CN101838830B - Electrolyte of electroplating palladium-nickel alloy - Google Patents
Electrolyte of electroplating palladium-nickel alloy Download PDFInfo
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Abstract
The invention relates to electrolyte of an electroplating palladium-nickel alloy, in particular to electrolyte. The invention provides electrolyte which can electroplate bright, compact and needle-hole-free electroplating palladium-nickel alloy with different nickel contents (10 to 40 percent), which comprises major salt, complexing agent, additive, conductive salt and pH stabilizer; the major salt comprises a palladium salt and a nickel salt, calculating at the metal palladium, the content of the palladium salt is 1 to 10 g/L, and the mol ratio of the palladium salt and the nickel slat is 1: 1 to 3; the concentration of the complexing agent is 0.2 to 1.0 mol/L; the content of the additive is 0.01 to 1.0 g/L; the content of the conductive salt is 20 to 100 g/L; and the pH stabilizer is of 20 to 50 g/L boric acid or 30 to 90 g/L pyroborate.
Description
Technical field
The present invention relates to a kind of electrolytic solution, especially relate to a kind of electrolytic solution of electroplating palladium-nickel alloy.
Background technology
Gold utensil has good solidity to corrosion, electroconductibility and ductility, in electronic industry, is widely used as the covering with paint metal of electric contactor and junctor.The price of gold lattice are expensive, and substitute, the saving cost of seeking gold plate have caused people's extensive concern.Many character of palladium are all similar with gold, and like solidity to corrosion, ductility etc., and the price of palladium is more cheap, and density is lower, and application cost is well below gold.Palldium alloy coating not only can make cost further reduce, and can also significantly reduce the suction hydrogen phenomenon of pure palladium coating, improves ductility, wear resistance, contact resistance and the luminance brightness etc. of palladium coating.Therefore, palladium and alloy thereof are considered to the most possible metal or alloy that replaces or practice thrift gold.
In addition, palladium and alloy thereof also can be used as high-grade ornamental bottom, blocking layer, electrically contact coating, patch coating, be widely used in industries such as ornamental industry, electronic industry, micro electronmechanical processing.
Palladium and nickel belong to gang together, and character is approaching.The thermodynamic stability of Pd-Ni alloy is better.Because the low price of nickel, solidity to corrosion is better, and contact resistance is lower, so Pd-Ni alloy is a kind of palldium alloy of at present widespread usage.
At present, domestic research about electroplating palladium-nickel alloy is few.The emphasis of foreign study is, through the selection of complexing agent and additive, to reach high speed electrodeposition and the galvanized purpose of no ammonia.To electroplating high nickel content, again can be as requested, the research of electroplating the Technology of different Ni contents Pd-Ni alloy does not appear in the newspapers; The additive research that high nickel content and different Ni contents Pd-Ni alloy coating luminance brightness, compactness and porosity are played a decisive role does not appear in the newspapers yet.
In the Pd-Ni alloy, nickel content is bigger to the property effect of coating, and the Pd-Ni alloy coating of different Ni contents has different hardness, different thermodynamic stabilities, and different application is also arranged certainly.At present, the nickel mass content is that about 20% Pd-Ni alloy coating is widely used, but the Pd-Ni alloy of nickelic mass content is not seen industrial application.
For with a kind of plating bath, in the certain current density scope, electroplate the Pd-Ni alloy coating that obtains, the mass content of nickel is constant basically.U.S. Pat .4849303 points out that behind a spot of iodide ion of adding, under the different electric flow density, the nickel quality change is no more than 3% in the Pd-Ni alloy coating that obtains in the plating bath.
Summary of the invention
The present invention aims to provide the electrolytic solution of the electroplating palladium-nickel alloy of a kind of light that can electroplate out different nickel mass content (10%～40%), densification, free of pinholes.
The electrolytic solution of electroplating palladium-nickel alloy according to the invention comprises main salt, complexing agent, additive, conducting salt and pH stablizer; Said main salt comprises palladium salt and nickel salt, calculates with palladium metal, and the content of palladium salt is 1～10g/L, and in molar ratio, palladium salt: nickel salt is 1: (1～3); The concentration of said complexing agent is 0.2～1.0mol/L; Said content of additive is 0.01～1.0g/L; The content of said conducting salt is 20～100g/L; Said pH stablizer is 20～50g/L boric acid or 30～90g/L pyroborate.
Said palladium salt can be selected from least a in Palladous chloride, dichloro diamino palladium, dichloro four ammonia palladiums, sulfuric acid diamino palladium, sulfuric acid four ammonia palladiums, nitrous acid ammonia palladium, nitric acid ammonia palladium, the oxalic acid diamino palladium etc.
Optional at least a in single nickel salt, nickelous chloride, nickel sulfamic acid etc. of said nickel salt.
Said complexing agent can be selected from least a in ammoniacal liquor, quadrol, Padil, trolamine, thanomin, diethylene diamine, triethylene tetramine, Hydrocerol A and salt thereof, tartrate and the salt thereof etc.
Said additive can be selected from least a in propenyl thiocarbamide, nicotinic acid, nicotinic acid amide, pyridine trisulfonic acid, acrylic amide, asccharin, benzene sulfinic acid sodium salt, propiolic alcohol, the butynediol etc.
Said conducting salt can be selected from least a in ammonium chloride, sodium-chlor, Repone K, sodium sulfate, ammonium sulfate, an ammonium nitrate, the saltpetre etc.
Galvanized condition is: the bath pH value scope is 6.5～10; Current density is 0.1～2.0A/dm
2Bath temperature is 20～50 ℃; During electrolysis, middling speed stirs; Adopting platinized titanium net, graphite, stainless steel etc. is insoluble anode, and ratio of cathodic to anodic area is 1: (1～3).
The nickel mass content is the highest can to reach 40%.
Electrolytic solution according to the invention; Palladium salt is mainly introduced with forms such as Palladous chloride, dichloro diamino palladium, dichloro four ammonia palladiums, sulfuric acid diamino palladium, sulfuric acid four ammonia palladiums, nitrous acid ammonia palladium, nitric acid ammonia palladium or oxalic acid diamino palladiums, and nickel salt is mainly introduced with forms such as single nickel salt, nickelous chloride or nickel sulfamic acids.The ratio of palladium and nickel content increases and increases along with the ratio of palladium salt and nickel salt in the plating bath in the coating, but after nickel mass content in the coating was above 40%, the nickel mass content basically no longer changed with the further raising of nickel salt content in the plating bath.The content of palladium salt (in palladium metal) is 1～10g/L.Palladium content is high more in the plating bath, and plating speed is fast more, but the palladium loss is also big more; Palladium content is too low in the plating bath, then will often add palladium, and maintenance cost increases.Nickel salt is pressed palladium salt and nickel salt mol ratio 1: (1～3) adds.
Electrolytic solution according to the invention, complexing agent mainly are ammoniacal liquor, quadrol, Padil, trolamine, thanomin, diethylene diamine, triethylene tetramine, Hydrocerol A and salt thereof, one or more in tartrate and the salt thereof.Concentration is 0.2～1.0mol/L.In containing the electrolytic solution of these complexing agents, can obtain the Pd-Ni alloy coating of light.When using ammoniacal liquor, should note suitably reducing the temperature and of the volatilization of pH value of plating bath with obstruction ammoniacal liquor as complexing agent.
Electrolytic solution according to the invention; Additive mainly is one or more in propenyl thiocarbamide, nicotinic acid, nicotinic acid amide, pyridine trisulfonic acid, acrylic amide, asccharin, benzene sulfinic acid sodium salt, sodium laurylsulfonate, propiolic alcohol or the butynediol, and content is 0.01～1.0g/L.Sodium laurylsulfonate had both played influence of surfactant, played brightening agent again, and propenyl thiocarbamide, acrylic amide, asccharin, nicotinic acid amide, propiolic alcohol, butynediol, benzene sulfinic acid sodium salt etc. are brightening agents.When current density is high, also need add a spot of nicotinic acid, pyridine trisulfonic acid or nicotinic acid amide.Additive is used, and just can obtain the Pd-Ni alloy coating of light, densification, free of pinholes.
Electrolytic solution according to the invention, conducting salt are one or more in ammonium chloride, sodium-chlor, Repone K, sodium sulfate, ammonium sulfate, an ammonium nitrate or the saltpetre.Content is 20～100g/L.
Electrolytic solution according to the invention, pH stablizer are 20～50g/L boric acid or 30～90g/L pyroborate.In this pH scope, the electrolytic solution stable in properties, the coating performance that obtains is superior.When bath pH value was on the low side, coating was the lime look; When bath pH value was higher, nickel content can reduce in the coating.
Plating condition of the present invention, electrolytic solution is weakly alkaline, and preferred pH value scope is 6.5～10.
Plating condition of the present invention, plating is at 0.1～2.0A/dm
2Current density under carry out.When current density was excessive, coating nickel content can reduce.This is because along with the raising of current density, the increase of palladium sedimentation velocity is greater than nickel deposition speed to be increased.But to a kind of plating bath, current density is at 0.1～2.0A/dm
2In the scope, the variation of the nickel mass content of the Pd-Ni alloy coating that obtains is no more than 4%.When current density was too small, electrodeposition efficiency reduced, and cost increases.
Plating condition of the present invention, temperature are 20～50 ℃.When temperature was too high, coating surface was sent out mist.Cross when low when temperature, the nickel mass content can reduce in the coating.
Form and the plating condition through regulating plating bath, can obtain the Pd-Ni alloy coating of different Ni contents, the nickel mass content is the highest can to reach 40%.Be used additive, can obtain the Pd-Ni alloy coating of different Ni contents, light, densification, free of pinholes.
Embodiment
Below provide the compound method (being upgraded to example) of the electrolytic solution of said electroplating palladium-nickel alloy to prepare 1:
1. main salt palladium salt is added and contain in the container of 100mL deionized water, heating, dropping ammonia stirs, and dissolving gets solution A;
2. main salt nickel salt is added and contain in the container of 100mL deionized water, heating is stirred, and dissolving gets solution B;
3. complexing agent, conducting salt and pH stablizer are added and contain in the container of 400mL deionized water, heating is stirred, and dissolving gets solution C;
4. solution A and solution B are added in the solution C, stir, get solution D;
5. additive is added and contain in the container of 100mL deionized water, heating is stirred, and after the dissolving, adds in the solution D, gets solution E;
6. with alkali lye such as ammoniacal liquor, sodium hydroxide or potassium hydroxide solution, add in the solution E, making its pH value scope is 6.5～10.Add deionized water, the TV that makes solution is 1000mL.
Embodiment 1
1) plating bath composition and plating condition are following
Dichloro diamino palladium (in palladium) 2g/L
Nickel sulfate hexahydrate 25g/L
Ammonium chloride 30～50g/L
Boric acid 40～50g/L
Ammoniacal liquor 30～60ml/L
Sodium laurylsulfonate 0.1～0.5g/L
Propiolic alcohol 0.05～0.4g/L
Asccharin 0.1～0.5g/L
PH (transferring) 6.5～8 with ammoniacal liquor
Current density 0.5～1A/dm
2
45 ℃ of temperature
Anode platinized titanium net
Negative electrode and anodic area were than 1: 2
Middling speed stirs in the electroplating process.
2) coating test result: referring to table 1, contact resistance evaluation criteria: SJ2431-84, general gold plate contact resistance is less than 0.6m Ω.
Table 1
Embodiment 2
1) plating bath composition and plating condition are following
Sulfuric acid four ammonia palladium (in palladium) 6g/L
Six water nickelous chloride 25g/L
Sodium-chlor 30～50g/L
Ten water sodium pyroborates, 50～80g/L
Quadrol 10～30g/L
Sodium laurylsulfonate 0.1～0.5g/L
Nicotinic acid 0.05～0.4g/L
Benzene sulfinic acid sodium salt 0.05～0.5g/L
PH (transferring) 6.5～7.5 with ammoniacal liquor
Current density 1～1.5A/dm
2
50 ℃ of temperature
Anode graphite
Negative electrode and anodic area were than 1: 2
Middling speed stirs in the electroplating process.
2) coating test result: referring to table 2.
Table 2
Embodiment 3
1) plating bath composition and plating condition are following
Nitrous acid ammonia palladium (in palladium) 8g/L
Nickel sulfamic acid 40g/L
Ammonium sulfate 30～60g/L
Boric acid 30～40g/L
Padil 15～30g/L
Acrylic amide 0.2～0.5g/L
Nicotinic acid amide 0.05～0.4g/L
Sodium laurylsulfonate 0.05～0.5g/L
PH (transferring) 7～9 with ammoniacal liquor
Current density 1～1.5A/dm
2
30 ℃ of temperature
The anode stainless steel
Negative electrode and anodic area were than 1: 3
Middling speed stirs in the electroplating process.
2) coating test result: referring to table 3.
Table 3
Embodiment 4
1) plating bath composition and plating condition are following
Oxalic acid diamino palladium (in palladium) 10g/L
Nickel sulfate hexahydrate 45g/L
Repone K 30～50g/L
Ten water sodium pyroborates, 40～80g/L
Tripotassium Citrate 40～60g/L
Butynediol 0.1～0.5g/L
Pyridine trisulfonic acid 0.05～0.2g/L
Sodium laurylsulfonate 0.05～0.5g/L
PH (transferring) 6.5～8 with ammoniacal liquor
Current density 1～2A/dm
2
40 ℃ of temperature
The anode stainless steel
Negative electrode and anodic area were than 1: 2
Middling speed stirs in the electroplating process.
2) coating test result: referring to table 4.
Table 4
In the present invention, along with the increase of nickel mass content in the coating, the hardness of coating significantly increases, and wear resistance also significantly improves, thereby can improve it greatly as the work-ing life that electrically contacts coating.Nickelic mass content Pd-Ni alloy coating still has lower contact resistance, qualified weldability, and coating light, fine and close, free of pinholes reach the requirement of on electronic industry, using fully.
In the present invention, same plating bath is 0.1～2.0A/dm in current density
2The coating that obtains in the scope, the variation of nickel mass content is no more than 4%.
The present invention is through the ratio and the proper technical conditions of palladium salt and nickel salt in the adjusting plating bath, and the mass content of nickel can change between 10%～40% as required in the Pd-Ni alloy coating that obtains, and can reach 40%.And the Pd-Ni alloy coating of the different nickel mass content that obtain all has lower contact resistance, qualified weldability, wear resistance preferably.
Claims (1)
1. the electrolytic solution of an electroplating palladium-nickel alloy is characterized in that comprising main salt, complexing agent, additive, conducting salt and pH stablizer; Said main salt comprises palladium salt and nickel salt, calculates with palladium metal, and the content of palladium salt is 1～10g/L, and in molar ratio, palladium salt: nickel salt is 1: (1～3); The concentration of said complexing agent is 0.2～1.0mol/L; Said content of additive is 0.01～1.0g/L; The content of said conducting salt is 20～100g/L; Said pH stablizer is 20～50g/L boric acid or 30～90g/L pyroborate;
Said palladium salt is selected from least a in Palladous chloride, dichloro diamino palladium, dichloro four ammonia palladiums, sulfuric acid diamino palladium, sulfuric acid four ammonia palladiums, nitrous acid ammonia palladium, nitric acid ammonia palladium, the oxalic acid diamino palladium;
Said nickel salt is selected from least a in single nickel salt, nickelous chloride, the nickel sulfamic acid;
Said complexing agent is selected from least a in ammoniacal liquor, quadrol, Padil, trolamine, thanomin, diethylene diamine, triethylene tetramine, Hydrocerol A and salt thereof, tartrate and the salt thereof;
Said additive is selected from least a in propenyl thiocarbamide, nicotinic acid, nicotinic acid amide, pyridine trisulfonic acid, acrylic amide, asccharin, benzene sulfinic acid sodium salt, propiolic alcohol, the butynediol;
Said conducting salt is selected from least a in ammonium chloride, sodium-chlor, Repone K, sodium sulfate, ammonium sulfate, an ammonium nitrate, the saltpetre;
The compound method of the electrolytic solution of said electroplating palladium-nickel alloy is following:
(1) adding of palladium salt is contained in the container of 100mL deionized water, heating, dropping ammonia stirs, and dissolving gets solution A;
(2) the nickel salt adding is contained in the container of 100mL deionized water, heating is stirred, and dissolving gets solution B;
(3) complexing agent, conducting salt and the adding of pH stablizer are contained in the container of 400mL deionized water, heating is stirred, and dissolving gets solution C;
(4) solution A and solution B are added in the solution C, stir, get solution D;
(5) the additive adding is contained in the container of 100mL deionized water, heating is stirred, and after the dissolving, adds in the solution D, gets solution E;
(6) add in the solution E with alkali lye, making its pH value scope is 6.5～10, adds deionized water, and the TV that makes solution is 1000mL, and said alkali lye is selected from ammoniacal liquor, hydrochlorinate sodium or hydrochlorinate potassium solution.
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