CN102995085B - Method for producing roughened nickel foil by electrolytic process - Google Patents

Method for producing roughened nickel foil by electrolytic process Download PDF

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CN102995085B
CN102995085B CN201210499727.XA CN201210499727A CN102995085B CN 102995085 B CN102995085 B CN 102995085B CN 201210499727 A CN201210499727 A CN 201210499727A CN 102995085 B CN102995085 B CN 102995085B
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nickel
alligatoring
nickel foil
electrolyzer
treatment
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CN102995085A (en
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刘言清
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Shandong Yongshen Electronic Technology Co ltd
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YANTAI CHENYU ELECTRONICS CO Ltd
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Abstract

The invention relates to a method for producing a roughened nickel foil by an electrolytic process, which is applied to the field of electrolytic process production of the nickel foil. The method comprises the steps of 1, selecting a semi-bright nickel foil as a base material of the roughened nickel foil, carrying out activating treatment on the semi-bright nickel foil; 2, putting the activated semi-bright nickel foil in the step 1 into a roughened electrolytic cell formed by 18-25g/L of nickel sulfate and 21-23g/L of ammonium sulfate, electrifying the cathode and the anode of the roughened electrolytic cell, and carrying out roughening treatment on the roughened electrolytic cell; 3, putting the roughened nickel foil in the step 2 into a curing electrolytic cell of solution formed by 200-250g/L of nickel sulfate, 40-45g/L of boric acid and 40g/L of nickel chloride, electrifying the cathode and the anode of the curing electrolytic cell, and carrying out curing treatment; and 4, drying the nickel foil cured in the step 3. The process is fewer in selected material varieties, simple to operate and easy to achieve, and the produced nickel foil is high in accuracy and good in ductibility.

Description

A kind of method of electrolytic process production alligatoring nickel foil
Technical field
The present invention relates to a kind of method of electrolytic process production alligatoring nickel foil, be applied to the electrolytic process production field of nickel foil.
Background technology
The technician of electroplating industry knows, ensure stability and the persistence of coating on base material, only leans on single alligatoring to be far from being enough.Therefore, must send and the alligatoring coating plated is enclosed in firmly on (or solid exist) coating with electric current
Summary of the invention
Technical problem to be solved by this invention is to provide a kind ofly chooses the few and method of electrolytic process production alligatoring nickel foil simple to operate of raw material type, and it can overcome prior art and produces complicated defect and obtain that a kind of surfaceness is large, antistripping good and the alligatoring nickel foil that ductility is good.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of method of electrolytic process production alligatoring nickel foil, comprises the following steps:
Step one: choose the base material of semi-bright nickel paper tinsel as alligatoring nickel foil, and activation treatment is carried out to described semi-bright nickel paper tinsel;
Step 2: the described semi-bright nickel paper tinsel after process activated described in step one is placed in be made up of the single nickel salt of 18 ~ 25g/L and the ammonium sulfate of 21 ~ 23g/L and pH value is the alligatoring electrolyzer of the solution of 3.5 ~ 4.5, to the negative electrode of described alligatoring electrolyzer and anodal closure, carry out roughening treatment at described alligatoring electrolyzer;
Step 3: the nickel foil in step 2 after roughening treatment is placed in be made up of the single nickel salt of 200g/L ~ 250g/L and the boric acid of 40 ~ 45g/L and 40g/L nickelous chloride and pH value is the solidification electrolyzer of the solution of 4 ~ 4.5, to the negative electrode of described solidification electrolyzer and anodal closure, be cured process;
Step 4: the nickel foil after solidification treatment described in step 3 is dried.
The invention has the beneficial effects as follows: first, the lower positively charged of sulphur content of semi-bright nickel paper tinsel, as easy as rolling off a logly on it cross the high electronegative nickel dam of last layer sulphur content, and in conjunction with effective, should not peel off; Its deuterzooid technique to choose raw material type few, simple to operate being easy to realizes; The nickel foil precision that production obtains is high and ductility good.
On the basis of technique scheme, the present invention can also do following improvement.
Further, the activation treatment in described step one is that the hydrochloric acid being 20 ~ 25g/L by the described semi-bright nickel paper tinsel activation solution chosen carries out chemical corrosion process to its surface.Described activation solution is the hydrochloric acid of 22g/L.
Adopt the beneficial effect of above-mentioned further scheme to be by chemical corrosion surface treatment, nickel foil base material is activated, is easy to the carrying out of the alligatoring in step 2.
Further, the solution temperature in described step 2 during roughening treatment in described alligatoring electrolyzer controls at 29 DEG C ~ 31 DEG C, and pH value maintains 3.8 ~ 4.0 simultaneously.Passing to current density in the coarsening process of described step 2 is 28A/dm 2electric current carry out electrolysis.
Further, described alligatoring electrolyzer adopts titanium plate as anode, and described solidification electrolyzer adopts titanium plate or nickel as anode.When solidifying electrolyzer and using nickel as anode, sulfur-bearing nickel cake or nickel foil offal are placed in titanium frame as anode.
The beneficial effect of above-mentioned further scheme is adopted to be replace to use stainless steel, chlorion is especially strong to Corrosion of Stainless Steel, and stainless steel can be made to separate out hexavalent chromium, thus cause systemic contamination to affect quality of coating, time serious (when content surpasses 0.01g/L) coating uniformity and covering power can be had a strong impact on, cause the problems such as coating peeling, decortication.And adopt Ni―Ti anode can avoid above problem.And use sulfur-bearing nickel cake or nickel foil offal, decrease the pollution of cupric ion, and take full advantage of nickel foil offal waste product, cost-saving.
Further, passing to current density in the solidification process of described step 3 is 12A/dm 2electric current carry out electrolysis.
Further, the bake out temperature in described step 4 controls at 50 ~ 70 DEG C.
The beneficial effect of above-mentioned further scheme is adopted to be that the resistance of the nickel foil of gained is low, effective.
Further, described step 2 and three alligatoring, be solidificated in plating the ascent stage all reduce primary current and adopt current density 1.5 ~ 2A/dm 2small area analysis carry out coating envelope point process.
Adopt the beneficial effect of above-mentioned further scheme to be adopt the process of small area analysis envelope point, make coating firm, strengthen the bonding force of coating.
Further, electrolyzer backflow place respectively in activation treatment, roughening treatment, solidification treatment three processes passes to 0.1A/dm 2~ 0.2A/dm 2direct current carry out impurity and purification process.
The beneficial effect of above-mentioned further scheme is adopted to be that System Solution purifies by reasonable foreign ion of removing.
Embodiment
Example, only for explaining the present invention, is not intended to limit scope of the present invention.
The present invention includes following steps:
Step one: choose the base material of semi-bright nickel paper tinsel as alligatoring nickel foil, and activation treatment is carried out to described semi-bright nickel paper tinsel; Activation treatment: usually by mechanical process or chemical process, workpiece surface is processed (mechanical grinding or small area analysis corrosion).What this technique adopted is only the most simply fill a prescription, and need not carry out the small area analysis etch of Yin/Yang pole, just carry out common pre-erosion i.e. the chemical etching known to electroplating work procedure technician.
Step 2: the described semi-bright nickel paper tinsel after process activated described in step one is placed in be made up of the single nickel salt of 18 ~ 25g/L and the ammonium sulfate of 21 ~ 23g/L and pH value is the alligatoring electrolyzer of the solution of 3.5 ~ 4.5, to the negative electrode of described alligatoring electrolyzer and anodal closure, passing to current density is 28A/dm 2electric current carry out electrolysis.Roughening treatment is carried out at described alligatoring electrolyzer; Roughening treatment: by the process of electrolysis nickel plating on Ni-based paper tinsel.
Step 3: the nickel foil in step 2 after roughening treatment is placed in be made up of the single nickel salt of 200g/L ~ 250g/L and the boric acid of 40 ~ 45g/L and 40g/L nickelous chloride and pH value is the solidification electrolyzer of the solution of 4 ~ 4.5, to the negative electrode of described solidification electrolyzer and anodal closure, be cured process; Solidification treatment: by electrolysis nickel plating on the Ni-based paper tinsel of alligatoring again, strengthens the power that be combined with each other of nickel layer and Ni-based paper tinsel.
Step 4: dried by the nickel foil after solidification treatment described in step 3, bake out temperature controls at 50 ~ 70 DEG C.
Alligatoring, be solidificated in plating the ascent stage all reduce primary current and adopt current density 1.5 ~ 2A/dm 2small area analysis carry out coating envelope point process.When after the process of employing small area analysis envelope point, coating can be made firmer, strengthen the bonding force of coating.Activation treatment in described step one is that the hydrochloric acid being 20 ~ 25g/L by the described semi-bright nickel paper tinsel activation solution chosen carries out chemical corrosion process to its surface.The hydrochloric acid of described activation solution optimal choice 22g/L.By chemical corrosion surface treatment, nickel foil base material is activated, is easy to the carrying out of the alligatoring in step 2.Solution temperature in described step 2 during roughening treatment in described alligatoring electrolyzer controls at 29 DEG C ~ 31 DEG C, and pH value maintains 3.8 ~ 4.0 simultaneously.Passing to current density in the coarsening process of described step 2 is 28A/dm 2electric current carry out electrolysis.Described alligatoring electrolyzer adopts titanium plate as anode, and described solidification electrolyzer adopts titanium plate or nickel as anode.When solidifying electrolyzer and using nickel as anode, sulfur-bearing nickel cake or nickel foil offal are placed in titanium frame as anode.Titanium plate or nickel foil replace use stainless steel, chlorion is especially strong to Corrosion of Stainless Steel, and stainless steel can be made to separate out hexavalent chromium, thus cause systemic contamination to affect quality of coating, time serious (when content surpasses 0.01g/L) coating uniformity and covering power can be had a strong impact on, cause the problems such as coating peeling, decortication.And adopt Ni―Ti anode can avoid above problem.And use sulfur-bearing nickel cake or nickel foil offal, decrease the pollution of cupric ion, and take full advantage of nickel foil offal waste product, cost-saving.Semi-bright nickel sulphur content is low, current potential calibration, the bright nickel coating current potential that sulfur acid is high is more negative, a microbattery is created between two-layer nickel dam, namely the semi-bright nickel of current potential calibration is negative electrode, and the bright nickel coating that current potential is comparatively born is anode, and that is matrix is semi-bright nickel, if plate the high nickel of one deck sulphur content in its outside, should than to be easier to and bonding force is relatively good.
The nickel cake that this technique adopts is sulfur-bearing nickel cake, and containing S nickel cake, it has following advantage in employing:
1, spongy nickel, nickel cake can not be generated without sharp edge, not easily hinder hand.
2, improve the sedimentation of nickel in basket, level of residue is less.
3, the operating voltage of starting vessel voltage and coating bath is reduced.
4, under various plating conditions, activity is very high.
5, higher current density can be used.
6, residue and solution type have nothing to do.
7, containing " S " nickel is round pie, and easy to use, do not have objectionable, anode basket can need not be cleared up for a long time.
8, the pollution of copper is reduced.Because cupric ion impurity can remove by sulfur-containing anion.Nickelous sulfide and Cu 2+react, generate copper sulfide precipitation.Cu 2++NiS→CuS↓+Ni 2+
Improve plating qualification rate.Solution loss can reduce about 11%.Anode basket outside adopts terylene cloth bag, and in addition, anode basket also can contain the waste leftover material of nickel foil, saves production cost.
Electrolyzer backflow place respectively in activation treatment, roughening treatment, solidification treatment three processes passes to 0.1A/dm 2~ 0.2A/dm 2direct current carry out impurity and purification process, electrolytic cleaning disposes the foreign ion in electrolytic solution, decreasing pollution, makes product purity higher.
Embodiment 1
Choose the base material of semi-bright nickel paper tinsel as alligatoring nickel foil, described alligatoring electrolyzer adopts titanium plate as anode, and described solidification electrolyzer adopts nickel as anode, is placed in titanium frame sulfur-bearing nickel cake or nickel foil offal as anode.And activation treatment is carried out to described semi-bright nickel paper tinsel; What this technique adopted is only the most simply fill a prescription, the small area analysis etch of Yin/Yang pole need not be carried out, just carry out common pre-erosion i.e. the chemical etching known to electroplating work procedure technician, the hydrochloric acid being 20g/L by the semi-bright nickel paper tinsel activation solution chosen carries out chemical corrosion process to its surface.By chemical corrosion surface treatment, nickel foil base material is activated.Described semi-bright nickel paper tinsel after activated process is placed in be made up of the single nickel salt of 18g/L and the ammonium sulfate of 21g/L and pH value is the alligatoring electrolyzer of the solution of 3.5, to the negative electrode of described alligatoring electrolyzer and anodal closure, passing to current density is 28A/dm 2electric current carry out electrolysis, the solution temperature in alligatoring electrolyzer controls at 29 DEG C, carries out roughening treatment at described alligatoring electrolyzer.The plating ascent stage in roughening treatment process, reduce primary current and adopt current density 1.5A/dm 2small area analysis carry out coating envelope point process.Nickel foil after roughening treatment is placed in be made up of the single nickel salt of 200g/L and the boric acid of 40g/L and 40g/L nickelous chloride and pH value is the solidification electrolyzer of the solution of 4, to the negative electrode of described solidification electrolyzer and anodal closure, passing to current density in solidification process is 12A/dm 2be cured process.In the plating ascent stage of solidification treatment, reduce primary current and adopt current density 1.5A/dm 2small area analysis carry out coating envelope point process.Dried by nickel foil after solidification treatment, bake out temperature controls at 50 DEG C.Products obtained therefrom surface roughness Ra=0.9um RZ=6.0um bonding force (skimming resistance) is >2.5kgf/cm, and resistance is 6m Ω, unit elongation >3.5%.
Embodiment 2
Choose the base material of semi-bright nickel paper tinsel as alligatoring nickel foil, described alligatoring electrolyzer adopts titanium plate as anode, and described solidification electrolyzer adopts nickel as anode, is placed in titanium frame sulfur-bearing nickel cake or nickel foil offal as anode.And activation treatment is carried out to described semi-bright nickel paper tinsel; What this technique adopted is only the most simply fill a prescription, the small area analysis etch of Yin/Yang pole need not be carried out, just carry out common pre-erosion i.e. the chemical etching known to electroplating work procedure technician, the hydrochloric acid being 22g/L by the semi-bright nickel paper tinsel activation solution chosen carries out chemical corrosion process to its surface.By chemical corrosion surface treatment, nickel foil base material is activated.Described semi-bright nickel paper tinsel after activated process is placed in be made up of the single nickel salt of 20g/L and the ammonium sulfate of 22g/L and pH value is the alligatoring electrolyzer of the solution of 3.8, to the negative electrode of described alligatoring electrolyzer and anodal closure, passing to current density is 28A/dm 2electric current carry out electrolysis, the solution temperature in alligatoring electrolyzer controls at 30 DEG C, carries out roughening treatment at described alligatoring electrolyzer.The plating ascent stage in roughening treatment process, reduce primary current and adopt current density 2A/dm 2small area analysis carry out coating envelope point process.Nickel foil after roughening treatment is placed in be made up of the single nickel salt of 250g/L and the boric acid of 45g/L and 40g/L nickelous chloride and pH value is the solidification electrolyzer of the solution of 4.5, to the negative electrode of described solidification electrolyzer and anodal closure, passing to current density in solidification process is 12A/dm 2be cured process.In the plating ascent stage of solidification treatment, reduce primary current and adopt current density 2A/dm 2small area analysis carry out coating envelope point process.Dried by nickel foil after solidification treatment, bake out temperature controls at 55 DEG C.Products obtained therefrom surface roughness Ra=0.95um RZ=6.5um bonding force (skimming resistance) is >2.5kgf/cm, and resistance is 8m Ω, unit elongation >3.5%.
Embodiment 3
Choose the base material of semi-bright nickel paper tinsel as alligatoring nickel foil, described alligatoring electrolyzer adopts titanium plate as anode, and described solidification electrolyzer adopts nickel as anode, is placed in titanium frame sulfur-bearing nickel cake or nickel foil offal as anode.And activation treatment is carried out to described semi-bright nickel paper tinsel; What this technique adopted is only the most simply fill a prescription, the small area analysis etch of Yin/Yang pole need not be carried out, just carry out common pre-erosion i.e. the chemical etching known to electroplating work procedure technician, the hydrochloric acid being 23g/L by the semi-bright nickel paper tinsel activation solution chosen carries out chemical corrosion process to its surface.By chemical corrosion surface treatment, nickel foil base material is activated.Described semi-bright nickel paper tinsel after activated process is placed in be made up of the single nickel salt of 24g/L and the ammonium sulfate of 23g/L and pH value is the alligatoring electrolyzer of the solution of 3.9, to the negative electrode of described alligatoring electrolyzer and anodal closure, passing to current density is 28A/dm 2electric current carry out electrolysis, the solution temperature in alligatoring electrolyzer controls at 31 DEG C, carries out roughening treatment at described alligatoring electrolyzer.The plating ascent stage in roughening treatment process, reduce primary current and adopt current density 1.8A/dm 2small area analysis carry out coating envelope point process.Nickel foil after roughening treatment is placed in be made up of the single nickel salt of 220g/L and the boric acid of 43g/L and 40g/L nickelous chloride and pH value is the solidification electrolyzer of the solution of 4.5, to the negative electrode of described solidification electrolyzer and anodal closure, passing to current density in solidification process is 12A/dm 2be cured process.In the plating ascent stage of solidification treatment, reduce primary current and adopt current density 2A/dm 2small area analysis carry out coating envelope point process.Dried by nickel foil after solidification treatment, bake out temperature controls at 58 DEG C.Products obtained therefrom surface roughness Ra=0.95um RZ=6.5um bonding force (skimming resistance) is >2.5kgf/cm, and resistance is 11m Ω, unit elongation >3.5%.
Embodiment 4
Choose the base material of semi-bright nickel paper tinsel as alligatoring nickel foil, described alligatoring electrolyzer adopts titanium plate as anode, and described solidification electrolyzer adopts nickel as anode, is placed in titanium frame sulfur-bearing nickel cake or nickel foil offal as anode.And activation treatment is carried out to described semi-bright nickel paper tinsel; What this technique adopted is only the most simply fill a prescription, the small area analysis etch of Yin/Yang pole need not be carried out, just carry out common pre-erosion i.e. the chemical etching known to electroplating work procedure technician, the hydrochloric acid being 25g/L by the semi-bright nickel paper tinsel activation solution chosen carries out chemical corrosion process to its surface.By chemical corrosion surface treatment, nickel foil base material is activated.Described semi-bright nickel paper tinsel after activated process is placed in be made up of the single nickel salt of 25g/L and the ammonium sulfate of 23g/L and pH value is the alligatoring electrolyzer of the solution of 4, to the negative electrode of described alligatoring electrolyzer and anodal closure, passing to current density is 28A/dm 2electric current carry out electrolysis, the solution temperature in alligatoring electrolyzer controls at 31 DEG C, carries out roughening treatment at described alligatoring electrolyzer.The plating ascent stage in roughening treatment process, reduce primary current and adopt current density 2A/dm 2small area analysis carry out coating envelope point process.Nickel foil after roughening treatment is placed in be made up of the single nickel salt of 250g/L and the boric acid of 45g/L and 40g/L nickelous chloride and pH value is the solidification electrolyzer of the solution of 4.5, to the negative electrode of described solidification electrolyzer and anodal closure, passing to current density in solidification process is 12A/dm 2be cured process.In the plating ascent stage of solidification treatment, reduce primary current and adopt current density 2A/dm 2small area analysis carry out coating envelope point process.Dried by nickel foil after solidification treatment, bake out temperature controls at 70 DEG C.Products obtained therefrom surface roughness Ra=1.0um RZ=7.0um bonding force (skimming resistance) is >2.5kgf/cm, and resistance is 15m Ω, unit elongation >3.5%.
Embodiment 5
Choose the base material of semi-bright nickel paper tinsel as alligatoring nickel foil, described alligatoring electrolyzer adopts titanium plate as anode, and described solidification electrolyzer adopts nickel as anode, is placed in titanium frame sulfur-bearing nickel cake or nickel foil offal as anode.And activation treatment is carried out to described semi-bright nickel paper tinsel; What this technique adopted is only the most simply fill a prescription, the small area analysis etch of Yin/Yang pole need not be carried out, just carry out common pre-erosion i.e. the chemical etching known to electroplating work procedure technician, the hydrochloric acid being 25g/L by the semi-bright nickel paper tinsel activation solution chosen carries out chemical corrosion process to its surface.By chemical corrosion surface treatment, nickel foil base material is activated.Described semi-bright nickel paper tinsel after activated process is placed in be made up of the single nickel salt of 25g/L and the ammonium sulfate of 23g/L and pH value is the alligatoring electrolyzer of the solution of 4.5, to the negative electrode of described alligatoring electrolyzer and anodal closure, passing to current density is 28A/dm 2electric current carry out electrolysis, the solution temperature in alligatoring electrolyzer controls at 31 DEG C, carries out roughening treatment at described alligatoring electrolyzer.The plating ascent stage in roughening treatment process, reduce primary current and adopt current density 2A/dm 2small area analysis carry out coating envelope point process.Nickel foil after roughening treatment is placed in be made up of the single nickel salt of 250g/L and the boric acid of 45g/L and 40g/L nickelous chloride and pH value is the solidification electrolyzer of the solution of 4.5, to the negative electrode of described solidification electrolyzer and anodal closure, passing to current density in solidification process is 12A/dm 2be cured process.In the plating ascent stage of solidification treatment, reduce primary current and adopt current density 2A/dm 2small area analysis carry out coating envelope point process.Dried by nickel foil after solidification treatment, bake out temperature controls at 70 DEG C.Products obtained therefrom surface roughness Ra=1.0um RZ=7.0um bonding force (skimming resistance) is >2.5kgf/cm, and resistance is 15m Ω, unit elongation >3.5%.
This operation item is simple, and raw material relates to and only has single nickel salt, nickelous chloride, boric acid and ammonium sulfate.Medicine used is plating level.Owing to only having four raw materials, configure also more convenient.Operation is very simple, is extremely suitable for industrial application.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (11)

1. a method for electrolytic process production alligatoring nickel foil, is characterized in that, comprise the following steps: step one: choose the base material of semi-bright nickel paper tinsel as alligatoring nickel foil, and carries out activation treatment to described semi-bright nickel paper tinsel;
Step 2: the described semi-bright nickel paper tinsel after process activated described in step one is placed in be made up of the single nickel salt of 18 ~ 25g/L and the ammonium sulfate of 21 ~ 23g/L and pH value is the alligatoring electrolyzer of the solution of 3.5 ~ 4.5, to the negative electrode of described alligatoring electrolyzer and anodal closure, carry out roughening treatment at described alligatoring electrolyzer;
Step 3: the nickel foil in step 2 after roughening treatment is placed in be made up of the single nickel salt of 200g/L ~ 250g/L and the boric acid of 40 ~ 45g/L and 40g/L nickelous chloride and pH value is the solidification electrolyzer of the solution of 4 ~ 4.5, to the negative electrode of described solidification electrolyzer and anodal closure, be cured process;
Step 4: the nickel foil after solidification treatment described in step 3 is dried.
2. want the method for a kind of electrolytic process production alligatoring nickel foil described in 1 according to right, it is characterized in that: the hydrochloric acid that the described semi-bright nickel paper tinsel activation solution chosen is specifically 20 ~ 25g/L by the activation treatment in described step one carries out chemical corrosion process to its surface.
3. the method for a kind of electrolytic process production alligatoring nickel foil according to claim 2, is characterized in that: described activation solution is the hydrochloric acid of 22g/L.
4. want the method for a kind of electrolytic process production alligatoring nickel foil described in 1 according to right, it is characterized in that:
Solution temperature in described step 2 during roughening treatment in described alligatoring electrolyzer controls at 29 DEG C ~ 31 DEG C, and pH value maintains 3.8 ~ 4.0 simultaneously.
5. want the method for a kind of electrolytic process production alligatoring nickel foil described in 4 according to right, it is characterized in that: passing to current density during the roughening treatment of described step 2 is 28A/dm 2electric current carry out electrolysis.
6. the method for a kind of electrolytic process production alligatoring nickel foil according to claim 1, is characterized in that: described alligatoring electrolyzer adopts titanium plate as anode, and described solidification electrolyzer adopts titanium plate or nickel as anode.
7. the method for a kind of electrolytic process production alligatoring nickel foil according to claim 6, is characterized in that: when solidifying electrolyzer and using nickel as anode, be placed in titanium frame sulfur-bearing nickel cake or nickel foil offal as anode.
8. the method for a kind of electrolytic process production alligatoring nickel foil according to claim 7, is characterized in that: passing to current density during the solidification treatment of described step 3 is 12A/dm 2electric current carry out electrolysis.
9. want the method for a kind of electrolytic process production alligatoring nickel foil described in 1 according to right, it is characterized in that: the bake out temperature in described step 4 controls at 50 ~ 70 DEG C.
10. want the method for 1 to 9 arbitrary described a kind of electrolytic process production alligatoring nickel foil according to right, it is characterized in that: described step 2 and three roughening treatment, solidification treatment all reduce primary current in the plating ascent stage, and adopt current density 1.5 ~ 2A/dm 2small area analysis to coating seal point process.
11. want the method for a kind of electrolytic process production alligatoring nickel foil described in 10 according to right, it is characterized in that: electrolyzer backflow place respectively in activation treatment, roughening treatment, solidification treatment three processes passes to 0.1A/dm 2~ 0.2A/dm 2direct current carry out purifying treatment.
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