CN114000179A - Easy-to-weld copper strip for vacuum device - Google Patents
Easy-to-weld copper strip for vacuum device Download PDFInfo
- Publication number
- CN114000179A CN114000179A CN202111315715.2A CN202111315715A CN114000179A CN 114000179 A CN114000179 A CN 114000179A CN 202111315715 A CN202111315715 A CN 202111315715A CN 114000179 A CN114000179 A CN 114000179A
- Authority
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- China
- Prior art keywords
- copper
- copper strip
- base band
- easy
- electroplating
- Prior art date
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Links
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 146
- 239000010949 copper Substances 0.000 title claims abstract description 146
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 143
- 238000009713 electroplating Methods 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000003223 protective agent Substances 0.000 claims abstract description 23
- 238000002844 melting Methods 0.000 claims abstract description 19
- 230000008018 melting Effects 0.000 claims abstract description 19
- 238000003466 welding Methods 0.000 claims abstract description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 11
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 5
- 229910052742 iron Inorganic materials 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 36
- 239000002585 base Substances 0.000 claims description 35
- 239000002994 raw material Substances 0.000 claims description 33
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 26
- 239000012535 impurity Substances 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 26
- 238000002156 mixing Methods 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000003822 epoxy resin Substances 0.000 claims description 19
- 229920000647 polyepoxide Polymers 0.000 claims description 19
- 238000004140 cleaning Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 230000003647 oxidation Effects 0.000 claims description 16
- 238000007254 oxidation reaction Methods 0.000 claims description 16
- 239000002893 slag Substances 0.000 claims description 16
- 238000007670 refining Methods 0.000 claims description 14
- 239000001488 sodium phosphate Substances 0.000 claims description 14
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 14
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 14
- 229910001868 water Inorganic materials 0.000 claims description 14
- 239000004698 Polyethylene Substances 0.000 claims description 13
- -1 polyethylene Polymers 0.000 claims description 13
- 229920000573 polyethylene Polymers 0.000 claims description 13
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 13
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 12
- 239000003513 alkali Substances 0.000 claims description 12
- 239000011248 coating agent Substances 0.000 claims description 11
- 238000000576 coating method Methods 0.000 claims description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 235000012239 silicon dioxide Nutrition 0.000 claims description 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 238000000137 annealing Methods 0.000 claims description 10
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 claims description 10
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims description 10
- 229940112669 cuprous oxide Drugs 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000005498 polishing Methods 0.000 claims description 9
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 7
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 7
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 7
- 239000004327 boric acid Substances 0.000 claims description 7
- DLDJFQGPPSQZKI-UHFFFAOYSA-N but-2-yne-1,4-diol Chemical compound OCC#CCO DLDJFQGPPSQZKI-UHFFFAOYSA-N 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 239000000155 melt Substances 0.000 claims description 7
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 7
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 7
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 7
- 238000003723 Smelting Methods 0.000 claims description 6
- 238000007872 degassing Methods 0.000 claims description 6
- 238000003801 milling Methods 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 2
- 238000005476 soldering Methods 0.000 claims 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 8
- 238000005096 rolling process Methods 0.000 abstract description 7
- 238000012545 processing Methods 0.000 abstract description 5
- 229910052759 nickel Inorganic materials 0.000 abstract description 4
- 238000007747 plating Methods 0.000 abstract description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 239000011574 phosphorus Substances 0.000 abstract description 3
- 238000005452 bending Methods 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000003792 electrolyte Substances 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- 238000002360 preparation method Methods 0.000 description 12
- 239000000243 solution Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 8
- 238000005520 cutting process Methods 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 239000007788 liquid Substances 0.000 description 6
- 238000005507 spraying Methods 0.000 description 6
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 6
- 238000001125 extrusion Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 239000003610 charcoal Substances 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- QOHMWDJIBGVPIF-UHFFFAOYSA-N n',n'-diethylpropane-1,3-diamine Chemical group CCN(CC)CCCN QOHMWDJIBGVPIF-UHFFFAOYSA-N 0.000 description 4
- 238000010008 shearing Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229910001887 tin oxide Inorganic materials 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000005097 cold rolling Methods 0.000 description 1
- 238000009749 continuous casting Methods 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 229940071182 stannate Drugs 0.000 description 1
- 125000005402 stannate group Chemical group 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
-
- 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
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Mechanical Engineering (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses an easily-welded copper strip for a vacuum device, which belongs to the technical field of nonferrous metal processing, wherein a small amount of phosphorus can increase the mechanical property of copper, has good effect on welding performance and can improve the fluidity of molten copper; the content of iron is improved, the weldability and the processing formability of copper are improved, and the copper strip does not crack during rolling and is easy to weld; the easy-to-weld copper strip is plated with a layer of nickel in the electroplating process, so that the corrosion of the copper strip can be slowed down in the subsequent use process of the copper strip, and the service life of the copper strip is prolonged; the protective agent is coated on the side which is not plated with the plating layer before electroplating, the melting point of the protective agent is higher than 100 ℃ and far higher than the temperature during electroplating, so that the protective agent can not be dissolved in electrolyte during electroplating, one side of the copper strip can not be plated with the plating layer, the subsequent welding use is convenient, the protective agent has better toughness, the bending resistance of the copper strip is improved, and meanwhile, the copper strip can not easily fall off, and the electroplating operation is convenient to protect.
Description
Technical Field
The invention belongs to the technical field of nonferrous metal processing, and particularly relates to an easily-welded copper strip for a vacuum device.
Background
The vacuum device comprises an electric vacuum device. The electric vacuum device is a device which converts one form of electromagnetic energy into another form of electromagnetic energy by utilizing the interaction of electrons and an electromagnetic field in vacuum or protective gas, and is widely applied to the technical fields of broadcasting, radar, navigation and the like. The vacuum device has the characteristics of high working efficiency, long service life and good stability, but has a complex structure and higher requirements on various materials and the whole device.
The publication No. CN106140862B discloses a production process of a copper strip for an electric vacuum device, which comprises the steps of upward continuous casting, continuous extrusion, cold rolling, annealing, re-rolling, cleaning, passivation and slitting, and ensures the high purity of the copper material by utilizing copper liquid online degassing and deoxidation equipment, thereby meeting the use conditions of the electric vacuum device. However, the copper strip with high purity is not easy to weld and use, the copper strip is broken after being used for a long time due to poor welding performance of the copper strip, and the copper strip is easy to corrode under severe conditions, so that the service life of a vacuum device is shortened, the maintenance cost of equipment is increased, and resource waste is caused.
Disclosure of Invention
The invention aims to provide an easily-welded copper strip for a vacuum device, which solves the problems in the background technology by increasing the processing formability of the copper strip and adding a plating layer.
The purpose of the invention can be realized by the following technical scheme: an easily-welded copper strip for a vacuum device comprises a base band and a coating; the base band comprises the following components in percentage by mass: 99.4 to 99.45 percent of Cu, 0.48 to 0.5 percent of Fe0.03 to 0.04 percent of P, and the balance of impurities;
further, the easily-welded copper strip for the vacuum device is prepared by the following steps:
the method comprises the following steps: adding 60 percent of the total amount of the raw material copper into a rotary refining furnace, enabling the furnace temperature of the rotary refining furnace to reach 1320-; the covering agent plays a role in isolating external oxygen; continuously introducing nitrogen during the heat preservation oxidation period, wherein the flow speed of the nitrogen is 0.118Nm3H, the refractory oxide at the bottom of the molten copper is convenient to blow to the surface of the molten copper,the slag is convenient to remove; adding the rest raw material copper accounting for 40% of the total mass of the raw material copper after the first slag removal operation, adding an impurity removing agent accounting for 40% of the total mass of the raw material copper after melting, and performing the second slag removal operation after melting for 50-60 min;
the first slag removal increases the purity of the molten copper and keeps the fluidity of the copper liquid, and the solid waste residues in the molten copper can easily flow to the surface of the copper liquid from the bottom during the second slag removal, so that the second slag removal operation is facilitated; removing gas from the remaining melt by using an ultrasonic degassing method, adding iron powder and sodium phosphate, smelting for 50-60min, and pouring the melt into an ingot; the dosage of the iron powder is 0.5 percent of the mass of the melt after deslagging, and the dosage of the sodium phosphate is 0.21 percent of the mass of the melt after deslagging; the covering agent is charcoal;
step two: heating the cast ingot to 480-540 ℃, extruding by using a continuous extrusion unit, pressing the cast ingot into a copper plate, cutting the corner of the copper plate and cleaning broken copper scraps; annealing the copper plate by using a resistance type annealing furnace at the temperature of 350-360 ℃, cooling the annealed copper plate to room temperature, pressing the copper plate into a copper strip blank with the thickness of 0.2-0.25mm by using a rolling press unit, and milling the edge of the copper strip blank to obtain a base band;
step three: polishing the base band by using a 600-mesh polishing roller until the surface is bright, cleaning the base band by using alkali liquor at 85-90 ℃ for 15-20min, soaking the base band subjected to alkali cleaning by using acid liquor at 40-50 ℃ for 3-5min, drying, coating a protective agent with the thickness of 0.3-0.5mm on one surface of the base band, and then placing the base band in electroplating solution for electroplating to obtain the easily-welded copper strip; after electroplating, cleaning the copper strip with distilled water, drying and then cutting with a shearing device;
the electroplating solution comprises nickel sulfate, nickel chloride, boric acid, 1, 4-butynediol, sodium dodecyl sulfate and water; the dosage ratio of the nickel sulfate, the nickel chloride, the boric acid, the 1, 4-butynediol, the sodium dodecyl sulfate and the water is 25 g: 4.8 g: 4.2 g: 0.03 g: 0.005 g: 100 mL; the electroplating temperature is 45-65 ℃ and the time is 10-20 min;
further, the impurity removing agent is prepared by the following steps:
mixing silicon dioxide and cuprous oxide according to the weight ratio of 3: 1, calcining for 40-60min at the temperature of 650-710 ℃, and grinding and crushing the calcined silicon dioxide and cuprous oxide to obtain an oxidation composition; mixing calcium carbonate and sodium carbonate according to the mass ratio of 4:1 to obtain a carbonate composition; stirring and mixing the oxidation composition and the carbonate composition, grinding by using a ball mill, and sieving by using a 80-mesh sieve to obtain an impurity removing agent; the dosage ratio of the oxidation composition to the carbonate composition is 1 g: 5g of the total weight of the mixture;
further, the alkali liquor in the third step is prepared by the following steps: mixing sodium carbonate, sodium hydroxide, sodium phosphate and water, and stirring for 25-30min to obtain alkali solution; the dosage ratio of sodium carbonate, sodium hydroxide, sodium phosphate and water is 3 g: 5 g: 1 g: 100 mL; in the third step, 15% of hydrofluoric acid and 10% of hydrochloric acid are mixed according to the mass ratio of 1: 1.
Further, the protective agent is prepared by the following steps: heating the epoxy resin at the temperature of 100-105 ℃ to reduce the viscosity of the epoxy resin, melting polyethylene wax at the temperature of 150-160 ℃, adding the molten polyethylene wax into the epoxy resin, stirring at the temperature of 135-145 ℃ for 40-50min to obtain a component A, adding a curing agent into the component A when in use, and stirring for 8-10min to obtain a protective agent; the dosage ratio of the epoxy resin, the polyethylene wax and the curing agent is 200 g: 90-95 g: 70-80 g; the curing agent is diethylaminopropylamine.
The invention has the beneficial effects that:
1. refining raw material copper by using an impurity removing agent, wherein tin is oxidized into tin oxide and tin dioxide in molten copper, the tin oxide is alkaline and reacts with acidic silicon dioxide to generate stannate, and the tin dioxide and sodium carbonate react with boron oxide generated in the raw material copper to generate carbon dioxide and refractory crystals; the impurities are removed by slagging, so that the purity of copper is increased; phosphorus and iron are added in the subsequent smelting process, and a small amount of phosphorus can increase the mechanical property of copper, has good effect on welding performance and can improve the fluidity of molten copper; the content of iron is increased, so that the weldability and the processing formability of copper can be improved; the manufactured copper strip does not crack during rolling and is easy to weld.
2. The easy-to-weld copper strip is plated with a layer of nickel in the electroplating process, so that the corrosion of the copper strip can be slowed down in the subsequent use process of the copper strip, and the service life of the copper strip is prolonged; the side that does not plate the coating is coated with the protectant before the electroplating, the fusing point of protectant is higher than 100 ℃, the temperature far above when electroplating, so can not dissolve in electrolyte when electroplating, wherein raw materials epoxy resin and polyethylene wax intermiscibility are relatively poor, form the heterogeneous system, can increase the mechanical properties after its solidification, prevent its fragility too high and increase its toughness, can prevent that the copper strips from bending in the electroplating process after coating in copper strips one side, make one side of copper strips not plated the coating, be convenient for follow-up welding use, and reduced the adhesive action of epoxy resin and metal, be convenient for get rid of after copper strips nickel plating.
3. This copper strips is not equipped with the one side of coating and is melt-connected when the welding, and the cladding material of opposite side links up each other, so structural can not receive the influence than the copper of the melting point of nickel cladding material, still levels than welding seam department, and the mechanical properties of the welding seam of formation is still better, satisfies vacuum device's operation requirement.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The preparation of the impurity removing agent comprises the following preparation steps:
mixing 300g of silicon dioxide and 100g of cuprous oxide, calcining for 40min at 650 ℃, and grinding and crushing the calcined silicon dioxide and cuprous oxide to obtain an oxidation composition; mixing 1.6kg of calcium carbonate and 400g of sodium carbonate to obtain a carbonate composition; 400g of the oxidation composition and 2kg of the carbonate composition were mixed with stirring, ground with a ball mill, and sieved through a 80 mesh sieve to obtain the impurity removing agent.
Example 2
The preparation of the impurity removing agent comprises the following preparation steps:
mixing 300g of silicon dioxide and 100g of cuprous oxide, calcining for 50min at 680 ℃, and grinding and crushing the calcined silicon dioxide and cuprous oxide to obtain an oxidation composition; mixing 1.6kg of calcium carbonate and 400g of sodium carbonate to obtain a carbonate composition; 400g of the oxidation composition and 2kg of the carbonate composition were mixed with stirring, ground with a ball mill, and sieved through a 80 mesh sieve to obtain the impurity removing agent.
Example 3
The preparation of the impurity removing agent comprises the following preparation steps:
mixing 300g of silicon dioxide and 100g of cuprous oxide, calcining for 60min at 710 ℃, and grinding and crushing the calcined silicon dioxide and cuprous oxide to obtain an oxidation composition; mixing 1.6kg of calcium carbonate and 400g of sodium carbonate to obtain a carbonate composition; 400g of the oxidation composition and 2kg of the carbonate composition were mixed with stirring, ground with a ball mill, and sieved through a 80 mesh sieve to obtain the impurity removing agent.
Example 4
The preparation of the protective agent comprises the following steps:
heating 2kg of epoxy resin at 100-105 ℃ to reduce the viscosity of the epoxy resin, melting 900-950g of polyethylene wax at 150-160 ℃, adding the molten polyethylene wax into the epoxy resin, stirring at 135-145 ℃ for 40-50min to obtain a component A, adding 700-800g of diethylaminopropylamine into the component A when in use, and stirring for 8-10min to obtain the protective agent.
Example 5
The preparation of the protective agent comprises the following steps:
heating 2kg of epoxy resin at 100-105 ℃ to reduce the viscosity of the epoxy resin, melting 900-950g of polyethylene wax at 150-160 ℃, adding the molten polyethylene wax into the epoxy resin, stirring at 135-145 ℃ for 40-50min to obtain a component A, adding 700-800g of diethylaminopropylamine into the component A when in use, and stirring for 8-10min to obtain the protective agent.
Example 6
The preparation of the protective agent comprises the following steps:
heating 2kg of epoxy resin at 100-105 ℃ to reduce the viscosity of the epoxy resin, melting 900-950g of polyethylene wax at 150-160 ℃, adding the molten polyethylene wax into the epoxy resin, stirring at 135-145 ℃ for 40-50min to obtain a component A, adding 700-800g of diethylaminopropylamine into the component A when in use, and stirring for 8-10min to obtain the protective agent.
Example 7
The method for preparing the easily-welded copper strip for the vacuum device comprises the following preparation steps:
the method comprises the following steps: adding 60 percent of the total amount of raw material copper into a rotary refining furnace, enabling the furnace temperature of the rotary refining furnace to reach 1320 ℃, after the raw material copper is melted, adding an impurity removing agent accounting for 0.6 percent of the total mass of the raw material copper into the refining furnace by using a powder spraying tank, continuously stirring, spraying a covering agent on the surface of the melted raw material copper, preserving heat, oxidizing for 1.5 hours, and then carrying out primary slag removal operation; continuously introducing nitrogen during the heat preservation oxidation period, wherein the flow speed of the nitrogen is 0.118Nm3H; adding the rest raw material copper accounting for 40% of the total mass of the raw material copper after the first slag removal operation, adding an impurity removing agent accounting for 40% of the total mass of the raw material copper after melting, carrying out the second slag removal operation after melting for 50min, removing gas in the left melt by using an ultrasonic degassing method, adding iron powder and sodium phosphate, and pouring the melt into an ingot after melting for 50 min; the covering agent is charcoal, and the impurity removing agent is prepared in example 2;
step two: heating the cast ingot to 480 ℃, extruding by using a continuous extrusion machine set, pressing the cast ingot into a copper plate, cutting the corners of the copper plate and cleaning broken copper scraps; annealing the copper plate by using a resistance type annealing furnace at 350 ℃, cooling the annealed copper plate to room temperature, pressing the copper plate into a copper strip blank with the thickness of 0.2mm by using a rolling press unit, and milling the edge of the copper strip blank to obtain a base band;
step three: mixing 3kg of sodium carbonate, 5kg of sodium hydroxide, 1kg of sodium phosphate and 100L of water, and stirring for 25min to obtain an alkali liquor; mixing 20L of 15 mass percent hydrofluoric acid and 20L of 10 mass percent hydrochloric acid to obtain acid liquid; uniformly mixing 25kg of nickel sulfate, 4.8kg of nickel chloride, 4.2kg of boric acid, 30g of 1, 4-butynediol, 5g of sodium dodecyl sulfate and 100L of water to obtain electroplating solution;
polishing the base band by using a 600-mesh polishing roller until the surface is bright, cleaning the base band for 15min by using an alkaline solution at 85 ℃, soaking the base band subjected to alkaline cleaning for 3min by using an acid solution at 40 ℃, drying, coating the protective agent prepared in the embodiment 5 with the thickness of 0.3mm on one surface of the base band, and then placing the base band in an electroplating solution for electroplating at the electroplating temperature of 45 ℃ for 10 min; removing the protective agent to obtain the easily-welded copper strip; and after electroplating, cleaning the copper strip with distilled water, drying and then cutting with a shearing device.
Example 8
The method for preparing the easily-welded copper strip for the vacuum device comprises the following preparation steps:
the method comprises the following steps: adding 60 percent of the total amount of the raw material copper into a rotary refining furnace, enabling the furnace temperature of the rotary refining furnace to reach 1330 ℃, after the raw material copper is melted, adding an impurity removing agent accounting for 0.6 percent of the total mass of the raw material copper into the refining furnace by using a powder spraying tank, continuously stirring, spraying a covering agent on the surface of the melted raw material copper, preserving heat, oxidizing for 1.8 hours, and then carrying out primary slag removal operation; continuously introducing nitrogen during the heat preservation oxidation period, wherein the flow speed of the nitrogen is 0.118Nm3H; adding the rest raw material copper accounting for 40% of the total mass of the raw material copper after the first slag removal operation, adding an impurity removing agent accounting for 40% of the total mass of the raw material copper after melting, carrying out the second slag removal operation after smelting for 55min, removing gas in the left melt by using an ultrasonic degassing method, adding iron powder and sodium phosphate, and pouring the melt into an ingot after smelting for 55 min; the covering agent is charcoal, and the impurity removing agent is prepared in example 2;
step two: heating the cast ingot to 510 ℃, extruding by using a continuous extrusion machine set, pressing the cast ingot into a copper plate, cutting the corners of the copper plate and cleaning broken copper scraps; annealing the copper plate by using a resistance type annealing furnace at 355 ℃, cooling the annealed copper plate to room temperature, pressing the copper plate into a copper strip blank with the thickness of 0.2mm by using a rolling press unit, and milling the edge of the copper strip blank to obtain a base band;
step three: mixing 3kg of sodium carbonate, 5kg of sodium hydroxide, 1kg of sodium phosphate and 100L of water, and stirring for 25min to obtain an alkali liquor; mixing 20L of 15 mass percent hydrofluoric acid and 20L of 10 mass percent hydrochloric acid to obtain acid liquid; uniformly mixing 25kg of nickel sulfate, 4.8kg of nickel chloride, 4.2kg of boric acid, 30g of 1, 4-butynediol, 5g of sodium dodecyl sulfate and 100L of water to obtain electroplating solution;
polishing the base band by using a 600-mesh polishing roller until the surface is bright, cleaning the base band by using alkali liquor at 88 ℃ for 18min, soaking the base band subjected to alkali cleaning by using acid liquor at 45 ℃ for 4min, drying, coating the protective agent prepared in the embodiment 5 with the thickness of 0.4mm on one surface of the base band, and then placing the base band in electroplating solution for electroplating, wherein the electroplating temperature is 55 ℃ and the electroplating time is 15 min; removing the protective agent to obtain the easily-welded copper strip; and after electroplating, cleaning the copper strip with distilled water, drying and then cutting with a shearing device.
Example 9
The method for preparing the easily-welded copper strip for the vacuum device comprises the following preparation steps:
the method comprises the following steps: adding 60 percent of the total amount of the raw material copper into a rotary refining furnace, enabling the furnace temperature of the rotary refining furnace to reach 1340 ℃, after the raw material copper is molten, adding an impurity removing agent accounting for 0.6 percent of the total mass of the raw material copper into the refining furnace by using a powder spraying tank, continuously stirring, spraying a covering agent on the surface of the molten raw material copper, and carrying out primary slag removal operation after heat preservation and oxidation for 2 hours; continuously introducing nitrogen during the heat preservation oxidation period, wherein the flow speed of the nitrogen is 0.118Nm3H; adding the rest raw material copper accounting for 40% of the total mass of the raw material copper after the first slag removal operation, adding an impurity removing agent accounting for 40% of the total mass of the raw material copper after melting, carrying out the second slag removal operation after melting for 60min, removing gas in the left melt by using an ultrasonic degassing method, adding iron powder and sodium phosphate, and pouring the melt into an ingot after melting for 60 min; the covering agent is charcoal, and the impurity removing agent is prepared in example 2;
step two: heating the cast ingot to 540 ℃, extruding by using a continuous extrusion unit, pressing the cast ingot into a copper plate, cutting the corners of the copper plate and cleaning broken copper scraps; annealing the copper plate by using a resistance type annealing furnace at 360 ℃, cooling the annealed copper plate to room temperature, pressing the copper plate into a copper strip blank with the thickness of 0.25mm by using a rolling press unit, and milling the edge of the copper strip blank to obtain a base band;
step three: mixing 3kg of sodium carbonate, 5kg of sodium hydroxide, 1kg of sodium phosphate and 100L of water, and stirring for 30min to obtain an alkali liquor; mixing 20L of 15 mass percent hydrofluoric acid and 20L of 10 mass percent hydrochloric acid to obtain acid liquid; uniformly mixing 25kg of nickel sulfate, 4.8kg of nickel chloride, 4.2kg of boric acid, 30g of 1, 4-butynediol, 5g of sodium dodecyl sulfate and 100L of water to obtain electroplating solution;
polishing the base band by using a 600-mesh polishing roller until the surface is bright, cleaning the base band for 20min by using an alkaline solution at 90 ℃, soaking the base band subjected to alkaline cleaning for 5min by using an acid solution at 50 ℃, drying, coating the protective agent prepared in the embodiment 5 with the thickness of 0.5mm on one surface of the base band, and then placing the base band in an electroplating solution for electroplating at the electroplating temperature of 65 ℃ for 20 min; removing the protective agent to obtain the easily-welded copper strip; and after electroplating, cleaning the copper strip with distilled water, drying and then cutting with a shearing device.
Comparative example 1: an impurity removing agent is prepared on the basis of the embodiment 2 without adding an oxidizing composition, and then the easily-weldable copper strip is prepared by the steps in the embodiment 8.
Comparative example 2: on the basis of the embodiment 8, sodium phosphate is not added in the process of further smelting in the step one, and the other steps are kept unchanged to prepare the easily-weldable copper strip.
Comparative example 3: copper strips 0.2mm thick were prepared according to the method described in the background application publication No. CN 106140862B.
And (3) carrying out performance test on the examples 7-9 and the comparative examples 1-3, wherein the performance test method is to verify the mechanical performance of the welding part of the easily-welded copper strip through a welding test, specifically, a TIG automatic welding machine is used, and the TIG automatic welding process parameters are firstly debugged: arc length: 1-2 mm; tungsten electrode tip angle: 30 degrees; extension length of tungsten electrode: 5-6 mm; the misalignment degree is less than 0.05 tt; taking the copper strips in the examples 4-6 and the comparative examples 1-3, milling the copper strips into square pieces of 4cm multiplied by 4cm, carrying out sampling analysis on the welded joints after butt welding, and obtaining the results shown in the table 1:
TABLE 1
| Item | Example 7 | Example 8 | Example 9 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| HV/1kg | 256 | 256 | 258 | 232 | 205 | 158 |
| σb(MPa) | 685.5 | 685.7 | 689.0 | 606.3 | 559.1 | 486.9 |
| δ％ | 0.5 | 0.5 | 0.6 | 0.4 | 0.3 | 0.3 |
As can be seen from Table 1, the thicker the copper strip thickness, the greater the Vickers hardness at the weld, the better the strength, and the greater the elongation in examples 7-9.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. An easily-welded copper strip for a vacuum device is characterized by comprising a base band and a coating; the base band comprises the following components in percentage by mass: 99.4 to 99.45 percent of Cu, 0.48 to 0.5 percent of Fe, 0.03 to 0.04 percent of P and the balance of impurities; the easy-welding copper strip for the vacuum device is prepared by the following steps:
the method comprises the following steps: adding iron powder and sodium phosphate in the raw material copper refining process, smelting for 50-60min, and pouring the melt into an ingot;
step two: pressing the cast ingot into a copper plate, annealing the copper plate at the temperature of 350-360 ℃, cooling and pressing into a copper strip blank with the thickness of 0.2-0.25mm, and milling the edge of the copper strip blank to obtain a base band;
step three: polishing the base band until the surface is bright, cleaning the base band for 15-20min at 85-90 ℃ by using an alkali solution, soaking the base band for 3-5min at 40-50 ℃ by using an acid solution, drying the base band, coating a protective agent with the thickness of 0.3-0.5mm on one surface of the base band, placing the base band in an electroplating solution for electroplating, and removing the protective agent to obtain the easily-welded copper strip for the vacuum device.
2. The easy-to-weld copper strip for vacuum devices as claimed in claim 1, wherein the refining step in the first step is: melting 60% of the total amount of the raw material copper at the temperature of 1320-; adding raw material copper accounting for 40% of the total mass of the raw material copper, melting, adding an impurity removing agent accounting for 40% of the total mass of the raw material copper, melting for 50-60min, and then performing secondary slag removal operation and degassing operation.
3. The easy-to-weld copper strip for vacuum devices as claimed in claim 2, wherein the impurity removing agent is prepared by the following steps:
mixing silicon dioxide and cuprous oxide according to the weight ratio of 3: 1, calcining for 40-60min at the temperature of 650-710 ℃, and grinding and crushing the calcined silicon dioxide and cuprous oxide to obtain an oxidation composition; mixing calcium carbonate and sodium carbonate according to the mass ratio of 4:1 to obtain a carbonate composition; and stirring and mixing the oxidation composition and the carbonate composition, grinding by using a ball mill, and sieving by using a 80-mesh sieve to obtain the impurity removing agent.
4. The easy-soldering copper tape for vacuum devices as claimed in claim 3, wherein the amount ratio of the oxidizing composition to the carbonate composition is 1 g: 5g of the total weight.
5. The easy-soldering copper strip for vacuum devices as claimed in claim 1, wherein the alkali solution in step three is prepared by the following steps: mixing sodium carbonate, sodium hydroxide, sodium phosphate and water, and stirring for 25-30min to obtain alkali solution; the dosage ratio of sodium carbonate, sodium hydroxide, sodium phosphate and water is 3 g: 5 g: 1 g: 100 mL.
6. The easy-to-weld copper strip for vacuum devices as claimed in claim 1, wherein the acid solution in the third step is prepared by mixing 15% hydrofluoric acid and 10% hydrochloric acid in a mass ratio of 1: 1.
7. The solderable copper strip for vacuum devices of claim 1 wherein the electroplating solution in step three comprises the following components: nickel sulfate, nickel chloride, boric acid, 1, 4-butynediol, sodium dodecyl sulfate and water; the dosage ratio of the nickel sulfate, the nickel chloride, the boric acid, the 1, 4-butynediol, the sodium dodecyl sulfate and the water is 25 g: 4.8 g: 4.2 g: 0.03 g: 0.005 g: 100 mL.
8. The easy-soldering copper strip for vacuum devices as claimed in claim 1, wherein the protective agent is prepared by the following steps in the third step: heating the epoxy resin at the temperature of 100-105 ℃ to reduce the viscosity of the epoxy resin, melting polyethylene wax at the temperature of 150-160 ℃, adding the molten polyethylene wax into the epoxy resin, stirring at the temperature of 135-145 ℃ for 40-50min to obtain a component A, adding a curing agent into the component A when in use, and stirring for 8-10min to obtain a protective agent; the dosage ratio of the epoxy resin, the polyethylene wax and the curing agent is 200 g: 90-95 g: 70-80 g.
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