CN108315779A - A kind of nickel-plating additive and electro-plating method - Google Patents
A kind of nickel-plating additive and electro-plating method Download PDFInfo
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- CN108315779A CN108315779A CN201810351953.0A CN201810351953A CN108315779A CN 108315779 A CN108315779 A CN 108315779A CN 201810351953 A CN201810351953 A CN 201810351953A CN 108315779 A CN108315779 A CN 108315779A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
- C25D3/14—Electroplating: Baths therefor from solutions of nickel or cobalt from baths containing acetylenic or heterocyclic compounds
- C25D3/16—Acetylenic compounds
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Abstract
The invention discloses a kind of nickel-plating additive and electro-plating methods.Wherein, nickel-plating additive of the invention includes：60 150g/L of propine sodium sulfonate, 10 80g/L of Sodium Allyl Sulfonate, 2 ethylhexylsulfate sodium salt, 10 50g/L, 10 50g/L of polyoxyethylated alkyl phenol sodium sulfate salt, 10 30g/L of 1 20g/L of polyetheramine, 5 15g/L of organic polysulfide and boric acid.Several substances in the present invention are not superimposed not instead of simply, by centainly acting synergistically, using the characteristic of various substances, play the role of mutually promoting, few side effects, and effect is good.In a variety of nickel-plating additives, additive formulations of the invention are simple, are easy to get, and the dosage of various substances is few.The nickel-plating additive of the present invention reduces the voidage of coating, improves the brightness of coating, enhances the dispersibility of plating solution, increases the ductility of coating, prevents coating from generating pin hole and point.
Description
Technical field
The present invention relates to electroplating technology more particularly to a kind of nickel-plating additive and electro-plating methods.
Background technology
Additive is added in nickel plating solution, not only can prevent or postpone the Auto-decomposition of nickel plating solution, play stabilization
The effect of plating solution can also be accelerated to react sometimes, improve the phosphorus content and internal stress of nickel coating, thus, ripe for one
For nickel plating product, additive is essential important component.
Nickel-plating additive is developed so far, and experienced four-stage：First stage is to use inorganic brightener, such as cadmium salt；
Second stage is butynediols and saccharin；Phase III is the condensation product and saccharin of butynediols and epoxide；Fourth order
Section is the second-class brightener and the softening agent as primary brightener, as forth generation nickel plating brightener of intermediate compounding.
Wherein, forth generation nickel plating brightener increasingly meets the needs of market in continuous improvement.
Forth generation nickel plating primary brightener is generally compounded by 3~5 kinds of intermediates, and some of which component is completely free of
Acetylene series system.Butynediols, but the addition product of propilolic alcohol are less used using acetylene series class.Directly fourth is replaced with propilolic alcohol
Acetylenic glycols, brightening and leveling is much better, but coating brittleness is very big, therefore should not be directly added into.Forth generation nickel plating primary brightener is
Softening agent is actually also to be compounded by several intermediates, and product differentiation is very big.
Currently, forth generation nickel plating brightener has following several respects the problem of reflecting：
First, intermediate is mostly sulfur-containing compound, therefore coating activity is high.Advantage is：When nickel in pairs with semi-bright nickel group
Easily reach the requirement of 120mV or more potential differences, the disadvantage is that：Coating corrosion resistance itself is not very good.The bright nickel plating in stainless steel test piece,
Then 1：It is impregnated in 1 (volume ratio) hydrochloric acid, the coating obtained with BE class sugaring essences, immersion will not for a long time change colour；And with containing pyrrole
The coating that the forth generation nickel plating brightener sugaring essence of piperidine derivatives etc obtains, is soaked for a period of time, coating starts to shade, in turn
Black and there is minute bubbles generation, nickel layer to dissolve, last coating is completely dissolved in hydrochloric acid.
The second, the common white haze in low current density area or blackspot.
Third, the obfuscation of low area, height, middle area's brightness decline.
Invention content
Technical problem to be solved by the present invention lies in provide a kind of nickel-plating additive, which reduces coating
Voidage, improve the brightness of coating, enhance the dispersibility of plating solution, increase the ductility of coating, prevent coating generate needle
Hole and point.
Technical problem to be solved by the present invention lies in provide a kind of electro-plating method, it is possible to reduce the use of nickel-plating additive
Amount improves electroplating effect.
In order to solve the above technical problem, the present invention provides a kind of nickel-plating additives, including：
Propine sodium sulfonate 60-150g/L；
Sodium Allyl Sulfonate 10-80g/L；
2- ethylhexylsulfate sodium salts 10-50g/L；
Polyoxyethylated alkyl phenol sodium sulfate salt 10-50g/L；
Polyetheramine 1-20g/L；
Organic polysulfide 5-15g/L；
Boric acid 10-30g/L.
As the improvement of said program, nickel-plating additive of the present invention includes：
Propine sodium sulfonate 80-120g/L；
Sodium Allyl Sulfonate 30-60g/L；
2- ethylhexylsulfate sodium salts 20-45g/L；
Polyoxyethylated alkyl phenol sodium sulfate salt 20-45g/L；
Polyetheramine 5-12g/L；
Organic polysulfide 7-12g/L；
Boric acid 15-25g/L.
As the improvement of said program, nickel-plating additive of the present invention includes：
Propine sodium sulfonate 90-110g/L；
Sodium Allyl Sulfonate 40-50g/L；
2- ethylhexylsulfate sodium salts 10-50g/L；
Polyoxyethylated alkyl phenol sodium sulfate salt 10-50g/L；
Polyetheramine 7-10g/L；
Organic polysulfide 9-11g/L；
Boric acid 18-22g/L.
As the improvement of said program, nickel-plating additive of the present invention further includes：0.5-1.8g/L saccharin.
As the improvement of said program, the content of saccharin is 0.6-1.5g/L.
Correspondingly, the present invention also provides a kind of electro-plating methods using nickel-plating additive described above, including：
Nickel-plating additive is added into nickel solution, mixed liquor is formed；
Mixed liquor is stirred, mixing speed 800-2000r/min；
The temperature of mixed liquor is 45-60 DEG C, pH value 4.0-5.0；
Consumption when plating into the mixed liquor according to 80-120ml/kA.h adds nickel-plating additive.
As the improvement of said program, nickel-plating additive is added into nickel solution according to the dosage of 0.1-1ml/L, is formed
Mixed liquor.
As the improvement of said program, mixing speed 1000-1600r/min.
As the improvement of said program, the temperature of mixed liquor is 51-56 DEG C.
As the improvement of said program, the pH value of mixed liquor is 4.5-4.8.
Implement the present invention, has the advantages that：
1, a kind of nickel-plating additive provided by the invention, including：Propine sodium sulfonate 60-150g/L, Sodium Allyl Sulfonate 10-
80g/L, 2- ethylhexylsulfate sodium salt 10-50g/L, polyoxyethylated alkyl phenol sodium sulfate salt 10-50g/L, polyetheramine 1-
20g/L, organic polysulfide 5-15g/L and boric acid 10-30g/L.Several substances in the present invention be not be simply superimposed, and
It is, using the characteristic of various substances, to play the role of mutually promoting by centainly acting synergistically, few side effects, effect is good.
In a variety of nickel-plating additives, additive formulations of the invention are simple, are easy to get, and the dosage of various substances is few.The plating of the present invention
Nickel additive reduces the voidage of coating, improves the brightness of coating, enhances the dispersibility of plating solution, increases the extension of coating
Property, prevent coating from generating pin hole and point.
2, the nickel-plating additive of the present invention is added into nickel solution a kind of electro-plating method provided by the invention, is formed mixed
Liquid is closed, and mixed liquor is stirred, the temperature and pH of mixed liquor is controlled, can not only reduce the dosage of nickel-plating additive, also
Improve the quality of coating.
Specific implementation mode
To make the object, technical solutions and advantages of the present invention clearer, the present invention will be made below further detailed
Description.The each component content unit g/L of nickel-plating additive indicates a certain constituent mass contained in every liter of additive.Nickel plating adds
Dosage units/ml/L that tank liquor is prepared in agent is added to indicate to add in every liter of nickel plating bath (nickel plating solution for being not added with nickel-plating additive)
The additive volume added.The consumption additional amount of nickel-plating additive refers to being come with the consumption of additive in electroplate liquid in electroplating process
Additive is added in batches, and unit kA.h is the usual unit that this field calculates consumption, and the specific calculating as consumption has been
Known to those skilled in the art, details are not described herein.
The present invention provides a kind of nickel-plating additives, including：
Propine sodium sulfonate 60-150g/L；
Sodium Allyl Sulfonate 10-80g/L；
2- ethylhexylsulfate sodium salts 10-50g/L；
Polyoxyethylated alkyl phenol sodium sulfate salt 10-50g/L；
Polyetheramine 1-20g/L；
Organic polysulfide 5-15g/L；
Boric acid 10-30g/L.
Propine sodium sulfonate is both a kind of primary brightener and a kind of second-class brightener, it is possible to reduce other reagents add
Enter, reduce the reaction between various chemical substances and stress, avoids generating some side effects.The present invention is made using propine sodium sulfonate
For primary brightener, can crystal grain thinning, reduce coating tensile stress, coating made to generate sub-dued lustre；In addition, using propine sodium sulfonate
Stronger suction-operated can be generated as second-class brightener, cathodic polarization can be increased substantially, makes plating solution that there is preferable Surface flat
And dispersibility, the careful light of coating.
Sodium Allyl Sulfonate can improve the brightness coverage capability of plating solution as a kind of auxiliary brightener, reduce pin hole, accelerate
Light extraction and leveling speed, and the consumption of other brighteners is reduced, reduce susceptibility of the plating solution to impurity.
Specifically, the present invention makes full use of primary, secondary, auxiliary brightener synergistic effect, using propine sodium sulfonate as base
Plinth is equipped with Sodium Allyl Sulfonate, the dosage of propine sodium sulfonate is 60-150g/L, the dosage of Sodium Allyl Sulfonate is 10-80g/
Under conditions of L, entire bright, high leveling and the good coating of ductility, and the dispersion energy of cathode efficiency and plating solution can get
Power is relatively high, and coating bright current density range is wide, flexibility is good.
2- ethylhexylsulfates sodium salt and polyoxyethylated alkyl phenol sodium sulfate salt can significantly extend low as wetting agent
The areas Jc bright range, wetting agent generate Characteristic Adsorption in cathode surface, show cathodic polarization function.In addition, 2- ethylhexyls
Sulfuric ester sodium salt and polyoxyethylated alkyl phenol sodium sulfate salt cooperate, and can effectively reduce the surface tension of plating solution, to
Prevent coating from generating pin hole and point.When the content of 2- ethylhexylsulfates sodium salt and polyoxyethylated alkyl phenol sodium sulfate salt
When respectively less than 10g/L, when wetting agent deficiency, the low areas Jc coating bright property is bad.
Organic polysulfide can not only eliminate " tomography " phenomenon of low current density area brightness as the agent that walks of low area,
The common white haze in low current density area or blackspot can be also eliminated simultaneously, can more offset a part causes because second-class brightener is excessive
Coating brittleness.When the content of organic polysulfide is less than 5g/L, brittleness can be brought to coating；Work as organic polysulfide
Content when being more than 15g/L, the obfuscation of coating low area, high, middle area's brightness can be made to decline.
Polyetheramine is compounded as intermediate and saccharin, and the brittleness of nickel coating is made to reduce, and corrosion resistance improves, and can improve
The anti-impurity ability of plating solution.
Boric acid not only plays the cushioning effect of stable pH value (in plating solution or cathode interface liquid layer), can also refine coating knot
Brilliant, raising coating bright property, has the function of certain cathodic polarization.When boric acid content is less than 10g/L, the low areas the Jc brightness of coating
It is insufficient.
Several substances in the present invention are not superimposed not instead of simply, by centainly acting synergistically, utilize various substances
Characteristic, play the role of mutually promoting, few side effects, effect is good.In a variety of nickel-plating additives, additive of the invention is matched
Side is simple, is easy to get, the dosage of various substances is few.The nickel-plating additive of the present invention reduces the voidage of coating, improves coating
Brightness, enhance the dispersibility of plating solution, increase the ductility of coating, coating is made to obtain covering for good low current density area
Lid ability.
Preferably, nickel-plating additive of the invention, including propine sodium sulfonate 80-120g/L, Sodium Allyl Sulfonate 30-60g/
L, 2- ethylhexylsulfates sodium salt 20-45g/L, polyoxyethylated alkyl phenol sodium sulfate salt 20-45g/L, polyetheramine 5-12g/
L, organic polysulfide 7-12g/L and boric acid 15-25g/L.
More preferably, nickel-plating additive of the invention, including propine sodium sulfonate 90-110g/L, Sodium Allyl Sulfonate 40-50g/
L, 2- ethylhexylsulfates sodium salt 30-40g/L, polyoxyethylated alkyl phenol sodium sulfate salt 30-40g/L, polyetheramine 7-10g/
L, organic polysulfide 9-11g/L and boric acid 18-22g/L.
The nickel-plating additive of the present invention further includes 0.6-1.5g/L saccharin.
Saccharin is a main additive in bright nickel plating, can reduce second-class brightener and answer caused by coating
Power reduces the brittleness of nickel layer, increases the function of coating ductility, that is, improves the toughness of coating.When saccharin content is less than 0.6g/L,
Coating on high current density region becomes dim, and brightness is deteriorated, or even is easy to burn, and coating is hard, easy tos produce crackle.Saccharin contains
Measure it is too low it will cause coating brittleness decortication etc. failures.Saccharin content is more than 1.5g/L, nickel coating can be made cloud occur dim in vain.
When covering chromium on this nickel coating, chrome plating is easy floating, and the deep recess of part is made to be not easy to put on chromium.When the content mistake of saccharin
Gao Shi can cause nickel layer to be easily passivated, and cause to cover chromium difficulty.Preferably, the content of saccharin is 0.8-1.2g/L.
Correspondingly, the present invention also provides a kind of electro-plating methods using above-mentioned nickel-plating additive, including：
Nickel-plating additive is added into nickel solution, mixed liquor is formed；
Mixed liquor is stirred, mixing speed 800-2000r/min；
The temperature of mixed liquor is 45-60 DEG C, pH value 4.0-5.0；
Consumption when plating into the mixed liquor according to 80-120ml/kA.h adds nickel-plating additive.
Have, nickel-plating additive is added into nickel solution according to the dosage of 0.1-1ml/L, forms mixed liquor.With it is existing
Some additives are compared, and the nickel-plating additive dosage of the application is few, and effect is good.
The convective mass transfer speed of mixed liquor can be improved by being stirred to mixed liquor, be conducive to main salt metal in cathode interface liquid layer
The supplement of ion is burnt to reduce.But when mixing speed is more than 2000r/min, cathode concentration polarization can be reduced, is made bright whole
Flat Jc ranges are moved to the areas Jc high.When being electroplated using small Jc and requiring the low areas Jc bright property good, stirring intensity is not preferably greater than
1600r/min may decrease slightly stroke to the movable cathode of set speed；To compressed air stirring, air inlet can be suitably reduced
Amount.Preferably, mixing speed 1000-1600r/min.
The temperature of mixed liquor plays a crucial role plating, even if brightener is good again, the temperature of mixed liquor is less than
At 45 DEG C, it is also difficult to obtain bright coating, the low areas Jc effect is worse.Preferably, the temperature of mixed liquor is 51-56 DEG C.
The pH value of mixed liquor influences the absorption property of multiple additives, when pH value is less than 4.0, the dosage of additive and consumption
Amount is bigger, and the low areas Jc bright property is deteriorated.Preferably, the pH value of mixed liquor is 4.5-5.8.
The nickel-plating additive of the present invention is added into nickel solution the electro-plating method of the present invention, forms mixed liquor, and to mixed
It closes liquid to be stirred, controls the temperature and pH of mixed liquor, can not only reduce the dosage of nickel-plating additive, also improve coating
Quality.
It will illustrate the present invention with specific embodiment below
Embodiment 1
A kind of nickel-plating additive, including propine sodium sulfonate 60g/L, Sodium Allyl Sulfonate 10g/L, 2- ethylhexylsulfate
Sodium salt 10g/L, polyoxyethylated alkyl phenol sodium sulfate salt 10g/L, polyetheramine 1g/L, organic polysulfide 5g/L and boric acid
10g/L。
A kind of electro-plating method using above-mentioned nickel-plating additive, including：
Above-mentioned nickel-plating additive is added into nickel solution according to the dosage of 1ml/L, forms mixed liquor；
Mixed liquor is stirred, mixing speed 800r/min；
The temperature of mixed liquor is 45 DEG C, pH value 4.0；
Consumption when plating into the mixed liquor according to 120ml/kA.h adds nickel-plating additive.
Embodiment 2
A kind of nickel-plating additive, including propine sodium sulfonate 70g/L, Sodium Allyl Sulfonate 20g/L, 2- ethylhexylsulfate
Sodium salt 14g/L, polyoxyethylated alkyl phenol sodium sulfate salt 14g/L, polyetheramine 3g/L, organic polysulfide 7g/L and boric acid
14g/L。
A kind of electro-plating method using above-mentioned nickel-plating additive, including：
Above-mentioned nickel-plating additive is added into nickel solution according to the dosage of 0.8ml/L, forms mixed liquor；
Mixed liquor is stirred, mixing speed 1200r/min；
The temperature of mixed liquor is 48 DEG C, pH value 4.2；
Consumption when plating into the mixed liquor according to 110ml/kA.h adds nickel-plating additive.
Embodiment 3
A kind of nickel-plating additive, including propine sodium sulfonate 90g/L, Sodium Allyl Sulfonate 35g/L, 2- ethylhexylsulfate
Sodium salt 19g/L, polyoxyethylated alkyl phenol sodium sulfate salt 19g/L, polyetheramine 7g/L, organic polysulfide 9g/L and boric acid
18g/L。
A kind of electro-plating method using above-mentioned nickel-plating additive, including：
Above-mentioned nickel-plating additive is added into nickel solution according to the dosage of 0.6ml/L, forms mixed liquor；
Mixed liquor is stirred, mixing speed 1400r/min；
The temperature of mixed liquor is 50 DEG C, pH value 4.4；
Consumption when plating into the mixed liquor according to 100ml/kA.h adds nickel-plating additive.
Embodiment 4
A kind of nickel-plating additive, including propine sodium sulfonate 110g/L, Sodium Allyl Sulfonate 50g/L, 2- ethylhexyl sulfuric acid
Ester sodium salt 25g/L, polyoxyethylated alkyl phenol sodium sulfate salt 25g/L 1.2g/L, polyetheramine 11g/L, organic polysulfide
11g/L and boric acid 21g/L.
A kind of electro-plating method using above-mentioned nickel-plating additive, including：
Above-mentioned nickel-plating additive is added into nickel solution according to the dosage of 0.6ml/L, forms mixed liquor；
Mixed liquor is stirred, mixing speed 1500r/min；
The temperature of mixed liquor is 55 DEG C, pH value 4.6；
Consumption when plating into the mixed liquor according to 90ml/kA.h adds nickel-plating additive.
Embodiment 5
A kind of nickel-plating additive, including propine sodium sulfonate 120g/L, Sodium Allyl Sulfonate 60g/L, 2- ethylhexyl sulfuric acid
Ester sodium salt 30g/L, polyoxyethylated alkyl phenol sodium sulfate salt 30g/L, polyetheramine 12g/L, organic polysulfide 12g/L and boron
Sour 25g/L.
A kind of electro-plating method using above-mentioned nickel-plating additive, including：
Above-mentioned nickel-plating additive is added into nickel solution according to the dosage of 0.5ml/L, forms mixed liquor；
Mixed liquor is stirred, mixing speed 1600r/min；
The temperature of mixed liquor is 55 DEG C, pH value 4.8；
Consumption when plating into the mixed liquor according to 90ml/kA.h adds nickel-plating additive.
Embodiment 6
A kind of nickel-plating additive, including propine sodium sulfonate 140g/L, Sodium Allyl Sulfonate 70g/L, 2- ethylhexyl sulfuric acid
Ester sodium salt 40g/L, polyoxyethylated alkyl phenol sodium sulfate salt 40g/L, polyetheramine 15g/L, organic polysulfide 12g/L and boron
Sour 28g/L.
A kind of electro-plating method using above-mentioned nickel-plating additive, including：
Above-mentioned nickel-plating additive is added into nickel solution according to the dosage of 0.3ml/L, forms mixed liquor；
Mixed liquor is stirred, mixing speed 1800r/min；
The temperature of mixed liquor is 58 DEG C, pH value 5.0；
Consumption when plating into the mixed liquor according to 80ml/kA.h adds nickel-plating additive.
Embodiment 7
A kind of nickel-plating additive, including propine sodium sulfonate 150g/L, Sodium Allyl Sulfonate 80g/L, 2- ethylhexyl sulfuric acid
Ester sodium salt 50g/L, polyoxyethylated alkyl phenol sodium sulfate salt 50g/L, polyetheramine 20g/L, organic polysulfide 15g/L and boron
Sour 30g/L.
A kind of electro-plating method using above-mentioned nickel-plating additive, including：
Above-mentioned nickel-plating additive is added into nickel solution according to the dosage of 0.1ml/L, forms mixed liquor；
Mixed liquor is stirred, mixing speed 2000r/min；
The temperature of mixed liquor is 60 DEG C, pH value 5.0；
Consumption when plating into the mixed liquor according to 80ml/kA.h adds nickel-plating additive.
Embodiment 8
A kind of nickel-plating additive, including propine sodium sulfonate 120g/L, Sodium Allyl Sulfonate 60g/L, 2- ethylhexyl sulfuric acid
Ester sodium salt 30g/L, polyoxyethylated alkyl phenol sodium sulfate salt 30g/L, saccharin 1.3g/L, polyetheramine 12g/L, organic polysulfide close
Object 12g/L and boric acid 25g/L.
A kind of electro-plating method using above-mentioned nickel-plating additive, including：
Above-mentioned nickel-plating additive is added into nickel solution according to the dosage of 0.5ml/L, forms mixed liquor；
Mixed liquor is stirred, mixing speed 1600r/min；
The temperature of mixed liquor is 55 DEG C, pH value 4.8；
Consumption when plating into the mixed liquor according to 90ml/kA.h adds nickel-plating additive.
Comparative example 1
A kind of electro-plating method using above-mentioned nickel-plating additive, not doping are directly electroplated.
Comparative example 2
A kind of electro-plating method using above-mentioned nickel-plating additive, including：
The BE nickel brighteners of commercial type are added into nickel solution according to the dosage of 3ml/L, form mixed liquor；
Consumption when plating into the mixed liquor according to 80ml/kA.h adds nickel-plating additive.
The mixed liquor prepared with the additive or brightener of embodiment 1-8 and comparative example 1-2 is prepared into nickel coating, specifically
For：By workpiece to be plated (the A3 steel discs of 35mm × 25mm × 1mm) the successively heat chemistry alkali liquor oil removing through sodium hydroxide/sodium carbonate,
Absolute ethyl alcohol oil removing, distilled water are cleaned, merging electroplating bath carries out electrochemical deposition after the activation process of 4% dilute hydrochloric acid immersion,
Workpiece to be plated is then taken out, is dried wash with distilled water.
By obtained by embodiment 1-8 and comparative example 1-2 workpiece to be plated and mixed liquor tested as follows, the results are shown in Table 1.
Dispersibility is tested：It is measured using far and near cathode method (Haring-Blue methods).It measures slot and uses Haring cell, it is internal
Size is 150mm × 50mm × 70mm.It is the copper sheet of 0.5mm that cathode, which selects thickness, and working face size is 50mm × 50mm；Anode
For plating nickel plate with holes；Plating electric current 1A, electroplating time 30min.
The dispersibility calculation formula of plating solution is：
The dispersibility of plating solution=[K- (Δ M1/ Δ M2)]/(K-1) (result is expressed as a percentage；K is remote cathode in formula
To the distance of anode and nearly cathode to the ratio of distances constant of anode, K takes 2 in this test；Δ M1 is the increment after being electroplated on nearly cathode
(g)；Δ M2 is the increment (g) after being electroplated on remote cathode.
Covering power is tested：It is measured using endoporus method.It is the copper pipe of 50mm, an end seal that cathode, which selects internal diameter l10mm, pipe range,
It closes.When test, nozzle is fixed on 80mm, test current 0.2A, electroplating time 30min at a distance from anode.According to following formula
It calculates：
Covering power=endoporus coating length/pipe range (result is expressed as a percentage).
Porosity test：Porosity size will be directly related to the corrosion resisting property of coating, and GB5935-86 is pressed using paster method
Standard detection.
The etchant solution of the potassium ferricyanide solution of 10g/L and the sodium chloride solution of 20g/L as porosity test.Operation
Step is：Coating surface is deoiled after wiped clean, is tightly attached to coating surface with the filter paper for being impregnated with etchant solution, the two cannot have
Gap.Etchant solution solution is bought with glass bar or degreasing swab stick and fully soaks filter paper, and a solution, 5min are supplemented at interval of lmin
Filter paper is taken off afterwards, with distilled water flushing it is clean after dry, record hole points.It is placed on airing on cleaned glass plate, number Bluepoint
Number.It substitutes into following formula and calculates voidage：
The number of porosity=spot/tested area (a/cm2)
When calculating number of apertures, make following calculate by spot diameter size：
Corrode spot diameter and be less than lmm, every with a porosimeter；It is less than 3mm every more than lmm with three porosimeters；
It is less than 5mm more than 3mm, with ten porosimeters at every.
Microhardness (HV)：The microhardness of coating, load 100g are measured using HV-71 type microhardness testers.
Wearability measures：On M5-10 type wear testers, the sample after heat treatment is loaded into lotus 2kg, loads 6h rotating speeds
10r min, stroke 8mm, test specimens are weightless, then are converted to wear extent (mgh-1cm-1).
Corrosion resistance measures：Workpiece to be plated impregnates 72h in 10% hydrochloric acid solution, then measures its weightlessness, and is converted to corruption
Lose rate (mgh-1cm-1).
Brightness is tested：Make reference with the minute surface that light reflectivity is 100%, with Shimadzu UV-240 type UV-vis spectroscopies
The light reflectivity of photometric determination coating, wave-length coverage characterize the brightness of coating for 600-800nm with light reflectivity.
The test result of 1 coating of table
As can be known from Table 1, the dispersibility of the mixed liquor of embodiment 1-8 and covering power are obviously higher than 1 He of comparative example
2, thus illustrate that the brightener of the present invention significantly improves the dispersibility and covering power of mixed liquor.In addition embodiment 1-8
Coating brightness, hardness, porosity, abrasion resistance properties and corrosion resistance are superior to comparative example 1 and 2, thus illustrate, of the invention
Nickel-plating additive significantly increases the brightness of coating, reduces the porosity of coating, improves the hardness of coating, increases prolonging for coating
Malleability increases the wear resistance and corrosion resistance of coating, prevents coating from generating pin hole and point.
It is above disclosed to be only a preferred embodiment of the present invention, the power of the present invention cannot be limited with this certainly
Sharp range, therefore equivalent changes made in accordance with the claims of the present invention, are still within the scope of the present invention.
Claims (10)
1. a kind of nickel-plating additive, which is characterized in that including：
Propine sodium sulfonate 60-150g/L；
Sodium Allyl Sulfonate 10-80g/L；
2- ethylhexylsulfate sodium salts 10-50g/L；
Polyoxyethylated alkyl phenol sodium sulfate salt 10-50g/L；
Polyetheramine 1-20g/L；
Organic polysulfide 5-15g/L；
Boric acid 10-30g/L.
2. nickel-plating additive as described in claim 1, which is characterized in that including：
Propine sodium sulfonate 80-120g/L；
Sodium Allyl Sulfonate 30-60g/L；
2- ethylhexylsulfate sodium salts 20-45g/L；
Polyoxyethylated alkyl phenol sodium sulfate salt 20-45g/L；
Polyetheramine 5-12g/L；
Organic polysulfide 7-12g/L；
Boric acid 15-25g/L.
3. nickel-plating additive as claimed in claim 2, which is characterized in that including：
Propine sodium sulfonate 90-110g/L；
Sodium Allyl Sulfonate 40-50g/L；
2- ethylhexylsulfate sodium salts 30-40g/L；
Polyoxyethylated alkyl phenol sodium sulfate salt 30-40g/L；
Polyetheramine 7-10g/L；
Organic polysulfide 9-11g/L；
Boric acid 18-22g/L.
4. nickel-plating additive as described in claim 1, which is characterized in that further include 0.6-1.5g/L saccharin.
5. nickel-plating additive as claimed in claim 4, which is characterized in that the content of saccharin is 0.8-1.2g/L.
6. a kind of electro-plating method using any one of claim 1-5 nickel-plating additives, which is characterized in that including：
Nickel-plating additive is added into nickel solution, mixed liquor is formed；
Mixed liquor is stirred, mixing speed 800-2000r/min；
The temperature of mixed liquor is 45-60 DEG C, pH value 4.0-5.0；
Consumption when plating into the mixed liquor according to 80-120ml/kA.h adds nickel-plating additive.
7. electro-plating method as claimed in claim 6, which is characterized in that add nickel-plating additive according to the dosage of 0.1-1ml/L
Enter into nickel solution, forms mixed liquor.
8. electro-plating method as claimed in claim 6, which is characterized in that mixing speed 1000-1600r/min.
9. electro-plating method as claimed in claim 6, which is characterized in that the temperature of mixed liquor is 51-56 DEG C.
10. electro-plating method as claimed in claim 6, which is characterized in that the pH value of mixed liquor is 4.5-4.8.
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