CN110106383B - WC reinforced Cu-Cr composite material and preparation method thereof - Google Patents

WC reinforced Cu-Cr composite material and preparation method thereof Download PDF

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CN110106383B
CN110106383B CN201910498484.XA CN201910498484A CN110106383B CN 110106383 B CN110106383 B CN 110106383B CN 201910498484 A CN201910498484 A CN 201910498484A CN 110106383 B CN110106383 B CN 110106383B
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CN110106383A (en
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宋克兴
国秀花
冯江
李韶林
王旭
刘海涛
程楚
赵培峰
周延军
张彦敏
皇涛
林焕然
张祥峰
杨豫博
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Henan University of Science and Technology
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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
    • B22F3/02—Compacting only
    • B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007—Atmosphere
    • 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
    • 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
    • C22C1/10—Alloys containing non-metals
    • C22C1/1036—Alloys containing non-metals starting from a melt
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon

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Abstract

The invention belongs to the technical field of non-ferrous metal alloys, and particularly relates to a WC (wolfram carbide) reinforced Cu-Cr composite material and a preparation method thereof. The preparation method of the WC reinforced Cu-Cr composite material comprises the following steps: 1) melting the consumable electrode by adopting vacuum consumable arc to obtain an ingot; the consumable electrode mainly comprises the following components in percentage by mass: 0.5-20% of WC, 80-99.5% of Cu and Cr, wherein the mass ratio of Cu to Cr is 100: (0.4 to 1.1); 2) and carrying out aging treatment on the cast ingot. The preparation method further improves the friction and wear resistance of the composite material. The composite material prepared by the preparation method has better plasticity and toughness, and further improves the strength and the frictional wear resistance.

Description

WC reinforced Cu-Cr composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of non-ferrous metal alloys, and particularly relates to a WC (wolfram carbide) reinforced Cu-Cr composite material and a preparation method thereof.
Background
The copper-based composite material is widely applied to the fields of rail transit, power industry, electronic information and the like due to good electric conductivity. Precipitation strengthened Cu-Cr alloys are well known for their high strength and high electrical conductivity. The nanometer Cr particles formed by the precipitation of Cr element in the Cu-Cr alloy are uniformly distributed in the copper matrix in the aging treatment process, thereby increasing the mechanical property of the composite material. The submicron or micron-sized particles can play a good supporting role for the material during friction, thereby improving the friction and wear resistance of the material. Particle-reinforced copper-based composites find use in many commercial products due to their outstanding high strength and high wear resistance, as well as low coefficient of thermal expansion.
At present, the common preparation methods of WC reinforced copper-based composite materials in the prior art include a powder metallurgy method and a mechanical alloying method. The powder metallurgy method is to mix copper alloy powder and high-melting-point reinforcing phase WC powder, and then to prepare the copper-based composite material through blank pressing, forming and sintering. For example, chinese patent document No. CN105220004B discloses a copper-based electrical contact composite material and a method for preparing the same. The copper-based electric contact composite material comprises the following components in percentage by mass: 10-30% of chromium, 1-5% of tungsten carbide and the balance of copper; the raw materials of each component are mixed and then are prepared into the composite material by a spark plasma sintering process. However, the composite material prepared by the method has poor matrix ductility and toughness, relatively poor interface bonding and low density, and the application of the composite material is severely restricted. The mechanical alloying method comprises the following steps: the copper alloy powder and the reinforcing phase in a certain proportion are ground in a high-energy ball mill for a long time, so that the organization structure of the metal powder is continuously refined in the frequent collision process, and the reinforcing phase is uniformly distributed.
Disclosure of Invention
The invention aims to provide a preparation method of a WC reinforced Cu-Cr composite material, which further improves the friction and wear resistance of the composite material.
The invention also aims to provide the WC reinforced Cu-Cr composite material prepared by the preparation method, and the composite material has higher friction and wear resistance.
In order to realize the purpose, the preparation method of the WC reinforced Cu-Cr composite material adopts the technical scheme that:
a preparation method of a WC reinforced Cu-Cr composite material comprises the following steps:
1) melting the consumable electrode by adopting vacuum consumable arc to obtain an ingot; the consumable electrode mainly comprises the following components in percentage by mass: 0.5-20% of WC, 80-99.5% of Cu and Cr, wherein the mass ratio of Cu to Cr is 100: (0.4 to 1.1);
2) and carrying out aging treatment on the cast ingot.
During the melting process, the copper matrix in the consumable electrode melts into a liquid phase under the action of the electric arc, and the reinforcing phase WC keeps a granular state and is hardly melted. The reinforced phase WC particles form molten drops along with the liquid phase of the copper matrix and drop from the consumable electrode to gradually form an ingot, so that the WC particles are uniformly distributed in the copper matrix, the interface bonding strength between the reinforced phase WC and the copper matrix is effectively improved, the matrix plasticity and the density of the composite material are improved, and the strength and the friction and wear resistance of the composite material are further improved. Meanwhile, the preparation method avoids introducing impurity elements and has low cost.
The consumable electrode is prepared by a method comprising the steps of: mixing the mixed powder of Cu powder and Cr powder or Cu-Cr alloy powder with WC powder to obtain mixed powder, and then sequentially pressing and sintering the mixed powder to obtain the alloy powder. The raw material powders are uniformly mixed, so that the reinforcing phase WC is further uniformly distributed in the copper matrix.
The pressing pressure is 150-300 MPa, and the pressing time is 5-10 min. Pressing is a process of compacting metal powder into a compact having a certain shape and strength, and during pressing, new particle contacts are generated, so that the particles are more densely packed, the pores are reduced, and preparation is made for subsequent sintering.
The sintering comprises the following steps: preserving heat for 1-4 h at 550-750 ℃, and then preserving heat for 1-5 h at 900-1070 ℃. Isothermal sintering is carried out in two steps to reduce the stress of the blank and homogenize the temperature of the blank, so as to prepare for obtaining a compact composite material.
The step 1) also comprises the ultrasonic treatment of the formed metal molten pool in the smelting process. Ultrasonic treatment is carried out simultaneously in the smelting process, the contents of impurities and gases in the material are effectively reduced under the double actions of ultrasonic and vacuum in the furnace, the ingot is purified, and the density of the composite material is improved. The microstructure with metallurgical quality can be obtained by ultrasonic-vacuum consumable arc melting, the interface combination of a matrix and a reinforcing phase is improved, and the wear resistance of the copper-based composite material is improved.
The ultrasonic frequency of the ultrasonic treatment is 5-15 kHz.
The initial power of ultrasonic treatment is 300-400W, and the power of ultrasonic treatment is increased along with the increase of the height of a smelting pool.
The speed of increase of power of the sonication was: when the height of the metal molten pool is increased by 9-11 mm, the ultrasonic vibration power is increased by 9-11W.
In order to ensure the smelting and reduce the energy consumption, the smelting current in the step 1) is 1000-4500A.
The technical scheme adopted by the WC reinforced Cu-Cr composite material is as follows:
a WC reinforced Cu-Cr composite material prepared by the preparation method of the WC reinforced Cu-Cr composite material.
The Cr particles in the WC reinforced Cu-Cr composite material improve the strength and hardness of a copper matrix, and the WC particles further improve the strength and hardness, play a role of a wear-resistant phase and a supporting phase in a friction and wear process and improve the friction and wear resistance of the composite material. Meanwhile, the composite material has a microstructure with metallurgical quality, the interface bonding strength between the reinforced phase WC and the copper matrix is enhanced, the compactness is high, the strength is higher, and the friction and wear resistance is higher.
Drawings
FIG. 1 is an SEM image of a composite material in example 1 of a WC reinforced Cu-Cr composite material according to the invention;
fig. 2 is an SEM image of the composite material in example 3 of the WC reinforced Cu-Cr composite material of the present invention.
Detailed Description
The preparation method of the WC reinforced Cu-Cr composite material comprises the following steps:
1) melting the consumable electrode by adopting vacuum consumable arc to obtain an ingot; the consumable electrode mainly comprises the following components in percentage by mass: 0.5-20% of WC, 85-99.5% of Cu and Cr, wherein the mass ratio of Cu to Cr is 100: (0.4 to 1.1);
2) and carrying out aging treatment on the cast ingot.
The consumable electrode is prepared by a method comprising the steps of: mixing the mixed powder of Cu powder and Cr powder or Cu-Cr alloy powder with WC powder to obtain mixed powder, and then sequentially pressing and sintering the mixed powder to obtain the alloy powder.
Preferably, the consumable electrode in the step 1) is composed of the following components in percentage by mass: 8-15.5% of WC, and 84.5-92% of Cu and Cr. Further preferably, the mass ratio of Cu to Cr is 100: (0.5-0.9).
The mixing is carried out in a mixer.
The mixing time is 2-16 h.
The pressing comprises the following steps: and (3) loading the mixture into a die, vibrating, rolling and reversely upsetting, and then pressing.
Preferably, the mold is a gum cover.
Preferably, the vibration is a mechanical vibration. The vibration time is 40-70 s.
Preferably, the material rolling time is 4-8 min.
Preferably, the reverse material upsetting times are 4-6.
Preferably, the pressing is performed by cold isostatic pressing. Further preferably, the pressing pressure is 180 to 300 MPa. The pressing time is 6-8 min.
The sintering is carried out under a protective atmosphere or under vacuum conditions.
Preferably, the protective atmosphere is at least one of hydrogen, nitrogen, argon and helium. The protective atmosphere protects the consumable electrode from oxidation during sintering.
Preferably, the degree of vacuum during sintering under vacuum is 1X 10-3～1×10-1Pa. The vacuum sintering effectively reduces the gas content in the consumable electrode, and is beneficial to improving the density of the material.
Preferably, the temperature of vacuum sintering is 950-1060 ℃.
And 2) the aging treatment is carried out for 1-6 h at the temperature of 400-600 ℃.
The smelting process comprises the following specific steps: and smelting the sintered consumable electrode bar in a vacuum consumable electrode furnace, vacuumizing the vacuum consumable electrode furnace after a furnace door is closed, then filling protective gas, smelting in the vacuum consumable electrode furnace, controlling the smelting voltage to be 23-28V, and dripping the consumable electrode into a water-cooled copper crucible after the consumable electrode is molten under the action of electric arc, so as to quickly solidify the consumable electrode bar into an ingot.
Preferably, the current during smelting is 3800-4300A.
The invention is further described with reference to the following specific embodiments and the accompanying drawings.
Example 1 of a method for preparing a WC-reinforced Cu-Cr composite
The preparation method of the WC reinforced Cu-Cr composite material comprises the following steps:
(1) weighing 18.21kg of copper powder, 0.09kg of Cr powder (the mass of the Cr powder is 0.5 percent of that of the Cu powder) and 1.7kg of WC powder (the average grain diameter is 0.5 mu m), and then mixing for 4h in a mixer to obtain a mixture;
(2) loading the mixture into a rubber sleeve, mechanically vibrating for 45s, rolling for 5min (the concrete operation process of rolling is that the mixture is horizontally placed on the ground and rolls), reversely upsetting for 5 times (the concrete operation process of reversely upsetting is that the bottom of the mixture is upward and the material is downward), and then carrying out cold isostatic pressing for 10min under the condition of 200MPa to obtain a press-formed consumable electrode;
(3) the pressed consumable electrode is sintered in a vacuum sintering furnace in vacuum (the vacuum degree is 1 multiplied by 10)-3Pa), the temperature is preserved for 2h at 650 ℃ during sintering, and then the temperature is preserved for 2h at 1020 ℃;
(4) putting the sintered consumable electrode into a vacuum consumable arc furnace for smelting, wherein the current is 3800A during smelting to obtain an ingot;
(5) machining the obtained cast ingot, and then carrying out aging treatment at the temperature of 450 ℃ for 4 h.
Example 2 of a method for preparing a WC-reinforced Cu-Cr composite
The preparation method of the WC reinforced Cu-Cr composite material comprises the following steps:
(1) weighing 16.75kg of copper powder, 0.15kg of Cr powder (the mass of the Cr powder is 0.9 percent of that of the Cu powder) and 3kg of WC powder (the average grain diameter is 10 mu m), and then mixing for 6 hours in a mixer to obtain a mixture;
(2) loading the mixture into a rubber sleeve, mechanically vibrating for 60s, rolling for 4min, reversely upsetting for 5 times, and carrying out cold isostatic pressing for 7min under the condition of 230MPa to obtain a press-formed consumable electrode;
(3) the pressed consumable electrode is sintered in a vacuum sintering furnace in vacuum (the vacuum degree is 1 multiplied by 10)-3Pa), the temperature is preserved for 2h at 650 ℃ during sintering, and then the temperature is preserved for 5h at 1020 ℃;
(4) putting the sintered consumable electrode into a vacuum consumable arc furnace for smelting, wherein the current is 4300A during smelting, after the smelting starts to arc, starting an ultrasonic generator to carry out ultrasonic treatment on a metal molten pool after the metal molten pool is formed at the bottom of a crucible, the ultrasonic frequency is 15kHz, the initial power is 350W, the ultrasonic power is increased along with the smelting, the ultrasonic treatment is carried out at the speed of 10W power increase every 10mm increase of the height of the metal molten pool until the smelting stops to obtain an ingot;
(5) machining the obtained cast ingot, and then carrying out aging treatment at the temperature of 450 ℃ for 4 h.
Example 3 of a method for preparing a WC-reinforced Cu-Cr composite
The preparation method of the WC reinforced Cu-Cr composite material comprises the following steps:
(1) weighing 18.3kg of Cu-Cr alloy powder (the mass content of Cr is 0.5 percent) and 1.7kg of WC powder (the average grain diameter is 0.5 mu m), and then mixing for 5 hours in a mixer to obtain a mixture;
(2) loading the mixture into a rubber sleeve, mechanically vibrating for 50s, rolling for 5min, reversely upsetting for 5 times, and carrying out cold isostatic pressing for 5min under the condition of 220MPa to obtain a press-formed consumable electrode;
(3) sintering the pressed consumable electrode in a vacuum sintering furnace (vacuum degree of 1 × 10)-3Pa), the temperature is preserved for 2h at 700 ℃ during sintering, and then the temperature is preserved for 2.5h at 1020 ℃;
(4) putting the sintered consumable electrode into a vacuum consumable arc furnace for smelting, wherein the current is 3800A during smelting, after the smelting starts to be in an arc state, after a metal molten pool is formed at the bottom of a crucible, starting an ultrasonic generator to carry out ultrasonic treatment on the metal molten pool, wherein the ultrasonic frequency is 15kHz, the initial power is 350W, the ultrasonic power is increased along with the smelting, and the ultrasonic treatment is carried out at the speed of 10W power increase every 10mm increase of the height of the metal molten pool until the smelting stops in an arc state, so that an ingot is obtained;
(5) machining the obtained cast ingot, and then carrying out aging treatment at the temperature of 450 ℃ for 4 h.
Example 4 of a method for preparing a WC-reinforced Cu-Cr composite
The preparation method of the WC reinforced Cu-Cr composite material comprises the following steps:
(1) weighing 17kg of Cu-Cr alloy powder (the mass content of Cr is 0.9%) and 3kg of WC powder (the average grain diameter is 10 mu m), and mixing for 5 hours in a mixer to obtain a mixture;
(2) loading the mixture into a rubber sleeve, mechanically vibrating for 50s, rolling for 5min, reversely upsetting for 5 times, and carrying out cold isostatic pressing for 7min under the condition of 230MPa to obtain a press-formed consumable electrode;
(3) the pressed consumable electrode is sintered in a vacuum sintering furnace in vacuum (the vacuum degree is 1 multiplied by 10)-3Pa), the sintering is carried out by preserving the heat for 2h at 700 ℃,then preserving the heat for 2h at 1020 ℃;
(4) putting the sintered consumable electrode into a vacuum consumable arc furnace for smelting, wherein the current is 4300A during smelting, after the smelting starts to arc, after a metal molten pool is formed at the bottom of a crucible, starting an ultrasonic generator to carry out ultrasonic treatment on the metal molten pool, wherein the ultrasonic frequency is 10kHz, the initial power is 380W, the ultrasonic power is increased along with the smelting, the ultrasonic treatment is carried out at the speed of 10W power increase every 10mm increase of the height of the metal molten pool until the smelting stops to obtain an ingot;
(5) machining the obtained cast ingot, and then carrying out aging treatment at the temperature of 450 ℃ for 4 h.
Example 1 of WC reinforced Cu-Cr composite
The WC-reinforced Cu-Cr composite material of the present example was obtained by the preparation method of example 1 of the preparation method of the WC-reinforced Cu-Cr composite material.
Example 2 of WC reinforced Cu-Cr composite
The WC-reinforced Cu-Cr composite material of the present example was obtained by the preparation method of example 2 of the preparation method of the WC-reinforced Cu-Cr composite material.
Example 3 of WC reinforced Cu-Cr composite
The WC-reinforced Cu-Cr composite material of the present example was obtained by the preparation method of example 3 of the preparation method of the WC-reinforced Cu-Cr composite material.
Example 4 of WC reinforced Cu-Cr composite
The WC-reinforced Cu-Cr composite material of the present example was obtained by the preparation method of example 4 of the preparation method of the WC-reinforced Cu-Cr composite material.
Test example 1
SEM characterization was performed on the composites of examples 1 and 3 of the WC reinforced Cu — Cr composite of the present invention, and the test results are shown in fig. 1 and 2. In fig. 1 and 2, the black part is a Cu — Cr composite matrix, and the white part is WC, and it is known from fig. 1 and 2 that the WC particles can be dispersed more uniformly by introducing ultrasonic waves.
Test example 2
The performance of the composite materials of examples 1 to 4 of the WC-reinforced Cu-Cr composite material of the present invention was tested. Wherein, the processing and the detection strength of the sample are carried out according to GB/T228.1-2010, and the hardness is detected according to a GB/T231.1-2009 metal Brinell hardness test method; the detection standard of the wear resistance is as follows: detecting in a self-made HST-100 high-speed current-carrying frictional wear tester (pin-disc type contact mode: pressure 40N, current 60A); the conductivity was measured according to the GB/T32791-2016 copper and copper alloy conductivity eddy current test method, and the measurement results are shown in Table 1.
TABLE 1 Properties of the composites
Figure BDA0002089403170000061
As can be seen from Table 1, the WC reinforced Cu-Cr composite material has high strength, good plasticity and good wear resistance, and WC particles can be better dispersed by introducing ultrasonic waves in the process of vacuum consumable arc melting so as to be uniformly distributed in a copper matrix.

Claims (6)

1. A preparation method of a WC reinforced Cu-Cr composite material is characterized by comprising the following steps:
1) melting the consumable electrode by adopting vacuum consumable arc to obtain an ingot; the consumable electrode mainly comprises the following components in percentage by mass: 0.5-20% of WC, 80-99.5% of Cu and Cr, wherein the mass ratio of Cu to Cr is 100: (0.4 to 1.1); the consumable electrode is prepared by a method comprising the steps of: mixing mixed powder of Cu powder and Cr powder or Cu-Cr alloy powder with WC powder to obtain mixed powder, and then sequentially pressing and sintering the mixed powder to obtain the alloy powder; the pressing pressure is 150-300 MPa, and the pressing time is 5-10 min; the sintering comprises the following steps: preserving heat for 1-4 h at 550-750 ℃, and then preserving heat for 1-5 h at 900-1070 ℃; the smelting current is 1000-4500A, and the smelting voltage is 23-28V;
2) machining the cast ingot obtained in the step 1), and then performing aging treatment to obtain a WC reinforced Cu-Cr composite material; the aging treatment is carried out for 1-6 h at the temperature of 400-600 ℃.
2. The method of preparing a WC reinforced Cu-Cr composite according to claim 1, characterized in that in step 1) the molten metal bath formed is sonicated during the smelting process.
3. The method for preparing a WC-reinforced Cu-Cr composite material according to claim 2, wherein the ultrasonic frequency of the ultrasonic treatment is 5-15 kHz.
4. The method for preparing a WC-reinforced Cu-Cr composite material according to claim 2, wherein the initial power of the ultrasonic treatment is 300-400W, and the power of the ultrasonic treatment is increased along with the increase of the height of a metal molten pool.
5. The method of preparing a WC reinforced Cu-Cr composite according to claim 4, wherein the power of the ultrasonic treatment is increased at a rate of: when the height of the metal molten pool is increased by 9-11 mm, the ultrasonic power is increased by 9-11W.
6. A WC-reinforced Cu-Cr composite material prepared by the method of claim 1.
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