CN108166024A - The technique that a kind of electrodeposition process prepares iron-nickel alloy foil - Google Patents

The technique that a kind of electrodeposition process prepares iron-nickel alloy foil Download PDF

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Publication number
CN108166024A
CN108166024A CN201711454555.3A CN201711454555A CN108166024A CN 108166024 A CN108166024 A CN 108166024A CN 201711454555 A CN201711454555 A CN 201711454555A CN 108166024 A CN108166024 A CN 108166024A
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anode
iron
alloy foil
nickel
nickel alloy
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王奇
王敏雪
立群
谷爱俊
程晓龙
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Anhui Mai De Fu New Materials Co Ltd
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Anhui Mai De Fu New Materials Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00Electroforming
    • C25D1/04Wires; Strips; Foils

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating Methods And Accessories (AREA)
  • Electroplating And Plating Baths Therefor (AREA)

Abstract

The invention discloses the techniques that a kind of electrodeposition process prepares iron-nickel alloy foil, it is related to electrochemical deposition technique field, installation, plating, cleaning, passivation, drying including electroplanting device, winding and etc., the present invention is 5 microns up to 1350mm, minimum thickness using the iron-nickel alloy foil breadth of electrodeposition process production, just correspond to 1/10th of common A4 paper thickness, product thickness error is can be controlled within 8%, and this method has many advantages, such as the recyclable of low energy consumption, low emission and raw material.

Description

The technique that a kind of electrodeposition process prepares iron-nickel alloy foil
Technical field
The present invention relates to electrochemical deposition technique fields, and in particular to a kind of electrodeposition process prepares the work of iron-nickel alloy foil Skill.
Background technology
Soft magnetic materials has the history of more than 100 years from pure iron, silicon steel, permalloy to invar steel.Traditionally these soft magnetisms Alloy be all by smelting, forging, numerous and diverse technique such as hot rolling or cold rolling crystal alloy band is made, then thermally treated to improve its magnetic Energy.Production cost is high, product specification (breadth, thickness) is limited, magnetic property is not also highly desirable.The amorphous alloy developed in recent years With nano-crystal soft-magnetic strip metal material production technology, be using chilling technique, by melt alloy on the roll surface of rotation chilling The strip of dozens of micron thickness is directly formed, although magnetic property significantly improves, production cost is very high, and product breadth is very narrow, thick Degree not easy-regulating, it is rough surface, brittle, using being limited to.
Iron-nickel alloy is otherwise known as permalloy, is a kind of critically important soft magnetic materials.Iron-nickel alloy foil has excellent Magnetic shield performance, the magnetic screen of low frequency magnetic field in being suitble to.The preparation process of conventional alloys metal foil be by mental section by thickness by Grade rolls thinning process.There is technical limitation in breadth, absolute thickness, metal fatigue, processing loss, the uniformity of becoming a useful person. Electrodeposition process is a kind of reverse preparation method, and foil is grown naturally by thin to thick.Need not improve cost just can prepare big breadth, Every stability of characteristics, homogeneous metal foil section bar.The Alloy Foil maximum breadth of conventional preparation techniques production is 300mm, most Small thickness is 30 microns.There are still improved spaces.
China Patent Publication No. discloses a kind of electro-deposition of one nickel of nano crystal iron, one evanohm foil for CN102839399A Preparation method belongs to electro-deposited alloy field, is to use the method for electrochemical deposition in one trivalent chromium water of sulfate monochloride One nickel of nano crystal iron, one evanohm foil is continuously prepared in electro-deposition in solution system.The Alloy Foil that this method is produced is simple for process, Electrolyte environmental protection, stable, waste liquid is disposable.Chromium content is higher in Alloy Foil, and ingredient and thickness are easily controllable, and surface is smooth, With excellent mechanics, electricity, magnetics and corrosion resisting property, can partial alternative stainless steel foil band etc. be widely used in electricity, communication, The industrial circles such as electromechanics can be used as excellent magnetic material, battery framework material and electromagnetic shielding material.But it is produced The Alloy Foil gone out equal Shortcomings in terms of thickness and breadth.
Invention content
Problem to be solved by this invention is to provide a kind of simple for process, stable, the excellent electrodeposition process preparation of product quality The technique of iron-nickel alloy foil.
To achieve these goals, the technical solution taken of the present invention is:A kind of electrodeposition process provided prepares iron nickel The technique of Alloy Foil, it is specific as follows:
(1) electroplating solution is injected into electrolytic cell, it is molten that the Ka band lower end for ensureing to connect with cathode roll is immersed in plating In liquid, anode conducting device is put into electrolytic cell, and iron anode plate and Nickel Anode Plate are alternately put into anode conducting device, Increase filter screen in anode upper end, anode conducting device and cathode roll are connected to the anode and cathode of power supply respectively;
(2) voltage regulating device is connected between anode conducting device and positive pole, what opening was connect with electrolytic cell follows Loop system starts motor and drives cathode roll rotation, and the reload temperature control device in electrolytic cell, and the interior plating of control electrolytic cell is molten The temperature of liquid is 51-54 DEG C, meanwhile, control current parameters are 3.6-4.0A/dm2, and the pH value for adjusting electroplating solution is 2.2- 2.4;
(3) plating enters Cleaning and Passivation device in the stripped device of iron-nickel alloy foil of cathode belt surface, is cleaned And Passivation Treatment, then drying device obtains dry clean and tidy iron-nickel alloy foil, is wound finally by rolling-up mechanism.
Preferably, the Ka band uses the annular strip of surface titanium-nitride.
Preferably, the anode conducting device includes graphite cake and graphite rod, a connection of graphite rod and graphite cake, separately One outside for extending to electrolytic cell is connect with positive pole, and the iron anode and nickel anode are arranged alternately on graphite cake, and Iron anode and nickel anode are provided with insulating materials, and iron anode is in parallel with nickel anode.
Preferably, the electroplating solution includes following component (mass-volume concentration g/L):Nickel sulfate 80-100, nickel chloride 30-40, ferrous sulfate 40-100, boric acid 20-40, polyethylene glycol 5-8, saccharin 5-40, surfactant 1-5.
Preferably, metal molybdenum powder 15-20g has been further included in the electroplating solution.
Preferably, in electroplating process, when electroplating solution volume is reduced, it is to pH by deionized water processing with dilute sulfuric acid 2.2-2.4 is then added in electroplating solution, when electroplating solution pH value rises, with a concentration of 5% sulfuric acid and sodium hydroxide solution PH is adjusted to zone of reasonableness.
Preferably, the iron anode and nickel anode are tabular, width 5-6cm, thickness 0.6-1.2cm.
Preferably, the circulatory system includes water circulating pump, return duct, reservoir and filter, and electroplating solution passes through successively Water circulating pump, return duct, reservoir and filter is crossed to re-enter into electrolytic cell.
Beneficial effects of the present invention:
(1) present invention is 5 microns up to 1350mm, minimum thickness using the iron-nickel alloy foil breadth of electrodeposition process production, / 10th of common A4 paper thickness are just corresponded to, product thickness error is can be controlled within 8%, and this method has low energy Consumption, low emission and raw material it is recyclable the advantages that.
(2) for the present invention by strictly controlling each technological parameter in production process, the temperature, electric current such as electroplating solution are close The ingredient of degree, the pH value of electroplating solution, the rotating speed of cathode roll and electroplating solution, can obtain satisfactory to the maximum extent Iron-nickel alloy foil, cathode roller surface plate the stripping that titanium nitride is conducive to coating.
Description of the drawings
Fig. 1 is the structural diagram of the present invention.
Wherein:1- electrolytic cells, 2- iron anodes, 3- cathode rolls, 4- strainers, 5- reservoirs, 6- return ducts, 7- water circulating pumps, 8- cleaning devices, 9- passivating devices, 10- drying units, 11- voltage regulating devices, 12- anode conducting devices, 13- filters, 14- nickel anodes.
Specific embodiment
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, the embodiment It is only used for explaining the present invention, be not intended to limit the scope of the present invention..
Embodiment 1
A kind of electrodeposition process prepares the technique of iron-nickel alloy foil, specific as follows:
(1) electroplating solution is injected into electrolytic cell 1, it is molten that the Ka band lower end for ensureing to connect with cathode roll is immersed in plating In liquid, anode conducting device 12 is put into electrolytic cell 1, can be supported by means of the support plate of an arc, and iron is positive 2 plate of pole and 14 plate of nickel anode are alternately put into anode conducting device 12, increase filter screen 4 in 2 upper end of anode, anode conducting is filled Put 12 and cathode roll connect the anode and cathode of power supply respectively;
(2) voltage regulating device 11 is connected between anode conducting device 12 and positive pole, opening is connect with electrolytic cell 1 The circulatory system, start motor and drive cathode roll rotation, and the reload temperature control device in electrolytic cell 1 is controlled in electrolytic cell 1 The temperature of electroplating solution is 51 DEG C, meanwhile, control current parameters are 3.6A/dm2, and the pH value for adjusting electroplating solution is 2.2;
(3) plating enters Cleaning and Passivation device in the stripped device of iron-nickel alloy foil of cathode belt surface, is cleaned (i.e. cleaning device 8) and Passivation Treatment (i.e. passivating device 9), then drying device 10 obtain dry clean and tidy iron-nickel alloy foil, It is wound finally by rolling-up mechanism.
In the present embodiment, the Ka band uses the annular strip of surface titanium-nitride.
In the present embodiment, the anode conducting device 12 includes graphite cake and graphite rod, and the one of graphite rod and graphite cake Head connection, the outside that other end extends to electrolytic cell 1 are connect with positive pole, and the iron anode 2 and nickel anode 14 are alternately arranged On graphite cake, and iron anode 2 and nickel anode 14 are provided with insulating materials, and iron anode 2 is in parallel with nickel anode 14.
In the present embodiment, the electroplating solution includes following constituent mass volumetric concentration g/L:Nickel sulfate 80, nickel chloride 30, ferrous sulfate 40, boric acid 20, polyethylene glycol 5, saccharin 5, surfactant 1.
In the present embodiment, metal molybdenum powder 15g has been further included in the electroplating solution.
In the present embodiment, in electroplating process, when electroplating solution volume is reduced, deionized water is handled to pH with dilute sulfuric acid It is then added in electroplating solution for 2.2, when electroplating solution pH value rises, sulfuric acid and sodium hydroxide solution tune with a concentration of 5% PH is saved to zone of reasonableness.
In the present embodiment, the iron anode 2 and nickel anode 14 are tabular, width 5cm, thickness 0.6cm.
In addition, the circulatory system includes water circulating pump 7, return duct 6, reservoir 5 and filter 12, electroplating solution is successively It is re-entered into electrolytic cell 1 by water circulating pump 7, return duct 6, reservoir 5 and filter 12.
Embodiment 2
A kind of electrodeposition process prepares the technique of iron-nickel alloy foil, specific as follows:
(1) electroplating solution is injected into electrolytic cell 1, it is molten that the Ka band lower end for ensureing to connect with cathode roll is immersed in plating In liquid, anode conducting device 12 is put into electrolytic cell 1, can be supported by means of the support plate of an arc, and iron is positive 2 plate of pole and 14 plate of nickel anode are alternately put into anode conducting device 12, increase filter screen 4 in 2 upper end of anode, anode conducting is filled Put 12 and cathode roll connect the anode and cathode of power supply respectively;
(2) voltage regulating device 11 is connected between anode conducting device 12 and positive pole, opening is connect with electrolytic cell 1 The circulatory system, start motor and drive cathode roll rotation, and the reload temperature control device in electrolytic cell 1 is controlled in electrolytic cell 1 The temperature of electroplating solution is 53 DEG C, meanwhile, control current parameters are 3.8A/dm2, and the pH value for adjusting electroplating solution is 2.3;
(3) plating enters Cleaning and Passivation device in the stripped device of iron-nickel alloy foil of cathode belt surface, is cleaned (i.e. cleaning device 8) and Passivation Treatment (i.e. passivating device 9), then drying device 10 obtain dry clean and tidy iron-nickel alloy foil, It is wound finally by rolling-up mechanism.
In the present embodiment, the Ka band uses the annular strip of surface titanium-nitride.
In the present embodiment, the anode conducting device 12 includes graphite cake and graphite rod, and the one of graphite rod and graphite cake Head connection, the outside that other end extends to electrolytic cell 1 are connect with positive pole, and the iron anode 2 and nickel anode 14 are alternately arranged On graphite cake, and iron anode 2 and nickel anode 14 are provided with insulating materials, and iron anode 2 is in parallel with nickel anode 14.
In the present embodiment, the electroplating solution includes following constituent mass volumetric concentration g/L:Nickel sulfate 90, nickel chloride 35, ferrous sulfate 80, boric acid 30, polyethylene glycol 7, saccharin 25, surfactant 3.
In the present embodiment, metal molybdenum powder 18g has been further included in the electroplating solution.
In the present embodiment, in electroplating process, when electroplating solution volume is reduced, deionized water is handled to pH with dilute sulfuric acid It is then added in electroplating solution for 2.3, when electroplating solution pH value rises, sulfuric acid and sodium hydroxide solution tune with a concentration of 5% PH is saved to zone of reasonableness.
In the present embodiment, the iron anode 2 and nickel anode 14 are tabular, width 5cm, thickness 1.0cm.
In addition, the circulatory system includes water circulating pump 7, return duct 6, reservoir 5 and filter 12, electroplating solution is successively It is re-entered into electrolytic cell 1 by water circulating pump 7, return duct 6, reservoir 5 and filter 12.
Embodiment 3
A kind of electrodeposition process prepares the technique of iron-nickel alloy foil, specific as follows:
(1) electroplating solution is injected into electrolytic cell 1, it is molten that the Ka band lower end for ensureing to connect with cathode roll is immersed in plating In liquid, anode conducting device 12 is put into electrolytic cell 1, can be supported by means of the support plate of an arc, and iron is positive 2 plate of pole and 14 plate of nickel anode are alternately put into anode conducting device 12, increase filter screen 4 in 2 upper end of anode, anode conducting is filled Put 12 and cathode roll connect the anode and cathode of power supply respectively;
(2) voltage regulating device is connected between anode conducting device and positive pole, what opening was connect with electrolytic cell follows Loop system starts motor and drives cathode roll rotation, and the reload temperature control device in electrolytic cell, and the interior plating of control electrolytic cell is molten The temperature of liquid is 54 DEG C, meanwhile, control current parameters are 4.0A/dm2, and the pH value for adjusting electroplating solution is 2.4;
(3) plating enters Cleaning and Passivation device in the stripped device of iron-nickel alloy foil of cathode belt surface, is cleaned (i.e. cleaning device 8) and Passivation Treatment (i.e. passivating device 9), then drying device 10 obtain dry clean and tidy iron-nickel alloy foil, It is wound finally by rolling-up mechanism.
In the present embodiment, the Ka band uses the annular strip of surface titanium-nitride.
In the present embodiment, the anode conducting device 12 includes graphite cake and graphite rod, and the one of graphite rod and graphite cake Head connection, the outside that other end extends to electrolytic cell 1 are connect with positive pole, and the iron anode 2 and nickel anode 14 are alternately arranged On graphite cake, and iron anode 2 and nickel anode 14 are provided with insulating materials, and iron anode 2 is in parallel with nickel anode 14.
In the present embodiment, the electroplating solution includes following constituent mass volumetric concentration g/L:Nickel sulfate 100, nickel chloride 40, ferrous sulfate 100, boric acid 40, polyethylene glycol 8, saccharin 40, surfactant 5.
In the present embodiment, metal molybdenum powder 20g has been further included in the electroplating solution.
In the present embodiment, in electroplating process, when electroplating solution volume is reduced, deionized water is handled to pH with dilute sulfuric acid It is then added in electroplating solution for 2.4, when electroplating solution pH value rises, sulfuric acid and sodium hydroxide solution tune with a concentration of 5% PH is saved to zone of reasonableness.
In the present embodiment, the iron anode 2 and nickel anode 14 are tabular, width 6cm, thickness 1.2cm.
In addition, the circulatory system includes water circulating pump 7, return duct 6, reservoir 5 and filter 12, electroplating solution is successively It is re-entered into electrolytic cell 1 by water circulating pump 7, return duct 6, reservoir 5 and filter 12.
The iron-nickel alloy foil of above-mentioned 3 embodiments is tested for the property, it is as a result as follows:
Obviously present invention specific implementation is not subject to the restrictions described above, as long as employing the method structure of the present invention.

Claims (8)

1. the technique that a kind of electrodeposition process prepares iron-nickel alloy foil, which is characterized in that specific as follows:
(1) electroplating solution is injected into electrolytic cell (1), the Ka band lower end for ensureing to connect with cathode roll is immersed in electroplating solution In, anode conducting device (12) is put into, and iron anode (2) plate and nickel anode (14) plate are alternately put into sun electrolytic cell (1) is inner In pole electric installation (12), increase filter screen (4) in anode (2) upper end, anode conducting device (12) and cathode roll are connected respectively Connect the anode and cathode of power supply;
(2) voltage regulating device (11) is connected between positive pole in anode conducting device (12), opened with electrolytic cell (1) even The circulatory system connect starts motor and drives cathode roll rotation, and in the interior reload temperature control device of electrolytic cell (1), control electrolysis The temperature of slot (1) interior electroplating solution is 51-54 DEG C, meanwhile, control current parameters are 3.6-4.0A/dm2, and adjust electroplating solution PH value be 2.2-2.4;
(3) plating enters Cleaning and Passivation device in the stripped device of iron-nickel alloy foil of cathode belt surface, clean and blunt Change is handled, then drying device (10) obtains dry clean and tidy iron-nickel alloy foil, is wound finally by rolling-up mechanism.
2. the technique that a kind of electrodeposition process according to claims 1 prepares iron-nickel alloy foil, which is characterized in that described the moon Pole band uses the annular strip of surface titanium-nitride.
3. the technique that a kind of electrodeposition process according to claims 1 prepares iron-nickel alloy foil, which is characterized in that the sun Pole electric installation (12) includes graphite cake and graphite rod, and a connection of graphite rod and graphite cake, other end extends to electrolytic cell (1) outside is connect with positive pole, and the iron anode (2) and nickel anode (14) are arranged alternately on graphite cake, and iron anode (2) and nickel anode (14) is provided with insulating materials, and iron anode (2) is in parallel with nickel anode (14).
4. the technique that a kind of electrodeposition process according to claims 1 prepares iron-nickel alloy foil, which is characterized in that the electricity Plating liquor includes following component (mass-volume concentration g/L):Nickel sulfate 80-100, nickel chloride 30-40, ferrous sulfate 40-100, Boric acid 20-40, polyethylene glycol 5-8, saccharin 5-40, surfactant 1-5.
5. the technique that a kind of electrodeposition process according to claims 4 prepares iron-nickel alloy foil, which is characterized in that the electricity Metal molybdenum powder 15-20g has been further included in plating liquor.
6. the technique that a kind of electrodeposition process according to claims 1 prepares iron-nickel alloy foil, which is characterized in that be electroplated Cheng Zhong, when electroplating solution volume is reduced, it is that 2.2-2.4 is then added to electroplating solution to be handled deionized water to pH with dilute sulfuric acid In, when electroplating solution pH value rises, pH is adjusted to zone of reasonableness with a concentration of 5% sulfuric acid and sodium hydroxide solution.
7. the technique that a kind of electrodeposition process according to claims 1 prepares iron-nickel alloy foil, which is characterized in that the iron Anode (2) and nickel anode (14) are tabular, width 5-6cm, thickness 0.6-1.2cm.
8. the technique that a kind of electrodeposition process according to claims 1 prepares iron-nickel alloy foil, which is characterized in that described to follow Loop system includes water circulating pump (7), return duct (6), reservoir (5) and filter (12), and electroplating solution passes through recirculated water successively Pump (7), return duct (6), reservoir (5) and filter (12) are re-entered into electrolytic cell (1).
CN201711454555.3A 2017-12-28 2017-12-28 The technique that a kind of electrodeposition process prepares iron-nickel alloy foil Pending CN108166024A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108914167A (en) * 2018-07-13 2018-11-30 安徽迈德福新材料有限责任公司 A kind of technique that electrodeposition process prepares invor alloy foil

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Publication number Priority date Publication date Assignee Title
CN1641072A (en) * 2004-01-15 2005-07-20 中南大学 Method for preparing Fe-Ni, Fi-Ni-Cr alloy foil
CN1793433A (en) * 2005-12-06 2006-06-28 钢铁研究总院 Process for preparing invor alloy foil
CN101660181A (en) * 2009-09-21 2010-03-03 菏泽天宇科技开发有限责任公司 Metal foil and manufacturing method and manufacturing device thereof
CN102839399A (en) * 2012-09-25 2012-12-26 中南大学 Preparation method of nanocrystal iron-nickel-chromium alloy foil by electrodeposition
CN103243356A (en) * 2012-10-11 2013-08-14 湖南理工学院 Preparation method of iron-nickel-cobalt-molybdenum alloy foil by electrodeposition
CN103726082A (en) * 2012-10-11 2014-04-16 湖南理工学院 Electrodeposition iron-nickel-molybdenum alloy foil composite electrolyte and preparation method
CN104818512A (en) * 2015-04-18 2015-08-05 北京工业大学 Device and method for preparing magnetically soft alloy continuous films through electric deposition of soluble separated anodes

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1641072A (en) * 2004-01-15 2005-07-20 中南大学 Method for preparing Fe-Ni, Fi-Ni-Cr alloy foil
CN1793433A (en) * 2005-12-06 2006-06-28 钢铁研究总院 Process for preparing invor alloy foil
CN101660181A (en) * 2009-09-21 2010-03-03 菏泽天宇科技开发有限责任公司 Metal foil and manufacturing method and manufacturing device thereof
CN102839399A (en) * 2012-09-25 2012-12-26 中南大学 Preparation method of nanocrystal iron-nickel-chromium alloy foil by electrodeposition
CN103243356A (en) * 2012-10-11 2013-08-14 湖南理工学院 Preparation method of iron-nickel-cobalt-molybdenum alloy foil by electrodeposition
CN103726082A (en) * 2012-10-11 2014-04-16 湖南理工学院 Electrodeposition iron-nickel-molybdenum alloy foil composite electrolyte and preparation method
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108914167A (en) * 2018-07-13 2018-11-30 安徽迈德福新材料有限责任公司 A kind of technique that electrodeposition process prepares invor alloy foil

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