CN101864584A - Plating solution for tumble-plating and tumble-plating method of steel battery shell - Google Patents
Plating solution for tumble-plating and tumble-plating method of steel battery shell Download PDFInfo
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- CN101864584A CN101864584A CN201010185248A CN201010185248A CN101864584A CN 101864584 A CN101864584 A CN 101864584A CN 201010185248 A CN201010185248 A CN 201010185248A CN 201010185248 A CN201010185248 A CN 201010185248A CN 101864584 A CN101864584 A CN 101864584A
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Abstract
The invention relates to a treatment process of a carrier of a device which is used to directly change chemical energy to electrical energy, in particular to a plating solution for tumble-plating and a tumble-plating method of a steel battery shell. The plating solution comprises the following components in parts by weight: 80-120 or 200-350 parts of main salt, 30-100 parts of anode activator, 3-60 parts of buffering agent, 20-30 or 180-250 parts of complexant, 0.5-2.5 parts of stress reducer, 0.005-0.1 part of main brightener and 0.3-1.0 part of auxiliary agent and is prepared by dissolving the components in water. The tumble-plating method of the invention comprises the following steps in turn: degreasing, tumble-plating and bleaching, wherein during tumble-plating, the pH value of the plating solution is 4.0-4.6 or 6.5-8.5, the temperature is 40-70 DEG C, the current density is 0.2-3A/dm<2>, the rotational speed of the drum is 4-12rpm, and the tumble-plating time is 180-300 minutes. The coating of the invention has write and bright appearance, high luminance brightness and powerful corrosion resistance.
Description
Technical field
The present invention relates to be used for directly changing the treatment process of used carrier on the device that chemical energy is an electric energy, be specially barrel plating with electroplate liquid and battery steel shell barrel plating method.
Background technology
At present, alkaline cell with its electrical capacity height, long service life, environmental pollution is few and obtain more and more widely application.The shell of alkaline cell generally is stamped to form with steel, and as the container of electrolytic solution and the leading-out end of electrode, battery case requires that erosion resistance is strong, good airproof performance, excellent conductivity, so battery steel shell is generally made Nickel Plating Treatment to improve every performance index.Battery steel shell is typical blind hole part, and a lot of model is again the deep hole part simultaneously, however to the requirement of electrolytic coating, but very high as the thickness and the bright degree of the conjugation of coating and base material, coating, so the plating difficulty of battery steel shell is very big.Traditional vitriol nickel plating technology can't deposit fastness, thickness and all satisfactory nickel dam of luminance brightness at the inwall and the inner bottom surface of blind hole deep hole, therefore, all the time, the first nickel plating technology of punching press is more generally adopted in the manufacturing of battery steel shell, and also must implement degreasing and antirust processing respectively after the punching press.Adopt this working method, plasticity is relative reduces because the hardness of steel in the nickel plating rear surface all can increase with stress, has so just improved when stamping-out draws the tonnagedemand of equipment, has weakened punch process.Still can keep original punch process after making nickel plating, steel can only be selected the softer kind of quality, and this just causes rammed box hat impact strength to descend, and machinery takes place easily damage.In addition, owing to be damaged at the lattice through nickel coating after the punching press, porosity increases, and the punching press incision do not have nickel coating, so this class box hat gets rusty easily, and therefore the battery storing cycle also shortens.Find by prior art documents, Chinese patent CN1484714A discloses a kind of " Nickeled Steel Plate and the anodal jar of alkaline manganese battery that are used for anodal jar of alkaline manganese battery " on March 24th, 2004, this technical scheme is used for the steel plate of anode jar (being battery case), by adding interspersed one section heat treatment step of in non-oxidizing atmosphere, operating in man-hour, and plating bath, current density when careful selection is electroplated, thereby forming nickel on a surface of steel plate is diffusion coating, and this one side is as the internal surface of jar; Be formed with the nickel coating of iron-nickel diffusion coating and process recrystallize softening on another surface, this one side is as the outside surface of jar.Though this Nickeled Steel Plate is making moderate progress aspect the lattice of nickel coating and the porosity, but the adding of heat treatment step and the requirement comparatively harsh to plating bath, current density, make that difficulty of processing is big, efficient is low, cost is high, and the problem that the punching press incision does not have a nickel coating is not solved effectively yet.
Summary of the invention
For overcoming aforementioned the deficiencies in the prior art, solve the defective that solidity to corrosion is poor, intensity is low of the present prepared battery steel shell of nickel plating method, the invention discloses a kind of barrel plating with electroplate liquid and battery steel shell barrel plating method.
A kind of barrel plating electroplate liquid, form by main salt, anode activator, buffer reagent, complexing agent, stress relieving agent, main brightener and auxiliary, the mass fraction of each component is as described below: main salt 80～120 or 200～350, anode activator 30～100, buffer reagent 3～60, complexing agent 20～30 or 180～250, stress relieving agent 0.5～2.5, main brightener 0.005～0.1, auxiliary 0.3～1.0.Wherein: main salt is selected NiSO for use
4The anode activator is selected NiCl for use
2Buffer reagent is selected H for use
3BO
3, NH
3H
2In O and the ammonium citrate any one; Complexing agent is selected any one in 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid, potassium pyrophosphate and the Trisodium Citrate for use; The stress relieving agent selects naphthalene disulfonic acid, benzoic sulfimide for use, in benzsulfamide and the o-benzoic sulfimide any one; Main brightener selects 1 for use, any one in 4-butynediol, alkynol propoxylation compound, diethylin propine, propiolic alcohol, propiolic alcohol propoxylation compound and the oxyethyl group alkynol compound; Auxiliary is selected any two or more composite with arbitrary proportion in an alkali metal salt of an alkali metal salt of an alkali metal salt, propine sulfonic acid of propine drone an alkali metal salt, butyl ether drone an alkali metal salt, allyl sulphonic acid and vinyl sulfonic acid for use.Above each component all is dissolved in deionized water or tap water, is made into the total mass umber and is 1000 solution, promptly get the barrel plating electroplate liquid.
A kind of battery steel shell barrel plating method, the battery steel shell that has been stamped to form is plated preceding skimming treatment by A., B. three steps in sequence of barrel plating and C. plating post-bleach processing are carried out, C step plating post-bleach is handled and carried out successively as follows: three road recovery → cleanings → bleaching → cleaning → neutralization → pure water is washed → antirust → dehydration → drying, citric acid is selected in bleaching for use, oxalic acid, oxyacetic acid, in 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid and the sulfuric acid any one, sodium hydroxide is selected in neutralization for use, in potassium hydroxide and the yellow soda ash any one, the characteristics in the step are: used electroplate liquid is a barrel plating as claimed in claim 1 electroplate liquid during B step barrel plating; During barrel plating, the pH value of electroplate liquid is controlled at 4.0～4.6 or 6.5～8.5,40 ℃～70 ℃ of temperature, current density 0.05A/dm
2～3A/dm
2, 4～12 rev/mins of drum rotating speeds, 180～300 minutes barrel plating time.
Described battery steel shell barrel plating method, the characteristics in the step are: skimming treatment is carried out as follows successively before the A step plating:
I. the degreasing of deoiling: with the battery steel shell of degreasing fluid washing electroplated, 50 ± 10 ℃ of wash temperatures, washing time 20～40 minutes, be that 40 ℃～60 ℃ deionized water or tap water cleans up with temperature after finishing, twice so repeatedly, degreasing fluid is by sodium hydroxide, water glass, yellow soda ash, sulfonic acid analog anion surfactants and deionized water are formed, the mass percent concentration of each component is as described below: sodium hydroxide 5%～10%, water glass 2%～8%, yellow soda ash 1%～10%, sulfonic acid analog anion surfactants 2%～5%, deionized water or tap water surplus, sulfonic acid analog anion surfactants is selected sodium laurylsulfonate or Sodium dodecylbenzene sulfonate for use.
Ii acid-wash activation: will finish i step and deoil the battery steel shell of degreasing with acid solution pickling at room temperature 1～3 minute, clean up with deionized water or tap water after finishing, twice so repeatedly, it is 10%～45% hydrochloric acid that pickle solution is selected mass percent concentration for use, or mass percent concentration is 10%～25% sulfuric acid.
Adopt technical scheme disclosed in this invention, can fundamentally solve the prior art elder generation nickel plating drawback brought of the technology of punching press again, because the every processing parameter when having adopted special electroplate liquid and having selected barrel plating meticulously, make this class blind hole deep-hole type parts surface of battery steel shell especially internal surface also can deposit with the base material bonding force strong, the high nickel coating of certain thickness and bright degree is arranged, outside surface nickel coating thickness is between 1.5 μ m～6 μ m, the inwall nickel coating is between 0.1 μ m～1.0 μ m, box hat is no longer implemented mechanical workout after nickel plating is finished like this, the nickel coating lattice is not damaged still can keep original fine and close state, porosity is little, thereby improved corrosion resistance, and the surfaces externally and internally and the incision of box hat can both be by the electroplate liquid submergence during barrel plating, whole surface nickel coating does not have blind spot, so can not get rusty, the resting period of battery also just prolongs greatly like this.According to the contrast experiment; adopt the battery steel shell of technical scheme barrel plating disclosed in this invention; no matter be under hot and humid environment; still be immersed in the electrolyte solution; still in the activity metal salt solution lower, all both do not had rusty stain and generated, and do not had metal yet and replaced than iron; the box hat that fine and close nickel coating is protected effectively is described, makes it isolated with corrosive atmosphere.And the nickel coating bright appearance, be different from by the nickel plated steel strip punching press make battery steel shell presented that ash is dark-coloured, the battery outward appearance is more attractive in appearance.
Description of drawings
Fig. 1 adopts its coating of battery steel shell of barrel plating of the present invention to be amplified to 400 times image;
Fig. 2 be adopt traditional first nickel plating again its coating of battery steel of making of Sheet Metal Forming Technology be amplified to 400 times image.
Embodiment
Below further specify the utility model by specific embodiment.
Embodiment 1
A. degreasing before the plating:
I. the degreasing of deoiling:
Getting the LR6 number used not galvanized box hat of alkaline zinc-manganese battery places in the degreasing tank, pouring degreasing fluid into washs, degreasing fluid is to be as the criterion the whole submergences of box hat, the mass percent concentration of each component of degreasing fluid is as described below: sodium hydroxide 5%, water glass 2%, yellow soda ash 1%, sodium laurylsulfonate 2%, tap water surplus.
During washing, the temperature in the degreasing tank is 40 ℃, and washing time 20 minutes is that 40 ℃ deionized water or tap water cleans up with temperature after washing is finished.Above-mentioned washing-cleaning process is carried out twice repeatedly.
The ii acid-wash activation:
Deoil the battery steel shell of degreasing with acid solution pickling at room temperature 1 minute with finishing i step, and it is 10% hydrochloric acid that acid solution is selected mass percent concentration for use, cleans up with deionized water or tap water after pickling is finished.Above-mentioned pickling-cleaning process is carried out twice repeatedly.
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 4.00,50 ℃ of temperature, current density 0.2A/dm
2, 4 rev/mins of drum rotating speeds, 180 minutes barrel plating time.
C. plate post-bleach
Carrying out successively as follows: three road recovery → cleanings → bleaching → cleaning → neutralization → pure water washes → and pure water washes → antirust → dehydration → drying.
Wherein, select organic acid during bleaching for use,, also can select sulfuric acid for use as citric acid, oxalic acid, oxyacetic acid or 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid.In and the time select sodium hydroxide, potassium hydroxide or yellow soda ash for use.Select for use Japan to go up the village rising sun light company rust-preventive agent when antirust.
Embodiment 2
A. degreasing before the plating:
I. the degreasing of deoiling:
The mass percent concentration of each component of degreasing fluid is as described below: sodium hydroxide 7%, water glass 5%, yellow soda ash 5%, Sodium dodecylbenzene sulfonate 3%, tap water surplus.
Temperature in the degreasing tank is 50 ℃, and washing time 30 minutes is that 50 ℃ deionized water or tap water cleans up with temperature after washing is finished.
The ii acid-wash activation:
It is 25% hydrochloric acid that mass percent concentration is selected in pickling 2 minutes, acid solution for use.
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 4.30,53 ℃ of temperature, current density 0.4A/dm
2, 8 rev/mins of drum rotating speeds, 240 minutes barrel plating time.
Other steps are all with embodiment one.
Embodiment 3
A. degreasing before the plating:
I. the degreasing of deoiling:
The mass percent concentration of each component of degreasing fluid is as described below: sodium hydroxide 10%, water glass 8%, yellow soda ash 10%, sodium laurylsulfonate 5%, tap water surplus.
Temperature in the degreasing tank is 60 ℃, and washing time 40 minutes is that 60 ℃ tap water cleans up with temperature after washing is finished.
The ii acid-wash activation:
It is 45% hydrochloric acid that mass percent concentration is selected in pickling 3 minutes, acid solution for use.
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 4.45,57 ℃ of temperature, current density 0.8A/dm
2, 12 rev/mins of drum rotating speeds, 300 minutes barrel plating time.
Other steps are all with embodiment one.
Embodiment 4
A. degreasing before the plating:
I. the degreasing of deoiling:
The mass percent concentration of each component of degreasing fluid is as described below: sodium hydroxide 5%, water glass 2%, yellow soda ash 1%, Sodium dodecylbenzene sulfonate 2%, deionized water surplus.
Temperature in the degreasing tank is 40 ℃, and washing time 20 minutes is that 40 ℃ tap water cleans up with temperature after washing is finished.
The ii acid-wash activation:
It is 10% sulfuric acid that mass percent concentration is selected in pickling 1 minute, acid solution for use.
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
| Component | Select material for use | Quality (g) |
| Main salt | ??NiSO 4 | ??80 |
| The anode activator | ??NiCl 2 | ??50 |
| Buffer reagent | Ammonium citrate | ??10 |
| Complexing agent | Potassium pyrophosphate | ??200 |
| Component | Select material for use | Quality (g) |
| The stress relieving agent | Naphthalene disulfonic acid | ??2 |
| Main brightener | 1, the 4-butynediol | ??0.1 |
| Auxiliary | Propine drone sodium salt | ??0.8 |
| The sodium salt of vinyl sulfonic acid | ??0.2 |
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 4.60,60 ℃ of temperature, current density 1.0A/dm
2
Other steps are all with embodiment one.
Embodiment 5
A. degreasing before the plating:
I. the degreasing of deoiling:
The mass percent concentration of each component of degreasing fluid is as described below: sodium hydroxide 8%, water glass 5%, yellow soda ash 6%, sodium laurylsulfonate 4%, deionized water surplus.
Temperature in the degreasing tank is 50 ℃, and washing time 30 minutes is that 50 ℃ washed with de-ionized water is clean with temperature after washing is finished.
Ii. acid-wash activation:
It is 15% sulfuric acid that mass percent concentration is selected in pickling 2 minutes, acid solution for use.
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 6.50,50 ℃ of temperature, current density 0.2A/dm
2
Other steps are all with embodiment one.
Embodiment 6
A. degreasing before the plating:
I. the degreasing of deoiling:
The mass percent concentration of each component of degreasing fluid is as described below: sodium hydroxide 10%, water glass 8%, yellow soda ash 10%, Sodium dodecylbenzene sulfonate 5%, tap water surplus.
Temperature in the degreasing tank is 60 ℃, and washing time 40 minutes is that 60 ℃ tap water cleans up with temperature after washing is finished.
The ii acid-wash activation:
It is 25% sulfuric acid that mass percent concentration is selected in pickling 3 minutes, acid solution for use.
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 6.70,53 ℃ of temperature, current density 0.4A/dm
2
Other steps are all with embodiment one.
Embodiment 7
A. degreasing before the plating:
I. the degreasing of deoiling:
The mass percent concentration of each component of degreasing fluid is as described below: sodium hydroxide 5%, water glass 2%, yellow soda ash 1%, sodium laurylsulfonate 2%, tap water surplus.
Temperature in the degreasing tank is 40 ℃, and washing time 20 minutes is that 40 ℃ deionized water or washed with de-ionized water is clean with temperature after washing is finished.
Ii. acid-wash activation:
It is 10% hydrochloric acid that mass percent concentration is selected in pickling 1 minute, acid solution for use.
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 6.85,55 ℃ of temperature, current density 0.6A/dm
2
Other steps are all with embodiment one.
Embodiment 8
A. degreasing before the plating:
I. the degreasing of deoiling:
The mass percent concentration of each component of degreasing fluid is as described below: sodium hydroxide 7%, water glass 5%, yellow soda ash 5%, Sodium dodecylbenzene sulfonate 3%, tap water surplus.
Temperature in the degreasing tank is 50 ℃, and washing time 30 minutes is that 50 ℃ tap water cleans up with temperature after washing is finished.
Ii. acid-wash activation:
It is 25% hydrochloric acid that mass percent concentration is selected in pickling 2 minutes, acid solution for use.
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 7.00,57 ℃ of temperature, current density 0.8A/dm
2
Other steps are all with embodiment one.
Embodiment 9
A. degreasing before the plating:
I. the degreasing of deoiling:
The mass percent concentration of each component of degreasing fluid is as described below: sodium hydroxide 10%, water glass 8%, yellow soda ash 10%, sodium laurylsulfonate 5%, deionized water surplus.
Temperature in the degreasing tank is 60 ℃, and washing time 40 minutes is that 60 ℃ washed with de-ionized water is clean with temperature after washing is finished.
The ii acid-wash activation:
It is 45% hydrochloric acid that mass percent concentration is selected in pickling 3 minutes, acid solution for use.
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 7.15,60 ℃ of temperature, current density 1A/dm
2
Other steps are all with embodiment one.
Embodiment 10
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 7.30,50 ℃ of temperature, current density 0.2A/dm
2
Other steps are all with embodiment two.
Embodiment 11
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 7.45,53 ℃ of temperature, current density 0.5A/dm
2
Other steps are all with embodiment two.
Embodiment 12
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 7.60,57 ℃ of temperature, current density 0.8A/dm
2
Other steps are all with embodiment two.
Embodiment 13
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 7.75,60 ℃ of temperature, current density 1A/dm
2
Other steps are all with embodiment two.
Embodiment 14
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 7.90,65 ℃ of temperature, current density 0.5A/dm
2
Other steps are all with embodiment two.
Embodiment 15
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 8.05,67 ℃ of temperature, current density 2A/dm
2
Other steps are all with embodiment two.
Embodiment 16
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 8.20,70 ℃ of temperature, current density 3A/dm
2
Other steps are all with embodiment two.
Embodiment 17
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 6.5,65 ℃ of temperature, current density 0.5A/dm
2
Other steps are all with embodiment two.
Embodiment 18
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 6.7,68 ℃ of temperature, current density 1.5A/dm
2
Other steps are all with embodiment two.
Embodiment 19
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 6.85,70 ℃ of temperature, current density 3A/dm
2
Other steps are all with embodiment two.
Embodiment 20
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 7.00,65 ℃ of temperature, current density 0.5A/dm
2
Other steps are all with embodiment two.
Embodiment 21
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 7.15,67 ℃ of temperature, current density 2A/dm
2
Other steps are all with embodiment two.
Embodiment 22
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 7.30,70 ℃ of temperature, current density 3A/dm
2
Other steps are all with embodiment two.
Embodiment 23
A. degreasing before the plating:
I. the degreasing of deoiling:
Degreasing fluid is prepared by following requirement:
| Component | Mass percent concentration (%) |
| Commercially available grease-removing agent | ??40 |
| ??NaOH | ??10 |
| Deionized water | Surplus |
The grease-removing agent that commercially available grease-removing agent selects for use Shanghai detergents and cosmetic company limited to produce.
Temperature in the degreasing tank is 60 ℃, and washing time 40 minutes is that 60 ℃ washed with de-ionized water is clean with temperature after washing is finished.
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 7.45,50 ℃ of temperature, current density 0.05A/dm
2
Other steps are all with embodiment one.
Embodiment 24
A. degreasing before the plating:
I. the degreasing of deoiling:
Degreasing fluid is prepared by following requirement:
| Component | Mass percent concentration (%) |
| Commercially available grease-removing agent | ??45 |
| ??NaOH | ??15 |
| Tap water | Surplus |
The grease-removing agent that commercially available grease-removing agent selects for use Shanghai detergents and cosmetic company limited to produce.
Temperature in the degreasing tank is 60 ℃, and washing time 40 minutes is that 60 ℃ tap water cleans up with temperature after washing is finished.
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 7.60,50 ℃ of temperature, current density 0.08A/dm
2
Other steps are all with embodiment one.
Embodiment 25
A. degreasing before the plating:
I. the degreasing of deoiling:
Degreasing fluid is prepared by following requirement:
| Component | Mass percent concentration (%) |
| Commercially available grease-removing agent | ??50 |
| ??NaOH | ??20 |
| Tap water | Surplus |
The grease-removing agent that commercially available grease-removing agent selects for use Shanghai detergents and cosmetic company limited to produce
Temperature in the degreasing tank is 60 ℃, and washing time 40 minutes is that 60 ℃ tap water cleans up with temperature after washing is finished.
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 7.75,55 ℃ of temperature, current density 0.08A/dm
2
Other steps are all with embodiment one.
Embodiment 26
A. degreasing before the plating:
I. the degreasing of deoiling:
Degreasing fluid is prepared by following requirement:
| Component | Mass percent concentration (%) |
| Commercially available grease-removing agent | ??60 |
| ??NaOH | ??25 |
| Tap water | Surplus |
The grease-removing agent that commercially available grease-removing agent selects for use Shanghai detergents and cosmetic company limited to produce.
Temperature in the degreasing tank is 60 ℃, and washing time 40 minutes is that 60 ℃ tap water cleans up with temperature after washing is finished.
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 7.90,55 ℃ of temperature, current density 0.1A/dm
2
Other steps are all with embodiment one.
Embodiment 27
A. degreasing before the plating:
I. the degreasing of deoiling:
Degreasing fluid is prepared by following requirement:
| Component | Mass percent concentration (%) |
| Commercially available grease-removing agent | ??40 |
| ??NaOH | ??10 |
| Tap water | Surplus |
The grease-removing agent that commercially available grease-removing agent selects for use Shanghai detergents and cosmetic company limited to produce.
Temperature in the degreasing tank is 60 ℃, and washing time 40 minutes is that 60 ℃ tap water cleans up with temperature after washing is finished.
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 8.05,50 ℃ of temperature, current density 0.05A/dm
2
Other steps are all with embodiment one.
Embodiment 28
A. degreasing before the plating:
I. the degreasing of deoiling:
Degreasing fluid is prepared by following requirement:
| Component | Mass percent concentration (%) |
| Commercially available grease-removing agent | ??50 |
| ??NaOH | ??15 |
| Tap water | Surplus |
The grease-removing agent that commercially available grease-removing agent selects for use Shanghai detergents and cosmetic company limited to produce.
Temperature in the degreasing tank is 60 ℃, and washing time 40 minutes is that 60 ℃ tap water cleans up with temperature after washing is finished.
Ii. acid-wash activation:
It is 25% sulfuric acid that mass percent concentration is selected in pickling 3 minutes, acid solution for use.
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
| Component | Select material for use | Quality (g) |
| Main salt | ??NiSO 4 | ??300 |
| The anode activator | ??NiCl 2 | ??40 |
| Buffer reagent | ??H 3BO 3 | ??45 |
| Complexing agent | Trisodium Citrate | ??20 |
| The stress relieving agent | Naphthalene disulfonic acid | ??0.5 |
| Component | Select material for use | Quality (g) |
| Main brightener | Alkynol propoxylation compound | ??0.05 |
| Auxiliary | Butyl ether drone sodium salt | ??0.2 |
| The sodium salt of propine sulfonic acid | ??0.3 |
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 8.20,50 ℃ of temperature, current density 0.08A/dm
2
Other steps are all with embodiment one.
Embodiment 29
A. degreasing before the plating:
I. the degreasing of deoiling:
Degreasing fluid is prepared by following requirement:
| Component | Mass percent concentration (%) |
| Commercially available grease-removing agent | ??55 |
| ??NaOH | ??20 |
| Tap water | Surplus |
The grease-removing agent that commercially available grease-removing agent selects for use Shanghai detergents and cosmetic company limited to produce.
Temperature in the degreasing tank is 60 ℃, and washing time 40 minutes is that 60 ℃ tap water cleans up with temperature after washing is finished.
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 8.35,55 ℃ of temperature, current density 0.08A/dm
2
Other steps are all with embodiment one.
Embodiment 30
A. degreasing before the plating:
I. the degreasing of deoiling:
Degreasing fluid is prepared by following requirement:
| Component | Mass percent concentration (%) |
| Commercially available grease-removing agent | ??60 |
| ??NaOH | ??25 |
| Tap water | Surplus |
The grease-removing agent that commercially available grease-removing agent selects for use Shanghai detergents and cosmetic company limited to produce.During the preparation degreasing fluid, also can replace deionized water with tap water.
Temperature in the degreasing tank is 60 ℃, and washing time 40 minutes is that 60 ℃ tap water cleans up with temperature after washing is finished.
B. barrel plating:
The box hat of finishing the preceding skimming treatment of aforementioned A step plating is put into the barrel plating groove, pour electroplate liquid into and carry out barrel plating, electroplate liquid is prepared by following requirement:
Above each component all is dissolved in deionized water, is made into the solution that total mass is 1000g, promptly get the barrel plating electroplate liquid.During barrel plating, the pH value of electroplate liquid is controlled at 8.50,55 ℃ of temperature, current density 0.1A/dm
2
Other steps are all with embodiment one.
The contrast experiment 1
Battery steel shell so that embodiment 2 described methods make is made as sample A; In addition, be made as sample B with traditional first nickel plating battery steel shell of making of Sheet Metal Forming Technology again.
Sample A and sample B respectively get 5, measure the thickness of coating of outer wall, and data are as shown in the table:
| Sample | The position | ??1 | ??2 | ??3 | ??4 | ??5 | Mean value |
| ??A | Outer wall | ??2.50 | ??2.76 | ??2.37 | ??2.68 | ??2.67 | ??2.596 |
| ??B | Outer wall | ??1.96 | ??2.01 | ??2.09 | ??2.00 | ??1.99 | ??2.01 |
As seen from the above table, the outer wall coating of sample A is than thick about 30% of sample B.
Fig. 1 is that the coating of sample A is amplified to 400 times image, and Fig. 2 is that the coating of sample B is amplified to 400 times image, can obviously find out, the coating of sample A is much finer and close than sample B's.
The contrast experiment 2
High temperature and humidity test contrast: take out sample A and sample B placed five hours simultaneously in 65 ℃, the environment of 90% humidity after, sample A outer wall still be that inwall does not all have rusty stain, and sample B outer wall and inwall all have the rusty stain generation.The battery case that explanation makes with the method disclosed in the present, the fine and close strong adhesion of coating can be effectively isolated with extraneous corrodibility atmosphere steel, thereby play the effect of protection.
The contrast experiment 3
Bluepoint test contrast: filter paper is wetting with the Tripotassium iron hexacyanide+sodium chloride solution, after be covered in sample A and sample B last 5 minute respectively.It is blue that the filter paper of sample A does not show, and it is blue that the filter paper of sample B shows.The battery steel shell that explanation makes with the method disclosed in the present, coating evenly do not have blind spot, and otch also has fine and close coating to cover the corrosion strength and the life-span of having improved shell.
The contrast experiment 4
Copper sulfate soak test contrast: with sample A and sample B all in 5% CuSO4 solution submergence take out after 2 minutes, the outer wall of sample A and inwall still are the silvery white of original light, the outer wall of sample B and inwall all have a little copper to separate out.The reaction equation of iron and copper sulfate is as follows:
Fe+CuSO
4＝FeSO
4+Cu
Chemical reaction does not take place in Ni and CuSO4.
The battery case that explanation makes with the method disclosed in the present, the fine and close strong adhesion of coating can be effectively isolated with extraneous corrodibility atmosphere steel, thereby play the effect of protection.
The contrast experiment 5
Saline soak test contrast: with sample A and sample B all in 5% NaCl solution submergence takes out after 2 hours, sample A otch, outer wall still are that inwall does not all have rusty stain, and sample B otch, outer wall and inwall all have the rusty stain generation.The battery case that explanation makes with the method disclosed in the present, coating evenly do not have blind spot, and otch also has fine and close coating to cover the corrosion strength and the life-span of having improved shell.The fine and close strong adhesion of coating can be effectively isolated with extraneous corrodibility atmosphere steel, thereby play the effect of protection.
The contrast experiment 6
The salt-fog test contrast: sample A and sample B are used NaCl solution spraying taking-up after 1 hour continuously of 5%, and sample A outer wall still is that inwall does not all have rusty stain, and sample B outer wall and inwall all have rusty stain to generate.The battery case that explanation makes with the method disclosed in the present, the fine and close strong adhesion of coating can be effectively isolated with extraneous corrodibility atmosphere steel, thereby play the effect of protection.
Claims (3)
1. a barrel plating electroplate liquid is made up of main salt, anode activator, buffer reagent, complexing agent, stress relieving agent, main brightener and auxiliary, and it is characterized in that: the mass fraction of each component is as described below:
Main salt 80～120 or 200～350, anode activator 30～100, buffer reagent 3～60, complexing agent 20～30 or 180～250, stress relieving agent 0.5～2.5, main brightener 0.005～0.1, auxiliary 0.3～1.0,
Wherein:
Main salt is selected NiSO for use
4
The anode activator is selected NiCl for use
2
Buffer reagent is selected H for use
3BO
3, NH
3H
2In O and the ammonium citrate any one;
Complexing agent is selected any one in 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid, potassium pyrophosphate and the Trisodium Citrate for use;
The stress relieving agent selects naphthalene disulfonic acid, benzoic sulfimide for use, in benzsulfamide and the o-benzoic sulfimide any one;
Main brightener selects 1 for use, any one in 4-butynediol, alkynol propoxylation compound, diethylin propine, propiolic alcohol, propiolic alcohol propoxylation compound and the oxyethyl group alkynol compound;
Auxiliary is selected any two or more composite with arbitrary proportion in an alkali metal salt of an alkali metal salt of an alkali metal salt, propine sulfonic acid of propine drone an alkali metal salt, butyl ether drone an alkali metal salt, allyl sulphonic acid and vinyl sulfonic acid for use;
Above each component all is dissolved in deionized water or tap water, is made into the total mass umber and is 1000 solution, promptly get the barrel plating electroplate liquid.
2. battery steel shell barrel plating method, the battery steel shell that has been stamped to form is plated preceding skimming treatment by A., B. three steps in sequence of barrel plating and C. plating post-bleach processing are carried out, C step plating post-bleach is handled and carried out successively as follows: three road recovery → cleanings → bleaching → cleaning → neutralization → pure water is washed → antirust → dehydration → drying, citric acid is selected in bleaching for use, oxalic acid, oxyacetic acid, in 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid and the sulfuric acid any one, sodium hydroxide is selected in neutralization for use, in potassium hydroxide and the yellow soda ash any one is characterized in that: used electroplate liquid is a barrel plating as claimed in claim 1 electroplate liquid during B step barrel plating; During barrel plating, the pH value of electroplate liquid is controlled at 4.0～4.6 or 6.5～8.5,40 ℃～70 ℃ of temperature, current density 0.05A/dm
2～3A/dm
2, 4～12 rev/mins of drum rotating speeds, 180～300 minutes barrel plating time.
3. battery steel shell barrel plating method as claimed in claim 2 is characterized in that: skimming treatment is carried out as follows successively before the A step plating:
I. the degreasing of deoiling: with the battery steel shell of degreasing fluid washing electroplated, 50 ± 10 ℃ of wash temperatures, washing time 20～40 minutes, be that 40 ℃～60 ℃ deionized water or tap water cleans up with temperature after finishing, twice so repeatedly, degreasing fluid is by sodium hydroxide, water glass, yellow soda ash, sulfonic acid analog anion surfactants and deionized water are formed, the mass percent concentration of each component is as described below: sodium hydroxide 5%～10%, water glass 2%～8%, yellow soda ash 1%～10%, sulfonic acid analog anion surfactants 2%～5%, tap water or deionized water surplus, sulfonic acid analog anion surfactants is selected sodium laurylsulfonate or Sodium dodecylbenzene sulfonate for use.
Ii acid-wash activation: will finish i step and deoil the battery steel shell of degreasing with acid solution pickling at room temperature 1～3 minute, clean up with deionized water or tap water after finishing, twice so repeatedly, it is 10%～45% hydrochloric acid that pickle solution is selected mass percent concentration for use, or mass percent concentration is 10%～25% sulfuric acid.
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|---|---|---|---|
| CN201010185248.1A CN101864584B (en) | 2010-05-26 | 2010-05-26 | Barrel plating electroplate liquid and battery steel shell method of barrel electroplating |
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| CN101864584B CN101864584B (en) | 2016-08-10 |
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| CN102021619A (en) * | 2010-12-10 | 2011-04-20 | 广州晋惠化工科技有限公司 | Electronickelling alloy solution for improving corrosion resistance of coating |
| CN102534695A (en) * | 2010-12-29 | 2012-07-04 | 京东方科技集团股份有限公司 | Metal substrate for flexible display and preparation method for metal substrate |
| CN105350033A (en) * | 2015-11-24 | 2016-02-24 | 安徽天思朴超精密模具股份有限公司 | Material combination of anticorrosion electroplating liquid and preparation method and application of anticorrosion electroplating liquid |
| CN105506722A (en) * | 2015-12-29 | 2016-04-20 | 上海金杨金属表面处理有限公司 | Battery shell discharge disc barrel plating device |
| CN105696031A (en) * | 2015-12-01 | 2016-06-22 | 江苏九天光电科技有限公司 | Method for manufacturing steel power lithium battery shell by using nickel pre-electroplated steel band |
| CN105951144A (en) * | 2016-06-21 | 2016-09-21 | 贵州振华群英电器有限公司（国营第八九厂） | Nickel plating process for deep-hole part |
| CN109137003A (en) * | 2018-08-09 | 2019-01-04 | 福鼎恒晟金属表面科技有限公司 | A kind of nickel plating technology of clipper |
| CN110484945A (en) * | 2019-09-03 | 2019-11-22 | 福建南平南孚电池有限公司 | Electroplate liquid and use its shell electric plating method to battery |
| CN111005044A (en) * | 2019-12-18 | 2020-04-14 | 宁波韵升股份有限公司 | Dark nickel barrel plating process for improving surface tension of neodymium iron boron magnet |
| CN111074308A (en) * | 2019-12-30 | 2020-04-28 | 福建南平南孚电池有限公司 | Method and device for electroplating nickel-cobalt alloy coating on surface of steel shell |
| CN111155151A (en) * | 2020-01-21 | 2020-05-15 | 福建南平南孚电池有限公司 | Electroplating solution and method for electroplating steel shell by using same |
| CN111398001A (en) * | 2020-04-01 | 2020-07-10 | 中国船舶重工集团公司第七二五研究所 | Method for preparing corrosion pit on metal material sample |
| CN114361592A (en) * | 2021-12-28 | 2022-04-15 | 大连中比动力电池有限公司 | Additive and application thereof in sodium ion battery electrolyte |
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| CN102021619A (en) * | 2010-12-10 | 2011-04-20 | 广州晋惠化工科技有限公司 | Electronickelling alloy solution for improving corrosion resistance of coating |
| CN102534695A (en) * | 2010-12-29 | 2012-07-04 | 京东方科技集团股份有限公司 | Metal substrate for flexible display and preparation method for metal substrate |
| CN102534695B (en) * | 2010-12-29 | 2015-06-17 | 京东方科技集团股份有限公司 | Metal substrate for flexible display and preparation method for metal substrate |
| CN105350033A (en) * | 2015-11-24 | 2016-02-24 | 安徽天思朴超精密模具股份有限公司 | Material combination of anticorrosion electroplating liquid and preparation method and application of anticorrosion electroplating liquid |
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| CN105506722A (en) * | 2015-12-29 | 2016-04-20 | 上海金杨金属表面处理有限公司 | Battery shell discharge disc barrel plating device |
| CN105951144A (en) * | 2016-06-21 | 2016-09-21 | 贵州振华群英电器有限公司（国营第八九厂） | Nickel plating process for deep-hole part |
| CN109137003A (en) * | 2018-08-09 | 2019-01-04 | 福鼎恒晟金属表面科技有限公司 | A kind of nickel plating technology of clipper |
| CN110484945A (en) * | 2019-09-03 | 2019-11-22 | 福建南平南孚电池有限公司 | Electroplate liquid and use its shell electric plating method to battery |
| CN111005044A (en) * | 2019-12-18 | 2020-04-14 | 宁波韵升股份有限公司 | Dark nickel barrel plating process for improving surface tension of neodymium iron boron magnet |
| CN111074308A (en) * | 2019-12-30 | 2020-04-28 | 福建南平南孚电池有限公司 | Method and device for electroplating nickel-cobalt alloy coating on surface of steel shell |
| CN111074308B (en) * | 2019-12-30 | 2021-03-12 | 福建南平南孚电池有限公司 | Method and device for electroplating nickel-cobalt alloy coating on surface of steel shell |
| CN111155151A (en) * | 2020-01-21 | 2020-05-15 | 福建南平南孚电池有限公司 | Electroplating solution and method for electroplating steel shell by using same |
| CN111398001A (en) * | 2020-04-01 | 2020-07-10 | 中国船舶重工集团公司第七二五研究所 | Method for preparing corrosion pit on metal material sample |
| CN114361592A (en) * | 2021-12-28 | 2022-04-15 | 大连中比动力电池有限公司 | Additive and application thereof in sodium ion battery electrolyte |
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