CN111893332A - Preparation method of copper alloy, copper alloy obtained by adopting preparation method, application of copper alloy, electronic component and mechanical component - Google Patents
Preparation method of copper alloy, copper alloy obtained by adopting preparation method, application of copper alloy, electronic component and mechanical component Download PDFInfo
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- CN111893332A CN111893332A CN202010793087.8A CN202010793087A CN111893332A CN 111893332 A CN111893332 A CN 111893332A CN 202010793087 A CN202010793087 A CN 202010793087A CN 111893332 A CN111893332 A CN 111893332A
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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
- C22C1/02—Making non-ferrous alloys by melting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- C22C32/001—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 only oxides
- C22C32/0015—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 only oxides with only single oxides as main non-metallic constituents
- C22C32/0021—Matrix based on noble metals, Cu or alloys thereof
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- 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
Abstract
The invention relates to the field of nonferrous metals, and particularly provides a preparation method of a copper alloy, the copper alloy obtained by the method, application of the copper alloy, an electronic component and a mechanical component. The preparation method of the copper alloy comprises the following steps: (a) pressing the nano particles into blocks to obtain powder blocks; (b) adding the powder blocks into the copper liquid, stirring for 2-4 times at a stirring speed of 60-120r/min for 20-30s, and then sequentially carrying out heat preservation, cooling and cooling to obtain the copper alloy. The preparation method adopts a mode of adding nano particles outside to disperse and strengthen the copper alloy, has simple process, short production period, low cost and excellent mechanical property, can be realized without using special equipment, and is suitable for industrial mass production.
Description
Technical Field
The invention relates to the field of nonferrous metals, in particular to a preparation method of a copper alloy, the copper alloy obtained by the method, application of the copper alloy, an electronic component and a mechanical component.
Background
The copper alloy is formed by adding one or more other elements into pure copper serving as a matrix, has excellent electrical conductivity, thermal conductivity, ductility and corrosion resistance, and has wide application prospect. In order to improve the comprehensive properties of the copper alloy and further expand the application range of the copper alloy, strengthening particles are generally added into the copper to block dislocation movement or crack propagation, so that the mechanical properties of the copper alloy are effectively improved.
At present, the main methods for introducing the second phase into the copper alloy matrix are as follows: internal oxidation and mechanical alloying. The aluminum oxide dispersion strengthening copper-based composite material prepared by adopting an internal oxidation method mainly has the following two forms: firstly, Cu-Al alloy powder and an oxidizing medium are uniformly mixed according to a certain proportion and then are subjected to internal oxidation under a closed condition, and the method has higher preparation cost because the oxidizing medium needs to be added, the powder is mixed for a long time and the redundant oxidizing medium is reduced by hydrogen; the other method is to oxidize Al element in the premise of ensuring that the substrate is not oxidized by strictly controlling the oxygen potential of the system, and the method needs to strictly control the oxygen partial pressure because of higher requirement on the vacuum degree. The mechanical alloying method is characterized in that pre-alloyed element powder is mixed, the pre-alloyed element powder runs at a high speed in a high-energy ball milling device, rotary mechanical energy is transferred to the powder, and the powder is impacted, extruded and repeatedly broken under a cold condition in the rotary process to form dispersed ultrafine particles so as to realize solid state alloying; however, this method is prone to generate impurities, contamination, oxidation and stress during the grinding process, it is difficult to obtain a clean nanocrystal surface, and the grain size of the material is not easy to control.
Therefore, the method has the problems of complex process, high requirements on production conditions, difficulty in controlling product quality, high production cost and the like, and is difficult to realize large-scale production, so that the further development, popularization and application of the dispersion strengthened copper alloy are limited.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide a preparation method of copper alloy, which adopts a mode of adding nano particles outside to dispersion strengthen the copper alloy, has simple process, short production period, low cost and excellent mechanical property, can be realized without using special equipment and is suitable for industrial mass production.
The second purpose of the invention is to provide the copper alloy prepared by the method.
The third purpose of the invention is to provide the application of the copper alloy.
A fourth object of the present invention is to provide an electronic component or a mechanical component.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
in a first aspect, the present invention provides a method for preparing a copper alloy, comprising the steps of: (a) pressing the nano particles into blocks to obtain powder blocks; (b) adding the powder blocks into the copper liquid, stirring for 2-4 times at a stirring speed of 60-120r/min for 20-30s, and then sequentially carrying out heat preservation, cooling and cooling to obtain the copper alloy.
As a further preferred technical solution, the melting point of the nanoparticles is higher than 2000 ℃;
preferably, the nanoparticles comprise inorganic nanoparticles;
preferably, the inorganic nanoparticles include MgO, Al2O3、TiN、ZrO2Or WC;
preferably, the nanoparticles have an average particle size of less than 20 nm.
As a further preferable technical proposal, the content of the nano particles is 0.05 to 0.25 weight percent.
As a further preferred technical solution, the method further comprises the steps of: pressing the nano particles into blocks, and then wrapping the blocks with copper foil to obtain powder blocks;
preferably, the method further comprises the steps of: fixing the powder block at one end of a connector which does not react with the copper liquid, placing one end of the connector, which is connected with the powder block, at the bottom of the copper liquid, and stirring for 2-4 times, wherein the melting point of the connector is higher than 2000 ℃;
preferably, the connector comprises a molybdenum rod.
As a further preferred technical solution, the copper liquid is obtained by the following steps: putting the copper block into a resistance furnace for heating, introducing inert gas in the heating process, and obtaining copper liquid after the copper block is completely melted;
preferably, the heating comprises: firstly, heating to 600-700 ℃ at the speed of 5-10 ℃/min, and preserving heat for 40-60 min; then, heating to 1200-1300 ℃ at the speed of 5-10 ℃/min;
preferably, the flow rate of the inert gas is 2 to 3m3/h。
As a further preferable technical proposal, the powder block is added into the copper liquid or is stirred, and the flow rate of the inert gas is 3-4m3/h；
Preferably, the agitating comprises: stirring once every 3-5min, wherein forward stirring and reverse stirring are adopted for single stirring, and the forward stirring time and the reverse stirring time are respectively 10-15 s.
As a further preferable technical scheme, in the step (b), the heat preservation time is 5-10 min;
preferably, the temperature is reduced to 1100-1150 ℃ after heat preservation;
preferably, the means of cooling comprises water cooling.
In a second aspect, the invention provides a copper alloy obtained by the above copper alloy preparation method.
In a third aspect, the present invention provides the use of a copper alloy as described above for the manufacture of electronic or mechanical components.
In a fourth aspect, the present invention provides an electronic or mechanical component.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method of the copper alloy provided by the invention adopts the nano particles as second phase strengthening particles, has small particle size, is added into the copper liquid after being pressed into blocks, and simultaneously adopts a stirring mode, compared with a mode of directly adding the nano particles, the method is easy to disperse and distribute the nano particles in the copper liquid. The method adopts a mode of adding nano particles outside to disperse and strengthen the copper alloy, has simple process, short production period, low cost and excellent mechanical property, can be realized without using special equipment, and is suitable for industrial mass production.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer.
According to one aspect of the present invention, there is provided in at least one embodiment a method of making a copper alloy, comprising the steps of: (a) pressing the nano particles into blocks to obtain powder blocks; (b) adding the powder blocks into the copper liquid, stirring for 2-4 times at a stirring speed of 60-120r/min for 20-30s, and then sequentially carrying out heat preservation, cooling and cooling to obtain the copper alloy.
The preparation method adopts the nano particles as second phase strengthening particles, has small particle size, is added into the copper liquid after being pressed into blocks, and simultaneously adopts a stirring mode, compared with a mode of directly adding the nano particles, the method is easy to disperse and distribute the nano particles in the copper liquid. The method adopts a mode of adding nano particles outside to disperse and strengthen the copper alloy, has simple process, short production period, low cost and excellent mechanical property, can be realized without using special equipment, and is suitable for industrial mass production.
The number of stirring is, for example, 2, 3 or 4. If the stirring is carried out only once, the nano particles in the powder block cannot be completely dispersed and distributed in the copper liquid, and the production efficiency is reduced if the stirring is carried out for too many times. In addition, the stirring frequency can also be seen, the invention adopts an interval stirring mode, on one hand, the interval stirring can effectively avoid the risk that the external gas is dissolved into the copper liquid caused by single long-time stirring, so as to ensure the performance of the copper alloy, on the other hand, the invention can also effectively protect the stirring tool, and the stirring tool can be fully cooled within the stirring interval time, so that the loss of the stirring tool is reduced, and the service life of the stirring tool is prolonged.
The stirring rate is, for example, 60, 65, 70, 75, 80, 85, 90, 95, 100, 105, 110, 115 or 120 r/min. The time of the above-mentioned single stirring is, for example, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29 or 30 seconds. When the stirring speed and the single stirring time are within the above ranges, the nano particles in the powder block can be uniformly dispersed in the copper liquid as much as possible, if the stirring speed is too slow or the stirring time is too short, the dispersion uniformity of the nano particles is poor, and if the stirring speed is too fast or the stirring time is too long, the dispersion uniformity of the nano particles is not further obviously improved, but time and energy are wasted.
In a preferred embodiment, the nanoparticles have a melting point above 2000 ℃. When the melting point of the nano particles is higher than 2000 ℃, the high-temperature stability of the nano particles is better, the nano particles cannot be melted in copper liquid, and the high-temperature stability of the copper alloy is ensured.
Preferably, the nanoparticles comprise inorganic nanoparticles.
Preferably, the inorganic nanoparticles include MgO, Al2O3、TiN、ZrO2Or WC. The nanoparticles are typically but not limited to MgO, Al2O3，TiN，ZrO2WC, MgO and Al2O3Combination of (A), TiN and ZrO2Combination of (A) and (B), ZrO2Combination with WC, MgO, Al2O3And TiN or TiN, ZrO2And WC, and the like. The nano particles have wide sources and higher hardness and melting point, and are favorable for further improving the mechanical property and the high-temperature stability of the copper alloy.
Preferably, the nanoparticles have an average particle size of less than 20 nm. The above average particle size is typically, but not limited to, 5, 10, 15 or 20 nm. If the average particle diameter of the nanoparticles is too high, the crack propagation preventing effect is deteriorated, and when the average particle diameter of the nanoparticles is less than 20nm, the mechanical properties of the copper alloy are higher.
The average particle size refers to a linear average particle size, and is measured by a laser particle sizer.
In a preferred embodiment, the nanoparticles are present in an amount of 0.05 to 0.25 wt.%. The above-mentioned content refers to the mass of the nanoparticles as a percentage of the total mass of the copper alloy, and is typically, but not limited to, 0.05 wt%, 0.06 wt%, 0.07 wt%, 0.08 wt%, 0.1 wt%, 0.12 wt%, 0.14 wt%, 0.16 wt%, 0.18 wt%, 0.2 wt%, 0.22 wt%, 0.24 wt%, or 0.25 wt%. A large number of experiments show that when the content of the nano particles is in the range, the nano particles have a better reinforcing effect on the copper alloy, the reinforcing effect is poor when the content is too low, the mechanical property of the copper alloy is poor, and the performance of the copper alloy is not favorably exerted when the content is too high.
In a preferred embodiment, the method further comprises the steps of: pressing the nano particles into blocks, and then wrapping the blocks by using copper foil to obtain powder blocks.
Preferably, the method further comprises the steps of: fixing the powder block at one end of a connector which does not react with the copper liquid, placing one end of the connector connected with the powder block at the bottom of the copper liquid, and stirring for 2-4 times, wherein the melting point of the connector is higher than 2000 ℃. In the preferred embodiment, the powder block is fixed at one end of the connector and then placed at the bottom of the copper liquid to realize the addition of the nano particles, and compared with the method for directly putting the powder block on the surface of the copper liquid, the method can avoid the direct putting to ensure that the nano particles float on the surface of the copper liquid, reduce the waste of the nano particles and simultaneously realize the dispersion distribution of the nano particles in the copper liquid.
Preferably, the connector comprises a molybdenum rod.
In a preferred embodiment, the copper liquid is obtained by the following steps: and (3) putting the copper block into a resistance furnace for heating, introducing inert gas in the heating process, and obtaining copper liquid after the copper block is completely melted. The preparation process of the copper liquid in the preferred embodiment is simple, and the copper blocks can be completely melted under the protection of inert gas by only adopting a common resistance furnace, so that pure copper liquid is obtained.
Optionally, the electric resistance furnace comprises a high temperature tube electric resistance furnace.
Optionally, during the heating process, the refractory brick is used for sealing the furnace mouth of the resistance furnace, so as to further prevent oxygen from entering and prevent copper from being oxidized.
Preferably, the heating comprises: firstly, heating to 600-700 ℃ at the speed of 5-10 ℃/min, and preserving heat for 40-60 min; then, the temperature is raised to 1200-1300 ℃ at the rate of 5-10 ℃/min. The temperature rise rate of the two temperature rises is, for example, 5, 6, 7, 8, 9 or 10 ℃/min, the temperature after the first temperature rise is, for example, 600, 610, 620, 630, 640, 650, 660, 670, 680, 690 or 700 ℃, the holding time is, for example, 40, 42, 44, 46, 48, 50, 52, 54, 56, 58 or 60min, and the temperature after the second temperature rise is, for example, 1200, 1210, 1220, 1230, 1240, 1250, 1260, 1270, 1280, 1290 or 1300 ℃. The temperature is raised to 600-700 ℃ for the first time, and the heat is preserved for 40-60min, which is beneficial to completely removing the moisture in the raw materials as far as possible.
Preferably, the flow rate of the inert gas is 2 to 3m3H is used as the reference value. Typical but not limiting of the above mentioned flow rates are 2, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9 or 3m3/h。
Alternatively, the inert gas includes helium, neon, argon, krypton, xenon, or the like.
In a preferred embodiment, the powder lump is added into the copper liquid or stirred, and the flow rate of the inert gas is 3-4m3H is used as the reference value. The above flow rates are typically, but not limited to, 3, 3.1, 3.2, 3.3, 3.4, 3.5, 3.6, 3.7, 3.8, 3.9 or 4m3H is used as the reference value. The powder block is added into the copper liquid or in the stirring process, the flow of the inert gas is increased, and the copper liquid can be prevented from being oxidized due to the suction of air.
Preferably, the agitating comprises: stirring once every 3-5min, wherein forward stirring and reverse stirring are adopted for single stirring, and the forward stirring time and the reverse stirring time are respectively 10-15 s. The "forward and reverse stirring" means a stirring method in which forward stirring and reverse stirring are sequentially performed, and the forward stirring and the reverse stirring are performed in opposite directions, for example, when the forward stirring is clockwise stirring, the reverse stirring is counterclockwise stirring. The time interval between two successive single stirrings is, for example, 3, 3.5, 4, 4.5 or 5 min. The time for forward or reverse stirring is, for example, 10, 11, 12, 13, 14 or 15 s. Through the preferable stirring mode, the nano particles can be more uniformly distributed in the copper liquid.
In a preferred embodiment, in step (b), the incubation time is 5-10 min. The above incubation times are typically, but not limited to, 5, 6, 7, 8, 9 or 10 min.
Preferably, the temperature is reduced to 1100-1150 ℃ after heat preservation. The reduced temperature is typically, but not limited to, 1100, 1120, 1130, 1140 or 1150 ℃.
Preferably, the means of cooling comprises water cooling.
According to another aspect of the present invention, there is provided a copper alloy obtained by the above-described production method. The copper alloy obtained by the method has the advantages of high mechanical property and low cost.
According to another aspect of the present invention, there is provided a use of the above copper alloy for manufacturing an electronic component or a mechanical component. The copper alloy is applied to the preparation of electronic elements or mechanical elements, and the mechanical property of the electronic elements or the mechanical elements can be effectively improved.
According to another aspect of the present invention, there is provided an electronic component or a mechanical component comprising the above copper alloy. The electronic or mechanical component comprises the above copper alloy, and thus has at least advantages of good mechanical properties, simple production and low cost.
The present invention will be described in further detail with reference to examples and comparative examples.
Example 1
A preparation method of a copper alloy comprises the following steps:
(1) weighing 0.45g of MgO nano powder, pressing the MgO nano powder into blocks by using a hydraulic sample making machine, unloading and taking out the nano powder blocks after a pressing pressure pointer points to 7MPa, wrapping the nano powder blocks by using copper foil, and fixing the nano powder blocks at the end part of a molybdenum rod for later use;
(2) 900g of remelting pure copper block (namely the added MgO nano particles account for 0.05 percent of the mass of the copper liquid) is weighed, put into a magnesium oxide crucible and then placed inElectrifying and heating in a high-temperature tubular resistance furnace, heating to 600 ℃ at a heating rate of 10 ℃/min, preserving heat for 60min to remove moisture in raw materials and refractory materials as far as possible, then continuously heating to 1300 ℃ at the same rate for preserving heat, introducing argon as protective gas in the whole smelting process to prevent oxidation, and keeping the gas flow at 2m3/h。
(3) After the copper blocks in the crucible are completely melted into copper liquid, the introduction amount of argon is increased, and the gas flow is kept at 3.5m3And h, rapidly inserting one end of the molybdenum rod for fixing the nano powder block into the bottom of the crucible, and rapidly forward and backward stirring for 10s respectively at the stirring speed of 120 r/min. And then, the molybdenum rods are deeply inserted into the bottom of the crucible at intervals of 3min and are stirred for 3 times, and the furnace mouth is sealed by refractory bricks after the stirring is finished each time.
(4) And (3) after stirring is finished, keeping the temperature for 5min, then closing the tube furnace, clamping the crucible out by using crucible tongs when the temperature of the tube furnace is reduced to 1150 ℃, and cooling by water to obtain the dispersion strengthened copper alloy.
Examples 2 to 4
In examples 2-4, the weight of MgO nano powder was 0.911g, 1.382g, and 2.231g, respectively, and the weight of the re-melted pure copper ingot was 910g, 920g, and 890g, respectively (i.e., the weight percentages of the added MgO nano particles in the copper solution were 0.1%, 0.15%, and 0.25%, respectively), and the rest was the same as in example 1.
Comparative example 1
A preparation method of a copper alloy comprises the following steps:
(1) 850g of remelting pure copper block (namely, no nano particles are added) is weighed, placed in a magnesium oxide crucible and then placed in a high-temperature tubular resistance furnace, electrified for heating, heated to 600 ℃ at a heating rate of 10 ℃/min and kept warm for 60min to remove moisture in the copper block and refractory material as far as possible, then continuously heated to 1300 ℃ at the same rate for heat preservation, argon is introduced in the whole smelting process as protective gas to prevent copper liquid from oxidizing, and the gas flow is kept at 2m3/h。
(2) And after the copper blocks in the crucible are completely melted into copper liquid, closing the tube furnace, and clamping the crucible out by using crucible tongs for water cooling when the temperature of the tube furnace is reduced to 1150 ℃.
The copper alloys prepared in the above examples and comparative examples were respectively subjected to performance tests, tensile tests were carried out according to the method in GB/T228-2002, impact tests were carried out according to the method in GB/T229-.
TABLE 1
While particular embodiments of the present invention have been illustrated and described, it would be obvious that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
Claims (10)
1. The preparation method of the copper alloy is characterized by comprising the following steps of: (a) pressing the nano particles into blocks to obtain powder blocks; (b) adding the powder blocks into the copper liquid, stirring for 2-4 times at a stirring speed of 60-120r/min for 20-30s, and then sequentially carrying out heat preservation, cooling and cooling to obtain the copper alloy.
2. The method of claim 1, wherein the nanoparticles have a melting point above 2000 ℃;
preferably, the nanoparticles comprise inorganic nanoparticles;
preferably, the inorganic nanoparticles include MgO, Al2O3、TiN、ZrO2Or WC;
preferably, the nanoparticles have an average particle size of less than 20 nm.
3. The method of claim 1, wherein the content of the nanoparticles is 0.05 to 0.25 wt%.
4. The method of producing a copper alloy according to claim 1, further comprising the steps of: pressing the nano particles into blocks, and then wrapping the blocks with copper foil to obtain powder blocks;
preferably, the method further comprises the steps of: fixing the powder block at one end of a connector which does not react with the copper liquid, placing one end of the connector, which is connected with the powder block, at the bottom of the copper liquid, and stirring for 2-4 times, wherein the melting point of the connector is higher than 2000 ℃;
preferably, the connector comprises a molybdenum rod.
5. The method for preparing a copper alloy according to claim 1, wherein the molten copper is obtained by the steps of: putting the copper block into a resistance furnace for heating, introducing inert gas in the heating process, and obtaining copper liquid after the copper block is completely melted;
preferably, the heating comprises: firstly, heating to 600-700 ℃ at the speed of 5-10 ℃/min, and preserving heat for 40-60 min; then, heating to 1200-1300 ℃ at the speed of 5-10 ℃/min;
preferably, the flow rate of the inert gas is 2 to 3m3/h。
6. The method according to claim 1, wherein the inert gas is supplied at a flow rate of 3 to 4m during the addition of the powder to the molten copper or the stirring3/h；
Preferably, the agitating comprises: stirring once every 3-5min, wherein forward stirring and reverse stirring are adopted for single stirring, and the forward stirring time and the reverse stirring time are respectively 10-15 s.
7. The method for producing a copper alloy according to any one of claims 1 to 6, wherein in the step (b), the holding time is 5 to 10 min;
preferably, the temperature is reduced to 1100-1150 ℃ after heat preservation;
preferably, the means of cooling comprises water cooling.
8. A copper alloy obtained by the method for producing a copper alloy according to any one of claims 1 to 7.
9. Use of the copper alloy of claim 8 for the production of electronic or mechanical components.
10. An electronic or mechanical component comprising the copper alloy of claim 8.
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Application publication date: 20201106 |