10mm multiplied by 7mm, aluminum content 5%wt and hardness 30.2 GPa) into a tantalum package, then placing 0.1g of nickel-based soldering flux (BNi-2:Ni > 82%) on the upper surface of the silicon carbide block, placing the processed block polycrystalline diamond thereon, and finally pre-pressing (100-200 MPa) the packaged package together for molding.
The inclusion after pre-pressing forming is placed into a large-cavity static high-pressure device, and sintered under the conditions of high temperature and high pressure (temperature and pressure: 5GPa,1200 ℃ and sintering time: 600 s) to obtain the drilling tooth blank with high bonding strength, wherein the sintering temperature and the sintering pressure are matched so as to avoid diamond graphitization.
Silicon carbide is adopted because of high hardness, high thermal conductivity, high compressive strength and stable structure at high temperature. Taking out the sintered diamond blank after high-temperature and high-pressure welding, grinding to remove the tantalum metal package outside, and polishing the front end surface of the diamond to a mirror surface to obtain the diamond with the transparent polycrystalline diamond end.
The hardness of the sample is about 115GPa, and the fracture toughness exceeds 19 MPa.m 1/2.
The sample is subjected to abrasion resistance detection, the cutting target is granite, the comparison is carried out by using the non-adhesive polycrystalline diamond sample and the experimental sample, and 6000m granite is cut (cutting conditions: wet cutting; cutting speed: 100m/min, feeding amount 0.4mm, and cutting depth: 0.2 mm).
Cutting comparison shows that the matrix loss volume of the transparent polycrystalline diamond prepared in the embodiment is 0.05mm 3 after cutting 6000m, and the abrasion volume of a commercial binderless polycrystalline diamond sample is 0.176mm 3 after cutting 6000m, and the abrasion amount is 3.52 times that of the transparent polycrystalline diamond sample.
And observing whether microcracks or other types of defects exist in each drilling tooth (shown in the fourth drawing) under an optical microscope, and simultaneously observing the welding condition of the high-temperature and high-pressure welding part of the diamond and the matrix, so that the performance of each drilling tooth is ensured to be kept uniform. And then embedding the inspected drilling teeth on the drill bit to form the drill bit with a plurality of transparent polycrystalline diamond end drilling teeth. The hardness of each drill tooth of the transparent polycrystalline diamond is about 110GPa, and meanwhile, the error of defect density in each drill tooth is within 5% because the transparent polycrystalline diamond is detectable. The practical drilling shows that the service life of the polycrystalline diamond tooth with the binder added in the oil and gas drilling is prolonged by more than 2.7 times compared with that of the polycrystalline diamond tooth with the binder added in the synthesis process, and the service life of the polycrystalline diamond tooth can reach more than 3240 meters when drilling underground strata once.
Example 4:
the present example is a weld made with silicon carbide powder and transparent polycrystalline diamond.
The transparent polycrystalline diamond obtained by sintering in example 1 was cut according to the processing method in example 2 to obtain two transparent polycrystalline diamond pieces having a size Φ10mm×2mm.
Subsequently, 10% by weight of alcohol was added to a commercially available silicon carbide powder (grain size 1 μm) and mixed well. And placing the uniformly mixed silicon carbide powder into a die with the diameter of 11mm for prepressing, wherein the prepressing pressure of the silicon carbide powder is 600MPa. After die stripping, a bulk silicon carbide of phi 11mm by 8.8mm is obtained, the compactness of which is 69%.
And placing the pre-pressed silicon carbide block into a tantalum package, then placing 0.3g of nickel-based soldering flux (BNi-2:Ni > 82%) on the upper surface of the pre-pressed silicon carbide block, and then placing the processed block polycrystalline diamond thereon. And then a silicon carbide ring with the diameter of phi 11mm multiplied by the diameter of phi 10mm multiplied by 2mm is pressed by a die to wrap the transparent polycrystalline diamond, wherein the pre-pressing pressure of the silicon carbide powder is 600MPa.
Finally, the packed inclusion is pre-pressed (100-200 MPa) together for molding. The inclusion after pre-pressing forming is put into a large-cavity static high-pressure device, and sintered under the conditions of high temperature and high pressure (temperature and pressure conditions: 5.5GPa,1300 ℃ and sintering time: 600 s) to obtain the drilling tooth blank with high bonding strength, wherein the sintering temperature and the sintering pressure are matched to avoid graphitization of diamond. Taking out the sintered diamond blank body (phi 10.2mm multiplied by 10.3 mm) after high-temperature and high-pressure welding, grinding to remove the tantalum metal package outside, cutting the sample to obtain the diamond with the diameter phi 10mm multiplied by 10mm, and polishing the front end surface of the diamond to a mirror surface to obtain the diamond with the transparent polycrystalline diamond end (figure four).
The hardness of the sample is about 115GPa, and the fracture toughness exceeds 19 MPa.m 1/2.
And (3) detecting the wear resistance of the sample, wherein the cutting target is granite, comparing the sample of the non-binder polycrystalline diamond with the experimental sample, and simultaneously cutting 6000m granite (cutting conditions: wet cutting; cutting speed: 100m/min, feeding amount 0.4mm, and cutting depth: 0.2 mm).
Cutting comparison shows that the matrix loss volume of the transparent polycrystalline diamond prepared in the embodiment is 0.047mm 3 after 6000m cutting, and the abrasion volume of a commercial binderless polycrystalline diamond sample is 0.176mm 3 after 6000m cutting, and the abrasion amount is 3.7 times that of the transparent polycrystalline diamond sample.
Meanwhile, the strength of the welded part of the sample welded in the third case and the fourth case is compared, and as the powder and the diamond are welded in the fourth case and the silicon carbide powder is better combined with the diamond interface under the action of the welding flux at high temperature and high pressure, the interface bonding strength of the welded sample in the fourth case is 1.2 times that in the third case, and the stability of the drilling teeth is improved. And observing whether microcracks or other types of defects exist in each drilling tooth under an optical microscope, and observing the welding condition of a high-temperature high-pressure welding part of the diamond and the matrix at the same time to ensure that the performance of each drilling tooth is kept uniform.
And then embedding the inspected drilling teeth on the drill bit to form the drill bit with a plurality of transparent polycrystalline diamond end drilling teeth. The hardness of each drill tooth of the transparent polycrystalline diamond is about 110GPa, and meanwhile, the error of defect density in each drill tooth is within 5% because the transparent polycrystalline diamond is detectable. The practical drilling shows that the service life of the polycrystalline diamond tooth with the binder added in the oil and gas drilling is prolonged by more than 3 times compared with that of the polycrystalline diamond tooth with the binder added in the synthesis process, and the service life of the polycrystalline diamond tooth can reach 3600 meters when drilling into underground strata at one time.
Example 5:
This example is a weld made with a transparent polycrystalline diamond using cubic boron nitride (cBN) powder.
The transparent polycrystalline diamond obtained by sintering in example 1 was cut according to the processing method in example 2 to obtain two transparent polycrystalline diamond pieces having a size Φ10mm×2mm.
Subsequently 10% wt of alcohol was added to a commercially available cBN powder (grain size 1 μm) and mixed well. And placing the uniformly mixed cBN powder into a die with the diameter of 11mm for prepressing, wherein the prepressing pressure of the cBN powder is 600MPa. After die stripping, a bulk silicon carbide of phi 11mm by 8.5mm is obtained, the compactness of which is 64%.
And placing the pre-pressed cBN block into a tantalum package, then placing 0.4g of nickel-based soldering flux (BNi-2:Ni > 82%) on the upper surface of the pre-pressed cBN block, and placing the processed block polycrystalline diamond thereon. And pressing a cBN ring with the diameter of phi 11mm multiplied by the diameter of phi 10mm multiplied by 2mm by using a die to wrap the transparent polycrystalline diamond, wherein the pre-pressing pressure of the cBN powder is 600MPa. Finally, the packed inclusion is pre-pressed (100-200 MPa) together for molding.
The inclusion after pre-pressing forming is put into a large-cavity static high-pressure device, and sintered under the conditions of high temperature and high pressure (temperature and pressure conditions: 5.5GPa,1300 ℃ and sintering time: 600 s) to obtain the drilling tooth blank with high bonding strength, wherein the sintering temperature and the sintering pressure are matched to avoid graphitization of diamond. Taking out the sintered diamond blank body (phi 10.5mm multiplied by 10.5 mm) after high-temperature and high-pressure welding, grinding to remove the tantalum metal package outside, cutting the sample to obtain the diamond with the diameter phi 10mm multiplied by 10mm (figure IV), and polishing the front end surface of the diamond to a mirror surface to obtain the diamond with the transparent polycrystalline diamond end.
The hardness of the sample is about 115GPa, and the fracture toughness exceeds 19 MPa.m 1/2.
And (3) detecting the wear resistance of the sample, wherein the cutting target is granite, comparing the sample of the non-binder polycrystalline diamond with the experimental sample, and simultaneously cutting 6000m granite (cutting conditions: wet cutting; cutting speed: 100m/min, feeding amount 0.4mm, and cutting depth: 0.2 mm).
Cutting comparison shows that the matrix loss volume of the transparent polycrystalline diamond prepared in the embodiment is 0.047mm 3 after 6000m cutting, and the abrasion volume of a commercial binderless polycrystalline diamond sample is 0.176mm 3 after 6000m cutting, and the abrasion amount is 3.7 times that of the transparent polycrystalline diamond sample.
And observing whether microcracks or other types of defects exist in each drilling tooth under an optical microscope, and observing the welding condition of a high-temperature high-pressure welding part of the diamond and the matrix at the same time to ensure that the performance of each drilling tooth is kept uniform. And then embedding the inspected drilling teeth on the drill bit to form the drill bit with a plurality of transparent polycrystalline diamond end drilling teeth. The hardness of each drill tooth of the transparent polycrystalline diamond is about 110GPa, and meanwhile, the error of defect density in each drill tooth is within 5% because the transparent polycrystalline diamond is detectable. The practical drilling shows that the service life of the polycrystalline diamond drill tooth added with the binder in the oil gas drilling process is prolonged by more than 3.4 times compared with that of the polycrystalline diamond drill tooth added with the binder in the synthesis process, and the service life of the polycrystalline diamond drill tooth can be prolonged by more than 4080 meters when drilling underground strata once (because the cBN has high thermal conductivity, heat generated by drilling can be conducted quickly, accumulation of the heat in the drill tooth is reduced, impact of the heat on a welded part is reduced, and the service life is prolonged).
The foregoing description of the embodiments has been provided for the purpose of illustrating the general principles of the invention, and is not meant to limit the scope of the invention, but to limit the invention to the particular embodiments, and any modifications, equivalents, improvements, etc. that fall within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (10)
1. A method of preparing a transparent diamond bit, comprising:
Putting a matrix into a metal material, paving a scaling powder on the surface of the matrix, putting the transparent polycrystalline diamond after impurity removal on the surface of the scaling powder, and tightly wrapping the transparent polycrystalline diamond with the metal material;
And (3) wrapping the whole polycrystalline diamond drill tooth at the pressure of 1.5 GPa-10 GPa and the temperature of 300 ℃ to 2000 ℃ for welding for 20 s-6000 s to obtain the transparent polycrystalline diamond drill tooth.
2. The method of preparing a transparent diamond bit according to claim 1, wherein the substrate is a high hardness ceramic material comprising: one or more of tungsten carbide, aluminum oxide, silicon nitride, titanium carbide, silicon carbide and chromium carbide.
3. The method of producing transparent diamond teeth according to claim 2, wherein the substrate is a sintered shaped block or unsintered powder.
4. The method of producing a transparent diamond bit according to claim 1, wherein the metal material comprises: one or more of tantalum, rhenium, molybdenum, niobium and platinum.
5. The method of preparing a transparent diamond bit according to claim 1, wherein the flux comprises: one or more of iron, chromium, nickel, silicon carbide, boron carbide and titanium carbide.
6. The method for producing transparent diamond teeth according to claim 1, wherein the flux is added in an amount of 2 to 15wt% of the base body.
7. The method of preparing a transparent diamond tooth according to claim 1, wherein the preparing transparent polycrystalline diamond comprises: under the heating condition, cleaning the diamond micro powder with hydrofluoric acid and hydrochloric acid in sequence to remove impurities;
The diamond micro powder after impurity removal is treated for 8 hours under the condition that the vacuum degree is 5 multiplied by 10 -3 Pa and the temperature is 800 ℃;
Placing the treated diamond powder into a metal wrapping material, and pre-pressing and forming under the pressure of 100-400 MPa;
and (3) wrapping the pre-pressed and molded transparent polycrystalline diamond with the pressure of 5-15GPa and the temperature of 1000-2200 ℃ for sintering for 0.5-15min, reducing the pressure and the temperature to normal pressure and room temperature, removing the wrapping material, and polishing to obtain the transparent polycrystalline diamond.
8. The method of preparing a transparent diamond bit according to claim 1, wherein the welding conditions are: 5GPa, and welding at 1200 ℃ for 300s.
9. A transparent diamond tooth produced by the method for producing a transparent diamond tooth according to any one of claims 1 to 8.
10. Use of a transparent diamond drilling tooth according to claim 9 in oil and gas drilling.
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