CN104818512A - 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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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, particularly relate to the device and method that a kind of solubility separation anodic electrodeposition prepares non-retentive alloy continuous film.
Background technology
Non-retentive alloy film is the magneticsubstance under low-intensity magnetic field with low-coercivity and high magnetic permeability.Soft magnetic materials is easy to magnetization, is also easy to demagnetization, is widely used in electrical equipment and electronics, and in magnetic field shielding field.
Non-retentive alloy preparation method has rolling, magnetron sputtering, galvanic deposit, wherein galvanic deposit prepare that iron-nickel alloy equipment is simple, cost is low, easy to operate.But in continuous electro-deposition iron nickel alloy film process, due to the metal ion in the continuous deposition consumes electroplate liquid of negative electrode, cause concentration of metal ions in plating solution to reduce, and then cause coated metal content ratio to lack of proper care, make the continuous band component content instability produced.Current continuous electro-deposition equipment supplements the metal ion reduced in plating solution by added metal ion.US Patent No. 5360525 and US4076597 describe a kind of method of supplementary metal ion, metal ion is obtained by dissolution of metals in acid, in plating solution, supplement metal ion, this method needs a large amount of strong acid dissolution metal, has disadvantageous effect to environment, product and personnel safety.Simultaneously, according to Chinese patent CN100564606C apparatus for continuous electrodepositing of metallic film and method introduction thereof, when after plating solution circulation plating for some time, plating solution metal ion will decline, by dissimilar metals ion liquid supply device, plate metal ions liquid is supplemented to the electroplate liquid in plating tank, reach concentration of metal ions balance.But the method for this supplementary metal ion needs not stop to dissolve various metallic salt in liquid supply device, complex process and tediously long, equipment requirements is high.
Summary of the invention
In order to overcome the technical problem that existing continuous electro-deposition device exists, the invention provides the device and method that a kind of solubility separation anodic electrodeposition prepares non-retentive alloy continuous film.The technical scheme adopted is: select suitable cathode material, use soluble anode, be separated by anode and be arranged in parallel, regulate electric current, the voltage of branch road anode, and then the meltage of controlling brancher anode equals cathodic metal ion deposition amount, reach cathodic deposition amount and anode dissolution amount balances, keep the metal ion content of plating solution to stablize, produce the object of the stable continuous soft magnetic film of excellent performance, component content.
Solubility is separated the device that anodic electrodeposition prepares non-retentive alloy continuous film, comprises the plating tank holding electroplate liquid; Can the endless metal negative electrode of cycle rotation; Soluble anode; Supply unit; Transmission gear for electric motor; Circulation device, filtration unit; Temperature-control device; Stripping off device; Washing unit; Passivating device; Drying unit; Tension control setting device and wrap-up, is characterized in that the negative electrode used in electrodeposition process is plated surface titanium nitride, the annular strip that the Stainless Steel Band of the back side and electrical-insulation polymeric film adhered formation insulation layer, titanium band are formed.
Further, in electrodeposition process, anode material is any two in pure iron, pure nickel, pure cobalt, and different metal anode forms and is separated anode, is alternately arranged, often kind of anodic formation assistant anode, and different metal anode is in parallel again forms comprehensive anode; Be separated anode by independent power supply or many Energy control, electric current, the voltage of different branch anode are adjustable.
Further, it is characterized in that being provided with an ion between negative electrode and anode by sexual isolation film, this film and Ka band are arranged in parallel; Plating solution horizontal flow between negative electrode and ion are by sexual isolation film is made by recycle pump.
Device described in utilization prepares the method for non-retentive alloy continuous film, it is characterized in that the annular titanium nitride negative electrode lower end leaching of cyclic motion in the plating solution, regulate parallel branch soluble anode electric current, voltage, controlling brancher anode dissolves in coated metal ratio, metal ion mixes under ion is by sexual isolation film and recycle pump effect, negative electrode deposits one deck alloy firm, and film rolling after stripping, cleaning, passivation, oven dry is become a useful person.
According to above-mentioned purpose, present invention employs following technical measures:
1. in order to produce continuous print soft magnetic film, needs easily can peel off lower deposition layer from Ka band, and this just requires that Ka band material smooth surface is clean and tidy, and good corrosion resistance, coating separability is good.The present invention uses thickness to be 0.05 ~ 0.5mm ring stainless steel strip and annular titanium strip, at the titanium nitride film that its plated surface one deck 0.0005 ~ 0.05mm is thick, and the back side and the film adhered formation insulation layer of electrical-insulation polymeric.Ring stainless steel and titanium band are welded by band head and the tail, and commissure existing defects, coating is not easy to peel off.The object one of titanium-nitride is the defect in order to shelter endless belt weld seam, and two is that coating on titanium nitride is easier than the coating on stainless steel, titanium strips down.
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 anode slot, has insulating material to isolate between two anode slots.Different metal anode is connected in parallel simultaneously, regulates electric current, the voltage of iron anode and nickel anode in shunt circuit, just can control the dissolution rate of different branch anode.In order to control electric current, the voltage of parallel branch anode, use two kinds of power supply modes, the independent power supply of a kind of use, parallel branch anode arranges electric current, voltage regulating device, comprises slide rheostat and reometer; Another kind of directly use two power supplys regulate electric current, the voltage of parallel branch anode respectively, and make the meltage of the first soluble anode equal this kind of metal deposition capability on negative electrode, the meltage of the second soluble anode equals this kind of metal deposition capability on negative electrode.
3. the component content in alloy layer determines primarily of solution composition, processing parameter.In order to obtain the iron-nickel alloy coating of iron-holder 5% ~ 95%, can be obtained by change solution composition and processing parameter, composition and the parameter of electroplate liquid comprise: single nickel salt 20 ~ 300g/L, ferrous sulfate 5g ~ 120g/L, the boric acid of 20 ~ 60g/L, Trisodium Citrate 5 ~ 50g/L, xitix 1g ~ 15/L, sodium lauryl sulphate 0.1 ~ 0.5g/L, asccharin 1 ~ 5g/L, benzene sulfinic acid sodium salt 0.1 ~ 0.6g/L, butynediol 0.1 ~ 0.8g/L, pH is 1.5 ~ 4.5, and temperature is 20 ~ 65 DEG C, and current density is 1 ~ 100A/dm
2.In order to obtain the stable alloy firm of coating iron nickel content ratio, need to keep each constituent concentration in above-mentioned plating solution to remain unchanged, this just requires that the meltage of iron anode equals the deposition of iron on negative electrode, and the meltage of nickel anode equals the deposition of nickel on negative electrode.Parallel branch iron anode is 1:17 ~ 20:1 with the scope of the ratio of the electric current of nickel anode.
The method of calculation of the ratio of parallel branch anodic current are as follows:
W
first soluble anodethe massfraction of the first soluble anode metal in-coating
W
second soluble anodethe massfraction of the second soluble anode metal in-coating
R
first soluble anodethe electrochemical equivalent of the-the first soluble anode
R
second soluble anodethe electrochemical equivalent of the-the second soluble anode
4. the plating solution localized metallic ionic concn difference in order to cause when eliminating the different metal anode dissolution be alternately arranged, the present invention places an ion permeability barrier film parallel with Ka band between negative electrode and positive electrode, the metal ion that this film can dissolve through soluble anode, different metal ion mixes through ionic isolation film, and this film also has the effect of impurity screening.Use water circulating pump to make plating solution horizontal flow between Ka band and ion permeability barrier film simultaneously, while eliminating concentration of metal ions difference, take away the gas that negative electrode produces.
Accompanying drawing explanation
Fig. 1 is the device schematic diagram for non-retentive alloy film continuous electro-deposition provided by the invention
Fig. 2 is plating tank schematic diagram
Fig. 3 is that single supply is separated plate circuit schematic diagram in parallel
Fig. 4 is that dual power supply is separated plate circuit schematic diagram in parallel
Embodiment
With specific embodiment, the present invention is elaborated by reference to the accompanying drawings now:
A kind of non-retentive alloy film continuous electro-deposition device, as Fig. 1, Fig. 2, Fig. 3, shown in Fig. 4, wherein 1 is the first support transfer roller, 4 is the second support transfer roller, 5 is the 3rd support transfer roller, 6 is the 4th support transfer roller, 2 is graphite cathode conductive rollers, 3 is annular titanium nitride Ka band, 7 is plating tank, 8 is electroplating solution, 9 is plating solution water-in, 10 is plating solution water outlet, 11 is anode filter net, 12 ion permeability barrier films, 13 is anode slot, 14 is water circulating pump, 15 is temperature-control device, 16 is strainer, 17 is coating stripper roll, 21 is coating cleaning, passivating device, comprise scavenging solution 18, liquid-storing box 19, passivating solution 20 and support rotating roller, 22 is drying unit, 23 is the first pressure deflector roll, 24 is the second pressure deflector roll, 25 is the 3rd pressure deflector roll, 26 is tension pick-up, 27 is tension controller, 28 is magnetic coupling mechanism, 29 is wind-up roll, 30 is graphite guide electroplax, 31 is graphite guide torch, 32 first soluble anodes, 33 is the second soluble anode, 34 is power lead, 35 is electroplating power supply, 36 is electric current, voltage regulating device.
With reference to figure 1, Fig. 2, Fig. 3 and Fig. 4, electroplating solution is injected in plating tank, and hollow cathode is enclosed within support transfer roller and makes galvanic deposit negative electrode, and Ka band lower end is immersed in electroplating solution, ensures that Ka band lower end keeps level.Anode conducting device graphite cake, graphite rod is put in anode slot, put into the first soluble anode, the second soluble anode, filtering net and ion permeability barrier film is added in anode upper end, graphite roller is close to the negative pole of the upper surface connection power supply of hollow cathode band, anode conducting device connects positive source, is connected electric current, voltage regulating device between positive source with anode.Open water circulating pump, temperature-control device and strainer, after for some time, electroplating solution reaches design temperature.Open stepper-motor, parameters, control cathode cycle rotation speed.Opening power, electric current, voltage regulating device is used to regulate electric current, the voltage of iron anode and nickel anode, at negative electrode substrates one deck alloy layer, when alloy layer turns to stripper roll, peel off coating, then obtain dry clean and tidy coating, finally by tension control system through Cleaning and Passivation device, drying unit, comprising pressure deflector roll, tension pick-up and tension controller, to control memberane stress constant, and the wrap-up of magnetic coupling mechanism, wind-up roll composition is curlingly become a useful person.Hollow cathode band cyclic motion, soluble anode constantly dissolves supplementary metal ion, and coating is constantly peeled off, and curlingly becomes a useful person, and material is thus formed continuous print non-retentive alloy film strip material.
The present invention uses thickness to be 0.05 ~ 0.5mm ring stainless steel strip and annular titanium strip, at the titanium nitride film that its plated surface one deck 0.0005 ~ 0.05mm is thick, the back side and the film adhered formation insulation layer of electrical-insulation polymeric, titanium-nitride object be shelter endless belt weld seam and be more prone to peel off cladding portion support deflector roll can soak in the plating solution, this will differentiate roller not with plating solution generation chemical corrosion and electrochemical reaction, and under power on condition, endless metal belt can produce heat, this will differentiate roller have must resistance toheat, the tetrafluoroethylene of the materials'use of the making deflector roll in the present invention.Stepper-motor is connected with the support rotating roller supporting hollow cathode.
The good graphite roller of electroconductibility is used to do cathode guide dielectric medium, the position of graphite roller can up-down adjustment, ensure that graphite roller surface is fitted closely with Ka band upper surface, graphite roller surface finish, scuffing can not be caused by anticathode band when there is relative movement, 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, graphite rod is connected with graphite cake one, and guarantee that conduction is good, other end extends to outside coating bath and is connected with positive source, the solubility first anode and second anode are arranged alternately on graphite cake, are immersed in electroplating solution.
The impurity produced to stop anode dissolution enters coating, adds terylene filtering net between anode and cathode, and in the recycle system, adds a strainer filter plating solution, regularly clears up filtration unit.In the recycle system, add a temperature-control device keeps bath temperature constant, and in a liquid-storing box, add well heater, thermopair, well heater is connected with temperature regulator with thermopair, setting and adjustment temperature value on temperature regulator.
Anode cathode separation can regulate between 5mm ~ 100mm, plating solution is caused to occur metal ion partial concn difference because soluble anode dissolves, add an ion permeability barrier film between a cathode and an anode, different metal ion mixes through ion permeability barrier film.
Water circulating pump makes plating solution horizontal flow between anode and cathode, and liquid flow direction is contrary with hollow cathode direction of motion, strengthens plating solution and negative electrode speed of relative movement.Eliminate bath concentration difference; take away purge of gas, passivating device that negative electrode produces to be made up of support rotating roller, liquid-storing box, scavenging solution and passivating solution simultaneously; mainly in order to clean the residual plating solution of coating surface; form layer protecting film at coating surface, drying unit is that the liquid residual to coating surface carries out drying and processing.
By regulating stepper-motor state modulator coiled material rolling speed, along with the increase of coil thickness, coiled material pulling tension increases, tension force too conference causes Film Tear, present invention uses a set of tension control system, comprise tension sensing device, tension controller, magnetic coupling mechanism, alloy firm is through tension sensing device, tension change is reacted on tension controller, tension controller changes galvanic action on the magnetic coupling mechanism be connected with wind-up roll, and electric current changes, and the torque of magnetic coupling mechanism changes, thus change rolling speed, become a useful person wind-up roll is curling.
Example:
Electroplate liquid forms: the single nickel salt of 78g/L.The ferrous sulfate of 9g/L, the boric acid of 40g/L, Trisodium Citrate 20g/L, xitix 5g/L, sodium lauryl sulphate 0.2g/L, asccharin 3g/L, benzene sulfinic acid sodium salt 0.3g/L, butynediol 0.5g/L
(1) electroplating iron-nickel alloy solution preparation
1. be the deionized water adding about 70% volume in the clean coating bath of 8L at capacity, be heated to 55 DEG C.
2. single nickel salt and the sodium-chlor of calculated amount is added, stirring and dissolving.
3. in independent container, with the boric acid of the deionized water dissolving calculated amount of more than 90 DEG C, every kilogram of boric acid 4 ~ 6kg deionized water dissolving.
4. the Trisodium Citrate of calculated amount is added, stirring and dissolving.
5. the ferrous sulfate of calculated amount is added, stirring and dissolving.
6. add the asccharin of calculated amount, xitix, benzene sulfinic acid sodium salt, butynediol, stirring and dissolving, add deionized water to volume required.
7. use the dilute sulphuric acid adjust ph of 5% to 2.5.
(2) be that the annular titanium nitride cathode sheath of 50mm is on support rotating roller by width, graphite guide roller is installed and is close to cathode outer surface, anode conducting device is put into anode slot, the thick soluble iron anode for 100mm*50mm*10mm of length and width and nickel anode are alternately arranged and are placed on anode conducting device, Anode-cathode Distance 35mm.
(3) open water circulating pump, adjustment pump capacity is 13L/min; Open temperature control unit, regulate temperature to be 55 DEG C; Open filtration unit.After for some time, electroplating solution reaches 55 DEG C.
(4) open high frequency electroplating power supply, arranging cathode current density is 3.5A/dm
2, the current ratio regulating iron anode and nickel anode is 1:5.5.Static plating for some time, coating is peeled off.
(5) stepper-motor is connected with supporting roll, opens motor, parameters, hollow cathode is rotated with 2m/h speed.
(6) when coating arrives stripper roll, peel off coating, coating obtains dry clean and tidy coating after cleaning, passivating device, drying unit, and eventually pass a control device and regulate rolling speed, on wrap-up, rolling is become a useful person.
Adopt solubility of the present invention to be separated the method for anodic electrodeposition non-retentive alloy continuous film, prepare the alloy continuous film of nickel content 85%, alloy firm width is 50mm, and thickness is 20 μm, and saturation magnetization is at 0.7T, and hardness is 460Hv.
Claims (4)
1. solubility is separated the device that anodic electrodeposition prepares non-retentive alloy continuous film, comprises the plating tank holding electroplate liquid; Can the endless metal negative electrode of cycle rotation; Soluble anode; Supply unit; Transmission gear for electric motor; Circulation device, filtration unit; Temperature-control device; Stripping off device; Washing unit; Passivating device; Drying unit; Tension control setting device and wrap-up, is characterized in that the negative electrode used in electrodeposition process is plated surface titanium nitride, the annular strip that the Stainless Steel Band of the back side and electrical-insulation polymeric film adhered formation insulation layer, titanium band are formed.
2. device according to claim 1, is characterized in that in electrodeposition process, and anode material is any two in pure iron, pure nickel, pure cobalt, different metal anode forms separation anode, be alternately arranged, often kind of anodic formation assistant anode, different metal anode is in parallel again forms comprehensive anode; Be separated anode by independent power supply or many Energy control, electric current, the voltage of different branch anode are adjustable.
3. device according to claim 1 and 2, it is characterized in that being provided with an ion between negative electrode and anode by sexual isolation film, this film and Ka band are arranged in parallel; Plating solution horizontal flow between negative electrode and ion are by sexual isolation film is made by recycle pump.
4. the method utilizing the device described in claim 2 or 3 to prepare non-retentive alloy continuous film, it is characterized in that the annular titanium nitride negative electrode lower end leaching of cyclic motion in the plating solution, regulate parallel branch soluble anode electric current, voltage, controlling brancher anode dissolves in coated metal ratio, metal ion mixes under ion is by sexual isolation film and recycle pump effect, negative electrode deposits one deck alloy firm, and film rolling after stripping, cleaning, passivation, oven dry is become a useful person.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106702468A (en) * | 2016-12-30 | 2017-05-24 | 北京工业大学 | Method for efficiently and continuously preparing metal film by vertically and completely immersing negative pole in equipotential mode |
| 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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| CN103031578A (en) * | 2012-11-29 | 2013-04-10 | 烟台晨煜电子有限公司 | Electrolysis method for producing nickel foil |
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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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106702468A (en) * | 2016-12-30 | 2017-05-24 | 北京工业大学 | Method for efficiently and continuously preparing metal film by vertically and completely immersing negative pole in equipotential mode |
| 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 |
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| 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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