CN110644025A - Ultrathin nickel-copper alloy foil and preparation method thereof - Google Patents
Ultrathin nickel-copper alloy foil and preparation method thereof Download PDFInfo
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- CN110644025A CN110644025A CN201911097580.XA CN201911097580A CN110644025A CN 110644025 A CN110644025 A CN 110644025A CN 201911097580 A CN201911097580 A CN 201911097580A CN 110644025 A CN110644025 A CN 110644025A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/06—Wires; Strips; Foils
- C25D7/0614—Strips or foils
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- 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
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- 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
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- 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
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
Abstract
The invention provides an ultrathin nickel-copper alloy foil material and a preparation method thereof, wherein the method comprises the following steps: 1. microetching the surface of the copper foil; 2. electrodepositing a nickel layer on the surface of the copper foil; 3. and (3) preparing the ultrathin nickel-copper alloy foil by vacuum sintering. The alloy foil has the thickness of less than 10 microns, uniform components, flat and bright foil surface and good corrosion resistance in seawater and hydrochloric acid environments, and can be widely applied to the technical fields of electronic devices, catalytic carriers, anti-counterfeiting, solar cells and the like.
Description
Technical Field
The invention relates to a continuous preparation technology of an ultrathin nickel-copper alloy foil material by combining an electrochemical method and a vacuum sintering method. The preparation method is simple, the technological parameters are easy to control, and the obtained ultrathin product is light and soft, can be bent at will and is strong in adjustability. Can be widely applied to the technical fields of electronic devices, catalytic carriers, anti-counterfeiting, solar cells and the like.
Background
The alloy foil has the characteristics of small volume, low power consumption, small resistance temperature coefficient, high long-term stability, small residual inductance and the like, is widely applied to industries such as automobile electronics, mobile communication and the like, and becomes a hotspot for research and development of electronic components. The alloy foil is usually prepared by a mechanical rolling method, the method can be completed by melting, casting, forging, repeated rolling and other processes, the production is complex, the cost is high, holes are easy to generate, the thickness is not uniform, and the micron-sized alloy foil is difficult to achieve. The thickness of alloy foil used for connectors and elastic elements is gradually reduced to micro-thinning and ultra-thinning, and the thickness specification of materials for some electronic products is smaller than 10 microns at present.
The nickel-copper alloy is mainly used as a corrosion-resistant alloy material in various industries, and has the advantages of excellent reduction resistance, particularly hydrofluoric acid corrosion resistance, so that the nickel-copper alloy is widely applied to the fluorination industry. The nickel-copper alloy has better corrosion resistance to halogen, neutral aqueous solution, caustic alkali with certain concentration and temperature, dilute hydrochloric acid, sulfuric acid, phosphoric acid and the like at certain temperature.
The invention adopts the electrodeposition method and the vacuum sintering technology, adopts the copper foil, the nickel plating solution and the microetching solution to prepare the ultrathin nickel-copper alloy foil, has simple preparation process, low cost, uniform thickness and components of the foil and smooth and bright surface of the foil, and is beneficial to large-scale industrial production and application.
Disclosure of Invention
The invention relates to an ultrathin nickel-copper alloy foil material and a preparation method thereof, wherein the thickness of the foil material prepared by the method can be adjusted within 0.005-0.010 mm. The invention adopts the electrodeposition method combined with the vacuum sintering technology, and compared with the prior art, the preparation process is simple, the process parameters are easy to control, and the invention is suitable for large-scale production. The technical scheme of the invention comprises the following steps:
1. microetching the surface of the copper foil: the copper foil is washed by a proper amount of deionized water, then is placed in a microetching solution to remove an oxide layer on the surface of the copper foil, and after a crystal boundary is fully exposed, the copper foil is washed by the deionized water to be neutral and then is dried in a vacuum drying oven.
2. Electrodepositing a nickel layer on the surface of the copper foil: and (3) placing the treated copper foil in an electrolytic tank filled with nickel deposition liquid, and setting electrodeposition parameters to obtain a nickel-copper alloy foil preform with a certain thickness.
3. Preparing an ultrathin nickel-copper alloy foil by vacuum sintering: and (3) placing the nickel-copper alloy foil preform in a sintering furnace in a vacuum environment, sintering at a controlled temperature, and obtaining the ultrathin nickel-copper alloy foil at a high temperature of 1000 ℃.
Drawings
FIG. 1 shows XRD spectra (JCPDS No) of two surfaces of the ultra-thin nickel-copper alloy foil obtained in the example.
65-7246), and Cu foil before sintering (JCPDS No.04-0836), nickel copper alloy foil preform XRD spectrum (JCPDS No.04-0850), with diffraction angle (unit: degree), and the ordinate is diffraction intensity (unit: a.u.);
FIG. 2 is the microstructure of the surface of the ultra-thin nickel-copper alloy foil obtained in the example;
FIG. 3 is an AC impedance curve of the ultra-thin nickel-copper alloy foil obtained in the example in hydrochloric acid of different concentrations, wherein the abscissa represents the real impedance part (unit: ohm) and the ordinate represents the imaginary impedance part (unit: ohm); compared with copper foil, the surface of the nickel-copper alloy foil has larger charge transfer resistance, which shows that the nickel-copper alloy foil has better corrosion resistance;
FIG. 4 is Tafel polarization curves of the ultra-thin nickel-copper alloy foils obtained in the examples in hydrochloric acid of different concentrations, with the abscissa being relative Hg/Hg2SO4Reference electrode potential (unit: V), ordinate log (i/A) (no unit); compared with the copper foil, the nickel-copper alloy foil has no pitting corrosion, has obviously excellent corrosion resistance and is consistent with the alternating current impedance test result.
Examples
Taking a 6 mu m thick copper foil with the area size of 5cm multiplied by 5cm, cleaning surface stains with a proper amount of deionized water, and placing the stains on FeCl3Standing for 450s in the mixed solution of (0.55mol/L) and HCl (1.0mol/L), washing with deionized water to neutrality, and placing in an electrolytic cell to electrodeposit a nickel layer by Hg/Hg2SO4As a reference electrode, a graphite plate counter electrode and a copper foil as a working electrode; the specific parameter is controlled to be the cathode current density of 10mA/cm2Electrodeposition temperature 30 ℃: drying in a vacuum drying oven at 50 ℃. Placing the dried sample on the surface of a flat alumina plate, separating with a porous alumina sheet, sintering in a vacuum sintering furnace at controlled temperature, heating to 600 deg.C at 5 deg.C/min, continuously maintaining at 600 deg.C, 700 deg.C, 900 deg.C for 60 min, and 120min respectivelyKeeping the temperature at 1000 ℃ for 50min, cooling along with the furnace to obtain an ultrathin nickel-copper alloy foil with the thickness of 6.8 mu m, wherein the X-ray diffraction analysis result of the sintered alloy foil is shown in the attached figure 1, the sample is alloyed, and the two surface compositions are completely matched; the surface micro-topography is shown in fig. 2, and the surface is flat, smooth and free of pores.
Claims (9)
1. The ultrathin nickel-copper alloy foil is characterized in that the ultrathin nickel-copper alloy foil is a copper-nickel solid solution alloy system, and the thickness of the ultrathin nickel-copper alloy foil can be adjusted within the range of 4.0-10.0 mu m.
2. The ultra-thin nickel-copper alloy foil according to claim 1, which is prepared by an electrodeposition method and a vacuum sintering technique.
3. The preparation method of the ultrathin nickel-copper alloy foil is characterized by comprising the following steps of:
(1) microetching the surface of the copper foil;
(2) in-situ electrodepositing a nickel layer on the surface of the copper foil;
(3) and (3) preparing the ultrathin nickel-copper alloy foil by vacuum sintering.
4. The method for preparing the ultrathin nickel-copper alloy foil according to claim 3, wherein the microetching solution used in the microetching treatment process of the surface of the copper foil in the step (1) is prepared from the following formula: FeCl3(0.5～5mol/L)+HCl(0.5～5mol/L)。
5. The method for preparing an ultrathin nickel-copper alloy foil according to claim 3, wherein the solution for electrodepositing nickel on the copper foil in the step (2) comprises 40-110 g/L of nickel sulfate, 3-15 g/L of nickel chloride and 3-12 g/L of boric acid.
6. The method for preparing an ultra-thin nickel-copper alloy foil according to claim 3, wherein the electrodeposition of nickel on the surface of the copper foil in the step (2) is performed by using a three-electrode system in Hg/Hg2SO4As reference electrode, graphite plate as counter electrode and copper foil as working electrodeAnd (4) a pole.
7. The method for preparing an ultrathin nickel-copper alloy foil according to claim 3, wherein the step (2) of electrodepositing nickel on the surface of the copper foil is as follows: controlling the parameters of the electrodeposition to be cathode current density of 10-20 mA/cm2(ii) a The electrodeposition temperature is 25-45 ℃.
8. The method for preparing an ultrathin nickel-copper alloy foil according to claim 3, wherein the step (3) of preparing the ultrathin nickel-copper alloy foil by vacuum sintering comprises the following steps: under vacuum environment (vacuum degree is lower than 1.0X 10)-4Pa), placing the alloy foil preform subjected to electrodeposition in a sintering furnace, and sintering at a controlled temperature to 1000 ℃ to obtain the ultrathin nickel-copper alloy foil.
9. The vacuum sintering process according to claim 8, wherein the temperature is increased to 1000 ℃, the liquid phase forming temperature is controlled, and the temperature is continuously maintained at 600-900 ℃ for 60-180 min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111710873A (en) * | 2020-06-23 | 2020-09-25 | 深圳市德立新材料科技有限公司 | Method for preparing ultrathin lithium battery copper foil through photocatalytic deposition |
| CN113430602A (en) * | 2021-06-22 | 2021-09-24 | 株洲鑫品硬质合金股份有限公司 | Preparation method of high-performance alloy coating |
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| CN108385158A (en) * | 2018-03-16 | 2018-08-10 | 江西宏业铜箔有限公司 | A kind of high smooth surface microetch treatment process and equipment for prolonging low peak extra thin copper foil |
| JP2018157173A (en) * | 2016-09-29 | 2018-10-04 | 株式会社クオルテック | Method for manufacturing power module, power module, method for manufacturing electronic component, and electronic component |
| CN108893760A (en) * | 2018-06-30 | 2018-11-27 | 青岛昊月鑫电子材料有限公司 | A kind of production method of lithium ion collector corronil foil |
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- 2019-11-12 CN CN201911097580.XA patent/CN110644025A/en active Pending
Patent Citations (6)
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| CN105779964A (en) * | 2016-05-23 | 2016-07-20 | 中国科学院上海微***与信息技术研究所 | Metal vapor-assisted preparation method of fast-growing few-layer graphene |
| JP2018157173A (en) * | 2016-09-29 | 2018-10-04 | 株式会社クオルテック | Method for manufacturing power module, power module, method for manufacturing electronic component, and electronic component |
| CN106848333A (en) * | 2017-02-22 | 2017-06-13 | 长沙理工大学 | A kind of preparation method of the cerium oxide load porous composite cathode of three-dimensional monel |
| CN108385158A (en) * | 2018-03-16 | 2018-08-10 | 江西宏业铜箔有限公司 | A kind of high smooth surface microetch treatment process and equipment for prolonging low peak extra thin copper foil |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111710873A (en) * | 2020-06-23 | 2020-09-25 | 深圳市德立新材料科技有限公司 | Method for preparing ultrathin lithium battery copper foil through photocatalytic deposition |
| CN111710873B (en) * | 2020-06-23 | 2021-09-17 | 深圳市德立新材料科技有限公司 | Method for preparing ultrathin lithium battery copper foil through photocatalytic deposition |
| CN113430602A (en) * | 2021-06-22 | 2021-09-24 | 株洲鑫品硬质合金股份有限公司 | Preparation method of high-performance alloy coating |
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Application publication date: 20200103 |