CN111676386A - Method for improving performance of CuCrZr material - Google Patents
Method for improving performance of CuCrZr material Download PDFInfo
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- CN111676386A CN111676386A CN202010442901.1A CN202010442901A CN111676386A CN 111676386 A CN111676386 A CN 111676386A CN 202010442901 A CN202010442901 A CN 202010442901A CN 111676386 A CN111676386 A CN 111676386A
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- 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
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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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- B33—ADDITIVE MANUFACTURING TECHNOLOGY
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- B33—ADDITIVE MANUFACTURING TECHNOLOGY
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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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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Abstract
The invention discloses a method for improving the performance of a CuCrZr material, which mainly comprises the following steps: s1, preparing a copper alloy bar: according to the mass fraction, the CuCrZr alloy spherical powder comprises the following main chemical components in percentage by mass: 0.7-1.2% of Cr, 0.065-0.25% of Zr and the balance of Cu, and the rod blank with the relative density of more than or equal to 90% and no obvious loose and shrinkage cavity defects on the surface is obtained by smelting, casting and forging according to the proportioning mode; processing a copper alloy bar; secondarily refining the CuCrZr bar stock; preparing solid solution powder; starting 3D printing equipment to print a sample block with the diameter of 20mm and the height of 20 mm; hot isostatic pressing and annealing treatment. The CuCrZr alloy provided by the invention changes the dispersion distribution method of the second phase through the additive manufacturing process, can obviously improve the conditions of material component segregation and the like, meets the use requirements of key parts, and is suitable for wide popularization.
Description
Technical Field
The invention relates to the technical field of metal powder metallurgy, in particular to a method for improving the performance of a CuCrZr material.
Background
The 3D printing application research is most exciting and is the development of new materials in the metal field, and the 3D printing of the metal is more and more widely applied to the 3D printing field of materials such as stainless steel, copper alloy and aluminum alloy from the 3D printing application of high-end materials such as titanium alloy and nickel-based superalloy, so that the application prospect of 3D printing parts is expanded.
In practical application, the copper alloy 3D printing piece is gradually applied to key parts. When the Aero jet Rocketdyne company researches and manufactures a new generation RL10 engine, 3D printing copper alloy thrust chamber parts are used for replacing former RL10C-1 thrust chamber parts, which brings possibility for manufacturing the new generation engine. The alternative thrust chamber component is made by conventional processes and is welded from multiple stainless steel parts, while the 3D printed copper alloy thrust chamber component is constructed from two copper alloy parts. The lander and co-operating partner 3T, EOS of the civil aviation and aerospace enterprise also developed 3D printed copper alloy rocket engine components.
The application of 3D printing technique can reduce engine part quantity, shortens development time to be easier to make the integrated part of complex function, at present, the 3D of copper alloy prints key spare part and uses more and more, so to the promotion of copper alloy material performance, the speed and the effect that just can better promotion 3D printed.
Disclosure of Invention
In order to solve the technical problem, the invention provides a method for improving the performance of a CuCrZr material.
The technical points of the invention are as follows:
a method for improving the performance of a CuCrZr material mainly comprises the following steps:
s1, preparing a copper alloy bar: according to the mass fraction, the CuCrZr alloy spherical powder comprises the following main chemical components in percentage by mass: 0.7-1.2% of Cr, 0.065-0.25% of Zr and the balance of Cu, and the mixture ratio is used for smelting, casting and forging to obtain a bar blank with the relative density of more than or equal to 90% and no obvious loose or shrinkage cavity defects on the surface, and the prepared bar can be fully alloyed by the mixture ratio, so that the service performance is met;
s2, processing the copper alloy bar: processing the copper alloy bar material to meet the requirement of the feeding size of the vacuum induction melting furnace according to a sawing machine and a lathe, and processing the surface of the cut copper alloy bar material to ensure that the surface roughness is less than or equal to 1.6 mu m;
s3, secondary refining of the CuCrZr bar stock: placing CuCrZr bars into a crucible in a furnace to be melted, stirring the melted CuCrZr bars through electromagnetic induction, pre-vacuumizing the whole equipment, then filling inert protective gas, placing the CuCrZr bars into a graphite crucible coated with a special protective layer for preventing the solution from reacting with graphite, starting a vacuum pumping system until the vacuum degree reaches 4 x 10-2When Pa is reached, intermediate frequency heating is started, the raw material is remelted, when the temperature in the graphite crucible reaches 1350 ℃ and the pressure is-0.02 Mpa, the vacuum pumping system is closed, high-purity argon is filled, the raw material is stirred by electromagnetic induction, heating is continued until the raw material is in a completely molten state, secondary refining is carried out to further remove impurities and reduce gas elements, simultaneously the alloy bar stock is changed into a liquid state for subsequent atomization, and the vacuum degree reaches 4 x 10-2When Pa is needed, intermediate frequency heating is started again to prevent the alloy solution from being oxidized, so that the content of alloy components is ensured on one hand, and impurities are prevented from being introduced on the other hand;
s4, preparing solid solution powder: pouring the smelted raw material solution into a tundish, preserving heat, making up Zr content loss in the remelting process by pre-placing Zr wires in the heat preservation process, starting electromagnetic induction stirring, starting an inert gas heating device after half an hour, heating atomized gas, detecting by an infrared temperature measuring instrument, pouring a crucible into the tundish above an atomizing nozzle when the superheat degree of alloy melt reaches 150 ℃, preserving heat, standing for 15 minutes, starting the inert gas heat preservation device at the temperature of 1350 ℃, heating the atomized gas to 300 ℃, cooling and screening out 10-65 mu m solid solution powder after atomization, placing printing equipment, and drawing into 1 x 10-2Vacuum standby is carried out, the second phase can be refined by making up the Zr content in the remelting process, so that the second phase is dispersed and distributed, and the strength and the conductivity of the copper alloy are increased;
s5, starting the 3D printing device: starting the equipment, starting to print sample blocks for molding, and printing sample blocks with the diameter of 20mm and the height of 20 mm;
s6, hot isostatic pressing and annealing treatment: after printing, hot isostatic pressing treatment is firstly carried out, the compactness of the copper alloy product is increased, then annealing treatment is carried out, and hot isostatic pressing parameters are as follows: the temperature is 850 ℃, the pressure is 120MPa, the heat preservation and pressure maintaining time is 4h, and the temperature rising rate is 15 ℃/min; the annealing temperature is 450 ℃ and the time is 6 h.
Further, pure copper, CuCr intermediate alloy and CuZr intermediate alloy are additionally added when the metals are smelted according to the base metal component ratio in S1, when the alloys are smelted, the argon gas is introduced for 10min, the solution standing time is 20-30min, the casting speed is 30-40kg/min during casting, and the scum on the surface needs to be cleaned in time during casting, so that the low content of impurities and gas elements is ensured.
Further, the diameter of the Zr wire pre-placed in S4 is 1.5mm, and the Zr wire can refine the second phase, so that the second phase is dispersed and distributed, and the strength and the electric conductivity of the copper alloy are increased.
Further, in S5, the print attributes of the 3D printer are set, and the print data specifically include: printing laser power: 300W, laser spot diameter: 0.12mm, laser processing scanning speed: 1500mm/s, single layer height: 0.02mm, and the control voltage of the argon circulating air speed in the forming chamber is set as follows: 2.5V, and the performance hardness of the copper alloy sample block printed by the parameter can reach 178 HB.
Furthermore, the special protective layer coated in the graphite crucible is Sio2a/Mo plasma composite coating, the SiO2the/Mo plasma composite coating can prevent graphite from directly or indirectly undergoing carbonization reaction with other elements at high temperature to influence the performance of parts, and SiO2The thermal shock resistance of the/Mo plasma composite coating is stronger, and part of Mo element can also be used as Sio2Elemental catalyst, increasing Sio2The heat and pressure resistance of the material.
Further, the Sio2The manufacturing method of the/Mo plasma composite coating comprises the following steps:
s 1: the weight percentages are as follows: 65% of Sio2And the rest Mo element is used for preparing mixed powder, gaps on the surface of the graphite crucible are finely cleaned, and carbon and oxide residues on the surface of the graphite crucible are removed in a vacuum pressurization mode, so that the phenomenon that the crucible is carbonized due to the existence of pores in the middle of the prepared coating is avoided.
s 2: make Sio2the/Mo composite powder is uniformly coated on the surface of the graphite crucible, and Sio is also filled in the gap on the surface of the graphite crucible2a/Mo composite powder;
s3: will be coated with Sio2Placing a graphite crucible of the/Mo composite powder into a vacuum smelting furnace, and smelting under pressure to ensure that the SiO2Crystallizing the/Mo composite powder.
Further, the Sio2the/Mo plasma composite coating adopts a structure with thick middle and thin two sides, and adopts a fish scale-shaped structure which is overlapped layer by layer from the middle to the periphery, when the graphite crucible is subjected to vacuum melting, carbon elements in the graphite crucible are firstly gathered at the middle part, and the periphery is less, so that the Sio can be further improved by adopting the structure2the/Mo plasma composite coating plays the most role, and the service life of the graphite crucible is prolonged.
Compared with the prior art, the invention has the beneficial effects that:
firstly, according to the proportion of the alloy components in the invention, the prepared copper alloy can be fully alloyed so as to meet the service performance; in a specific adding mode: the addition of pure copper, CuCr intermediate alloy and CuZr intermediate alloy greatly improves the performance parameters of the prepared alloy; specific argon adding time, solution standing time and electromagnetic stirring strength during smelting and timely treatment of surface scum during casting; ensures low contents of impurities and gas elements, thereby enabling the refined alloy to be more pure.
Secondly, in the step S3, the invention adopts the medium-frequency induction furnace which has the advantages of high heat efficiency, short smelting time, less burning loss of alloy elements, wide smelting material, less environmental pollution, capability of accurately controlling the temperature and components of molten metal and the like, can greatly improve the alloying performance under the condition of saving the alloy cost, adds the pre-prepared Zr wire in the tundish crucible to participate in the process of making up for remelting, can refine the second phase, enables the second phase to be dispersed and distributed, and increases the strength and the conductivity of the copper alloy.
Thirdly, compared with the prior art, the tundish crucible has higher temperature, and can also be heated and electromagnetically stirred; the tundish crucible can be added with intermediate alloy in the standing process; the guide pipe is short; the atomized inert gas may be heated.
Drawings
FIG. 1 is a solid solution CuCrZr spherical powder of the present invention;
FIG. 2 is a second phase of the present invention dispersed on a substrate.
Detailed Description
The first embodiment is as follows:
a method for improving the performance of a CuCrZr material mainly comprises the following steps:
s1, preparing a copper alloy bar: according to the mass fraction, the CuCrZr alloy spherical powder comprises the following main chemical components in percentage by mass: 1.0 percent of Cr, 0.08 percent of Zr and the balance of Cu are smelted, cast and forged according to the proportion mode to obtain a bar blank with the relative density of more than or equal to 90 percent and no obvious loose and shrinkage cavity defects on the surface;
s2, processing the copper alloy bar: processing the copper alloy bar material to meet the requirement of the feeding size of the vacuum induction melting furnace according to a sawing machine and a lathe, and processing the surface of the cut copper alloy bar material to ensure that the surface roughness is less than or equal to 1.6 mu m;
s3, secondary refining of the CuCrZr bar stock: placing CuCrZr bars into a crucible in a furnace to be melted, stirring the melted CuCrZr bars through electromagnetic induction, pre-vacuumizing the whole equipment, then filling inert protective gas, placing the CuCrZr bars into a graphite crucible coated with a ceramic layer for preventing the solution from reacting with graphite, starting a vacuum pumping system until the vacuum degree reaches 4 x 10-2When Pa, starting intermediate frequency heating, remelting the raw materials, when the temperature in the graphite crucible reaches 1350 ℃ and the pressure is-0.02 Mpa, closing a vacuum pumping system, filling high-purity argon, stirring by electromagnetic induction, and continuing heating until the raw materials are in a completely molten state;
s4, preparing solid solution powder: pouring the melted raw material solution into a tundish, preserving heat, making up Zr content loss in the remelting process by pre-placing Zr wires in the heat preservation process, starting electromagnetic induction stirring, starting an inert gas heating device after half an hour, heating atomized gas, detecting by an infrared temperature measuring instrument, pouring a crucible into the tundish above an atomizing nozzle when the superheat degree of the alloy melt reaches 150 ℃, preserving heat, standing for 15 minutes, starting the inert gas heat preservation device at the heat preservation temperature of 1350 ℃, heating the atomized gas to 300 ℃, finally cooling and screening out solid solution powder of 45 mu m after atomization, placing printing equipment, and drawing into 1 x 10-2Vacuum for standby;
s5, starting the 3D printing device: starting the equipment, starting to print sample blocks for molding, and printing sample blocks with the diameter of 20mm and the height of 20 mm;
s6, hot isostatic pressing and annealing treatment: after printing, hot isostatic pressing treatment is firstly carried out, the compactness of the copper alloy product is increased, then annealing treatment is carried out, and hot isostatic pressing parameters are as follows: the temperature is 850 ℃, the pressure is 120MPa, the heat preservation and pressure maintaining time is 4h, and the temperature rising rate is 15 ℃/min; the annealing temperature is 450 ℃ and the time is 6 h.
In S1, when metal is smelted according to the base metal component ratio, pure copper, CuCr intermediate alloy and CuZr intermediate alloy with the same ratio are additionally added, when the alloy is smelted, argon is introduced for 10min, the solution standing time is 30min, the casting speed is 35kg/min during casting, and scum on the surface needs to be cleaned in time during casting.
The diameter of the Zr wire previously laid in S4 was 1.5 mm.
In S5, the print attributes of the 3D printer are set, and the print data specifically includes: printing laser power: 300W, laser spot diameter: 0.12mm, laser processing scanning speed: 1500mm/s, single layer height: 0.02mm, and the control voltage of the argon circulating air speed in the forming chamber is set as follows: 2.5V.
The special protective layer coated in the graphite crucible is Sio2a/Mo plasma composite coating, the SiO2the/Mo plasma composite coating can prevent the graphite from directly or indirectly undergoing carbonization reaction with other elements at high temperature to influence the performance of the part.
The special protective layer coated in the graphite crucible is Sio2a/Mo plasma composite coating, the SiO2the/Mo plasma composite coating can prevent the graphite from directly or indirectly undergoing carbonization reaction with other elements at high temperature to influence the performance of the part.
The Sio2The manufacturing method of the/Mo plasma composite coating comprises the following steps:
s 1: the weight percentages are as follows: 65% of Sio2And the residual Mo element is prepared into plasma mixed powder in an atomizing mode, the gap on the surface of the graphite crucible is finely cleaned, the carbon and oxide residue on the surface of the graphite crucible is removed in a vacuum pressurizing mode, and the phenomenon that pores exist in the middle of the prepared coating to cause crucible carbonization is prevented.
s 2: make Sio2the/Mo composite powder is uniformly coated on the surface of the graphite crucible, and Sio is also filled in the gap on the surface of the graphite crucible2a/Mo composite powder;
s 3: will be coated with Sio2Placing graphite crucible of/Mo composite powder in vacuum melting furnace, pressure smelting, raising temperature to 1800 deg.C in the form of 150 deg.C/min, and smelting to make SiO2Crystallizing the/Mo composite powder.
The Sio2The thick both sides of the thick structure that is thinner in centre is adopted to the Mo plasma composite coating, and from the middle part to adopting the fish scale column structure of overlapping layer upon layer all around, middle part thickness is 15um, and the minimum thickness all around is 10um, and every fish scale column step height is 0.2 um.
After the performance of the CuCrZr material is improved through the experimental steps, the hardness of the CuCrZr material can reach 178HB, and the electric conductivity is 60% IACS.
Example two:
the difference from the first embodiment is that this embodiment prepares a copper alloy bar in S1: according to the mass fraction, the CuCrZr alloy spherical powder comprises the following main chemical components in percentage by mass: 0.7% of Cr, 0.07% of Zr and the balance of Cu, and the balance of the copper alloy bar.
After the performance of the CuCrZr material is improved through the experimental steps, the hardness of the CuCrZr material can reach 139HB, and the electric conductivity is 72.4% IACS.
Example three:
the difference from the second example is that this example prepares a copper alloy bar in S1: according to the mass fraction, the CuCrZr alloy spherical powder comprises the following main chemical components in percentage by mass: 1.2 percent of Cr, 0.2 percent of Zr and the balance of Cu, and smelting the copper alloy bar.
After the performance of the CuCrZr material is improved through the experimental steps, the hardness of the CuCrZr material can reach 115HB, and the electric conductivity is 78.3% IACS.
Example four:
the difference from the third example is that this example prepares a copper alloy bar in S1: according to the mass fraction, the CuCrZr alloy spherical powder comprises the following main chemical components in percentage by mass: 0.9% of Cr, 0.15% of Zr and the balance of Cu, and smelting the copper alloy bar.
After the performance of the CuCrZr material is improved through the experimental steps, the hardness of the CuCrZr material can reach 142HB, and the electric conductivity is 76.9% IACS.
The experimental data of the above examples show that, under the same heat treatment, when the mass fraction ratio is: 1.0% of Cr, 0.08% of Zr and the balance of Cu, wherein the hardness of the CuCrZr material is the highest and is 178HB, and the mass fraction ratio is as follows: 1.2 percent of Cr, 0.2 percent of Zr and the balance of Cu, the highest conductivity is 78.3 percent of IACS, and the mass fraction ratio is as follows: 0.9% of Cr, 0.15% of Zr, and the balance of Cu, hardness: 142HB, conductivity: 76.9% IACS, the performance is more balanced.
Claims (6)
1. A method for improving the performance of a CuCrZr material is characterized by mainly comprising the following steps:
s1, preparing a copper alloy bar: according to the mass fraction: 0.7-1.2% of Cr, 0.065-0.25% of Zr and the balance of Cu, and the CuCrZr bar blank with the relative density of more than or equal to 90% is obtained by smelting, casting and forging according to the proportion;
s2, processing the copper alloy bar: processing the copper alloy bar material into a copper alloy bar material meeting the charging size requirement of the vacuum induction melting furnace according to a sawing machine and a lathe, and processing the surface of the cut copper alloy bar material to ensure that the surface roughness is less than or equal to 1.6 mu m;
s3, secondary refining of the CuCrZr bar stock: placing CuCrZr bars into a crucible in a furnace to be melted, stirring the melted CuCrZr bars through electromagnetic induction, pre-vacuumizing the whole equipment, then filling inert protective gas, placing the CuCrZr bars into a graphite crucible coated with a special protective layer for preventing the solution from reacting with graphite, starting a vacuum pumping system until the vacuum degree reaches 4 x 10-2When Pa, starting intermediate frequency heating, remelting the raw material, when the temperature in the graphite crucible reaches 1350 ℃ and the pressure is-0.02 Mpa, closing a vacuum pumping system, filling high-purity argon, stirring by electromagnetic induction, and continuing heating until the raw material is in a completely molten state;
s4, preparing solid solution powder: pouring the melted raw material solution into a tundish, preserving heat, making up the Zr content loss in the remelting process by placing Zr wires in advance in the heat preservation process, starting electromagnetic induction stirring, and starting inert gas after half an hourHeating the atomized gas by a body heating device, detecting by an infrared temperature measuring instrument, pouring a crucible into a tundish above an atomizing nozzle when the superheat degree of the alloy melt reaches 150 ℃, keeping the temperature for standing for 15 minutes, starting an inert gas heat preservation device at the heat preservation temperature of 1350 ℃, heating the atomized gas to 300 ℃, cooling and screening out 10-65 mu m of solid solution powder after atomization, placing printing equipment, and drawing into 1 x 10-2Vacuum for standby;
s5, starting the 3D printing device: starting the equipment, starting to print sample blocks for molding, and printing sample blocks with the diameter of 20mm and the height of 20 mm;
s6, hot isostatic pressing and annealing treatment: after printing, hot isostatic pressing treatment is firstly carried out to increase the compactness of the copper alloy product, then annealing treatment is carried out, and hot isostatic pressing parameters are as follows: the temperature is 850 ℃, the pressure is 120MPa, the heat preservation and pressure maintaining time is 4h, and the temperature rising rate is 15 ℃/min; the annealing temperature is 450 ℃ and the time is 6 h.
2. The method of claim 1, wherein pure copper, CuCr intermediate alloy and CuZr intermediate alloy are additionally added in S1 when the metal is smelted according to the base material composition ratio, argon gas is introduced for 10min when the alloy is smelted, the solution stationary time is 20-30min, the casting speed is 30-40kg/min when casting, and the scum on the surface needs to be cleaned in time when casting.
3. The method for improving the performance of the CuCrZr material, according to claim 1, wherein the diameter of the Zr wire pre-arranged in S4 is 1.5 mm.
4. The method for improving the performance of the CuCrZr material according to claim 1, wherein in S5, the printing attributes of the 3D printer are set, and the printing data specifically comprise: printing laser power: 300W, laser spot diameter: 0.12mm, laser processing scanning speed: 1500mm/s, single layer height: 0.02mm, and the control voltage of the argon circulating air speed in the forming chamber is set as follows: 2.5V.
5. The method for improving the performance of the CuCrZr material, according to claim 1, wherein the special protective layer coated in the graphite crucible is Sio2the/Mo plasma composite coating.
6. The method for improving the performance of the CuCrZr material according to claim 5, wherein the method for manufacturing the professional protective layer comprises the following steps:
s 1: the weight percentages are as follows: 65% of Sio2Preparing mixed powder with the balance of Mo element, finely cleaning gaps on the surface of the graphite crucible, and removing carbon and oxide residues on the surface of the graphite crucible by using a vacuum pressurization mode;
s 2: make Sio2the/Mo composite powder is uniformly coated on the surface of the graphite crucible, and Sio is also filled in the gap on the surface of the graphite crucible2a/Mo composite powder;
s3: will be coated with Sio2Placing a graphite crucible of the/Mo composite powder into a vacuum smelting furnace, and smelting under pressure to ensure that the SiO2Crystallizing the/Mo composite powder.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114318049A (en) * | 2021-12-16 | 2022-04-12 | 镇江市镇特合金材料有限公司 | Long-life copper alloy for welding head box body and preparation method thereof |
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| WO2024090446A1 (en) * | 2022-10-24 | 2024-05-02 | 三菱マテリアル株式会社 | Copper alloy powder for metal additive manufacturing (am) and method for producing laminate molded article |
| WO2024090447A1 (en) * | 2022-10-24 | 2024-05-02 | 三菱マテリアル株式会社 | Method for manufacturing copper alloy powder for metal am |
| WO2024090448A1 (en) * | 2022-10-24 | 2024-05-02 | 三菱マテリアル株式会社 | Copper alloy powder for metal additive manufacturing (am) and method for producing laminate molded article |
| JP7513223B1 (en) | 2022-10-24 | 2024-07-09 | 三菱マテリアル株式会社 | Manufacturing method of copper alloy powder for metal AM |
| JP7513224B1 (en) | 2022-10-24 | 2024-07-09 | 三菱マテリアル株式会社 | Copper alloy powder for metal AM and method for manufacturing laminated objects |
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