CN109852952A - A kind of hydrazine hydrate chemical nickel-plating plating solution and preparation method thereof and nickel plating process - Google Patents

A kind of hydrazine hydrate chemical nickel-plating plating solution and preparation method thereof and nickel plating process Download PDF

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CN109852952A
CN109852952A CN201910151189.7A CN201910151189A CN109852952A CN 109852952 A CN109852952 A CN 109852952A CN 201910151189 A CN201910151189 A CN 201910151189A CN 109852952 A CN109852952 A CN 109852952A
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plating
nickel
solution
hydrazine hydrate
chemical
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CN109852952B (en
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魏中华
陈小平
赵栋梁
宋玉
王向东
刘清友
贾书君
黄涛
汪兵
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Central Iron and Steel Research Institute
Zhejiang Innuovo Magnetics Industry Co Ltd
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Central Iron and Steel Research Institute
Zhejiang Innuovo Magnetics Industry Co Ltd
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Abstract

The invention discloses a kind of hydrazine hydrate chemical nickel-plating plating solution and preparation method thereof and nickel plating process, belong to chemical plating nickel technology field, solve destruction and pollution of the P elements to nickel-plating liquid and environment in sodium hypophosphite chemical nickel-plating liquid in the prior art, and using speed low problem when hydrazine hydrate progress chemical nickel plating.The plating solution of hydrazine hydrate chemical nickel plating of the invention, is made of nickel sulfate, hydrazine hydrate, sodium citrate, sodium potassium tartrate tetrahydrate, cobaltous sulfate and lead acetate.Chemical nickel plating suitable for basis material.

Description

A kind of hydrazine hydrate chemical nickel-plating plating solution and preparation method thereof and nickel plating process
Technical field
The invention belongs to chemical plating nickel technology field, in particular to a kind of hydrazine hydrate chemical nickel-plating plating solution and preparation method thereof And nickel plating process.
Background technique
Chemical nickel plating with its simple process, be not necessarily to additional power source, good evenness;In high molecular material and inorganic non-gold Belong to and being deposited on a variety of nonmetal basal bodies such as material;The excellent performances such as corrosion resistance, wear-resisting property and binding force of cladding material be strong etc. are special Point is rapidly developed and is widely applied.The plating solution composition of chemical nickel plating is particularly significant, and the ingredient of common chemical nickel-plating liquid has Metal salt, reducing agent, complexing agent, buffer, stabilizer, pH adjusting agent etc..
Reducing agent provides electronics needed for nickel ion in solution, mainly there is sodium hypophosphite, dimethylamino borine, hydroboration Potassium, hydrazine hydrate etc..Reducing agent is mostly sodium hypophosphite in chemical nickel-plating liquid at present, it has cheap, bath stability is good etc. Feature, while the nickel coating welding performance there is also some disadvantages as formed is poor, it is maximum the disadvantage is that P elements in plating solution Feature of environmental protection difference and destroy plating solution, there are contradictions for this development with green science and technology and chemical nickel plating itself, develop it based on this Its reducing agent chemical nickel-plating liquid is that inevitable choice also has huge prospect.
When hydrazine hydrate is reducing agent, plating nickel product is nitrogen, and safety and environmental protection meets the expected requirement of environmental protection, but simultaneously it It is slow that there is also reaction speeds, and easily decomposing under hydrazine hydrate high temperature causes plating solution unstable, and the nickel coating internal stress of formation is larger etc. asks Topic.Currently, it is that hydrazine hydrate reduction reaction speed is slow that hydrazine hydrate nickel chemical plating technology, which does not obtain the main reason for large-scale application, Chemical Ni-plating layer deposition velocity is too slow, causes chemical nickel plating efficiency too low, and general hydrazine hydrate chemical nickel plating speed is 1~2 μm/ h。
The research of hydrazine hydrate chemical nickel-plating plating solution is more, such as using hydrazine hydrate as initiator, uses hydrazine hydrate and sodium hypophosphite Nickel-phosphorus alloy is deposited on Copper substrate for co-reductant, the hydrazine hydrate in this research does not play weight in subsequent Ni-Speed It acts on;Some researchs are then on the biggish nano-particle surface of specific surface area using hydrazine hydrate chemical nickel plating, this and hydrazine hydrate The slow property of oxidation reaction is consistent, and such as prepares iron nickel bianry alloy nano-particle and forms nucleocapsid using nickel coated carbon Structure;Certain researchs are that fine and close pure-nickel-layer is such as prepared using hydrazine hydrate chemical nickel plating in nylon fabric in high molecular material, Also have simultaneously and such as utilizes hydrazine hydrate chemical plating nanometer nickel coated beta-silicon nitride powder in inorganic non-metallic material.We have found that because water Close that hydrazine redox reaction itself is relatively slow, the properties such as unstable under high temperature, it is few by hydrazine hydrate chemical nickel plating method in research It is applied on macroscopical matrix such as iron plate and preplating Ni substrate material.
Summary of the invention
In view of the above analysis, the present invention is intended to provide a kind of hydrazine hydrate chemical nickel-plating plating solution and preparation method thereof and nickel plating side Method, to solve destruction and pollution of the P elements to nickel-plating liquid and environment in sodium hypophosphite chemical nickel-plating liquid in the prior art, And solve the problems, such as that hydrazine hydrate chemical nickel plating speed is low.
The purpose of the present invention is mainly achieved through the following technical solutions:
A kind of plating solution of hydrazine hydrate chemical nickel plating, by nickel sulfate, hydrazine hydrate, sodium citrate, sodium potassium tartrate tetrahydrate, cobaltous sulfate and Lead acetate composition.
Further, the concentration range of each component is in plating solution: nickel sulfate 20~30g/L, 65wt.% hydrazine hydrate 50~ 70ml/L, 60~90g/L of sodium citrate, 8~14g/L of sodium potassium tartrate tetrahydrate, 6~15g/L of cobaltous sulfate, 5~15mg/L of lead acetate.
Further, the concentration range of each component is in plating solution: nickel sulfate 25~30g/L, 65wt.% hydrazine hydrate 60~ 70ml/L, 60~80g/L of sodium citrate, 8~12g/L of sodium potassium tartrate tetrahydrate, 6~10g/L of cobaltous sulfate, 5~10mg/L of lead acetate.
Further, the pH value of plating solution is 12~13, adjusts pH value using sodium hydroxide.
A kind of preparation method of hydrazine hydrate alkaline electroless plating nickel plating bath, comprising the following steps:
Step 1 measures various raw materials according to each component concentration in chemical nickel-plating liquid;
Step 2, with deionized water dissolving nickel sulfate, obtain solution A;
Step 3, with deionized water dissolving sodium citrate and sodium potassium tartrate tetrahydrate, obtain solution B, solution A be slowly added to molten In liquid B, it is uniformly mixed and stirs to get solution C;
Cobaltous sulfate, lead acetate are added separately in solution C by step 4, stir to obtain solution D;
The pH value of solution D is adjusted to 9 or more with the sodium hydroxide solution of 5wt% by step 5, is stirred after hydrazine hydrate is added It is uniformly mixed, deionized water is added to close to volumetric flask capacity, then with a small amount of sodium hydroxide, pH value is adjusted to 12~13, obtain To solution E, solution is transferred in volumetric flask, then with a small amount of deionized water constant volume, obtains hydrazine hydrate chemical nickel-plating plating solution.
A kind of nickel plating process is included the following steps: using above-mentioned hydrazine hydrate alkaline electroless plating nickel plating bath
Step 1 carries out pre-treatment to basis material;
Step 2, heating chemical nickel plating solution;
Basis material is put into nickel plating in chemical nickel-plating liquid by step 3;
Step 4, the nickel coating for obtaining basis material.
Further, in step 1, pre-treatment successively be polishing corner, cleaning, grease removal, washing, oil removing, washing, pickling, Cleaning.
Further, in step 2, the bath temperature of plating solution is 70 DEG C~90 DEG C.
Further, in step 3, plating time is 1~2h.
Further, in step 1, after carrying out pre-treatment to basis material, basis material is electroplated.
Compared with prior art, the present invention is at least able to achieve one of following technical effect:
1) reducing agent is mostly sodium hypophosphite in chemical nickel-plating plating solution in the prior art, and the P elements feature of environmental protection difference in plating solution is simultaneously And plating solution is destroyed, using hydrazine hydrate as reducing agent in the present invention, plating nickel product is nitrogen, and safety and environmental protection meets environmental requirement, is " phosphorus-free green environmental protection " alkaline electroless plating nickel plating bath, can make substrate material surface form bright nickel coating.
2) chemical plating of the invention speed is fast, and the addition of promotor cobaltous sulfate solves electroless nickel deposition speed issue very well, Highest deposition velocity can reach 7 μm/h or so, and deposition velocity can satisfy the requirement of business application completely;Chemical nickel-plating plating solution Stablize, the service life it is long, product is environmentally protective, directly can carry out chemical nickel plating to basis material, obtained nickel coating light is smooth, Crystal grain even compact, corrosion resistance are good.
3) preparation method of plating solution of the present invention can ensure the network between nickel sulfate and sodium citrate and sodium potassium tartrate tetrahydrate It closes, nickel ion exists in the solution with the complex form of nickel, and the nickel ion after complexing can be improved nickel coating quality.The present invention Environmentally protective, simple process has potential industrial application value.
4) present invention in chemical Ni-plating layer as surface layer play the role of sealing of hole enhance it is corrosion proof.It is first electric to basis material The form for plating again chemical plating can effectively reduce nickel plating layer thick, and chemical Ni-plating layer plays the role of to electroplated layer sealing of hole, relatively thin Coating can reach preferable corrosion resistance effect.
Other features and advantages of the present invention will illustrate in the following description, also, part can become from specification It obtains it is clear that understand through the implementation of the invention.The objectives and other advantages of the invention can be by written explanation It is achieved and obtained in book examples and drawings.
Detailed description of the invention
Attached drawing is only used for showing the purpose of specific embodiment, and is not to be construed as limiting the invention, in entire attached drawing In, identical appended drawing reference indicates identical component.
Fig. 1 is the scanning electron microscope diagram of coating prepared by the embodiment of the present invention 1;
Fig. 2 is the section metallographic microscope of coating prepared by the embodiment of the present invention 2;
Fig. 3 is coating polarization curve test result figure prepared by the embodiment of the present invention 3;
Fig. 4 is the scanning electron microscope diagram of 4 preplating nickel coating of the embodiment of the present invention;
Fig. 5 is the scanning electron microscope diagram of 4 chemical Ni-plating layer of the embodiment of the present invention.
Specific embodiment
Below in conjunction with specific embodiment to a kind of hydrazine hydrate chemical nickel-plating plating solution and preparation method thereof and nickel plating process make into The detailed description of one step, these embodiments are served only for the purpose for comparing and explaining, the present invention is not limited in these embodiments.
The invention discloses a kind of hydrazine hydrate chemical nickel-plating plating solutions, including nickel sulfate, hydrazine hydrate, sodium citrate, tartaric acid Potassium sodium, cobaltous sulfate and lead acetate.The concentration range of each component is in plating solution: nickel sulfate 20~30g/L, 65wt.% hydrazine hydrate 50 ~70ml/L, 60~90g/L of sodium citrate, 8~14g/L of sodium potassium tartrate tetrahydrate, 6~15g/L of cobaltous sulfate, 5~15mg/L of lead acetate.
Reducing agent is mostly sodium hypophosphite in chemical nickel-plating plating solution in the prior art, the P elements feature of environmental protection difference in plating solution and Destroy plating solution, using hydrazine hydrate as reducing agent in the present invention, plating nickel product is nitrogen, and safety and environmental protection meets environmental requirement.
Nickel sulfate is the main salt of chemical nickel-plating solution in the present invention, and concentration is 20~30g/L, and the too low nickel that can reduce of concentration sinks Self-catalyzed reaction easily occurs for product speed, excessive concentration plating solution, excessively high or too low can impact to the quality of nickel coating.
Hydrazine hydrate is the reducing agent in plating solution, provides electronics for nickel ion.When concentration of hydrazine hydrate is lower, chemical nickel plating is heavy Product speed is low, and the nickel layer of formation is thin, and performance is poor;When concentration of hydrazine hydrate is higher, the nickel content in solution is fixed, deposition velocity by Nickel ion concentration determines that more hydrazine hydrate can not play the role of accelerating reaction, volatilizees at high temperature instead, increases work Skill cost.Hydrazine hydrate reproducibility itself is weaker, and it is preferred range that selection concentration, which is 50~70ml/L, in this formula.
Sodium citrate is the complexing agent of nickel ion in plating solution, and concentration is 60~90g/L, and sodium citrate concentration is too low can shadow Ring nickel ion be complexed effect, and it is excessively high when will cause complexing agent residue, influence plating solution performance.
Sodium potassium tartrate tetrahydrate is compounding complexing agent, and concentration is 8~14g/L, similar with sodium citrate, is had to nickel ion The effect of compound complexing, potassium tartrate na concn is too low to will affect nickel ion complexing effect, and it is excessively high when to will cause complexing agent surplus It is remaining, influence plating solution performance.
Using cobaltous sulfate as additive, suitable cobalt element can play the role of increasing nucleation point, and it is heavy to accelerate nickle atom Product speed, so that nickel coating is fine and close, bright, smooth;It is found in research process, with the raising of cobalt sulfate concentration, the deposition of nickel Speed gradually increases, and nickel layer performance gradually increases, if but cobalt element too high levels, can have competition work deposit with nickel element With so that nickel element content score reduces in nickel layer, therefore cobalt sulfate concentration determination is more important.The present invention grinds the dense of cobaltous sulfate Degree is 6~15g/L, and the nickel coating of even compact function admirable can be obtained.
Use a small amount of lead acetate for stabilizer, concentration is 5~15mg/L, and the lead ion of low quality concentration is electric in the plating solution Electrode potential can be got higher, and be difficult to be reduced, and lead ion is slightly adsorbed in matrix surface, in the nickel hydroxide particle that hydrolysis generates Surface strong adsorption plays the forming core active site of masking nickel ion so that particle is positively charged mutually exclusive, stablizes the work of plating solution With.
Sodium hydroxide is pH adjusting agent, plays the role of adjusting bath pH value.
Preferably, the concentration range of each component is in plating solution: 25~30g/L of nickel sulfate, 60~70ml/L of hydrazine hydrate, lemon Sour 60~80g/L of sodium, 8~12g/L of sodium potassium tartrate tetrahydrate, 6~10g/L of cobaltous sulfate, 5~10mg/L of lead acetate.
The pH value of plating solution is 12~13, adjusts pH value using sodium hydroxide.When pH value is lower, hydrazine hydrate oxidation consumption hydrogen The reaction of oxygen root is slower, and nickel ion reactivity is low, and deposition velocity is slow, and nickel coating is relatively thin, and coating performance is poor;With the liter of pH value Height, redox reaction speed are accelerated, and deposition velocity increases;But when pH is excessively high, nickel ion core forming speed is too fast, crystallite dimension Excessive, nickel coating is coarse, coating performance decline.Preferably, pH value 12.5, deposition velocity is most fast at this time, and nickel coating is most thick, plating Layer performance is best.
The invention also discloses the preparation methods of above-mentioned hydrazine hydrate alkaline electroless plating nickel plating bath, comprising the following steps:
Step 1 measures various raw materials according to each component concentration in chemical nickel-plating liquid;
Step 2, with deionized water dissolving nickel sulfate, obtain solution A;
Step 3, with deionized water dissolving sodium citrate and sodium potassium tartrate tetrahydrate, obtain solution B, solution A be slowly added to molten In liquid B, it is uniformly mixed and stirs to get solution C;
Cobaltous sulfate, lead acetate are added separately in solution C by step 4, stir to obtain solution D;
The pH value of solution D is adjusted to 9 or more with the sodium hydroxide solution of 5wt% by step 5, is stirred after hydrazine hydrate is added It is uniformly mixed, deionized water is added to close to volumetric flask capacity, then with a small amount of sodium hydroxide, pH value is adjusted to 12~13, obtain To solution E, solution is transferred in volumetric flask, then with a small amount of deionized water constant volume, obtains hydrazine hydrate chemical nickel-plating plating solution.
Preparation method of the present invention can ensure the complexing between nickel sulfate and sodium citrate and sodium potassium tartrate tetrahydrate, nickel ion Exist in the solution with the complex form of nickel, the nickel ion after complexing can be improved nickel coating quality.
The invention also discloses a kind of nickel plating process, and using above-mentioned hydrazine hydrate chemical nickel-plating plating solution, method includes following step It is rapid:
Step 1 carries out pre-treatment to basis material;
Step 2, the heating chemical nickel-plating plating solution;
Basis material is put into nickel plating in chemical nickel-plating liquid by step 3;
Step 4, the nickel coating for obtaining basis material.
Hydrazine hydrate chemical nickel plating method of the present invention can ensure iron matrix, nickel preplating substrate material surface can directly into Row chemical nickel plating, obtained nickel coating is bright fine and close, and corrosion resistance is strong.
Preferably, in step 1, basis material is iron matrix or preplating Ni substrate;Pre-treatment is successively polishing corner, clear It washes, grease removal, washing, oil removing, washing, pickling, cleaning.
The present invention carries out pre-treatment to iron matrix, nickel preplating basis material, uses NaOH and Na by pre-treatment3PO4It is mixed Conjunction solution carries out grease removal, adds degreaser aqueous solution and acetone ultrasonic oil removal, obtains clean matrix surface, facilitates progress subsequent Chemical plating, acid cleaning process are affected to quality of coating, through overtesting, carry out pickling, acid using 5wt% dilute hydrochloric acid in this research Washing the time is 1~2min, it is therefore intended that activated matrix guarantees to have excellent performance nickel coating to obtain.Matrix is being removed through overpickling After the oxide on surface, unplated piece should enter chemical nickel plating slot as early as possible after cleaning, and secondary oxidation is avoided to influence quality of coating.
In step 2, temperature is 70 DEG C~90 DEG C when chemical nickel plating.When the temperature is low, hydrazine hydrate and nickel ion in plating solution Activity it is lower, deposition velocity is slow, and for nickel coating than relatively thin, performance is poor;Ni2+Reduction reaction be the endothermic reaction, deposition rate To accelerate with the raising of temperature, deposition rate about linearly increases with temperature, and deposition velocity is accelerated, and nickel plating layer thick increases, Performance enhancement.But when the temperature is excessively high, deionized water and hydrazine hydrate evaporation rate are accelerated, and each component changes of contents is big in solution, Deposition velocity can reduce instead.
Plating time is 1~2h in step 3.
The thickness range of prepared nickel coating is 5~14 μm in step 4.The thickness range of coating is set in 5~14 μ Between m, the quality of product nickel coating is effectively ensured, coating is too thin to will affect coating corrosion resistance, the too thick then chemical plating of coating Nickel higher cost.
Embodiment 1
Each component content is as shown in table 1 in a kind of hydrazine hydrate alkaline electroless plating nickel plating bath of the present embodiment:
Each component content in 1 hydrazine hydrate alkaline electroless plating nickel plating bath of table
A kind of preparation method of hydrazine hydrate alkaline electroless plating nickel plating bath of the present embodiment, specifically includes the following steps:
Step 1, weighed according to each component content in table 1 3kg nickel sulfate, 8kg sodium citrate, 1.2kg sodium potassium tartrate tetrahydrate, 0.6kg cobaltous sulfate, 0.5g lead acetate and 6L hydrazine hydrate;
20L deionized water is added in step 2 in container A, while stirring, 3kg nickel sulfate is added, stirs to complete Fully dissolved;
30L deionized water is added in step 3 in container B, while stirring, 8kg sodium citrate and 1.2kg is added Sodium potassium tartrate tetrahydrate, stirring to abundant dissolution;Nickel sulfate solution in container A is poured slowly into container B under stirring, continues to stir Mix complexing 2h;
0.6kg cobaltous sulfate and 0.5g lead acetate are added into container B for step 4, stir 30min;
It is 9 that step 5, addition 1L sodium hydroxide solution, which adjust pH value,;6L hydrazine hydrate is continuously added, 26L deionized water is added The solution close to total value is obtained, adding 4L sodium hydroxide solution and adjusting pH value is 12.5, and it is fixed to be eventually adding 0.2L deionized water Hold and 100L hydrazine hydrate alkaline electroless plating nickel plating bath is made.
Nickel plating process in the present embodiment specifically includes the following steps:
Step 1, by iron matrix material by polishing corner → cleaning → grease removal → washing → oil removing → washing → pickling → The pre-treating technologies such as cleaning;Chamfering carries out in beveler;Using NaOH and Na3PO4Mixed solution carry out grease removal;Oil removing is It is carried out using the aqueous solution and acetone of addition degreaser until the clean company of being formed of product surface oily waste degradation in ultrasonic environment Continuous moisture film;Pickling is 1~2min of pickling in 5wt% dilute hydrochloric acid solution, and removal Surface Rust is until leaking out homogeneous metal gloss Matrix;
Iron matrix material after pre-treatment is hung and is put into the coating bath equipped with chemical nickel-plating solution by step 2;
Step 3 carries out chemical plating 1 hour in the environment of temperature is 80 DEG C;
Step 4, the nickel plating layer thick for obtaining iron matrix material are about 6 μm.
Micro-analysis is carried out such as to nickel plating layer surface prepared by the present embodiment 1 by scanning electron microscope in the present invention Shown in Fig. 1, iron matrix surface, nickel particle close-packed arrays uniform in size are completely covered in chemical Ni-plating layer.
Embodiment 2
Each component content is as shown in table 2 in a kind of hydrazine hydrate alkaline electroless plating nickel plating bath of the present embodiment:
Each component content in 2 hydrazine hydrate alkaline electroless plating nickel plating bath of table
Nickel sulfate 25g/L
Hydrazine hydrate 70ml/L
Sodium citrate 60g/L
Sodium potassium tartrate tetrahydrate 8g/L
Cobaltous sulfate 10g/L
Lead acetate 10mg/L
The preparation method is the same as that of Example 1 for plating solution, the present embodiment nickel plating process, specifically includes the following steps:
Step 1, by iron matrix material by polishing corner → cleaning → grease removal → washing → oil removing → washing → pickling → The pre-treating technologies such as cleaning;
Sample Jing Guo pre-treatment is hung and is put into the coating bath equipped with chemical nickel-plating plating solution by step 2;
Step 3 carries out chemical plating 2 hours in the environment of temperature is 85 DEG C;
Step 4, the nickel plating layer thick for obtaining iron matrix material are about 13.5 μm.
The present embodiment carries out hydrazine hydrate alkaline chemical nickel-plating after iron matrix material surface is electroplated, micro- by inverted metallurgic Mirror carries out Metallographic Analysis to nickel plating layer cross section prepared by the present embodiment 2 as shown in Fig. 2, epoxy resin plays approved sample conveniently in figure The effect of metallographic observation, about 13.5 μm of the average thickness of nickel coating, it was demonstrated that chemical nickel plating fast speed of the present invention can reach about 6.75μm/h.It is combined between nickel coating and matrix very close.
Embodiment 3
Each component content is as shown in table 3 in a kind of hydrazine hydrate alkaline electroless plating nickel plating bath of the present embodiment:
Each component content in 3 hydrazine hydrate alkaline electroless plating nickel plating bath of table
Nickel sulfate 20g/L
65wt.% hydrazine hydrate 65ml/L
Sodium citrate 75g/L
Sodium potassium tartrate tetrahydrate 10g/L
Cobaltous sulfate 10g/L
Lead acetate 6mg/L
The preparation method is the same as that of Example 1 for plating solution, the present embodiment nickel plating process, specifically includes the following steps:
Step 1 takes basis material by polishing corner → cleaning → grease removal → washing → oil removing → washing → pickling → clear Wash equal pre-treating technologies;Using NaOH and Na3PO4Mixed solution carry out grease removal;Oil removing is in ultrasonic environment using addition The aqueous solution and acetone of degreaser carry out completely forming continuous moisture film until product surface oily waste degradation;Pickling is dilute in 5wt% 1~2min of pickling in hydrochloric acid solution, removal Surface Rust is until leaking out homogeneous metal gloss matrix;
Step 2 carries out nickel preplating to matrix using electroplating technology, then carries out strike copper plating technique.Take nickel preplating Copper substrate material Expect three pieces, then carries out chemical nickel plating;
Step 3 carries out chemical nickel plating 30min, 60min, 120min in the environment of temperature is 80 DEG C respectively.
Current existing basis material nickel plating technology is three plating process of ambrose alloy nickel, and bottom nickel, which plays, prevents copper facing corrosion base The effect of body, layers of copper play the role of enhance corrosion resistance, the present invention in chemical Ni-plating layer as surface layer play sealing of hole enhance it is anti-corrosion The effect of property.The form for basis material being first electroplated again chemical plating can effectively reduce nickel plating layer thick, and chemical Ni-plating layer plays Electroplated layer sealing of hole is acted on, relatively thin coating can reach preferable corrosion resistance effect.
Electro-chemical test is carried out to nickel plating layer surface prepared by the present embodiment 3 by scanning electron microscope in the present invention Polarization curve is obtained as shown in figure 3, chemical Ni-plating layer corrosion resistance enhances with the increase of chemical nickel plating time.
Embodiment 4
Each component content is as shown in table 4 in a kind of hydrazine hydrate alkaline electroless plating nickel plating bath of the present embodiment:
Each component content in 4 hydrazine hydrate alkaline electroless plating nickel plating bath of table
Nickel sulfate 30g/L
65wt.% hydrazine hydrate 70ml/L
Sodium citrate 80g/L
Sodium potassium tartrate tetrahydrate 8g/L
Cobaltous sulfate 8g/L
Lead acetate 5mg/L
The preparation method is the same as that of Example 1 for plating solution, the present embodiment nickel plating process, specifically includes the following steps:
Step 1 takes basis material by polishing corner → cleaning → grease removal → washing → oil removing → washing → pickling → clear Wash equal pre-treating technologies;
Step 2 carries out nickel preplating to matrix using electroplating technology, takes nickel preplating basis material chemical nickel plating 1h, while electricity Plate nickel preplating sample as a comparison;
Step 3 carries out chemical nickel plating 1h in the environment of temperature is 80 DEG C respectively.
The nickel coating nickel particle fine uniform that in the present invention prepared by hydrazine hydrate nickel chemical plating technology has to plating nickel preplating Layer carries out the effect of sealing of hole, by scanning electron microscope to preplating nickel coating prepared by embodiment 4 and chemical Ni-plating layer table Face carries out micro-analysis as illustrated in figures 4-5, and Fig. 4 is preplating nickel coating microscopic appearance, and Fig. 5 is the microcosmic shape of chemical nickel plating after nickel preplating Looks, it can be seen that electronickelling nickel particle is big, and gap is more, and chemical Ni-plating layer nickel particle is smaller, and part of nickel distribution of particles is in hole At gap, there are sealing of hole effects.
In conclusion the present invention provides one kind on iron matrix, nickel preplating body material, hydrazine hydrate alkaline chemical nickel-plating is plated Liquid, preparation method and plating method are prepared for a kind of stable chemical nickel-plating solution by optimizing chemical nickel-plating solution.This hair Bright chemical plating speed is fast, chemical nickel-plating plating solution is stable, the service life is long, and product is environmentally protective, can be directly to basis material Nickel plating is learned, obtained nickel coating light is smooth, crystal grain even compact, and corrosion resistance is good.Environmentally protective, simple process of the invention, tool There is potential industrial application value.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto, In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art, It should be covered by the protection scope of the present invention.

Claims (10)

1. a kind of hydrazine hydrate chemical nickel-plating plating solution, which is characterized in that the plating solution is by nickel sulfate, hydrazine hydrate, sodium citrate, winestone Sour potassium sodium, cobaltous sulfate and lead acetate composition.
2. hydrazine hydrate chemical nickel-plating plating solution according to claim 1, which is characterized in that the concentration range of each component in plating solution It is: nickel sulfate 20~30g/L, 65wt.% 50~70ml/L of hydrazine hydrate, 60~90g/L of sodium citrate, sodium potassium tartrate tetrahydrate 8~ 14g/L, 6~15g/L of cobaltous sulfate, 5~15mg/L of lead acetate.
3. hydrazine hydrate chemical nickel-plating plating solution according to claim 2, which is characterized in that the concentration range of each component in plating solution It is: nickel sulfate 25~30g/L, 65wt.% 60~70ml/L of hydrazine hydrate, 60~80g/L of sodium citrate, sodium potassium tartrate tetrahydrate 8~ 12g/L, 6~10g/L of cobaltous sulfate, 5~10mg/L of lead acetate.
4. hydrazine hydrate alkaline electroless plating nickel plating bath according to claim 1-3, which is characterized in that the plating solution PH value is 12~13, adjusts pH value using sodium hydroxide.
5. the preparation method of hydrazine hydrate alkaline electroless plating nickel plating bath according to claim 1-4, which is characterized in that The following steps are included:
Step 1 measures various raw materials according to each component concentration in chemical nickel-plating plating solution;
Step 2, with deionized water dissolving nickel sulfate, obtain solution A;
Step 3, with deionized water dissolving sodium citrate and sodium potassium tartrate tetrahydrate, obtain solution B, solution A be slowly added to solution B In, it is uniformly mixed and stirs to get solution C;
Cobaltous sulfate, lead acetate are added separately in solution C by step 4, stir to obtain solution D;
The pH value of solution D is adjusted to 9 or more with the sodium hydroxide solution of 5wt% by step 5, is stirred after hydrazine hydrate is added Uniformly, deionized water is added and pH value is adjusted to 12~13 to close to volumetric flask capacity, then with a small amount of sodium hydroxide, obtain molten Liquid E, solution is transferred in volumetric flask, then with a small amount of deionized water constant volume, obtains hydrazine hydrate chemical nickel-plating plating solution.
6. a kind of nickel plating process, which is characterized in that using the described in any item hydrazine hydrate alkaline chemical nickel-plating platings of claim 1-4 Liquid;Described method includes following steps:
Step 1 carries out pre-treatment to basis material;
Step 2, the heating chemical nickel-plating plating solution;
Basis material is put into nickel plating in chemical nickel-plating liquid by step 3;
Step 4, the nickel coating for obtaining basis material.
7. nickel plating process according to claim 6, which is characterized in that in the step 1, the pre-treatment is successively polishing Corner, cleaning, grease removal, washing, oil removing, washing, pickling, cleaning.
8. nickel plating process according to claim 6, which is characterized in that in the step 2, the bath temperature of plating solution is 70 DEG C ~90 DEG C.
9. nickel plating process according to claim 6, which is characterized in that in the step 3, plating time is 1~2h.
10. according to nickel plating process described in claim 6-9, which is characterized in that in the step 1, before being carried out to basis material After processing, basis material is electroplated.
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