CN111621664A - Method for preparing copper-iron alloy by spark plasma sintering - Google Patents
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- CN111621664A CN111621664A CN202010499734.4A CN202010499734A CN111621664A CN 111621664 A CN111621664 A CN 111621664A CN 202010499734 A CN202010499734 A CN 202010499734A CN 111621664 A CN111621664 A CN 111621664A
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- C22C9/00—Alloys based on copper
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- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0848—Melting process before atomisation
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0888—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid casting construction of the melt process, apparatus, intermediate reservoir, e.g. tundish, devices for temperature control
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0892—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid casting nozzle; controlling metal stream in or after the casting nozzle
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Abstract
The invention provides a method for preparing a copper-iron alloy by spark plasma sintering, which specifically comprises the following steps: preparing materials; smelting; atomizing to prepare powder: atomizing the melted alloy after the smelting treatment to prepare powder so as to obtain atomized alloy powder; screening; spark plasma sintering: pouring the screened atomized alloy powder into a graphite mold, placing the graphite mold in a plasma sintering furnace for vacuumizing and pressurizing, introducing 1500-2000A of pulse direct current when the pressure reaches 30-60 MPa, heating to 800-950 ℃ at the heating rate of 30-100 ℃/min, and keeping the temperature for 3-5 min; cooling, releasing pressure and discharging to obtain copper-iron alloy; the method has simple process and reasonable flow, prepares the copper-iron alloy material with excellent performance by vacuum atomization powder preparation and combining with the spark plasma sintering technology, and has the advantages of high density, less pore defects and high powder bonding strength.
Description
Technical Field
The invention relates to the technical field of powder metallurgy products, in particular to a method for preparing a copper-iron alloy by spark plasma sintering.
Background
In the powder metallurgy products, copper powder and iron powder are two kinds of powder with the largest dosage, the traditional powder metallurgy products are prepared by mixing the copper powder and the iron powder for use, the copper powder and the iron powder are not mixed uniformly, the melting temperature difference of the copper powder and the iron powder is large, the sintering temperature is difficult to determine, and the like, so that the quality and the performance of the finished products are seriously influenced; in addition, the production method of the copper-iron composite powder adopts a diffusion method, copper powder and iron powder are uniformly mixed according to a certain proportion, and then the mixture is heated to a certain temperature, so that the copper powder is coated on the surface of iron powder particles.
Compared with the common pressureless sintering and hot-pressing sintering, the spark plasma sintering process can obtain compact materials at lower sintering temperature. And the spark plasma sintering greatly shortens the sintering time, improves the production efficiency, reduces the production cost and improves the density of the metal ceramic composite material.
Aiming at the problems, the copper-iron alloy material with excellent performance is prepared by vacuum atomization powder preparation and a discharge plasma sintering technology.
Disclosure of Invention
Aiming at the problems, the invention provides a method for preparing a copper-iron alloy by spark plasma sintering, and the copper-iron alloy prepared by the method has the advantages of high density, few pore defects and high powder bonding strength.
The technical scheme of the invention is as follows: a method for preparing a copper-iron alloy by spark plasma sintering specifically comprises the following steps:
the method comprises the following steps: ingredients
According to the percentage content, the percentage content of Fe element in the raw material is 5-50%, and the balance is Cu element;
step two: melting
Smelting in a vacuum smelting mode;
step three: atomized powder
Atomizing the melted alloy after the smelting treatment to prepare powder so as to obtain atomized alloy powder;
step four: screening
Collecting atomized alloy powder and then screening and grading; wherein the granularity of the screened atomized alloy powder is 200-650 meshes;
step five: spark plasma sintering
Pouring the screened atomized alloy powder into a graphite mold, placing the graphite mold in a plasma sintering furnace for vacuumizing and pressurizing, introducing 1500-2000A of pulse direct current when the pressure reaches 30-60 MPa, heating to 800-950 ℃ at the heating rate of 30-100 ℃/min, and keeping the temperature for 3-5 min; and (5) cooling, releasing pressure and discharging to obtain the copper-iron alloy.
Further, in the first step, Fe element is added in the form of CuFe master alloy, and Cu element is added in the form of electrolytic copper plate and CuFe master alloy; the adoption of the raw materials with higher purity can effectively reduce impurities contained in the alloy at the later stage from the source.
Furthermore, the CuFe master alloy and the electrolytic copper plate need to be pretreated before smelting, and the pretreatment comprises the following specific steps: polishing the CuFe master alloy and the electrolytic copper plate respectively by a laser polishing machine; the polishing treatment can effectively remove the oxide film on the surface of the raw material, and can effectively improve the purity.
Further, the smelting in the second step comprises the following specific steps: uniformly mixing the raw materials prepared in the step one, putting the mixture into a carbon-free crucible, putting the crucible into a vacuum smelting furnace, and when the vacuum degree is pumped to a value that the pH value is less than or equal to 4Pa, heating to 850-1050 ℃ and preserving heat for 3-5 min; and then raising the temperature to 1350-1450 ℃, preserving the temperature for 5-8 min, and then slowly filling high-purity argon into the vacuum smelting furnace body for protection.
Further, the smelting in the second step comprises the following specific steps: uniformly mixing the raw materials prepared in the step one, putting the mixture into a carbon-free crucible, putting the crucible into a vacuum smelting furnace, when the vacuum degree is pumped to the pH value of less than or equal to 4Pa, heating to 800-950 ℃ at the heating rate of 5 ℃/s, preserving heat for 30-45 s, heating to 1250-1350 ℃ at the heating rate of 50 ℃/min, and preserving heat for 3-5 min; and then heating to 1400-1450 ℃ at a heating rate of 5 ℃/s, filling high-purity argon into the vacuum smelting furnace body while heating, stopping filling the high-purity argon when the pressure in the furnace rises to 0.08Mpa, and then continuously preserving the temperature for 2.5-3 min at 1400-1450 ℃.
Furthermore, the crucible is a corundum crucible; the carbon in the carbon-containing crucible seriously affects the smelting of the copper-iron alloy.
Further, the atomization powder preparation in the third step comprises the following specific steps: pouring molten alloy liquid into a drain ladle, spraying compressed gas with the pressure of 0.5-10 MPa to disperse the molten alloy liquid into fine liquid drops in the process that the molten alloy liquid flows out through a drain nozzle, and cooling and solidifying the fine liquid drops in the process of falling to prepare atomized alloy powder; wherein the flow rate of the compressed gas is controlled to be 4-20L/min; the compressed gas is high-purity argon gas, and the molten alloy can be dispersed into fine liquid drops by using pressure.
Further, the atomization powder preparation in the third step comprises the following specific steps: pouring molten alloy liquid into a drain ladle, spraying compressed gas with the pressure of 5-8 MPa in the process that the alloy liquid flows out through a drain nozzle to disperse the alloy liquid into fine liquid drops, and cooling and solidifying the fine liquid drops in the process of falling to prepare atomized alloy powder; wherein the flow rate of the compressed gas is controlled to be 12-15L/min.
Compared with the prior art, the invention has the beneficial effects that: the method has simple process and reasonable flow; the adopted raw materials with higher purity are prepared, so that impurities can be effectively reduced from the source; the crucible which does not contain carbon is adopted during smelting, so that the influence of carbon elements on the smelting of the copper-iron alloy can be effectively avoided; the copper-iron alloy material with excellent performance is prepared by vacuum atomization powder preparation and a discharge plasma sintering technology, and has the advantages of high density, few pore defects and high powder bonding strength.
Drawings
FIG. 1 is a metallographic structure diagram of a copper-iron alloy prepared in example 1 of the present invention after spark plasma sintering under a 100-fold mirror;
FIG. 2 is a metallographic structure diagram of a copper-iron alloy prepared in example 1 of the present invention after spark plasma sintering under a 50-fold mirror.
Detailed Description
Example 1: a method for preparing a copper-iron alloy by spark plasma sintering specifically comprises the following steps:
the method comprises the following steps: ingredients
According to the percentage content, the percentage content of Fe element in the raw material is 5%, and the balance is Cu element; wherein, Fe element is added in the form of CuFe master alloy, and Cu element is added in the form of electrolytic copper plate and CuFe master alloy;
step two: melting
Smelting in a vacuum smelting mode; the method specifically comprises the following steps: uniformly mixing the raw materials prepared in the step one, putting the mixture into a carbon-free crucible, putting the crucible into a vacuum smelting furnace, and when the vacuum degree is pumped to reach a pH value of less than or equal to 4Pa, heating to 850 ℃ and preserving heat for 3 min; then, the temperature is raised to 1350 ℃, the temperature is preserved for 5min, and then high-purity argon is slowly filled into the furnace body of the vacuum smelting furnace for protection; wherein the crucible is a corundum crucible;
step three: atomized powder
Atomizing the melted alloy after the smelting treatment to prepare powder so as to obtain atomized alloy powder; the method specifically comprises the following steps: pouring molten alloy liquid into a drain ladle, dispersing the molten alloy liquid into fine liquid drops through the injection of compressed gas with the pressure of 0.5MPa in the process of flowing out of a drain nozzle, and cooling and solidifying in the process of falling to prepare atomized alloy powder; wherein the flow rate of the compressed gas is controlled to be 4L/min; the compressed gas is specifically argon with the concentration of 99.99 percent;
step four: screening
Collecting atomized alloy powder and then screening and grading; wherein the granularity of the screened atomized alloy powder is 200-650 meshes;
step five: spark plasma sintering
Pouring the screened atomized alloy powder into a graphite mold, placing the graphite mold in a plasma sintering furnace, vacuumizing and pressurizing, introducing 1500A pulse direct current when the pressure reaches 30MPa, heating to 800 ℃ at the heating rate of 30 ℃/min, and keeping the temperature for 3 min; and (5) cooling, releasing pressure and discharging to obtain the copper-iron alloy.
The density of the copper-iron alloy prepared by the embodiment is more than 97%, and the iron phase is uniformly distributed and dispersed.
Example 2: a method for preparing a copper-iron alloy by spark plasma sintering specifically comprises the following steps:
the method comprises the following steps: ingredients
According to the percentage content, the percentage content of Fe element in the raw material is 15%, and the balance is Cu element; wherein, Fe element is added in the form of CuFe master alloy, and Cu element is added in the form of electrolytic copper plate and CuFe master alloy;
step two: melting
Smelting in a vacuum smelting mode; the method specifically comprises the following steps: uniformly mixing the raw materials prepared in the step one, putting the mixture into a carbon-free crucible, putting the crucible into a vacuum smelting furnace, and when the vacuum degree is pumped to reach a pH value of less than or equal to 4Pa, heating to 950 ℃ and preserving heat for 4 min; then raising the temperature to 1400 ℃, preserving the heat for 7min, and then slowly filling high-purity argon into the furnace body of the vacuum smelting furnace for protection; wherein the crucible is a corundum crucible;
step three: atomized powder
Atomizing the melted alloy after the smelting treatment to prepare powder so as to obtain atomized alloy powder; the method specifically comprises the following steps: pouring molten alloy liquid into a drain ladle, dispersing the molten alloy liquid into fine liquid drops through the injection of compressed gas with the pressure of 8MPa in the process of flowing out of a drain nozzle, and cooling and solidifying in the process of falling to prepare atomized alloy powder; wherein the flow rate of the compressed gas is controlled to be 15L/min;
step four: screening
Collecting atomized alloy powder and then screening and grading; wherein the granularity of the screened atomized alloy powder is 300-500 meshes;
step five: spark plasma sintering
Pouring the screened atomized alloy powder into a graphite mold, placing the graphite mold in a plasma sintering furnace, vacuumizing and pressurizing, introducing 1800A pulse direct current when the pressure reaches 50MPa, heating to 850 ℃ at the heating rate of 50 ℃/min, and keeping the temperature for 4 min; and (5) cooling, releasing pressure and discharging to obtain the copper-iron alloy.
The density of the copper-iron alloy prepared by the embodiment is more than 98%, and the iron phase is uniformly distributed and dispersed.
Example 3: a method for preparing a copper-iron alloy by spark plasma sintering specifically comprises the following steps:
the method comprises the following steps: ingredients
According to the percentage content, the percentage content of Fe element in the raw material is 50%, and the balance is Cu element; wherein, Fe element is added in the form of CuFe master alloy, and Cu element is added in the form of electrolytic copper plate and CuFe master alloy;
step two: melting
Smelting in a vacuum smelting mode; the method specifically comprises the following steps: uniformly mixing the raw materials prepared in the step one, putting the mixture into a carbon-free crucible, putting the crucible into a vacuum smelting furnace, and when the vacuum degree is pumped to reach a pH value of less than or equal to 4Pa, heating to 1050 ℃ and preserving heat for 5 min; then raising the temperature to 1450 ℃, preserving the temperature for 8min, and then slowly filling high-purity argon into the vacuum smelting furnace body for protection; wherein the crucible is a corundum crucible;
step three: atomized powder
Atomizing the melted alloy after the smelting treatment to prepare powder so as to obtain atomized alloy powder; the method specifically comprises the following steps: pouring molten alloy liquid into a drain ladle, dispersing the molten alloy liquid into fine liquid drops through the injection of compressed gas with the pressure of 10MPa in the process of flowing out of a drain nozzle, and cooling and solidifying in the process of falling to prepare atomized alloy powder; wherein the flow rate of the compressed gas is controlled to be 20L/min;
step four: screening
Collecting atomized alloy powder and then screening and grading; wherein the granularity of the screened atomized alloy powder is 350-450 meshes;
step five: spark plasma sintering
Pouring the screened atomized alloy powder into a graphite mold, placing the graphite mold in a plasma sintering furnace for vacuumizing and pressurizing, introducing 2000A pulse direct current when the pressure reaches 60MPa, heating to 950 ℃ at the heating rate of 100 ℃/min, and keeping the temperature for 5 min; and (5) cooling, releasing pressure and discharging to obtain the copper-iron alloy.
The density of the copper-iron alloy prepared by the embodiment is more than 97%, and the iron phase is uniformly distributed and dispersed.
Example 4: the difference from example 1 is: the CuFe master alloy and the electrolytic copper plate need to be pretreated before smelting, and the pretreatment comprises the following specific steps: and respectively polishing the CuFe master alloy and the electrolytic copper plate by a laser polishing machine.
The density of the copper-iron alloy prepared by the embodiment is more than 98%, and the iron phase is uniformly distributed and dispersed.
Example 5: the difference from example 1 is: the smelting in the second step comprises the following specific steps: uniformly mixing the raw materials prepared in the step one, putting the mixture into a carbon-free crucible, putting the crucible into a vacuum smelting furnace, when the vacuum degree is pumped to reach a pH value of less than or equal to 4Pa, heating to 800 ℃ at a heating rate of 5 ℃/s, preserving heat for 30s, heating to 1250 ℃ at a heating rate of 50 ℃/min, and preserving heat for 3 min; then heating to 1400 ℃ at the heating rate of 5 ℃/s, filling high-purity argon into the vacuum smelting furnace body while heating, stopping filling the high-purity argon when the pressure in the furnace rises to 0.08Mpa, and keeping the temperature for 2.5min at 1400 ℃.
The density of the copper-iron alloy prepared by the embodiment is more than 98%, and the iron phase is uniformly distributed and dispersed.
Example 6: the difference from example 1 is: the smelting in the second step comprises the following specific steps: uniformly mixing the raw materials prepared in the step one, putting the mixture into a carbon-free crucible, putting the crucible into a vacuum smelting furnace, when the vacuum degree is pumped to reach a pH value of less than or equal to 4Pa, heating to 900 ℃ at a heating rate of 5 ℃/s, preserving heat for 35s, heating to 1300 ℃ at a heating rate of 50 ℃/min, and preserving heat for 4 min; then heating to 1425 ℃ at a heating rate of 5 ℃/s, filling high-purity argon into the vacuum smelting furnace body while heating, stopping filling the high-purity argon when the pressure in the furnace rises to 0.08Mpa, and keeping the temperature for 3min at 1425 ℃.
The density of the copper-iron alloy prepared by the embodiment is more than 99%, and the iron phase is uniformly distributed and dispersed.
Example 7: the difference from example 1 is: the smelting in the second step comprises the following specific steps: uniformly mixing the raw materials prepared in the step one, putting the mixture into a carbon-free crucible, putting the crucible into a vacuum smelting furnace, when the vacuum degree is pumped to reach a pH value of less than or equal to 4Pa, heating to 950 ℃ at a heating rate of 5 ℃/s, preserving heat for 45s, heating to 1350 ℃ at a heating rate of 50 ℃/min, and preserving heat for 5 min; and then heating to 1450 ℃ at the heating rate of 5 ℃/s, filling high-purity argon into the vacuum smelting furnace body while heating, stopping filling the high-purity argon when the pressure in the furnace rises to 0.08Mpa, and keeping the temperature for 3min at 1450 ℃.
The density of the copper-iron alloy prepared by the embodiment is more than 98%, and the iron phase is uniformly distributed and dispersed.
Claims (8)
1. A method for preparing a copper-iron alloy by spark plasma sintering is characterized by specifically comprising the following steps:
the method comprises the following steps: ingredients
According to the percentage content, the percentage content of Fe element in the raw material is 5-50%, and the balance is Cu element;
step two: melting
Smelting in a vacuum smelting mode;
step three: atomized powder
Atomizing the melted alloy after the smelting treatment to prepare powder so as to obtain atomized alloy powder;
step four: screening
Collecting atomized alloy powder and then screening and grading; wherein the granularity of the screened atomized alloy powder is 200-650 meshes;
step five: spark plasma sintering
Pouring the screened atomized alloy powder into a graphite mold, placing the graphite mold in a plasma sintering furnace for vacuumizing and pressurizing, introducing 1500-2000A of pulse direct current when the pressure reaches 30-60 MPa, heating to 800-950 ℃ at the heating rate of 30-100 ℃/min, and keeping the temperature for 3-5 min; and (5) cooling, releasing pressure and discharging to obtain the copper-iron alloy.
2. The method for manufacturing a copper-iron alloy by spark plasma sintering as claimed in claim 1, wherein in said first step, the Fe element is added in the form of a CuFe master alloy, and the Cu element is added in the form of an electrolytic copper plate and in the form of a CuFe master alloy.
3. The method for preparing the copper-iron alloy by the spark plasma sintering as claimed in claim 2, wherein the CuFe master alloy and the electrolytic copper plate need to be pretreated before smelting, and the pretreatment comprises the following specific steps: and respectively polishing the CuFe master alloy and the electrolytic copper plate by a laser polishing machine.
4. The method for preparing the copper-iron alloy by the spark plasma sintering as claimed in claim 1, wherein the smelting in the second step comprises the following specific steps: uniformly mixing the raw materials prepared in the step one, putting the mixture into a carbon-free crucible, putting the crucible into a vacuum smelting furnace, and when the vacuum degree is pumped to a value that the pH value is less than or equal to 4Pa, heating to 850-1050 ℃ and preserving heat for 3-5 min; and then raising the temperature to 1350-1450 ℃, preserving the temperature for 5-8 min, and then slowly filling high-purity argon into the vacuum smelting furnace body for protection.
5. The method for preparing a copper-iron alloy by spark plasma sintering as claimed in claim 4, wherein said crucible is a corundum crucible.
6. The method for preparing the copper-iron alloy by the spark plasma sintering as claimed in claim 1, wherein the step three atomization pulverization comprises the following specific steps: pouring molten alloy liquid into a drain ladle, spraying compressed gas with the pressure of 0.5-10 MPa to disperse the molten alloy liquid into fine liquid drops in the process that the molten alloy liquid flows out through a drain nozzle, and cooling and solidifying the fine liquid drops in the process of falling to prepare atomized alloy powder; wherein the flow rate of the compressed gas is controlled to be 4-20L/min.
7. The method for preparing the copper-iron alloy by the spark plasma sintering as claimed in claim 1, wherein the step three atomization pulverization comprises the following specific steps: pouring molten alloy liquid into a drain ladle, spraying compressed gas with the pressure of 5-8 MPa in the process that the alloy liquid flows out through a drain nozzle to disperse the alloy liquid into fine liquid drops, and cooling and solidifying the fine liquid drops in the process of falling to prepare atomized alloy powder; wherein the flow rate of the compressed gas is controlled to be 12-15L/min.
8. The method for preparing the copper-iron alloy by the spark plasma sintering as claimed in claim 1, wherein the specific temperature of the sintering in the fifth step is 800-950 ℃.
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Cited By (4)
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| CN112387978A (en) * | 2020-10-21 | 2021-02-23 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of CuFe alloy powder for brake pad |
| CN113005325A (en) * | 2021-02-25 | 2021-06-22 | 宁波中超新材料有限公司 | Copper-iron alloy strip with microcrystalline structure and high iron content and preparation method thereof |
| CN113263161A (en) * | 2021-04-25 | 2021-08-17 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of soldering bit |
| CN115354180A (en) * | 2022-08-31 | 2022-11-18 | 西安理工大学 | Method for quickly preparing high-performance copper-tin alloy under action of thermal-force-electric multi-field coupling |
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| CN113005325B (en) * | 2021-02-25 | 2022-03-25 | 宁波中超新材料有限公司 | Copper-iron alloy strip with microcrystalline structure and high iron content and preparation method thereof |
| CN113263161A (en) * | 2021-04-25 | 2021-08-17 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of soldering bit |
| CN113263161B (en) * | 2021-04-25 | 2022-08-26 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of soldering bit |
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