CN105088290A - 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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- CN105088290A CN105088290A CN201510599887.5A CN201510599887A CN105088290A CN 105088290 A CN105088290 A CN 105088290A CN 201510599887 A CN201510599887 A CN 201510599887A CN 105088290 A CN105088290 A CN 105088290A
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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 stratiform tin coating is prepared in galvanic deposit.
Background technology
Tin is a kind of silvery white metal, has fusing point low (232 DEG C), the features such as ductility is high, easy polishing.Tin coating is to humid climate, and water-soluble salt solution and weak acid all have good erosion resistance, can form alloy with many metals, therefore, is widely used in the industries such as tinplate, alloy manufacture, printed circuit board (PCB), five metals.
Common the solution of electrotinning is divided into acid tin plating liquid and the large class of Alkaline Tin Plating Solntion two.In Alkaline Tin Plating Solntion, tin exists with the stannate radicle ion of tetravalence, and in acidity tin plating electrolyte, tin ion exists with the form of divalent cation.Vitriol tin plating technique is little and at room temperature can carry out plating because composition is simple, raw material is easy to get, with low cost, sedimentation velocity is fast, current efficiency is high, to equipment corrosion, and becomes the first-selection of bright tin plating layer.In traditional tin plating technique, no matter adopt Acidic Sn electroplating system or alkaline tin plating system, what obtain is all the fine and close coating of light, and the fine and close tin coating of light easily there is efflorescence as during lithium ion battery negative pole, thus affects cycle performance of battery.
Summary of the invention
The present invention will solve the problem being bright close coating prepared by existing tin plating method, provides a kind of galvanic deposit to prepare the method for stratiform tin coating.
The method that stratiform tin coating is prepared in a kind of galvanic deposit of the present invention is:
By plating piece alkaline degreasing, washing, pickling, then wash, after drying, obtain the negative electrode electroplated, the anode using simple substance tin as plating; The current density of plating is 2 ~ 5A/dm
2, electroplating temperature is 10 ~ 35 DEG C, and electroplating time is 3 ~ 9min, namely obtains stratiform tin coating; Wherein plating solution comprises stannous sulfate, the vitriol oil, gelatin, additive and xitix, in plating solution, the final concentration of stannous sulfate is 35 ~ 45g/L, the final concentration of the vitriol oil is 180 ~ 182g/L, the final concentration of gelatin is 0.2 ~ 1.0g/L, the final concentration of additive is 0.2 ~ 1.6mL/L, and the final concentration of xitix is 0.3 ~ 0.5g/L.
The present invention's tin coating with laminate structure that adopted the method for galvanic deposit to prepare, plating solution composition is simple, and electroplating technology is easy to control.Stratiform tin coating prepared by the present invention is compared with the tin coating of light densification, and specific surface area is larger, therefore can increase embedding lithium capacity.And due to the easy efflorescence distortion in working cycle of the tin coating of densification, cycle performance is poor, and laminate structure effectively can suppress the volumetric expansion of negative pole in charge and discharge process, therefore not easily deformation, improves the cycle performance of lithium ion battery.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of stratiform tin coating prepared by embodiment 1.
Embodiment
Embodiment one: the method that stratiform tin coating is prepared in a kind of galvanic deposit of present embodiment is: by plating piece alkaline degreasing, washing, pickling, then wash, obtains the negative electrode electroplated after drying, the anode using simple substance tin as plating; The current density of plating is 2 ~ 5A/dm
2, electroplating temperature is 10 ~ 35 DEG C, and electroplating time is 3 ~ 9min, namely obtains stratiform tin coating; Wherein plating solution comprises stannous sulfate, the vitriol oil, gelatin, additive and xitix, in plating solution, the final concentration of stannous sulfate is 35 ~ 45g/L, the final concentration of the vitriol oil is 180 ~ 182g/L, the final concentration of gelatin is 0.2 ~ 1.0g/L, the final concentration of additive is 0.2 ~ 1.6mL/L, and the final concentration of xitix is 0.3 ~ 0.5g/L.
Present embodiment adopts the method for galvanic deposit to prepare the tin coating with laminate structure, and plating solution composition is simple, and electroplating technology is easy to control.Stratiform tin coating prepared by present embodiment is compared with the tin coating of light densification, and specific surface area is larger, therefore can increase embedding lithium capacity.And due to the easy efflorescence distortion in working cycle of the tin coating of densification, cycle performance is poor.And laminate structure effectively can suppress the volumetric expansion of negative pole in charge and discharge process, therefore not easily deformation, improves the cycle performance of lithium ion battery.
Embodiment two: present embodiment and embodiment one unlike: be adopt mass concentration to be that the aqueous solution of 20%HCl carries out pickling.Other is identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two unlike: in described plating solution, the final concentration of stannous sulfate is 40g/L.Other is identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three unlike: in described plating solution, the final concentration of the vitriol oil is 181g/L.Other is identical with one of embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four unlike: in described plating solution, the final concentration of gelatin is 0.6g/L.Other is identical with one of embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five unlike: in described plating solution, the final concentration of additive is 0.8mL/L.Other is identical with one of embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six unlike: in described plating solution, the final concentration of gelatin is 0.4g/L.Other is identical with one of embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven unlike: in described plating solution, the final concentration of gelatin is 0.8g/L.Other is identical with one of embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight unlike: in described plating solution, the final concentration of additive is 1.2mL/L.Other is identical with one of embodiment one to eight.
Embodiment ten: one of present embodiment and embodiment one to nine unlike: in described plating solution, the final concentration of additive is 1.4mL/L.Other is identical with one of embodiment one to nine.
Embodiment 11: one of present embodiment and embodiment one to ten unlike: described additive by benzylideneacetone, ethanol, formaldehyde, ethyl acetate and dimethylsilane alcohol in molar ratio for the ratio of 6:3:1:1:1 forms.Other is identical with one of embodiment one to ten.
Embodiment 12: one of present embodiment and embodiment one to ten one unlike: in plating solution, the final concentration of xitix is 0.4g/L.Other is identical with one of embodiment one to ten one.
Embodiment 13: one of present embodiment and embodiment one to ten two unlike: described plating solution compound method is: the vitriol oil is poured into water dilution, leave standstill, to be cooled to room temperature, obtain sulphuric acid soln; Stannous sulfate is soluble in water, add xitix, stir, put into Ultrasonic Cleaners and disperse, obtain mixture; Mixture is poured in sulphuric acid soln, stir 12h, filter, in filtrate, add gelatin and additive, stir, namely prepared.Other is identical with one of embodiment one to ten two.
Embodiment 14: one of present embodiment and embodiment one to ten three unlike: the distance between described negative electrode and anode is 2cm.Other is identical with one of embodiment one to ten three.
The following examples will be further described the present invention, but not thereby limiting the invention.
Embodiment 1: the method that stratiform tin coating is prepared in the present embodiment galvanic deposit is: by plating piece alkaline degreasing, washing, be that the 20%HCl aqueous solution carries out pickling by mass concentration, wash again, obtain the negative electrode electroplated after drying, the anode using simple substance tin as plating, the distance between anode and cathode is 2cm; The current density of plating is 3A/dm
2, electroplating temperature is 10 DEG C, and electroplating time is 3min, namely obtains stratiform tin coating; Wherein plating solution comprises stannous sulfate, the vitriol oil, gelatin, additive and xitix, in plating solution, the final concentration of stannous sulfate is 40g/L, the final concentration of the vitriol oil is 181g/L, and the final concentration of gelatin is 0.6g/L, the final concentration of additive is 1.2mL/L, and the final concentration of xitix is 0.4g/L.
As shown in Figure 1, this coating has obvious laminate structure to the stereoscan photograph of stratiform tin coating prepared by the present embodiment as seen from Figure 1.
The method that embodiment 2, the present embodiment galvanic deposit prepare stratiform tin coating is: by plating piece alkaline degreasing, washing, be that the 20%HCl aqueous solution carries out pickling by mass concentration, wash again, obtain the negative electrode electroplated after drying, the anode using simple substance tin as plating, the distance between anode and cathode is 2cm; The current density of plating is 1.5A/dm
2, electroplating temperature is 20 DEG C, and electroplating time is 6min, namely obtains stratiform tin coating; Wherein plating solution comprises stannous sulfate, the vitriol oil, gelatin, additive and xitix, in plating solution, the final concentration of stannous sulfate is 40g/L, the final concentration of the vitriol oil is 181g/L, and the final concentration of gelatin is 0.4g/L, the final concentration of additive is 0.8mL/L, and the final concentration of xitix is 0.4g/L.Tin coating prepared by the present embodiment has obvious laminate structure.
The method that embodiment 3, the present embodiment galvanic deposit prepare stratiform tin coating is: by plating piece alkaline degreasing, washing, be that the 20%HCl aqueous solution carries out pickling by mass concentration, wash again, obtain the negative electrode electroplated after drying, the anode using simple substance tin as plating, the distance between anode and cathode is 2cm; The current density of plating is 4.5A/dm
2, electroplating temperature is 30 DEG C, and electroplating time is 9min, namely obtains stratiform tin coating; Wherein plating solution comprises stannous sulfate, the vitriol oil, gelatin, additive and xitix, in plating solution, the final concentration of stannous sulfate is 40g/L, the final concentration of the vitriol oil is 181/L, and the final concentration of gelatin is 0.8g/L, the final concentration of additive is 1.4mL/L, and the final concentration of xitix is 0.4g/L.Tin coating prepared by the present embodiment has obvious laminate structure.
The ratio that additive in embodiment 1 ~ 3 is 6:3:1:1:1 by benzylideneacetone, ethanol, formaldehyde, ethyl acetate and dimethylsilane alcohol in molar ratio forms.
Embodiment 1 ~ 3 adopts the method for galvanic deposit to prepare the tin coating with laminate structure, and plating solution composition is simple, and electroplating technology is easy to control.
Claims (9)
1. a method for stratiform tin coating is prepared in galvanic deposit, it is characterized in that the method is: by plating piece alkaline degreasing, washing, pickling, then wash, and obtains the negative electrode electroplated after drying, the anode using simple substance tin as plating; The current density of plating is 2 ~ 5A/dm
2, electroplating temperature is 10 ~ 35 DEG C, and electroplating time is 3 ~ 9min, namely obtains stratiform tin coating; Wherein plating solution comprises stannous sulfate, the vitriol oil, gelatin, additive and xitix, in plating solution, the final concentration of stannous sulfate is 35 ~ 45g/L, the final concentration of the vitriol oil is 180 ~ 182g/L, the final concentration of gelatin is 0.2 ~ 1.0g/L, the final concentration of additive is 0.2 ~ 1.6mL/L, and the final concentration of xitix is 0.3 ~ 0.5g/L.
2. the method for stratiform tin coating is prepared in a kind of galvanic deposit according to claim 1, it is characterized in that the final concentration of stannous sulfate in described plating solution is 40g/L.
3. the method for stratiform tin coating is prepared in a kind of galvanic deposit according to claim 1, it is characterized in that the final concentration of the vitriol oil in described plating solution is 181g/L.
4. the method for stratiform tin coating is prepared in a kind of galvanic deposit according to claim 1, it is characterized in that the final concentration of gelatin in described plating solution is 0.6g/L.
5. the method for stratiform tin coating is prepared in a kind of galvanic deposit according to claim 1, it is characterized in that the final concentration of additive in described plating solution is 0.8mL/L.
6. the method for stratiform tin coating is prepared in a kind of galvanic deposit according to claim 1 or 5, it is characterized in that described additive by benzylideneacetone, ethanol, formaldehyde, ethyl acetate and dimethylsilane alcohol in molar ratio for the ratio of 6:3:1:1:1 forms.
7. the method for stratiform tin coating is prepared in a kind of galvanic deposit according to claim 1, it is characterized in that the final concentration of xitix in described plating solution is 0.4g/L.
8. the method for stratiform tin coating is prepared in a kind of galvanic deposit according to claim 1, it is characterized in that described plating solution compound method is: the vitriol oil is poured into water dilution, leaves standstill, to be cooled to room temperature, obtains sulphuric acid soln; Stannous sulfate is soluble in water, add xitix, stir, put into Ultrasonic Cleaners and disperse, obtain mixture; Mixture is poured in sulphuric acid soln, stir 12h, filter, in filtrate, add gelatin and additive, stir, namely prepared.
9. the method for stratiform tin coating is prepared in a kind of galvanic deposit according to claim 1, it is characterized in that the distance between described negative electrode and anode is 2cm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| US10995797B2 (en) | 2017-07-05 | 2021-05-04 | Aktiebolaget Skf | Electroplated component of a rolling element bearing |
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| CN104716313A (en) * | 2015-03-16 | 2015-06-17 | 哈尔滨工业大学 | Preparation method for tin-based/graphene composite anode material of lithium ion battery |
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| JPH05106091A (en) * | 1991-10-15 | 1993-04-27 | Nippon Steel Corp | Material for welded can excellent in seam weldability and adhesive strength of paint |
| CN104716313A (en) * | 2015-03-16 | 2015-06-17 | 哈尔滨工业大学 | Preparation method for tin-based/graphene composite anode material of lithium ion battery |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105714347A (en) * | 2015-09-30 | 2016-06-29 | 安徽中盛罐业有限公司 | Tin case surface tinning process |
| US10995797B2 (en) | 2017-07-05 | 2021-05-04 | Aktiebolaget Skf | Electroplated component of a rolling element bearing |
| 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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| CN105088290B (en) | 2017-04-26 |
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