CN104818512B - Device and method for preparing magnetically soft alloy continuous films through electric deposition of soluble separated anodes - Google Patents
Device and method for preparing magnetically soft alloy continuous films through electric deposition of soluble separated anodes Download PDFInfo
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- CN104818512B CN104818512B CN201510185230.4A CN201510185230A CN104818512B CN 104818512 B CN104818512 B CN 104818512B CN 201510185230 A CN201510185230 A CN 201510185230A CN 104818512 B CN104818512 B CN 104818512B
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Abstract
The invention provides a device and a method for preparing magnetically soft alloy continuous films through electric deposition of soluble separated anodes. Annular thin strips plated with titanium nitride on the surfaces of a stainless steel strip and a titanium strip serve as cathodes; soluble monometal anodes are separately arranged in parallel; branch anodes are dissolved to a scale through adjusting the current and the voltage of the branch anodes to achieve the balance between the cathode deposition quantity and the anode dissolution amount; and the content of metal ions in plating liquid is kept stable. The device and the method prevent the addition of a plating liquid supplementation metal ion device, effectively solve the problems of metal ion stability and regenerability of the plating liquid in continuous production, keep the stability of the metal content in continuous alloy plating layers, and are suitable for continuous production of magnetically soft alloy films.
Description
Technical field
The invention belongs to field of electrochemical deposition, more particularly, to a kind of solubility separation anodic electrodeposition prepares magnetically soft alloy
The device and method of continuous film.
Background technology
Magnetically soft alloy thin film is the magnetic material under low-intensity magnetic field with low-coercivity and high magnetic permeability.Soft magnetic materials is easy to
Magnetization, is also easy to demagnetize, is widely used in electrical equipment and electronic equipment, and in magnetic field shielding field.
Magnetically soft alloy preparation method has rolling, magnetron sputtering, electro-deposition, and the letter of iron-nickel alloy equipment is prepared in wherein electro-deposition
List, low cost, easy to operate.But during continuous electro-deposition iron nickel alloy film, because negative electrode constantly deposits consumption electricity
Metal ion in plating solution, causes concentration of metal ions in plating solution to reduce, in turn results in the imbalance of coated metal content ratio, make life
The continuous band component content of output is unstable.Current continuous electro-deposition equipment is supplemented in plating solution by added metal ion and subtracts
Few metal ion.United States Patent (USP) us5360525 and us4076597 describe a kind of method of supplementary metal ion, by
In acid, dissolving metal obtains metal ion, supplements metal ion in plating solution, and this method needs a large amount of strong acid dissolution metals, right
Environment, product and personal safety adversely affect.Meanwhile, according to Chinese patent cn100564606c continuous electrodepositing of metallic film
Devices and methods therefor is introduced, and after plating solution circulation plating a period of time, plating solution metal ion will decline, by variety classes gold
Belong to ion liquid supply device and plate metal ions liquid is supplemented to the electroplate liquid in electroplating bath, reach concentration of metal ions balance.However,
The method of this supplementary metal ion needs not stop to dissolve in liquid supply device various metallic salts, complex process and tediously long, if
Standby have high demands.
Content of the invention
For the technical problem overcoming existing continuous electro-deposition device to exist, the invention provides a kind of solubility separates sun
The device and method of magnetically soft alloy continuous film is prepared in pole electro-deposition.The technical scheme being adopted is: selects suitable negative electrode material
Material, using soluble anode, is separated by anode and is arranged in parallel, and adjusts electric current, the voltage of branch road anode, and then controlling brancher sun
The meltage of pole is equal to cathodic metal ion deposition amount, reaches negative electrode deposition and balances with anodic solution amount, keeps the gold of plating solution
Belong to that ion concentration is stable, produce the purpose of the stable continuous soft magnetic film of excellent performance, component content.
A kind of solubility separation anodic electrodeposition prepares the device of magnetically soft alloy continuous film, including the electricity accommodating electroplate liquid
Coating bath；Can be with the endless metal negative electrode of cycle rotation；Soluble anode；Supply unit；Transmission gear for electric motor；Circulating device, mistake
Filter device；Temperature control equipment；Stripping off device；Cleaning device；Passivating device；Drying unit；Tension force adjusting means and receipts
Winding apparatus it is characterised in that used in electrodeposition process negative electrode be surface titanium-nitride, the back side and electrical-insulation polymeric thin film
The annular strip that laminating forms the stainless steel band of insulating barrier, titanium band is formed.
Further, in electrodeposition process, anode material is pure iron, pure nickel, any two in pure cobalt, different metal anode structure
Composition is from anode, alternately arranged, and every kind of anode forms an assistant anode, and different metal anode is again in parallel to constitute comprehensive anode；
Separate anode by independent power supply or many power supplies, the electric current of different branch anode, voltage are adjustable.
Further it is characterised in that being provided with an ion between negative electrode and anode to pass through sexual isolation's film, this film and Ka band
It is arranged in parallel；Plating solution is made to pass through bottom horizontal flow sheet between sexual isolation's film in negative electrode and ion by circulating pump.
Prepare the method for magnetically soft alloy continuous film using described device it is characterised in that the annular of shuttling movement nitrogenizes
Ti cathode lower end is soaked in the plating solution, adjusts parallel branch soluble anode electric current, voltage, and controlling brancher anode presses coated metal ratio
Example dissolving, metal ion passes through mix homogeneously under sexual isolation's film and circulation pumping action in ion, deposits a lamination gold on negative electrode
Thin film, thin film winds after peeling off, clean, be passivated, drying becomes a useful person.
According to above-mentioned purpose, present invention employs following technical measures:
1. in order to produce continuous soft magnetic film it is desirable to be able to lower deposition layer easily be peeled off from Ka band, this is just
Require negative electrode band smooth surface clean and tidy, good corrosion resistance, coating fissility is good.It is 0.05～0.5mm that the present invention uses thickness
Ring stainless steel strip and annular titanium strip, in the titanium nitride film that one layer of 0.0005～0.05mm of its plated surface is thick, the back side and electricity
Insulating polymer film adhered formation insulating barrier.Ring stainless steel and titanium band are to be welded by band head and the tail, and commissure is deposited
In defect, coating is unlikely to be peel off.The purpose one of titanium-nitride is the defect in order to shelter endless belt weld seam, and two is on titanium nitride
Coating be more easily peelable than the coating on rustless steel, titanium.
2. the soluble anode material that the present invention uses is pure iron, pure nickel, pure cobalt, and different metal anode is arranged alternately in sun
In the groove of pole, insulant between two anode slots, is had to isolate.Different metal anode is connected in parallel simultaneously, adjusts ferrum in parallel circuit
The electric current of anode and nickel anode, voltage, just can control the dissolution velocity of different branch anode.In order to control parallel branch anode
Electric current, voltage, using two kinds of power supply modes, one kind uses independent power supply, setting electric current, voltage-regulation on parallel branch anode
Device, including slide rheostat and ammeter；Another kind of directly using two power supplys adjust respectively parallel branch anode electric current,
Voltage, makes the meltage of the first soluble anode be equal to this kind of metal deposition capability on negative electrode, the meltage of the second soluble anode
Equal to metal deposition capability this kind of on negative electrode.
3. the component content in alloy layer is mainly determined by solution composition, technological parameter.In order to obtain iron-holder 5%～
95% iron-nickel alloy coating, can be obtained by changing solution composition and technological parameter, the composition of electroplate liquid and parameter include:
Nickel sulfate 20～300g/l, ferrous sulfate 5g～120g/l, the boric acid of 20～60g/l, sodium citrate 5～50g/l, ascorbic acid
1g～15/l, sodium lauryl sulphate 0.1～0.5g/l, saccharin 1～5g/l, benzene sulfinic acid sodium salt 0.1～0.6g/l, butynediols
0.1～0.8g/l, ph are 1.5～4.5, and temperature is 20～65 DEG C, and electric current density is 1～100a/dm2.In order to obtain coating ferrum
The stable alloy firm of nickel content ratio, needs to keep each constituent concentration in above-mentioned plating solution to keep constant, this requires iron anode
Meltage be equal to the deposition of ferrum on negative electrode, the meltage of nickel anode is equal to the deposition of nickel on negative electrode.Parallel branch ferrum sun
Pole is 1:17～20:1 with the scope of the ratio of the electric current of nickel anode.
The computational methods of the ratio of parallel branch anode current are as follows:
wFirst soluble anodeThe mass fraction of the first soluble anode metal in coating
wSecond soluble anodeThe mass fraction of the second soluble anode metal in coating
rFirst soluble anodeThe electrochemical equivalent of the first soluble anode
rSecond soluble anodeThe electrochemical equivalent of the second soluble anode
4. in order to eliminate the plating solution localized metallic ion concentration difference causing during alternately arranged different metal anodic solution,
The present invention places an ion permeability isolating membrane parallel with Ka band between negative electrode and anode, and this film can pass through solubility
The metal ion of anodic solution, different metal ions mix homogeneously when ionic isolation film, and this film also has impurity screening
Effect.Make plating solution bottom horizontal flow sheet between Ka band and ion permeability isolating membrane using water circulating pump simultaneously, eliminate metal
The gas producing is taken away while ion concentration difference on negative electrode.
Brief description
Fig. 1 is the schematic device provided by the present invention for magnetically soft alloy thin film continuous electro-deposition
Fig. 2 is electroplating bath schematic diagram
Fig. 3 separates anode circuit schematic diagram in parallel for single supply
Fig. 4 separates anode circuit schematic diagram in parallel for dual power supply
Specific embodiment
Presently in connection with the drawings and specific embodiments, the present invention is elaborated:
A kind of magnetically soft alloy thin film continuous electro-deposition device, as shown in Figure 1, Figure 2, shown in Fig. 3, Fig. 4, wherein 1 is first
Support transfer roller, 4 be second support transfer roller, 5 be the 3rd support transfer roller, 6 be the 4th support transfer roller, 2 lead for graphite cathode
Electric roller, 3 is annular titanium nitride Ka band, and 7 is electroplating bath, and 8 is electroplating solution, and 9 is plating solution water inlet, and 10 is plating solution outlet,
11 is anode filter net, 12 ion permeability isolating membrane, and 13 is anode slot, and 14 is water circulating pump, and 15 is temperature control equipment, 16
For filter, 17 is coating stripper roll, and 21 is coating cleaning, passivating device, including cleanout fluid 18, reserving liquid tank 19, passivating solution 20
With support rotating roller, 22 is drying unit, and 23 is first pressure deflector roll, 24 is second pressure deflector roll, 25 is the 3rd pressure deflector roll,
26 is tension pick-up, and 27 is tension controller, and 28 is magnetic powder bonder, and 29 is wind-up roll, and 30 is graphite guide electroplax, and 31 is stone
Black contact rod, 32 first soluble anodes, 33 is the second soluble anode, and 34 is power lead, and 35 is electroplating power supply, and 36 is electricity
Stream, voltage regulating device.
With reference to Fig. 1, Fig. 2, Fig. 3 and Fig. 4, electroplating solution is injected in electroplating bath, and hollow cathode is enclosed within support transfer roller and makees
Electro-deposition negative electrode, Ka band lower end is immersed in electroplating solution it is ensured that Ka band lower end holding level.Anode is put in anode slot
Electric installation graphite cake, graphite rod, put into the first soluble anode, the second soluble anode, anode upper end add drainage screen and
Ion permeability isolating membrane, graphite roller is close to the negative pole of the upper surface connection power supply of hollow cathode band, anode conducting device
Connect positive source, between positive source and anode, be connected electric current, voltage regulating device.Open water circulating pump, temperature control fills
Put and filter, after a period of time, electroplating solution reaches design temperature.Open motor, arrange parameter, control cathode circulation
Velocity of rotation.Turn on the power, using the electric current of electric current, voltage regulating device regulation iron anode and nickel anode, voltage, on negative electrode
Electro-deposition one lamination gold plate, when alloy layer turns to stripper roll, peels off coating, then through Cleaning and Passivation device, drying
Device obtains the clean and tidy coating of drying, finally by tension control system, including pressure deflector roll, tension pick-up and tension force
Device controls membrane tension constant, crimps and become a useful person on magnetic powder bonder, the wrap-up of wind-up roll composition.Hollow cathode band circulates
Motion, soluble anode constantly dissolves supplementary metal ion, and coating is constantly peeled off, and curling is become a useful person, and material is thus formed continuous
Soft magnetic alloy sheet film strips material.
It is 0.05～0.5mm ring stainless steel strip and annular titanium strip that the present invention uses thickness, in one layer of its plated surface
The thick titanium nitride film of 0.0005～0.05mm, the back side and electrical-insulation polymeric film adhered formation insulating barrier, titanium-nitride purpose
To shelter the weld seam of endless belt and be more prone to peel off cladding portion and support deflector roll can soak in the plating solution, this require deflector roll not with
There is chemical attack and electrochemical reaction in plating solution, and under power on condition, endless metal belt can produce heat, and this will derivation
Roller have must heat resistance, in the present invention making deflector roll materials'use politef.Motor and support ring
One support rotating roller of shape negative electrode is connected.
Do negative electrode conducting medium using the good graphite roller of electric conductivity, the position of graphite roller can be with up-down adjustment it is ensured that stone
Ink roller surface is fitted closely with Ka band upper surface, and graphite roller surface polishes, and occurs Ka band will not be caused during relative motion
Scratch, add a carbon brush in graphite roller one end, power cathode is connected to cathodal closing with carbon brush.
Anode conducting device is made up of graphite cake and graphite rod, and graphite rod and graphite cake one is connected it is ensured that well conducting,
Other end is extended to and is connected with positive source outside coating bath, and the solubility first anode and second plate are arranged alternately in graphite cake
On, it is immersed in electroplating solution.
Impurity in order to stop anodic solution from producing enters coating, adds terylene drainage screen, and following between anode and cathode
Add a filter in loop systems plating solution is filtered, periodically defecator is cleared up.Add one in blood circulation
Temperature control equipment keeps bath temperature constant, adds heater, thermocouple in a reserving liquid tank, heater and thermocouple with
Temperature controller is connected, and sets and adjust temperature value on temperature controller.
Anode cathode separation can be adjusted between 5mm～100mm, because soluble anode dissolving causes plating solution to go out cash
Belong to ion local concentration difference, between a cathode and an anode plus an ion permeability isolating membrane, different metal ions are through ion
Mix homogeneously during permeability isolating membrane.
Water circulating pump makes plating solution bottom horizontal flow sheet between anode and cathode, liquid flow direction and hollow cathode direction of motion phase
Instead, plating solution and negative electrode speed of related movement are increased.Eliminate bath concentration difference, take away simultaneously on negative electrode produce purge of gas,
Passivating device is made up of support rotating roller, reserving liquid tank, cleanout fluid and passivating solution, primarily to cleaning coating surface residual
Plating solution, forms layer protecting film in coating surface, and drying unit is that the liquid to coating surface residual carries out drying and processing.
By adjusting motor state modulator coiled material rolling speed, with the increase of coil thickness, coiled material pulling tension
Increase, tension force too conference causes Film Tear, present invention uses a set of tension control system, including tension sensing device, open
Force controller, magnetic powder bonder, through tension sensing device, tension change is reacted on tension controller alloy firm, tension force
Controller changes the function of current on the magnetic powder bonder being connected with wind-up roll, and electric current changes, and the torque of magnetic powder bonder changes,
Thus changing rolling speed, become a useful person in wind-up roll curling.
Example:
Electroplate liquid forms: the nickel sulfate of 78g/l.The ferrous sulfate of 9g/l, the boric acid of 40g/l, sodium citrate 20g/l, resist
Bad hematic acid 5g/l, sodium lauryl sulphate 0.2g/l, saccharin 3g/l, benzene sulfinic acid sodium salt 0.3g/l, butynediols 0.5g/l
(1) electroplating iron-nickel alloy solution is prepared
1. add the deionized water of about 70% volume in the cleaning coating bath for 8l for the capacity, be heated to 55 DEG C.
2. nickel sulfate and the sodium chloride of amount of calculation, stirring and dissolving are added.
3. in independent container, with the boric acid of more than 90 DEG C of deionized water dissolving amount of calculation, every kilogram of boric acid with 4～
6kg deionized water dissolving.
4. the sodium citrate of amount of calculation, stirring and dissolving are added.
5. the ferrous sulfate of amount of calculation, stirring and dissolving are added.
6. the saccharin of addition amount of calculation, ascorbic acid, benzene sulfinic acid sodium salt, butynediols, stirring and dissolving, plus deionized water is extremely
Volume required.
7. adjust ph value to 2.5 with 5% dilute sulfuric acid.
(2) by the annular titanium nitride cathode sheath for 50mm for the width on support rotating roller, graphite guide roller is installed and is close to the moon
Pole outer surface, anode conducting device is put in anode slot, grows the generous soluble iron anode for 100mm*50mm*10mm and nickel
Anode is alternately arranged to be placed on anode conducting device, Anode-cathode Distance 35mm.
(3) open water circulating pump, regulation pump capacity is 13l/min；Open attemperating unit, adjust temperature and be 55 DEG C；Open
Open defecator.After a period of time, electroplating solution reaches 55 DEG C.
(4) open high frequency electroplating power supply, setting cathode-current density is 3.5a/dm2, adjust the electricity of iron anode and nickel anode
Flow ratio is 1:5.5.Static plating a period of time, coating is enable to peel off.
(5) motor is connected with support roller, opens motor, arrange parameter, so that hollow cathode is rotated with 2m/h speed.
(6) when coating reaches stripper roll, peel off coating, coating is done after over cleaning, passivating device, drying unit
Dry clean and tidy coating, eventually passes a control device and adjusts rolling speed, wind and become a useful person on wrap-up.
Using the method for solubility separation anodic electrodeposition magnetically soft alloy continuous film of the present invention, prepare nickel content 85%
Alloy continuous film, alloy firm width is 50mm, and thickness is 20 μm, and in 0.7t, hardness is 460hv to saturation magnetization.
Claims (3)
1. a kind of solubility separation anodic electrodeposition prepares the device of magnetically soft alloy continuous film, including the plating accommodating electroplate liquid
Groove；Can be with the endless metal negative electrode of cycle rotation；Soluble anode；Supply unit；Transmission gear for electric motor；Circulating device, filtration
Device；Temperature control equipment；Stripping off device；Cleaning device；Passivating device；Drying unit；Tension force adjusting means and winding
Device it is characterised in that used in electrodeposition process negative electrode be surface titanium-nitride, the back side and electrical-insulation polymeric thin film paste
Close stainless steel band, the annular strip of titanium band formation forming insulating barrier；
In electrodeposition process, anode material is pure iron, pure nickel, any two in pure cobalt, and different metal anode constitutes and separates anode,
Alternately arranged, every kind of anode forms an assistant anode, and different metal anode is again in parallel to constitute comprehensive anode；Separate anode to pass through
Individually power supply or many power supplies, the electric current of different branch anode, voltage are adjustable.
2. device according to claim 1 passes through sexual isolation it is characterised in that being provided with an ion between negative electrode and anode
Film, this film and Ka band are arranged in parallel；Plating solution is made to pass through bottom horizontal flow sheet between sexual isolation's film in negative electrode and ion by circulating pump.
3. a kind of using the device described in claim 1 or 2 prepare magnetically soft alloy continuous film method it is characterised in that circulation
The annular nitridation Ti cathode lower end of motion is soaked in the plating solution, adjusts parallel branch soluble anode electric current, voltage, controlling brancher sun
Pole is dissolved in coated metal ratio, and metal ion passes through mix homogeneously under sexual isolation's film and circulation pumping action in ion, in negative electrode
Upper deposition one lamination gold thin film, thin film winds after peeling off, clean, be passivated, drying becomes a useful person.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510185230.4A CN104818512B (en) | 2015-04-18 | 2015-04-18 | Device and method for preparing magnetically soft alloy continuous films through electric deposition of soluble separated anodes |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510185230.4A CN104818512B (en) | 2015-04-18 | 2015-04-18 | Device and method for preparing magnetically soft alloy continuous films through electric deposition of soluble separated anodes |
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| CN104818512B true CN104818512B (en) | 2017-01-25 |
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| CN106702468B (en) * | 2016-12-30 | 2021-05-28 | 北京工业大学 | Method for efficiently and continuously preparing metal film by equipotential vertical full-immersion cathode |
| CN108103533A (en) * | 2017-12-28 | 2018-06-01 | 安徽迈德福新材料有限责任公司 | The technique that a kind of electrodeposition process prepares nickel foil |
| CN108166024A (en) * | 2017-12-28 | 2018-06-15 | 安徽迈德福新材料有限责任公司 | The technique that a kind of electrodeposition process prepares iron-nickel alloy foil |
| CN109735880A (en) * | 2019-03-04 | 2019-05-10 | 深圳市汇美新科技有限公司 | A kind of ultrathin film electrochemical deposition system |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US4076579A (en) * | 1973-08-06 | 1978-02-28 | The Regents Of The University Of California | Pulping of lignocellulosic material by sequential treatment thereof with nitric oxide and oxygen |
| JPS61291992A (en) * | 1985-06-20 | 1986-12-22 | Nippon Steel Corp | Plating method for controlling anodic electric conduction oxidation in iron series alloy plating |
| US5360525A (en) * | 1993-03-16 | 1994-11-01 | United Foils Inc. | Apparatus for making metal foil |
| CN100564606C (en) * | 2005-12-06 | 2009-12-02 | 安泰科技股份有限公司 | Apparatus for continuous electrodepositing of metallic film and method thereof |
| CN103031578B (en) * | 2012-11-29 | 2016-08-31 | 烟台晨煜电子有限公司 | A kind of electrolytic method producing nickel foil |
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