CN113234982B - Preparation method of PDC drill bit matrix material - Google Patents
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- CN113234982B CN113234982B CN202110431964.1A CN202110431964A CN113234982B CN 113234982 B CN113234982 B CN 113234982B CN 202110431964 A CN202110431964 A CN 202110431964A CN 113234982 B CN113234982 B CN 113234982B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/08—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on tungsten carbide
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
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- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1036—Alloys containing non-metals starting from a melt
- C22C1/1057—Reactive infiltration
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- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/067—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds comprising a particular metallic binder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
The invention discloses a preparation method of a PDC drill bit matrix material, which is characterized in that high-entropy alloy with a face-centered cubic and body-centered cubic eutectic structure is added into cast tungsten carbide and single-crystal tungsten carbide powder, agarose sol is added after mixing to form slurry, then the slurry is injected into a mold and dried to form the slurry, and finally copper-based dipping alloy is added to carry out infiltration in a vacuum furnace to form the PDC drill bit matrix material containing the high-entropy alloy with the face-centered cubic and body-centered cubic eutectic structures which are uniformly distributed. The preparation method solves the problems that tungsten carbide and metal additives existing in the existing preparation method of the PDC drill bit matrix material are difficult to uniformly disperse, and the like, the hardness is more than or equal to 30HRC, the bending strength is more than or equal to 600MPa, the impact toughness is more than or equal to 4J, and the comprehensive mechanical property is excellent.
Description
Technical Field
The invention relates to a preparation method of a matrix material, in particular to a preparation method of a PDC drill bit matrix material, and belongs to the field of composite materials.
Background
The use of PDC (diamond compact) drill bits is becoming increasingly common in oil production. The PDC drill bit is composed of PDC cutting teeth and a matrix material, the PDC cutting teeth are embedded in the matrix, and the comprehensive performances of hardness, wear resistance, strength, toughness and the like of the matrix are very important for the use performance of the PDC drill bit. The academic and industrial circles pay great attention to the research on the matrix material and the preparation method thereof. CN201911079586.4 discloses a drill bit matrix material and a preparation method thereof, wherein the components of the drill bit matrix material comprise 45.0-65.0% of tungsten carbide hard particles and 35.0-55.0% of copper-containing multi-principal element high-entropy alloy. The preparation method of the drill bit matrix material comprises the steps of carrying out die filling and compaction on tungsten carbide hard particles, and then infiltrating copper-containing multi-principal-element high-entropy alloy at high temperature to obtain the drill bit matrix material, wherein the wear resistance, the strength and the impact toughness of the drill bit matrix material can be greatly improved, so that the service life of the matrix drill bit can be remarkably prolonged, and the drill bit matrix material is particularly suitable for drilling of medium-hard strata. The bonding metal nickel powder is also added into the tungsten carbide cast by the matrix material framework powder, when the nickel content is 2 percent, the performance is in the best state, the bending strength reaches 960MPa, and the impact toughness reaches 3.62J/cm2(Weshifai et al. influence of nickel content on performance of infiltrated matrix material. protective engineering. 2 nd 2019). However, the existing preparation method of the carcass material has two problems: firstly, the added metal powder is difficult to be uniformly dispersed around the carbide hard phase by adopting a tap mode; secondly, although the performance of the matrix material can be improved by carrying out high entropy melting on the copper alloy for dipping the alloy, after the high entropy copper alloy is melted at high temperature in the infiltration process, low melting point metal in the high entropy copper alloy is easy to lose, and the high entropy alloy can have structural relaxation, so that the phase structure of the high entropy alloy is difficult to maintain, and the performance advantage of the high entropy alloy is difficult to be exerted. Therefore, a method for preparing a high-performance carcass material still needs to be continuously developed.
Disclosure of Invention
Aiming at the problems of the existing matrix material preparation method, the invention provides a PDC drill bit matrix material containing uniformly distributed face-centered cubic and body-centered cubic phase eutectic structure high-entropy alloy, which is prepared by adding the high-entropy alloy with the face-centered cubic and body-centered cubic phase eutectic structures into cast tungsten carbide and single-crystal tungsten carbide powder, mixing, adding agarose sol to form slurry, injecting the slurry into a mold, drying and molding, and finally adding copper-based dipping alloy to perform infiltration in a vacuum furnace.
The preparation method of the PDC drill bit matrix material is characterized by sequentially comprising the following steps of:
(1) preparing framework material powder containing high-entropy alloy: preparing framework material powder from cast tungsten carbide, single crystal tungsten carbide powder and AlCoCrFeNiCu high-entropy alloy powder, wherein the AlCoCrFeNiCu is a face-centered cubic and body-centered cubic eutectic structure, the proportion of the AlCoCrFeNiCu in the mixed powder is 2-6 wt.%, the single crystal tungsten carbide accounts for 20-60 wt.%, and the balance is cast tungsten carbide; putting the skeleton powder into a planetary ball mill for dry mixing for 2-4 h to prepare skeleton material powder containing the high-entropy alloy;
(2) preparing agarose sol: adding agarose into deionized water to prepare a solution of 1-5 wt.%, putting the solution into a constant-temperature water bath kettle, preserving heat for 2-3 hours at 80-90 ℃, stirring in the heat preservation process to form agarose sol, and keeping the temperature of the agarose sol at 50-60 ℃ after heat preservation;
(3) preparing framework material slurry: adding agarose sol into skeleton material powder containing high-entropy alloy, wherein the skeleton material powder accounts for 30-40 wt%, preserving heat at 50-60 ℃ for 30-40 min, stirring in the heat preservation process, and forming skeleton material slurry after heat preservation;
(4) molding a framework material blank: pouring the framework material slurry into a graphite mold, and drying in a vacuum drying oven at 100-110 ℃ for 1-2 h to form a framework material blank, wherein the cast tungsten carbide, the single crystal tungsten carbide and the high-entropy alloy are uniformly distributed in the blank;
(5) preparing a PDC drill bit matrix material: placing Cu-Ni-Mn-Sn alloy particles on the upper part of the framework material blank, wherein the weight ratio of the Cu-Ni-Mn-Sn alloy particles to the framework material blank is 1: 1-1.3: 1; then putting the framework material blank body in which the Cu-Ni-Mn-Sn alloy is placed and a graphite mould into a vacuum sintering furnace, keeping the temperature at 400-600 ℃ for 1-2 h to decompose and remove agarose, keeping the temperature at 1150-1200 ℃ for 1-2 h to melt the Cu-Ni-Mn-Sn alloy and immerse the Cu-Ni-Mn-Sn alloy into the framework material blank body, filling pores among cast tungsten carbide, single crystal tungsten carbide and high-entropy alloy and pores left after the agarose is removed, introducing Ar gas with the flow rate of 5-10L/h to rapidly cool after the heat preservation is finished, avoiding the structural relaxation of the high-entropy alloy, keeping the eutectic cubic and body-centered cubic phase structures of the AlCoCrFeNiCu high-entropy alloy, and enabling the tungsten carbide to have no solid solution in the high-entropy alloy, thereby preparing the PDC drill bit matrix material containing the face-centered cubic and body-centered cubic phase eutectic structure high-entropy alloy phases, the hardness is more than or equal to 30HRC, the bending strength is more than or equal to 600MPa, and the impact toughness is more than or equal to 4J.
The preparation method of the PDC drill bit matrix material is further characterized by comprising the following steps:
(1) when the skeleton powder is mixed in a planetary ball mill, the rotating speed of the ball mill is 100-300 r/min;
(2) the stirring speed during the preparation of the agarose sol is 60-100 r/min;
(3) the stirring speed during preparation of the framework material slurry is 60-100 r/min;
(4) when the framework material blank is formed, the drying vacuum degree is less than 20 Pa;
(5) the temperature rise speed during the preparation of the matrix material is 10 ℃/min, the Cu-Ni-Mn-Sn alloy comprises 9.5-11.5 wt% of nickel, 5.5-6.5 wt% of Sn, 5-6.5 wt% of Mn and the balance of Cu.
The invention has the advantages that: (1) the existing tire body preparation method takes high-entropy alloy as an impregnating material, and low-melting-point alloy is easy to run off after being melted and is difficult to maintain the phase structure of the high-entropy alloy; the high-entropy alloy is added into the framework material and uniformly dispersed, and the face-centered cubic structure and the body-centered cubic eutectic phase structure are maintained after infiltration, so that the strength and the toughness of the matrix material can be improved; (2) in the traditional method, a tap method is adopted, the difference between the granularity, the morphology, the specific gravity and the like of spherical cast tungsten carbide powder and other added metal or alloy powder is large, and the metal powder is difficult to be uniformly dispersed with the tungsten carbide powder in the tap process; in the invention, the skeleton material blank is prepared by adopting a dry ball milling and sol slurry forming mode, so that the high-entropy alloy powder and the tungsten carbide powder can be uniformly mixed, the gap uniformity among particles is higher, and the alloy after infiltration is more uniform. (3) The high-entropy alloy adopted in the invention has a delayed diffusion effect, and cannot dissolve in a tungsten carbide metal phase when metals such as nickel and the like are added, so that the content, volume fraction and morphology of tungsten carbide particles are maintained.
Drawings
FIG. 1 is a schematic diagram of a method for preparing a PDC bit matrix material of the present invention.
Detailed Description
Example 1: preparing PDC drill bit matrix material according to the following steps
(1) Preparing framework material powder containing high-entropy alloy: preparing framework material powder from cast tungsten carbide, single crystal tungsten carbide powder and AlCoCrFeNiCu high-entropy alloy powder, wherein AlCoCrFeNiCu is a face-centered cubic and body-centered cubic eutectic structure, the ratio of the AlCoCrFeNiCu in the mixed powder is 3wt.%, the single crystal tungsten carbide is 32wt.%, and the balance is cast tungsten carbide; putting the skeleton powder into a planetary ball mill for dry mixing for 4 hours, wherein the rotating speed of the ball mill is 150r/min, so that skeleton material powder containing the high-entropy alloy is prepared;
(2) preparing agarose sol: adding agarose into deionized water to prepare a 2wt.% solution, placing the solution into a constant-temperature water bath kettle, preserving heat for 2 hours at 85 ℃, stirring the solution at the stirring speed of 80r/min during the heat preservation process to form agarose sol, and keeping the temperature of the agarose sol at 52 ℃ after the heat preservation;
(3) preparing framework material slurry: adding agarose sol into skeleton material powder containing high-entropy alloy, wherein the skeleton material powder accounts for 30 wt%, preserving heat at 55 ℃ for 30min, stirring at the stirring speed of 70r/min during the heat preservation process, and forming skeleton material slurry after the heat preservation is finished;
(4) molding a framework material blank: pouring the framework material slurry into a graphite mold, drying for 1h in a vacuum drying oven at 100 ℃ and the drying vacuum degree of 19Pa to form a framework material blank, wherein the cast tungsten carbide, the single crystal tungsten carbide and the high-entropy alloy are uniformly distributed in the blank;
(5) preparing a PDC drill bit matrix material: placing Cu-Ni-Mn-Sn alloy particles on the upper part of a framework material blank, wherein the Cu-Ni-Mn-Sn alloy comprises the components of 10wt.% of nickel, 5.5wt.% of Sn, 5.5wt.% of Mn and the balance of Cu; the weight ratio of the Cu-Ni-Mn-Sn alloy particles to the framework material blank is 1: 1; then putting the framework material blank body in which the Cu-Ni-Mn-Sn alloy is placed and a graphite mold into a vacuum sintering furnace together, wherein the initial vacuum degree is 18Pa, the heating speed is 10 ℃/min, and the temperature is kept at 450 ℃ for 1h to decompose and remove the agarose; heating to 1150 ℃ at the speed of 10 ℃/min, preserving heat for 1h to melt Cu-Ni-Mn-Sn alloy, immersing the Cu-Ni-Mn-Sn alloy into a framework material blank, filling pores among cast tungsten carbide, monocrystal tungsten carbide and high-entropy alloy and pores left after agarose is removed, introducing Ar gas with the flow of 6L/h to rapidly cool after heat preservation is finished, avoiding structural relaxation of the high-entropy alloy, keeping a face-centered cubic and body-centered cubic eutectic structure of the AlCoCrFeNiCu high-entropy alloy, and preparing the PDC drill bit matrix material containing the high-entropy alloy phase with the face-centered cubic and body-centered cubic eutectic structures, wherein the hardness of the PDC drill bit matrix material is 31HRC, the bending strength of the PDC drill bit matrix material is 650MPa, and the impact toughness of the PDC drill bit matrix material is 4J.
Example 2: preparing PDC drill bit matrix material according to the following steps
(1) Preparing framework material powder containing high-entropy alloy: preparing framework material powder from cast tungsten carbide, single crystal tungsten carbide powder and AlCoCrFeNiCu high-entropy alloy powder, wherein the AlCoCrFeNiCu is a face-centered cubic and body-centered cubic eutectic structure, the proportion of the AlCoCrFeNiCu in the mixed powder is 4wt.%, the single crystal tungsten carbide is 45wt.%, and the balance is cast tungsten carbide; putting the skeleton powder into a planetary ball mill for dry mixing for 3 hours, wherein the rotating speed of the ball mill is 250r/min, so that skeleton material powder containing high-entropy alloy is prepared;
(2) preparing agarose sol: adding agarose into deionized water to prepare a 4wt.% solution, placing the solution into a constant-temperature water bath kettle, preserving heat for 3 hours at 90 ℃, stirring the solution during the heat preservation process at a stirring speed of 90r/min to form agarose sol, and keeping the temperature of the agarose sol at 60 ℃ after the heat preservation;
(3) preparing framework material slurry: adding agarose sol into framework material powder containing high-entropy alloy, wherein the framework material powder accounts for 40 wt%, preserving heat at 58 ℃ for 40min, stirring at the stirring speed of 80r/min in the heat preservation process, and forming framework material slurry after heat preservation;
(4) molding a framework material blank: pouring the framework material slurry into a graphite mold, drying for 2 hours in a vacuum drying oven at 110 ℃ under the drying vacuum degree of 15Pa to form a framework material blank, wherein the cast tungsten carbide, the single crystal tungsten carbide and the high-entropy alloy are uniformly distributed in the blank;
(5) preparing a PDC drill bit matrix material: placing Cu-Ni-Mn-Sn alloy particles on the upper part of a framework material blank, wherein the Cu-Ni-Mn-Sn alloy comprises the components of 11.5wt.% of nickel, 6.5wt.% of Sn, 6wt.% of Mn and the balance of Cu; the weight ratio of the Cu-Ni-Mn-Sn alloy particles to the framework material blank is 1.2: 1; then putting the framework material blank body in which the Cu-Ni-Mn-Sn alloy is placed and a graphite mold into a vacuum sintering furnace together, wherein the initial vacuum degree is 16Pa, the heating speed is 10 ℃/min, and the temperature is kept at 500 ℃ for 2h to decompose and remove the agarose; heating to 1180 ℃ at the speed of 10 ℃/min, preserving heat for 2 hours to melt and immerse the Cu-Ni-Mn-Sn alloy into a framework material blank, filling pores among cast tungsten carbide, monocrystal tungsten carbide and high-entropy alloy and pores left after agarose is removed, introducing Ar gas with the flow of 8L/h to rapidly cool after heat preservation is finished, avoiding structural relaxation of the high-entropy alloy, keeping a face-centered cubic and body-centered cubic eutectic structure of AlCoCrFeNiCu high-entropy alloy, and preparing the PDC drill bit matrix material containing the high-entropy alloy phase with the face-centered cubic and body-centered cubic eutectic structures, wherein the hardness is 33HRC, the bending strength is more than or equal to 760MPa, and the impact toughness is 5J.
Claims (2)
1. A preparation method of a PDC drill bit matrix material is characterized by sequentially comprising the following steps:
(1) preparing framework material powder containing high-entropy alloy: preparing framework material powder from cast tungsten carbide, single crystal tungsten carbide powder and AlCoCrFeNiCu high-entropy alloy powder, wherein the AlCoCrFeNiCu is a face-centered cubic and body-centered cubic eutectic structure, the proportion of the AlCoCrFeNiCu in the mixed powder is 2-6 wt.%, the single crystal tungsten carbide accounts for 20-60 wt.%, and the balance is cast tungsten carbide; putting the skeleton powder into a planetary ball mill for dry mixing for 2-4 h to prepare skeleton material powder containing the high-entropy alloy;
(2) preparing agarose sol: adding agarose into deionized water to prepare a solution of 1-5 wt.%, putting the solution into a constant-temperature water bath kettle, preserving heat for 2-3 hours at 80-90 ℃, stirring in the heat preservation process to form agarose sol, and keeping the temperature of the agarose sol at 50-60 ℃ after heat preservation;
(3) preparing framework material slurry: adding agarose sol into skeleton material powder containing high-entropy alloy, wherein the skeleton material powder accounts for 30-40 wt%, preserving heat at 50-60 ℃ for 30-40 min, stirring in the heat preservation process, and forming skeleton material slurry after heat preservation;
(4) molding a framework material blank: pouring the framework material slurry into a graphite mold, and drying in a vacuum drying oven at 100-110 ℃ for 1-2 h to form a framework material blank, wherein the cast tungsten carbide, the single crystal tungsten carbide and the high-entropy alloy are uniformly distributed in the blank;
(5) preparing a PDC drill bit matrix material: placing Cu-Ni-Mn-Sn alloy particles on the upper part of a framework material blank, wherein the Cu-Ni-Mn-Sn alloy comprises 9.5-11.5 wt% of nickel, 5.5-6.5 wt% of Sn, 5-6.5 wt% of Mn and the balance of Cu; the weight ratio of the Cu-Ni-Mn-Sn alloy particles to the framework material blank is 1: 1-1.3: 1; then putting the framework material blank body in which the Cu-Ni-Mn-Sn alloy is placed and a graphite mould into a vacuum sintering furnace, keeping the temperature at 400-600 ℃ for 1-2 h to decompose and remove agarose, keeping the temperature at 1150-1200 ℃ for 1-2 h to melt the Cu-Ni-Mn-Sn alloy and immerse the Cu-Ni-Mn-Sn alloy into the framework material blank body, filling pores among cast tungsten carbide, single crystal tungsten carbide and high-entropy alloy and pores left after the agarose is removed, introducing Ar gas with the flow rate of 5-10L/h to rapidly cool after the heat preservation is finished, avoiding the structural relaxation of the high-entropy alloy, keeping the eutectic cubic and body-centered cubic phase structures of the AlCoCrFeNiCu high-entropy alloy, and enabling the tungsten carbide to have no solid solution in the high-entropy alloy, thereby preparing the PDC drill bit matrix material containing the face-centered cubic and body-centered cubic phase eutectic structure high-entropy alloy phases, the hardness is more than or equal to 30HRC, the bending strength is more than or equal to 600MPa, and the impact toughness is more than or equal to 4J.
2. The method of preparing a PDC bit matrix material of claim 1, further characterized by:
(1) when the skeleton powder is mixed in a planetary ball mill, the rotating speed of the ball mill is 100-300 r/min;
(2) the stirring speed during the preparation of the agarose sol is 60-100 r/min;
(3) the stirring speed during preparation of the framework material slurry is 60-100 r/min;
(4) when the framework material blank is formed, the drying vacuum degree is less than 20 Pa;
(5) the temperature rise speed during the preparation of the matrix material is 10 ℃/min.
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