CN105088290B - Method for preparing layered tin coatings in electrolytic deposition manner - Google Patents
Method for preparing layered tin coatings in electrolytic deposition manner Download PDFInfo
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- CN105088290B CN105088290B CN201510599887.5A CN201510599887A CN105088290B CN 105088290 B CN105088290 B CN 105088290B CN 201510599887 A CN201510599887 A CN 201510599887A CN 105088290 B CN105088290 B CN 105088290B
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Abstract
The invention relates to a method for preparing layered tin coatings in an electrolytic deposition manner. According to the method, the problem that an existing tinning method can only prepare bright compact coatings is solved. The method comprises the steps of removing oil on a coated part in an alkaline manner, rinsing the coated part, and pickling the coated part; then rinsing the coated part again, and drying the coated part to obtain an electroplating negative pole and using elementary substance tin as an electroplating positive pole; and setting the electroplating current density as 2-5A/dm<2>, the electroplating temperature as 10-35 DEG C and the electroplating time as 3-9min to obtain the layered tin coatings. Plating solution comprises stannous mono sulphate, concentrated sulfuric acid, gelatin, additive and ascorbic acid. The method can be used for preparing tin coatings of a layered structure in the electrolytic deposition manner, the plating solution is simple in composition, and the electroplating process is easy to control. The method is applied to the field of material preparing.
Description
Technical field
The present invention relates to a kind of method that electro-deposition prepares stratiform tin coating.
Background technology
Stannum is a kind of silvery white non-ferrous metal, and with fusing point low (232 DEG C), ductility is high, the features such as easily polish.Tin coating is to tide
Dampness is waited, and water-soluble salt solution and weak acid are respectively provided with preferable corrosion resistance, can form alloy with many metals, therefore, extensively
It is applied to the industries such as tinplate, alloy manufacture, printed circuit board (PCB), five metals.
Common the solution of electrotinning is divided into two big class of acid tin plating liquid and Alkaline Tin Plating Solntion.In Alkaline Tin Plating Solntion, stannum is with four
What the stannic acid radical ion of valency was present, and in acidity tin plating electrolyte, tin ion is in the form of bivalent cation.Sulfate is plated
Process of tin as composition is simple, raw material is easy to get, with low cost, deposition velocity is fast, current efficiency is high, it is little to equipment corrosion and can be
Plating is carried out under room temperature, and becomes the first-selection of bright tin plating layer.In traditional tin plating technique, no matter using Acidic Sn electroplating system also
It is alkaline tin plating system, what is obtained is bright fine and close coating, and the fine and close tin coating of light is as lithium ion battery negative pole
When be susceptible to efflorescence, so as to affect cycle performance of battery.
The content of the invention
The present invention is to solve the problem for being bright close coating prepared by existing tin plating method, there is provided a kind of electro-deposition
The method for preparing stratiform tin coating.
A kind of electro-deposition of the present invention prepares the method for stratiform tin coating：
By plating piece alkaline degreasing, washing, pickling, then wash, the negative electrode electroplated is obtained after being dried, using simple substance stannum as plating
Anode；The electric current density of plating is 2～5A/dm2, electroplating temperature is 10～35 DEG C, and electroplating time is 3～9min, that is, obtain
Stratiform tin coating；Wherein plating solution includes stannous sulfate, concentrated sulphuric acid, gelatin, additive and ascorbic acid, stannous sulfate in plating solution
Final concentration of 35～45g/L, the final concentration of 180～182g/L of concentrated sulphuric acid, the final concentration of 0.2～1.0g/L of gelatin, addition
Final concentration of 0.2～the 1.6mL/L of agent, the final concentration of 0.3～0.5g/L of ascorbic acid.
The present invention is prepared for the tin coating with layer structure using the method for electro-deposition, and plating solution composition is simple, galvanizer
Skill is easily controllable., compared with bright fine and close tin coating, specific surface area is bigger, therefore can increase for stratiform tin coating prepared by the present invention
Big embedding lithium capacity.And the easy efflorescence deformation in cyclic process due to fine and close tin coating, cycle performance is poor, and layer structure can have
Effect suppresses the volumetric expansion of negative pole in charge and discharge process, therefore is difficult deformation, improves the cycle performance of lithium ion battery.
Description of the drawings
Fig. 1 is the stereoscan photograph of stratiform tin coating prepared by embodiment 1.
Specific embodiment
Specific embodiment one：A kind of electro-deposition of present embodiment prepares the method for stratiform tin coating：By plating piece alkalescence
Oil removing, washing, pickling, then wash, the negative electrode electroplated is obtained after being dried, using simple substance stannum as the anode of plating；The electric current of plating
Density is 2～5A/dm2, electroplating temperature is 10～35 DEG C, and electroplating time is 3～9min, that is, obtain stratiform tin coating；Wherein plate
Liquid includes stannous sulfate, concentrated sulphuric acid, gelatin, additive and ascorbic acid, the final concentration of 35～45g/ of stannous sulfate in plating solution
L, the final concentration of 180～182g/L of concentrated sulphuric acid, the final concentration of 0.2～1.0g/L of gelatin, final concentration of the 0.2 of additive～
1.6mL/L, the final concentration of 0.3～0.5g/L of ascorbic acid.
Present embodiment is prepared for the tin coating with layer structure using the method for electro-deposition, and plating solution composition is simple, electricity
Depositing process is easily controllable., compared with bright fine and close tin coating, specific surface area is bigger for stratiform tin coating prepared by present embodiment,
Therefore embedding lithium capacity can be increased.And in cyclic process, easy efflorescence deforms due to fine and close tin coating, cycle performance is poor.And stratiform
Structure can effectively suppress the volumetric expansion of negative pole in charge and discharge process, therefore be difficult deformation, improve the circulation of lithium ion battery
Performance.
Specific embodiment two：Present embodiment from unlike specific embodiment one：Be adopt mass concentration for
The aqueous solution of 20%HCl carries out pickling.Other are identical with specific embodiment one.
Specific embodiment three：Present embodiment from unlike specific embodiment one or two：Sulfur in described plating solution
The final concentration of 40g/L of sour stannous.Other are identical with specific embodiment one or two.
Specific embodiment four：Unlike one of present embodiment and specific embodiment one to three：Described plating solution
The final concentration of 181g/L of middle concentrated sulphuric acid.Other are identical with one of specific embodiment one to three.
Specific embodiment five：Unlike one of present embodiment and specific embodiment one to four：Described plating solution
The final concentration of 0.6g/L of middle gelatin.Other are identical with one of specific embodiment one to four.
Specific embodiment six：Unlike one of present embodiment and specific embodiment one to five：Described plating solution
The final concentration of 0.8mL/L of middle additive.Other are identical with one of specific embodiment one to five.
Specific embodiment seven：Unlike one of present embodiment and specific embodiment one to six：Described plating solution
The final concentration of 0.4g/L of middle gelatin.Other are identical with one of specific embodiment one to six.
Specific embodiment eight：Unlike one of present embodiment and specific embodiment one to seven：Described plating solution
The final concentration of 0.8g/L of middle gelatin.Other are identical with one of specific embodiment one to seven.
Specific embodiment nine：Unlike one of present embodiment and specific embodiment one to eight：Described plating solution
The final concentration of 1.2mL/L of middle additive.Other are identical with one of specific embodiment one to eight.
Specific embodiment ten：Unlike one of present embodiment and specific embodiment one to nine：Described plating solution
The final concentration of 1.4mL/L of middle additive.Other are identical with one of specific embodiment one to nine.
Specific embodiment 11：Unlike one of present embodiment and specific embodiment one to ten：Described adds
Plus agent be by benzylideneacetone, ethanol, formaldehyde, ethyl acetate and dimethyl silane alcohol in molar ratio be 6:3:1:1:1 ratio
Composition.Other are identical with one of specific embodiment one to ten.
Specific embodiment 12：Unlike one of present embodiment and specific embodiment one to ten one：In plating solution
The final concentration of 0.4g/L of ascorbic acid.Other are identical with one of specific embodiment one to ten one.
Specific embodiment 13：Unlike one of present embodiment and specific embodiment one to ten two：Described
Plating liquid making method is：Concentrated sulphuric acid is poured into water into dilution, is stood, is cooled to room temperature, obtains sulfuric acid solution；By stannous sulfate
It is soluble in water, add ascorbic acid, stirring to disperse in being put into ultrasonic washing unit, obtain mixture；Pour the mixture into sulphuric acid
In solution, 12h is stirred, filtered, gelatin and additive are added in filtrate, is stirred, that is, prepared and complete.Other and concrete reality
Apply one of mode one to ten two identical.
Specific embodiment 14：Unlike one of present embodiment and specific embodiment one to ten three：Described
The distance between negative electrode and anode are 2cm.Other are identical with one of specific embodiment one to ten three.
The following examples will be further described to the present invention, but not thereby limiting the invention.
Embodiment 1：The present embodiment electro-deposition prepares the method for stratiform tin coating：By plating piece alkaline degreasing, wash, use matter
Amount concentration carries out pickling for 20%HCl aqueous solutions, then washes, and obtains the negative electrode electroplated, using simple substance stannum as plating after being dried
The distance between anode, anode and cathode are 2cm；The electric current density of plating is 3A/dm2, electroplating temperature is 10 DEG C, and electroplating time is
3min, that is, obtain stratiform tin coating；Wherein plating solution includes stannous sulfate, concentrated sulphuric acid, gelatin, additive and ascorbic acid, plating solution
The final concentration of 40g/L of middle stannous sulfate, the final concentration of 181g/L of concentrated sulphuric acid, the final concentration of 0.6g/L of gelatin, additive
Final concentration of 1.2mL/L, the final concentration of 0.4g/L of ascorbic acid.
The stereoscan photograph of stratiform tin coating manufactured in the present embodiment is as shown in figure 1, the coating has as seen from Figure 1
There is obvious layer structure.
Embodiment 2, the present embodiment electro-deposition prepare the method for stratiform tin coating：By plating piece alkaline degreasing, wash, use matter
Amount concentration carries out pickling for 20%HCl aqueous solutions, then washes, and obtains the negative electrode electroplated, using simple substance stannum as plating after being dried
The distance between anode, anode and cathode are 2cm；The electric current density of plating is 1.5A/dm2, electroplating temperature is 20 DEG C, and electroplating time is
6min, that is, obtain stratiform tin coating；Wherein plating solution includes stannous sulfate, concentrated sulphuric acid, gelatin, additive and ascorbic acid, plating solution
The final concentration of 40g/L of middle stannous sulfate, the final concentration of 181g/L of concentrated sulphuric acid, the final concentration of 0.4g/L of gelatin, additive
Final concentration of 0.8mL/L, the final concentration of 0.4g/L of ascorbic acid.Tin coating manufactured in the present embodiment has obvious stratiform knot
Structure.
Embodiment 3, the present embodiment electro-deposition prepare the method for stratiform tin coating：By plating piece alkaline degreasing, wash, use matter
Amount concentration carries out pickling for 20%HCl aqueous solutions, then washes, and obtains the negative electrode electroplated, using simple substance stannum as plating after being dried
The distance between anode, anode and cathode are 2cm；The electric current density of plating is 4.5A/dm2, electroplating temperature is 30 DEG C, and electroplating time is
9min, that is, obtain stratiform tin coating；Wherein plating solution includes stannous sulfate, concentrated sulphuric acid, gelatin, additive and ascorbic acid, plating solution
The final concentration of 40g/L of middle stannous sulfate, the final concentration of 181/L of concentrated sulphuric acid, the final concentration of 0.8g/L of gelatin, additive
Final concentration of 1.4mL/L, the final concentration of 0.4g/L of ascorbic acid.Tin coating manufactured in the present embodiment has obvious stratiform knot
Structure.
Additive in embodiment 1～3 be by benzylideneacetone, ethanol, formaldehyde, ethyl acetate and dimethyl silane alcohol by
Mol ratio is 6:3:1:1:1 ratio composition.
Embodiment 1～3 is prepared for the tin coating with layer structure using the method for electro-deposition, and plating solution composition is simple, electricity
Depositing process is easily controllable.
Claims (8)
1. a kind of method that electro-deposition prepares stratiform tin coating, it is characterised in that the method is：By plating piece alkaline degreasing, washing,
Pickling, then wash, the negative electrode electroplated is obtained after being dried, using simple substance stannum as the anode of plating；The electric current density of plating be 2～
5A/dm2, electroplating temperature is 10～35 DEG C, and electroplating time is 3～9min, that is, obtain stratiform tin coating；Wherein plating solution includes sulphuric acid
Stannous, concentrated sulphuric acid, gelatin, additive and ascorbic acid, the final concentration of 35～45g/L of stannous sulfate in plating solution, concentrated sulphuric acid
Final concentration of 180～182g/L, the final concentration of 0.2～1.0g/L of gelatin, the final concentration of 0.2～1.6mL/L of additive, resist
Final concentration of 0.3～the 0.5g/L of bad hematic acid；Described additive is by benzylideneacetone, ethanol, formaldehyde, ethyl acetate and diformazan
Base silanol is 6 in molar ratio:3:1:1:1 ratio composition.
2. the method that a kind of electro-deposition according to claim 1 prepares stratiform tin coating, it is characterised in that described plating solution
The final concentration of 40g/L of middle stannous sulfate.
3. the method that a kind of electro-deposition according to claim 1 prepares stratiform tin coating, it is characterised in that described plating solution
The final concentration of 181g/L of middle concentrated sulphuric acid.
4. the method that a kind of electro-deposition according to claim 1 prepares stratiform tin coating, it is characterised in that described plating solution
The final concentration of 0.6g/L of middle gelatin.
5. the method that a kind of electro-deposition according to claim 1 prepares stratiform tin coating, it is characterised in that described plating solution
The final concentration of 0.8mL/L of middle additive.
6. the method that a kind of electro-deposition according to claim 1 prepares stratiform tin coating, it is characterised in that described plating solution
The final concentration of 0.4g/L of middle ascorbic acid.
7. the method that a kind of electro-deposition according to claim 1 prepares stratiform tin coating, it is characterised in that described plating solution
Compound method is：Concentrated sulphuric acid is poured into water into dilution, is stood, is cooled to room temperature, obtains sulfuric acid solution；Stannous sulfate is dissolved in
In water, ascorbic acid, stirring is added to disperse in being put into ultrasonic washing unit, obtain mixture；Pour the mixture into sulfuric acid solution
In, 12h is stirred, is filtered, gelatin and additive are added in filtrate, is stirred, that is, prepared and complete.
8. the method that a kind of electro-deposition according to claim 1 prepares stratiform tin coating, it is characterised in that described negative electrode
It is 2cm with the distance between anode.
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| CN105714347A (en) * | 2015-09-30 | 2016-06-29 | 安徽中盛罐业有限公司 | Tin case surface tinning process |
| CN108277508A (en) * | 2018-01-08 | 2018-07-13 | 河北师范大学 | A method of preparing tin lithium cell cathode material |
| CN111188069A (en) * | 2019-12-31 | 2020-05-22 | 大连长丰实业总公司 | Tin-plated bismuth alloy solution and preparation method thereof |
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| CN104716313B (en) * | 2015-03-16 | 2016-11-30 | 哈尔滨工业大学 | The preparation method of tinbase/graphene lithium ion battery composite negative pole material |
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