CN109680310A - A kind of nickel antimony electroplating solution and preparation method thereof - Google Patents

A kind of nickel antimony electroplating solution and preparation method thereof Download PDF

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Publication number
CN109680310A
CN109680310A CN201910007990.4A CN201910007990A CN109680310A CN 109680310 A CN109680310 A CN 109680310A CN 201910007990 A CN201910007990 A CN 201910007990A CN 109680310 A CN109680310 A CN 109680310A
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nickel
electroplating solution
acid
electroplate liquid
salt
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CN109680310B (en
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郑小美
张朋越
黄凌
屠国平
陶姗
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JIANGSU OLITER ENERGY TECHNOLOGY CO LTD
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China Jiliang University
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/56Electroplating: Baths therefor from solutions of alloys
    • C25D3/562Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/56Electroplating: Baths therefor from solutions of alloys

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating And Plating Baths Therefor (AREA)

Abstract

The present invention relates to electroplating technologies, more particularly to a kind of nickel antimony electroplating solution and preparation method thereof, the electroplate liquid contains boric acid, sodium hypophosphite, complexing agent and suitable quantity of water, the electroplate liquid also contains nickel salt and antimonic salt, and the electroplate liquid each component and its content are boric acid 20-80g/L, sodium hypophosphite 10-80g/L, complexing agent 10-80g/L, nickel salt 1-20g/L and antimonic salt 1-10g/L.Uniform nickel antimony coating is obtained using electro-plating method, in beautiful color, specific capacity is high, and the stability of electroplate liquid is good.

Description

A kind of nickel antimony electroplating solution and preparation method thereof
Technical field
The present invention relates to electroplating technologies, and in particular to a kind of nickel antimony electroplating solution and preparation method thereof.
Background technique
Plating have at low cost, simple process, it is easy to operate the advantages that, in life using very extensive.Dan Jin is electroplated Belong to far from meets modernize to functional material the needs of.Therefore, the rapid development of plating multicomponent alloy in recent years, type Various, excellent material performance has been widely used for magnetic industry, energy field etc. at present.
The theoretical capacity of antimony is up to 660mAh/g, and much higher than current commercialization carbon material, antimony and nickel antimony alloy are a kind of The extraordinary energy and material of prospect.Currently, the method for preparing nickel antimony alloy mainly has hydro-thermal method, cross-linking reaction method etc., and these Preparation method has the shortcomings that at high cost, the reaction time is long, is not easy large-scale production application.Therefore, the electricity for seeking low cost is heavy The nickel antimony alloy that product technology prepares height ratio capacity is of great significance.
Summary of the invention
The purpose of the present invention is to solve the above problem, a kind of nickel antimony electroplating solution and preparation method thereof is provided.The plating Liquid is free of corrosive substance, safety and environmental protection, and chemical stability is high, and preparation process is simply controllable, and stability is good.
In order to achieve the above object of the invention, the invention adopts the following technical scheme:
A kind of nickel antimony electroplating solution, containing boric acid, sodium hypophosphite, complexing agent and suitable quantity of water, the electroplate liquid also contains nickel Salt and antimonic salt, the electroplate liquid each component and its content are boric acid 20-80g/L, sodium hypophosphite 10-80g/L, complexing agent 10- 80g/L, nickel salt 1-20g/L and antimonic salt 1-10g/L.
Further, the electroplate liquid each component and its content are boric acid 40g/L, sodium hypophosphite 40g/L, complexing agent 60g/L, nickel salt 10g/L and antimonic salt 4g/L.
Further, the nickel salt is sulfate or chlorate.
Further, the antimonic salt is potassium antimony tartrate or antimony chloride.
Further, the complexing agent is sodium acetate, acetic acid ammonia, citric acid or ethylenediamine tetra-acetic acid.
Further, the pH value of the electroplate liquid is 0.5-3.0.
Further, the operating temperature of the electroplate liquid is 10-50 DEG C.
Further, the electroplate liquid further includes additive, and additive is tin tetrabromide and 4-dimethylaminopyridine, specifically Content is tin tetrabromide 2-5g/L and 4-dimethylaminopyridine 3-8g/L.Since the electroplate liquid is the alloy plating of nickel salt and antimonic salt Liquid, therefore above two substance is added, on the one hand purpose is the stability improved in storing process, be on the other hand to improve electricity Plating solution depositing homogeneous in the plating process and stability.
Further, the electroplate liquid further includes tartaric acid and sodium tartrate, the content difference of tartaric acid and sodium tartrate For 1-2g/L and 0.5-1g/L.Purpose is that the electroplate liquid is made to have stable polarization curve, it is ensured that is had during electro-deposition There is stably and controllable property, to improve the uniform and stable property of final products.
A kind of preparation method of nickel antimony electroplating solution, comprising the following steps:
(1) boric acid 20-80g, sodium hypophosphite 10-80g, complexing agent 10-80g, stirring and dissolving are added into deionized water Mixed liquor is made;
(2) pH for being adjusted with acid mixed liquor is 1.0-3.0;
(3) nickel salt 1-20g, antimonic salt 1-10g are added in Xiang Shangshu mixed liquor, stirring and dissolving adds the deionization of surplus Water is settled to 1L, and adjusting pH of mixed is 0.5-3.0, obtains antimony electroplating solution.
Further, acid described in step (2) is hydrochloric acid or sulfuric acid.
Compared with prior art, the present invention beneficial effect is: obtaining uniform nickel antimony coating, color beauty using electro-plating method It sees, specific capacity is high, and the stability of electroplate liquid is good.The electroplate liquid of the proportion has relatively stable polarization curve, can Cooperation obtains the preferably uniform product of performance reproducibility using relatively simple operation.
Specific embodiment
Below by specific embodiment the technical scheme of the present invention will be further described explanation.
If raw material employed in the embodiment of the present invention is raw material commonly used in the art without specified otherwise, implement Method employed in example, is the conventional method of this field.
Embodiment 1:
A kind of nickel antimony electroplating solution the preparation method is as follows:
Boric acid 20g, sodium hypophosphite 10g, complexing agent (sodium acetate) 10g are added into deionized water, stirring and dissolving is made Mixed liquor adjusts pH=1.0 with HCl, and potassium antimony tartrate 1g, nickel chloride 1g are added into mixed liquor, and stirring and dissolving adds remaining The deionized water of amount to total volume is 1L, and adjusting pH is 0.5, obtains nickel antimony electroplating solution.
Embodiment 2:
A kind of nickel antimony electroplating solution the preparation method is as follows:
Boric acid 80g, sodium hypophosphite 80g, complexing agent (acetic acid ammonia) 80g are added into deionized water, stirring and dissolving is made Mixed liquor adjusts pH=3.0 with HCl, and potassium antimony tartrate 10g, nickel sulfate 20g are added into mixed liquor, and stirring and dissolving adds The deionized water of surplus to total volume is 1L, and adjusting pH is 3.0, obtains nickel antimony electroplating solution.
Embodiment 3:
A kind of nickel antimony electroplating solution the preparation method is as follows:
Boric acid 40g, sodium hypophosphite 40g, complexing agent (sodium acetate) 60g are added into deionized water, stirring and dissolving is made Mixed liquor adjusts pH=2.0 with HCl, and potassium antimony tartrate 4g, nickel chloride 10g are added into mixed liquor, and stirring and dissolving adds The deionized water of surplus to total volume is 1L, and adjusting pH is 1.5, obtains nickel antimony electroplating solution.
Embodiment 4:
A kind of nickel antimony electroplating solution the preparation method is as follows:
Boric acid 60g, sodium hypophosphite 20g, complexing agent (citric acid) 20g are added into deionized water, stirring and dissolving is made Mixed liquor adjusts pH=1.0 with HCl, and potassium antimony tartrate 6g, nickel sulfate 5g are added into mixed liquor, and stirring and dissolving adds remaining The deionized water of amount to total volume is 1L, and adjusting pH is 1.0, obtains nickel antimony electroplating solution.
Embodiment 5:
A kind of nickel antimony electroplating solution the preparation method is as follows:
Boric acid 40g, sodium hypophosphite 60g, complexing agent (ethylenediamine tetra-acetic acid) 40g are added into deionized water, stirs molten Mixed liquor is made in solution, adjusts pH=3.0 with HCl, the addition potassium antimony tartrate 6g into mixed liquor, nickel chloride 10g, stirring and dissolving, Deionized water to the total volume for adding surplus is 1L, and adjusting pH is 1.5, obtains nickel antimony electroplating solution.
Embodiment 6:
A kind of nickel antimony electroplating solution the preparation method is as follows:
Boric acid 40g, sodium hypophosphite 40g, complexing agent (citric acid) 60g are added into deionized water, stirring and dissolving is made Mixed liquor adjusts pH=2.0 with HCl, and potassium antimony tartrate 4g, nickel chloride 20g are added into mixed liquor, and stirring and dissolving adds The deionized water of surplus to total volume is 1L, and adjusting pH is 1.5, obtains nickel antimony electroplating solution.
Embodiment 7:
On the basis of embodiment 5, tin tetrabromide 2g/L, 4-dimethylaminopyridine 8g/L is added, opportunity same boric acid is added It is equivalent.
Embodiment 8:
On the basis of embodiment 6, tin tetrabromide 5g/L, 4-dimethylaminopyridine 3g/L is added, opportunity same boric acid is added It is equivalent.
Embodiment 9:
On the basis of embodiment 5, tin tetrabromide 3g/L, 4-dimethylaminopyridine 5g/L is added, while tartaric acid is added It is equivalent with boric acid that opportunity is added in 2g/L and sodium tartrate 1g/L.
Embodiment 10:
On the basis of embodiment 6, tin tetrabromide 4g/L, 4-dimethylaminopyridine 7g/L is added, while tartaric acid is added It is equivalent with boric acid that opportunity is added in 1g/L and sodium tartrate 0.5g/L.
The nickel antimony coating that embodiment 1-6 is obtained is uniform, and in beautiful color, specific capacity is relatively high.
Embodiment 7-10 is further to improve, existing since the electroplate liquid is the electroplate liquid based on nickel salt and antimonic salt Complexing agent can not improve the stability of storage, it is therefore desirable to be modified to its storage stability, to reduce storage time Influence to its plating performance.Meanwhile the electroplate liquid of embodiment 1-6 is asked in technology controlling and process in the presence of repeatability is relatively weak Topic, this proposes more requirements to the manipulation precision of technique, in order to improve controllability, and improves the stability of plating solution deposition, Particularly improved.
Embodiment 7-8 is guaranteed the stability of its storage performance, and embodiment 1-6 is saved in long-time, technique Operation difficulty increases, and coating performance stability reduces, and after long-time is stored, coating performance reduces 3-10%;And embodiment After 7-8 is improved, in one month, very little is influenced on coating.Embodiment 9-10 is more the stability control to operating procedure System can obtain preferable repeated data as a result, operational difficulty reduces with more loose operating procedure.
From another point of view, it more tends to stablize by modified coating performance, technique is more controllable.
The coating that embodiment 1-6 is obtained using electrochemical property test test result is as follows table:
Project Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6
Lithium storage content/(mA h g-1) 600.0 535.2 530.0 560.6 540.5 537.1
The coating that embodiment 7-10 is obtained using electrochemical property test test result is as follows table:
Project Embodiment 7 Embodiment 8 Embodiment 9 Embodiment 10
Lithium storage content/(mA h g-1) 568.4 571.9 608.3 610.1
It can be seen that the specific capacity of the antimony coating obtained using electroplate liquid of the invention is high by upper table, the electricity shown Chemical property.
The above is only a better embodiment of the present invention and the applied technical principle.It will be appreciated by those skilled in the art that this hair It is bright to be not limited to specific embodiment described here, be able to carry out for a person skilled in the art it is various it is apparent variation, again Adjustment and substitution are without departing from protection scope of the present invention.Therefore, although by above embodiments to the present invention carried out compared with For detailed description, but the present invention is not limited to the above embodiments only, without departing from the inventive concept, can be with Including more other equivalent embodiments, and the scope of the invention is determined by the scope of the appended claims.

Claims (10)

1. a kind of nickel antimony electroplating solution, contains boric acid, sodium hypophosphite, complexing agent and suitable quantity of water, which is characterized in that the electroplate liquid Also contain nickel salt and antimonic salt, the electroplate liquid each component and its content are boric acid 20-80g/L, sodium hypophosphite 10-80g/L, network Mixture 10-80g/L, nickel salt 1-20g/L and antimonic salt 1-10g/L.
2. a kind of nickel antimony electroplating solution according to claim 1, which is characterized in that the electroplate liquid each component and its content For boric acid 40g/L, sodium hypophosphite 40g/L, complexing agent 60g/L, nickel salt 10g/L and antimonic salt 4g/L.
3. a kind of nickel antimony electroplating solution according to claim 1 or 2, which is characterized in that the antimonic salt be potassium antimony tartrate or Person's antimony chloride.
4. a kind of nickel antimony electroplating solution according to claim 1, which is characterized in that the complexing agent be sodium acetate, acetic acid ammonia, Citric acid or ethylenediamine tetra-acetic acid.
5. a kind of nickel antimony electroplating solution according to claim 1, which is characterized in that the pH value of the electroplate liquid is 0.5-3.0.
6. a kind of nickel antimony electroplating solution according to claim 1, which is characterized in that the operating temperature of the electroplate liquid is 10- 50℃。
7. a kind of nickel antimony electroplating solution according to claim 1, which is characterized in that the electroplate liquid further includes additive, is added Adding agent is tin tetrabromide and 4-dimethylaminopyridine, and concrete content is tin tetrabromide 2-5g/L and 4-dimethylaminopyridine 3-8g/ L。
8. a kind of nickel antimony electroplating solution according to claim 1, which is characterized in that the electroplate liquid further includes tartaric acid and wine The content of stone acid sodium, tartaric acid and sodium tartrate is respectively 1-2g/L and 0.5-1g/L.
9. a kind of preparation method of nickel antimony electroplating solution according to claim 1, which comprises the following steps:
(1) boric acid 20-80g, sodium hypophosphite 10-80g, complexing agent 10-80g are added into deionized water, stirring and dissolving is made Mixed liquor;
(2) pH for being adjusted with acid mixed liquor is 1.0-3.0;
(3) addition nickel salt 1-20g, antimonic salt 1-10g, stirring and dissolving in Xiang Shangshu mixed liquor, the deionized water for adding surplus are fixed Hold to 1L, adjusting pH of mixed is 0.5-3.0, obtains antimony electroplating solution.
10. a kind of preparation method of nickel antimony electroplating solution according to claim 9, which is characterized in that acid described in step (2) For hydrochloric acid or sulfuric acid.
CN201910007990.4A 2019-01-04 2019-01-04 Nickel-antimony electroplating solution and preparation method thereof Active CN109680310B (en)

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CN113248840A (en) * 2021-05-10 2021-08-13 宁波晶美科技有限公司 Automobile door handle and electroplating process thereof
CN114059115A (en) * 2021-12-20 2022-02-18 中国计量大学 Tin-antimony electroplating solution and preparation method thereof
CN114892226A (en) * 2022-01-12 2022-08-12 中国计量大学 Zinc-antimony electroplating solution and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN113248840A (en) * 2021-05-10 2021-08-13 宁波晶美科技有限公司 Automobile door handle and electroplating process thereof
CN113248840B (en) * 2021-05-10 2022-04-15 宁波晶美科技有限公司 Automobile door handle and electroplating process thereof
CN114059115A (en) * 2021-12-20 2022-02-18 中国计量大学 Tin-antimony electroplating solution and preparation method thereof
CN114892226A (en) * 2022-01-12 2022-08-12 中国计量大学 Zinc-antimony electroplating solution and preparation method thereof

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