CN116516268A - Alloy copper wire annealing process - Google Patents

Alloy copper wire annealing process Download PDF

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Publication number
CN116516268A
CN116516268A CN202310394921.XA CN202310394921A CN116516268A CN 116516268 A CN116516268 A CN 116516268A CN 202310394921 A CN202310394921 A CN 202310394921A CN 116516268 A CN116516268 A CN 116516268A
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Prior art keywords
copper wire
alloy copper
cooling
heat preservation
annealing process
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CN202310394921.XA
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Chinese (zh)
Inventor
朱雪江
张雪荣
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Changshu Puhua Electrical Material Co ltd
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Changshu Puhua Electrical Material Co ltd
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Priority to CN202310394921.XA priority Critical patent/CN116516268A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/02Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/52Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
    • C21D9/525Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length for wire, for rods
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C9/00Alloys based on copper
    • C22C9/04Alloys based on copper with zinc as the next major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/002Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/08Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Metal Extraction Processes (AREA)

Abstract

The invention discloses an alloy copper wire annealing process, and relates to the technical field of metal material processing. Heating and preserving heat for the first time under vacuum condition, preserving heat for the second time under the condition of introducing inert mixed gas of methane, hydrogen and argon, recovering the pressure to normal pressure, cooling for the first time, and then carrying out impact deformation treatment on the surface of the alloy copper wire by adopting a vacuum environment surface nanocrystallization tester under liquid nitrogen for cooling for the second time to obtain the annealed alloy copper wire; the alloy copper wire obtained by adopting the processes of vacuum heating, primary heat preservation, secondary heat preservation, primary cooling and secondary cooling has stronger yield strength, ductility and conductivity.

Description

Alloy copper wire annealing process
Technical Field
The invention relates to the technical field of metal material processing, in particular to an alloy copper wire annealing process.
Background
Annealing is a metal heat treatment process that involves slowly heating the metal to a temperature, holding for a sufficient period of time, and then cooling at a suitable rate. The aim is to reduce the hardness and improve the machinability; residual stress is eliminated, the size is stabilized, and the deformation and crack tendency is reduced; fine grains, adjust the structure and eliminate the defect of the structure. To be precise, annealing is a heat treatment process for materials, including metallic materials and nonmetallic materials. The annealing purpose of the new material is different from that of the traditional metal annealing, wherein the annealing of copper wires and other linear metals has certain requirements on both the steps of complete cooling and heating.
However, the existing copper wire annealing process has a number of technical drawbacks: for example, when brass wires are heated under vacuum in production, a 'vinasse' phenomenon sometimes occurs, namely, white edges appear on the surfaces or the surfaces of the brass wires become red copper after the brass wires are annealed under vacuum, so that the plasticity, tensile strength and electric conductivity of Huang Xisi are greatly reduced, and the brass wires become waste products which can only be remelted; therefore, the annealing process of the zinc-containing alloy copper wire such as brass needs to be improved so as to ensure the mechanical property and the electric conductivity of the alloy copper wire.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides an alloy copper wire annealing process, which comprises the following process steps: vacuum heating, primary heat preservation, secondary heat preservation, primary cooling and secondary cooling.
Further, the method comprises the following process steps:
(1) Vacuum heating: placing the alloy copper wire into a tube furnace for vacuumizing, and then heating to 950-1050 ℃ at the speed of 90-110 ℃/h;
(2) Primary heat preservation: maintaining the vacuum state of the tube furnace, and preserving the temperature for 5.5-6.5 hours at 950-1050 ℃;
(3) And (3) secondary heat preservation: then introducing inert mixed gas, and preserving the temperature for 1-2 hours at 950-1050 ℃;
(4) Primary cooling: restoring the pressure to normal pressure, and then cooling to normal temperature at 70-90 ℃/h;
(5) And (5) secondary cooling: and (3) carrying out impact deformation treatment on the surface of the alloy copper wire for 4-6 min by adopting a vacuum environment surface nanocrystallization tester under liquid nitrogen.
Further, the zinc content of the alloy copper wire is 10-30%.
Further, the inert mixed gas comprises methane, hydrogen and argon; the gas flow ratio of methane to hydrogen to argon is 1:4:400-2:6:500.
Further, the test frequency of the surface nanocrystallization testing machine is 20-50 Hz, the number of steel balls is 100-200, and the diameter of the steel balls is 6-8 mm.
Further, the vacuum degree of the vacuuming is 1 mbar.
Compared with the prior art, the invention has the following beneficial effects:
the annealing process of the alloy copper wire sequentially comprises the following process steps: vacuum heating, primary heat preservation, secondary heat preservation, primary cooling and secondary cooling; wherein the zinc content of the alloy copper wire is 10-30%; argon, hydrogen and methane mixed gas are introduced in the secondary heat preservation; the secondary cooling is deformation treatment under the liquid nitrogen environment.
After vacuum heating, zinc atoms on the surface of the alloy copper wire are evaporated to generate holes, and during one heat preservation period, the internal zinc atoms are diffused to the surface to form a large number of holes and hole channels on the surface and the inside of the alloy copper wire; during secondary heat preservation, the mixed gas rapidly enters and disperses into the alloy copper wire through the cavity channel to form a large amount of graphene, so that the mechanical property and the conductivity of the alloy copper wire are enhanced; the secondary cooling is deformed in the liquid nitrogen environment, and the gradient change from the fine crystal area to the coarse crystal area is formed in the alloy copper wire from outside to inside, so that the strength and the ductility of the alloy copper wire are enhanced.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In order to more clearly illustrate the method provided by the invention, the following examples are used for describing the detailed description, and the test method of each index of the alloy copper wire prepared in the following examples is as follows:
mechanical properties: the alloy copper wires prepared in the same quality examples and comparative examples were taken and tested for tensile strength and elongation according to GB/T228.
Conductivity: the alloy copper wires prepared in the same quality examples and comparative examples were used to test the conductivity of the alloy copper wires according to GB/T32791.
Example 1
An annealing process of an alloy copper wire comprises the following process steps: vacuum heating, primary heat preservation, secondary heat preservation, primary cooling and secondary cooling.
Further, the method comprises the following process steps:
(1) Vacuum heating: placing the alloy copper wire into a tube furnace, vacuumizing, and then heating to 950 ℃ at a speed of 90 ℃/h;
(2) Primary heat preservation: maintaining the vacuum state of the tube furnace, and preserving the temperature for 5.5 hours at 950 ℃;
(3) And (3) secondary heat preservation: then introducing inert mixed gas, and preserving heat for 1h at 950 ℃;
(4) Primary cooling: restoring the pressure to normal pressure, and then cooling to normal temperature at 70 ℃/h;
(5) And (5) secondary cooling: and (3) carrying out impact deformation treatment on the surface of the alloy copper wire for 4min by adopting a vacuum environment surface nanocrystallization tester under liquid nitrogen.
Further, the zinc content of the alloy copper wire is 10%.
Further, the inert mixed gas comprises methane, hydrogen and argon; the gas flow ratio of methane, hydrogen and argon is 1:4:400.
Further, the test frequency of the surface nanocrystallization testing machine is 20Hz, the number of steel balls is 100, and the diameter of the steel balls is 6mm.
Further, the vacuum degree of the vacuuming is 1 mbar.
Example 2
An annealing process of an alloy copper wire comprises the following process steps: vacuum heating, primary heat preservation, secondary heat preservation, primary cooling and secondary cooling.
Further, the method comprises the following process steps:
(1) Vacuum heating: placing the alloy copper wire into a tube furnace, vacuumizing, and then heating to 1000 ℃ at a speed of 100 ℃/h;
(2) Primary heat preservation: maintaining the vacuum state of the tube furnace, and preserving the heat for 6 hours at 1000 ℃;
(3) And (3) secondary heat preservation: then inert mixed gas is introduced, and the temperature is kept at 1000 ℃ for 1.5 hours;
(4) Primary cooling: restoring the pressure to normal pressure, and then cooling to normal temperature at 80 ℃/h;
(5) And (5) secondary cooling: and (3) carrying out impact deformation treatment on the surface of the alloy copper wire for 5min by adopting a vacuum environment surface nanocrystallization tester under liquid nitrogen.
Further, the zinc content of the alloy copper wire is 20%.
Further, the inert mixed gas comprises methane, hydrogen and argon; the gas flow ratio of methane, hydrogen and argon is 1.5:5:450.
Further, the test frequency of the surface nanocrystallization testing machine is 35Hz, the number of steel balls is 150, and the diameter of the steel balls is 7mm.
Further, the vacuum degree of the vacuuming is 1 mbar.
Example 3
An annealing process of an alloy copper wire comprises the following process steps: vacuum heating, primary heat preservation, secondary heat preservation, primary cooling and secondary cooling.
Further, the method comprises the following process steps:
(1) Vacuum heating: placing the alloy copper wire into a tube furnace, vacuumizing, and then heating to 950-1050 ℃ at a speed of 110 ℃/h;
(2) Primary heat preservation: maintaining the vacuum state of the tube furnace, and preserving the temperature for 6.5 hours at 1050 ℃;
(3) And (3) secondary heat preservation: then inert mixed gas is introduced, and the temperature is kept for 2 hours at 1050 ℃;
(4) Primary cooling: restoring the pressure to normal pressure, and then cooling to normal temperature at 90 ℃/h;
(5) And (5) secondary cooling: and (3) carrying out impact deformation treatment on the surface of the alloy copper wire for 6min by adopting a vacuum environment surface nanocrystallization tester under liquid nitrogen.
Further, the zinc content of the alloy copper wire is 30%.
Further, the inert mixed gas comprises methane, hydrogen and argon; the gas flow ratio of methane, hydrogen and argon is 2:6:500.
Further, the test frequency of the surface nanocrystallization testing machine is 50Hz, the number of steel balls is 200, and the diameter of the steel balls is 8mm.
Further, the vacuum degree of the vacuuming is 1 mbar.
Comparative example 1
An annealing process of an alloy copper wire comprises the following process steps: vacuum heating, primary heat preservation, primary cooling and secondary cooling.
Further, the method comprises the following process steps:
(1) Vacuum heating: placing the alloy copper wire into a tube furnace, vacuumizing, and then heating to 1000 ℃ at a speed of 100 ℃/h;
(2) Primary heat preservation: then inert mixed gas is introduced, and the temperature is kept at 1000 ℃ for 1.5 hours;
(3) Primary cooling: restoring the pressure to normal pressure, and then cooling to normal temperature at 80 ℃/h;
(4) And (5) secondary cooling: and (3) carrying out impact deformation treatment on the surface of the alloy copper wire for 5min by adopting a vacuum environment surface nanocrystallization tester under liquid nitrogen.
Further, the zinc content of the alloy copper wire is 20%.
Further, the inert mixed gas comprises methane, hydrogen and argon; the gas flow ratio of methane, hydrogen and argon is 1.5:5:450.
Further, the test frequency of the surface nanocrystallization testing machine is 35Hz, the number of steel balls is 150, and the diameter of the steel balls is 7mm.
Further, the vacuum degree of the vacuuming is 1 mbar.
Comparative example 2
An annealing process of an alloy copper wire comprises the following process steps: vacuum heating, primary heat preservation, secondary heat preservation, primary cooling and secondary cooling.
Further, the method comprises the following process steps:
(1) Vacuum heating: placing the alloy copper wire into a tube furnace, vacuumizing, and then heating to 1000 ℃ at a speed of 100 ℃/h;
(2) Primary heat preservation: maintaining the vacuum state of the tube furnace, and preserving the heat for 6 hours at 1000 ℃;
(3) Primary cooling: restoring the pressure to normal pressure, and then cooling to normal temperature at 80 ℃/h;
(4) And (5) secondary cooling: and (3) carrying out impact deformation treatment on the surface of the alloy copper wire for 5min by adopting a vacuum environment surface nanocrystallization tester under liquid nitrogen.
Further, the zinc content of the alloy copper wire is 20%.
Further, the test frequency of the surface nanocrystallization testing machine is 35Hz, the number of steel balls is 150, and the diameter of the steel balls is 7mm.
Further, the vacuum degree of the vacuuming is 1 mbar.
Comparative example 3
An annealing process of an alloy copper wire comprises the following process steps: vacuum heating, primary heat preservation, secondary heat preservation and primary cooling.
Further, the method comprises the following process steps:
(1) Vacuum heating: placing the alloy copper wire into a tube furnace, vacuumizing, and then heating to 1000 ℃ at a speed of 100 ℃/h;
(2) Primary heat preservation: maintaining the vacuum state of the tube furnace, and preserving the heat for 6 hours at 1000 ℃;
(3) And (3) secondary heat preservation: then inert mixed gas is introduced, and the temperature is kept at 1000 ℃ for 1.5 hours;
(4) Primary cooling: the pressure was restored to normal pressure, and then cooled to normal temperature at 80 c/h.
Further, the zinc content of the alloy copper wire is 20%.
Further, the inert mixed gas comprises methane, hydrogen and argon; the gas flow ratio of methane, hydrogen and argon is 1.5:5:450.
Further, the vacuum degree of the vacuuming is 1 mbar.
Comparative example 4
An annealing process of an alloy copper wire comprises the following process steps: vacuum heating, primary heat preservation, secondary heat preservation, primary cooling and secondary cooling.
Further, the method comprises the following process steps:
(1) Vacuum heating: placing the alloy copper wire into a tube furnace, vacuumizing, and then heating to 1000 ℃ at a speed of 100 ℃/h;
(2) Primary heat preservation: maintaining the vacuum state of the tube furnace, and preserving the heat for 6 hours at 1000 ℃;
(3) And (3) secondary heat preservation: then inert mixed gas is introduced, and the temperature is kept at 1000 ℃ for 1.5 hours;
(4) Primary cooling: restoring the pressure to normal pressure, and then cooling to normal temperature at 80 ℃/h;
(5) And (5) secondary cooling: and (3) carrying out impact deformation treatment on the surface of the alloy copper wire for 5min by adopting a vacuum environment surface nanocrystallization tester under liquid nitrogen.
Further, the alloy copper wire is copper-aluminum alloy.
Further, the inert mixed gas comprises methane, hydrogen and argon; the gas flow ratio of methane, hydrogen and argon is 1.5:5:450.
Further, the test frequency of the surface nanocrystallization testing machine is 35Hz, the number of steel balls is 150, and the diameter of the steel balls is 7mm.
Further, the vacuum degree of the vacuuming is 1 mbar.
Effect example
The following table 1 shows the analysis results of mechanical properties and electrical conductivity of the alloy copper wires prepared by using examples 1 to 3 and comparative examples 1 to 4 of the present invention.
TABLE 1
From Table 1, it can be found that the alloy copper wires prepared in examples 1, 2 and 3 have better toughness; from comparison of experimental data of examples 1, 2 and 3 and comparative examples 1 and 5, it can be found that the zinc-containing alloy copper wire is subjected to one-time heat preservation to prepare the alloy copper wire, and the prepared alloy copper wire has better yield strength; from comparison of experimental data of examples 1, 2 and 3 and comparative example 2, it can be found that the alloy copper wire prepared by heat preservation under inert mixed gas has better yield strength, elongation and electric conductivity; from the experimental data of examples 1, 2, 3 and comparative example 3, it can be found that the alloy copper wire is prepared by secondary cooling, and the prepared alloy copper wire has better yield strength and elongation.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (6)

1. An annealing process of an alloy copper wire is characterized by comprising the following process steps: vacuum heating, primary heat preservation, secondary heat preservation, primary cooling and secondary cooling.
2. An alloy copper wire annealing process according to claim 1, comprising the following process steps:
(1) Vacuum heating: placing the alloy copper wire into a tube furnace for vacuumizing, and then heating to 950-1050 ℃ at the speed of 90-110 ℃/h;
(2) Primary heat preservation: maintaining the vacuum state of the tube furnace, and preserving the temperature for 5.5-6.5 hours at 950-1050 ℃;
(3) And (3) secondary heat preservation: then introducing inert mixed gas, and preserving the temperature for 1-2 hours at 950-1050 ℃;
(4) Primary cooling: restoring the pressure to normal pressure, and then cooling to normal temperature at 70-90 ℃/h;
(5) And (5) secondary cooling: and (3) carrying out impact deformation treatment on the surface of the alloy copper wire for 4-6 min by adopting a vacuum environment surface nanocrystallization tester under liquid nitrogen.
3. An alloy copper wire annealing process according to claim 2, wherein the zinc content of said alloy copper wire is 10-30%.
4. An alloy copper wire annealing process according to claim 2, wherein said inert gas mixture comprises methane, hydrogen and argon; the gas flow ratio of methane to hydrogen to argon is 1:4:400-2:6:500.
5. The annealing process of the alloy copper wire according to claim 1, wherein the test frequency of the surface nanocrystallization tester is 20-50 Hz, the number of steel balls is 100-200, and the diameter of the steel balls is 6-8 mm.
6. An alloy copper wire annealing process according to claim 5, wherein said evacuated vacuum is 1mba.
CN202310394921.XA 2023-04-14 2023-04-14 Alloy copper wire annealing process Pending CN116516268A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014227594A (en) * 2013-05-27 2014-12-08 Jx日鉱日石金属株式会社 Copper foil for manufacturing graphene and method for manufacturing graphene
CN104451487A (en) * 2014-11-18 2015-03-25 昆明理工大学 Method for preparing copper alloy nanometer gradient material
CN105018770A (en) * 2014-04-30 2015-11-04 中国科学院金属研究所 Method for preparing porous metal material and application thereof
KR20150126195A (en) * 2014-05-02 2015-11-11 에스 알 씨 주식회사 A copper thin foil for manufacturing graphene and a method of manufacturing graphene using the same
CN105063524A (en) * 2015-07-31 2015-11-18 昆明理工大学 Surface strengthening processing method for pinchbeck alloy
CN108893647A (en) * 2018-07-18 2018-11-27 上海电机学院 A kind of Cu-base composites that high strength anti-corrosion is wear-resisting
CN110257795A (en) * 2019-05-31 2019-09-20 上海欣材科技有限公司 A kind of preparation method of three-dimensional structure graphene enhancing Cu-base composites
CN111809151A (en) * 2020-06-23 2020-10-23 佛山市东鹏陶瓷有限公司 Coating process for brass and zinc alloy base material

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014227594A (en) * 2013-05-27 2014-12-08 Jx日鉱日石金属株式会社 Copper foil for manufacturing graphene and method for manufacturing graphene
CN105018770A (en) * 2014-04-30 2015-11-04 中国科学院金属研究所 Method for preparing porous metal material and application thereof
KR20150126195A (en) * 2014-05-02 2015-11-11 에스 알 씨 주식회사 A copper thin foil for manufacturing graphene and a method of manufacturing graphene using the same
CN104451487A (en) * 2014-11-18 2015-03-25 昆明理工大学 Method for preparing copper alloy nanometer gradient material
CN105063524A (en) * 2015-07-31 2015-11-18 昆明理工大学 Surface strengthening processing method for pinchbeck alloy
CN108893647A (en) * 2018-07-18 2018-11-27 上海电机学院 A kind of Cu-base composites that high strength anti-corrosion is wear-resisting
CN110257795A (en) * 2019-05-31 2019-09-20 上海欣材科技有限公司 A kind of preparation method of three-dimensional structure graphene enhancing Cu-base composites
CN111809151A (en) * 2020-06-23 2020-10-23 佛山市东鹏陶瓷有限公司 Coating process for brass and zinc alloy base material

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