CN113249605A - Method for manufacturing metal ceramic matrix material - Google Patents
Method for manufacturing metal ceramic matrix material Download PDFInfo
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- CN113249605A CN113249605A CN202110432419.4A CN202110432419A CN113249605A CN 113249605 A CN113249605 A CN 113249605A CN 202110432419 A CN202110432419 A CN 202110432419A CN 113249605 A CN113249605 A CN 113249605A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/108—Mixtures obtained by warm mixing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F3/26—Impregnating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a method for manufacturing a metal ceramic matrix material, which is characterized in that spherical casting tungsten carbide and high-entropy alloy powder are firstly mixed in a dry mode, gelatin sol is utilized to form metal ceramic slurry, then the metal ceramic slurry is injected into a graphite mold to be dried to form a metal ceramic framework prefabricated member, and finally infiltration is carried out to prepare the metal ceramic matrix material which is uniform in structure and contains a face-centered cubic structure high-entropy alloy phase. The invention overcomes the problems of insufficient obdurability and the like existing in the existing manufacturing method of the matrix material, and has excellent mechanical property, the hardness is more than or equal to 25HRC, the bending strength is more than or equal to 500MPa, and the impact toughness is more than or equal to 5J.
Description
Technical Field
The invention relates to a manufacturing method of a matrix material, in particular to a manufacturing method of a metal ceramic matrix material, and belongs to the field of energy engineering materials.
Background
In an oil drilling tool, the function of the matrix material is to fix PDC cutting teeth and connect with a steel body of a drill bit, and the hardness, the strength, the wear resistance and the toughness of the matrix material are very important for the service performance of the drill bit. The current matrix material mainly adopts cast tungsten carbide as a framework phase and is formed by infiltration of copper-based alloy at high temperature.
As a typical cermet material, its toughness is still insufficient. At present, metal powder such as Ni is mainly added into skeleton powder, and CN110684935A discloses a drill bit matrix material and a preparation method thereof, wherein, tungsten carbide hard particles, nickel powder and 3-10% tungsten fiber are mixed and then are subjected to die filling and compaction; and then the copper alloy is melted and infiltrated at high temperature to obtain the bit matrix material, and the strength and the impact toughness of the bit matrix material are obviously improved, so that the drilling service life of the bit using the matrix material in a medium-soft stratum is greatly prolonged.
It should be noted that although the addition of metallic nickel to the matrix material can improve mechanical properties such as ductility and toughness, the strength of metallic nickel is not high, and tungsten carbide will dissolve in nickel at high temperature, resulting in a decrease in volume fraction of tungsten carbide particles and a decrease in wear resistance. Moreover, the prior tap-infiltration is not favorable for the uniform dispersion of the additional metal powder and the tungsten carbide powder, is difficult to obtain a uniform organization structure and is not favorable for the performance improvement of the matrix material. Therefore, it is very important to find a new method for preparing the cermet matrix material.
Disclosure of Invention
Aiming at the problem of the preparation of the current matrix material, the invention provides a method for preparing the metal ceramic matrix material which has uniform tissue and contains a face-centered cubic structure high-entropy alloy phase and has excellent mechanical property by dry-mixing spherical casting tungsten carbide and high-entropy alloy powder, forming metal ceramic slurry by using gelatin sol, injecting the metal ceramic slurry into a graphite mold for drying and removing the gelatin in vacuum to form a metal ceramic framework prefabricated part, and finally performing infiltration.
The manufacturing method of the metal ceramic matrix material is characterized by sequentially comprising the following steps of:
(1) preparing metal ceramic framework powder: preparing mixed powder by taking spherical cast tungsten carbide powder and CoCrFeNiMn high-entropy alloy powder as raw materials, wherein the CoCrFeNiMn is in a face-centered cubic structure, and the proportion of the CoCrFeNiMn in the mixed powder is 2-12 wt.%; putting the mixed powder into a planetary ball mill for dry mixing for 2-4 h to prepare metal ceramic skeleton powder;
(2) preparing metal ceramic slurry: adding gelatin into deionized water to prepare a solution of 5-15 wt%, placing the solution into a constant-temperature water bath kettle, preserving heat at 60-80 ℃, and continuously stirring for 2-3 hours to form gelatin sol; putting 20-35 g of metal ceramic framework powder into 100ml of gelatin sol, stirring for 30-40 min, and keeping the temperature at 60-80 ℃ in the stirring process to finally form metal ceramic slurry;
(3) preparing a metal ceramic framework prefabricated part: pouring the metal ceramic slurry into a graphite mold, and drying in a vacuum drying oven at 100-110 ℃ for 1-2 h to remove water; then putting the mixture into a vacuum sintering furnace, heating to 600-700 ℃ at the speed of 10 ℃/min, and preserving heat for 1-2 h to remove gelatin, so as to prepare a metal ceramic framework prefabricated part with uniformly dispersed cast tungsten carbide and high-entropy alloy;
(4) infiltration preparation of the metal ceramic matrix material: placing CuNiZnMn alloy particles on the surface of the metal ceramic framework prefabricated part, wherein the weight ratio of the CuNiZnMn alloy particles to the metal ceramic framework prefabricated part is 1: 1-1.2: 1; and then placing the prefabricated part with the copper alloy and a graphite mold into a box-type resistance furnace which is preheated to 1150-1200 ℃, preserving heat for 1-2 h to melt and immerse the CuNiZnMn alloy into the prefabricated part, filling pores between the tungsten carbide and the high-entropy alloy and pores left after gelatin removal, taking out for air cooling after heat preservation is finished, and avoiding structural relaxation, wherein the CoCrFeNiMn high-entropy alloy keeps a face-centered cubic phase, and the tungsten carbide does not have solid solution in the high-entropy alloy, so that the metal ceramic matrix material containing the face-centered cubic high-entropy alloy phase with uniform tissue is prepared, the hardness is more than or equal to HRC, the bending strength is more than or equal to 500MPa, and the impact toughness is more than or equal to 5J.
The manufacturing method of the metal ceramic matrix material of the invention is further characterized in that:
(1) when the metal framework powder is prepared, the rotating speed of the planetary ball mill is 100-300 r/min;
(2) the stirring speed during the preparation of the metal ceramic slurry is 60-100 r/min;
(3) when the metal ceramic framework prefabricated part is prepared, the drying vacuum degree is less than or equal to 20 Pa;
(4) the temperature rising speed of the infiltration preparation of the metal ceramic matrix material is 10 ℃/min, the components of the CuNiZnMn alloy are 40-60 wt% of Cu, 10-25 wt% of Ni, 5-15 wt% of Zn and 20-40 wt% of Mn.
The invention has the advantages that: (1) in the traditional method, a tap method is adopted, the difference between the particle size, morphology, specific gravity and the like of spherical cast tungsten carbide powder and metal powder such as Ni and the like is large, and the metal powder is difficult to be uniformly dispersed with the spherical cast tungsten carbide powder in the tap process; in the invention, the metal ceramic framework prefabricated part is prepared by light mixing, slurry drying, so that the high-entropy alloy powder and the spherical cast tungsten carbide powder can be uniformly mixed, and the uniformity of gaps among particles is higher. (2) After the high-entropy alloy is added, the face-centered cubic structure is kept, the toughness is higher, and the strength can be improved; (3) in the traditional method, Ni metal is added, and WC can be dissolved in Ni due to high solubility of the WC in the Ni, and the high-entropy alloy has a delayed diffusion effect and can avoid the dissolution of the WC in a metal phase, so that the content, volume fraction and morphology of WC particles are maintained.
Drawings
FIG. 1 is a schematic representation of a cermet matrix material of the present invention.
Detailed Description
Example 1: the metal ceramic matrix material is prepared by the following steps
(1) Preparing metal ceramic framework powder: spherical cast tungsten carbide powder and CoCrFeNiMn high-entropy alloy powder are used as raw materials to prepare mixed powder, CoCrFeNiMn is of a face-centered cubic structure, and the proportion of the CoCrFeNiMn in the mixed powder is 2 wt.%; putting the mixed powder into a planetary ball mill for dry mixing for 3 hours, wherein the rotating speed of the planetary ball mill is 180r/min, and preparing metal ceramic framework powder;
(2) preparing metal ceramic slurry: adding gelatin into deionized water to prepare 6wt.% solution, placing the solution into a constant-temperature water bath kettle, keeping the temperature at 65 ℃ and continuously stirring for 2 hours to form gelatin sol; putting 25g of metal ceramic framework powder into 100ml of gelatin sol, and stirring for 30min, wherein the temperature is kept at 65 ℃ in the stirring process, and the stirring speed is 65r/min, so as to finally form metal ceramic slurry;
(3) preparing a metal ceramic framework prefabricated part: pouring the metal ceramic slurry into a graphite mold, drying in a vacuum drying oven at 100 ℃ for 1h to remove water, and drying at a vacuum degree of 20 Pa; then putting the mixture into a vacuum sintering furnace, heating to 600 ℃ at the speed of 10 ℃/min, preserving the heat for 1h, removing gelatin, and obtaining a metal ceramic framework prefabricated part with uniformly dispersed cast tungsten carbide and high-entropy alloy, wherein the vacuum degree is 18 Pa;
(4) infiltration preparation of the metal ceramic matrix material: placing CuNiZnMn alloy particles on the surface of a metal ceramic framework prefabricated part, wherein the CuNiZnMn alloy comprises the components of 45wt.% of Cu, 15wt.% of Ni, 15wt.% of Zn and 25wt.% of Mn; the weight ratio of the CuNiZnMn alloy particles to the metal ceramic framework prefabricated part is 1: 1; and then placing the prefabricated member in which the CuNiZnMn alloy is placed and a graphite mold into a box-type resistance furnace which is preheated to 1150 ℃, preserving heat for 1h, melting and immersing the CuNiZnMn alloy into the prefabricated member, filling pores between the tungsten carbide and the high-entropy alloy and pores left after the gelatin is removed, taking out the prefabricated member for air cooling after finishing the heat preservation, and avoiding the occurrence of structural relaxation, wherein the CoCrFeNiMn high-entropy alloy keeps a face-centered cubic phase, and the tungsten carbide does not have solid solution in the high-entropy alloy, so that the metal ceramic matrix material containing the face-centered cubic high-entropy alloy phase with uniform tissue is prepared, and the hardness of the metal ceramic matrix material is 26HRC, the bending strength is 580MPa, and the impact toughness is 5J.
Example 2: the metal ceramic matrix material is prepared by the following steps
(1) Preparing metal ceramic framework powder: spherical cast tungsten carbide powder and CoCrFeNiMn high-entropy alloy powder are used as raw materials to prepare mixed powder, CoCrFeNiMn is of a face-centered cubic structure, and the proportion of the CoCrFeNiMn in the mixed powder is 10 wt.%; putting the mixed powder into a planetary ball mill for dry mixing for 4 hours, wherein the rotating speed of the planetary ball mill is 250r/min, and preparing metal ceramic framework powder;
(2) preparing metal ceramic slurry: adding gelatin into deionized water to prepare 10wt.% solution, placing the solution into a constant-temperature water bath kettle, keeping the temperature at 80 ℃ and continuously stirring for 3 hours to form gelatin sol; putting 30g of metal ceramic framework powder into 100ml of gelatin sol, and stirring for 40min, wherein the temperature is kept at 80 ℃ in the stirring process, and the stirring speed is 90r/min, so as to finally form metal ceramic slurry;
(3) preparing a metal ceramic framework prefabricated part: pouring the metal ceramic slurry into a graphite mold, drying for 2 hours at 110 ℃ in a vacuum drying oven to remove water, and drying to 18 Pa; then putting the mixture into a vacuum sintering furnace, heating to 700 ℃ at a speed of 10 ℃/min, preserving the heat for 1-2 h, and removing gelatin, wherein the vacuum degree is 20Pa, so as to prepare a metal ceramic framework prefabricated part with uniformly dispersed cast tungsten carbide and high-entropy alloy;
(4) infiltration preparation of the metal ceramic matrix material: placing CuNiZnMn alloy particles on the surface of a metal ceramic framework prefabricated part, wherein the CuNiZnMn alloy comprises 50wt.% of Cu, 20wt.% of Ni, 8wt.% of Zn and 22wt.% of Mn; the weight ratio of the CuNiZnMn alloy particles to the metal ceramic framework prefabricated part is 1.1: 1; then placing the prefabricated member with the CuNiZnMn alloy and a graphite mold into a box-type resistance furnace which is preheated to 1200 ℃, preserving heat for 1.5h to melt the CuNiZnMn alloy and immerse the CuNiZnMn alloy into the prefabricated member, filling pores between the tungsten carbide and the high-entropy alloy and pores left after gelatin removal, taking out the prefabricated member for air cooling after heat preservation is finished, avoiding structural relaxation, keeping the face-centered cubic phase in the CoCrFeNiMn high-entropy alloy, and enabling the tungsten carbide to have no solid solution in the high-entropy alloy, thereby preparing the metal ceramic matrix material containing the face-centered cubic high-entropy alloy phase with uniform tissue, wherein the hardness of the metal ceramic matrix material is HRC 28, the bending strength of 650MPa and the impact toughness of 5.5J.
Claims (2)
1. The manufacturing method of the ceramic matrix material is characterized by sequentially comprising the following steps of:
(1) preparing metal ceramic framework powder: preparing mixed powder by taking spherical cast tungsten carbide powder and CoCrFeNiMn high-entropy alloy powder as raw materials, wherein the CoCrFeNiMn is in a face-centered cubic structure, and the proportion of the CoCrFeNiMn in the mixed powder is 2-12 wt.%; putting the mixed powder into a planetary ball mill for dry mixing for 2-4 h to prepare metal ceramic skeleton powder;
(2) preparing metal ceramic slurry: adding gelatin into deionized water to prepare a solution of 5-15 wt%, placing the solution into a constant-temperature water bath kettle, preserving heat at 60-80 ℃, and continuously stirring for 2-3 hours to form gelatin sol; putting 20-35 g of metal ceramic framework powder into 100ml of gelatin sol, stirring for 30-40 min, and keeping the temperature at 60-80 ℃ in the stirring process to finally form metal ceramic slurry;
(3) preparing a metal ceramic framework prefabricated part: pouring the metal ceramic slurry into a graphite mold, and drying in a vacuum drying oven at 100-110 ℃ for 1-2 h to remove water; then putting the mixture into a vacuum sintering furnace, heating to 600-700 ℃ at the speed of 10 ℃/min, and preserving heat for 1-2 h to remove gelatin, so as to prepare a metal ceramic framework prefabricated part with uniformly dispersed cast tungsten carbide and high-entropy alloy;
(4) infiltration preparation of the metal ceramic matrix material: placing CuNiZnMn alloy particles on the surface of the metal ceramic framework prefabricated part, wherein the weight ratio of the CuNiZnMn alloy particles to the metal ceramic framework prefabricated part is 1: 1-1.2: 1; and then placing the prefabricated part with the copper alloy and a graphite mold into a box-type resistance furnace which is preheated to 1150-1200 ℃, preserving heat for 1-2 h to enable the CuNiZnMn alloy to be melted and immersed into the prefabricated part, filling pores between the tungsten carbide and the high-entropy alloy and pores left after gelatin is removed, taking out for air cooling after heat preservation is finished, and avoiding structural relaxation, wherein the CoCrFeNiMn high-entropy alloy keeps a face-centered cubic phase, and the tungsten carbide does not have solid solution in the high-entropy alloy, so that the metal ceramic matrix material containing the face-centered cubic high-entropy alloy phase with uniform tissue is prepared, the hardness is more than or equal to 25HRC, the bending strength is more than or equal to 500MPa, and the impact toughness is more than or equal to 5J.
2. The cermet matrix material manufacturing method according to claim 1, further characterized in that:
(1) when the metal framework powder is prepared, the rotating speed of the planetary ball mill is 100-300 r/min;
(2) the stirring speed during the preparation of the metal ceramic slurry is 60-100 r/min;
(3) when the metal ceramic framework prefabricated part is prepared, the drying vacuum degree is less than or equal to 20 Pa;
(4) the temperature rising speed of the infiltration preparation of the metal ceramic matrix material is 10 ℃/min, the components of the CuNiZnMn alloy are 40-60 wt% of Cu, 10-25 wt% of Ni, 5-15 wt% of Zn and 20-40 wt% of Mn.
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