CN101240437B - Method for plating zinc-nickel alloy in alkaline electroplate liquid - Google Patents
Method for plating zinc-nickel alloy in alkaline electroplate liquid Download PDFInfo
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Abstract
The invention discloses a method for electroplating alkaline Zn-Ni alloy, comprising the steps of: preparing alkali wash and acid wash, preparing electroplating Zn-Ni alloy plating solution, mechanical grinding, degreasing with organic solvent or water-based detergent, alkali washing, acid washing and electroplating. The invention provides a stable electroplating solution formula and complete electroplating process. The coating electroplated by the method is proved to have good flat surface, uniform coating distribution and alloy distribution, the coating is single gamma-phase, the nickel has a content of 10% to 15%; the coating has superior corrosion resistance, red rust appears on the non-passivated Zn-Ni coating after 1500 hours in a neutral salt spray test; compared with general alkali electroplating solution, the coating has high current efficiency, reaching up to 80% to 90%.
Description
Technical field
The invention belongs to the electroplating technology field, be specifically related to a kind of in alkali plating solution the method for electroplated zinc nickel alloy.
Background technology
Electroplated zinc nickel alloy has many excellent characteristic, like solidity to corrosion, thermostability and the low hydrogen embrittlement etc. of excellence.Compare with zinc coating, cadmium plating layer, can improve solidity to corrosion more than 3 times, its thermostability, hardness and wear resistance are significantly improved, and its hydrogen embrittlement can reduce again greatly.The plating bath of the electroplated zinc nickel alloy of using at present can be divided into acid system and alkaline system.Acid system adopts acidic bath; Space ripple etc. points out that the acidic bath composition is simple in " the aviation high-strength steel hangs down hydrogen embrittlement electroplating zinc-nickel alloy technical study " literary composition, cathode efficiency is high, bath stability; Easy to operate; But its uneven coating is even, and the composition of alloy layer is bigger with the variation of current density, makes the solidity to corrosion of coating descend.And alkaline system adopts alkali plating solution, and Wu Yinan analyzes alkali plating solution in " development of electroplating zinc alloy " literary composition.The dispersive ability of alkali plating solution is good, and coating alloying constituent ratio is even in broad current density range, and thickness of coating is even, and little to the corrodibility of equipment and workpiece, technological operation is easy, process stabilizing, and cost is lower.Zinc-nickel alloy electroplating technology has been carried out a large amount of research both at home and abroad; But belong to acidic zinc nickel alloy electricity depositing process mostly; And the number of processes of electroplated zinc nickel alloy is less in alkali plating solution, and that is that all right is ripe for technology, exists coating nickel content lower (7～9%); The coating phase structure is not single γ phase (corrosion resisting property of the admiro of single γ phase is good), low (50～70%) problem that waits of cathode efficiency.
Summary of the invention
The purpose of this invention is to provide a kind of in alkali plating solution the method for electroplated zinc nickel alloy; Adopt alkali plating solution; Through process treatment process such as preparation washing lotion, mechanical grinding, cleaning and plating; Obtained to have the zn-ni alloy deposits of good corrosion resisting property and current efficiency, and coating interalloy composition and thickness of coating are even.
Of the present invention a kind of in alkali plating solution the method for electroplated zinc nickel alloy comprise five steps:
The first step, preparation alkaline wash, pickle solution and electroplate liquid.
Alkaline wash is to contain NaOH, Na
3PO
412H
2O, Na
2CO
310H
2O, Na
2SiO
3NH
2The aqueous solution of O wherein preferably, contains NaOH 60～80g, Na in every liter of alkaline wash
3PO
412H
2O 20～40g, Na
2CO
310H
2O 20～40g, Na
2SiO
3NH
2 O 20～40g, all the other are water.
Pickle solution adopts HCl solution, and preferably, containing HCl in every liter of pickle solution is 4～8mL.
The Alkaline Zinc boron-tungsten-iron-nickel alloy electroplating is for containing ZnO, NiSO
4, NaOH, complexing agent, additive and brightening agent the aqueous solution, preferably, in every liter of plating bath, contain ZnO 10～30g, NiSO
45～13g, NaOH 100～140g contains an amount of complexing agent, additive and brightening agent and water in addition.
Described complexing agent can be two or more the material in lemon acid amide, trolamine, quadrol, diethylenetriamine, TEPA, Seignette salt, EDTA and the ammoniacal liquor.Preferably, the complexing agent components contents of required interpolation is (containing in every liter of plating bath) in plating bath: lemon acid amide 5～40g or trolamine 38～80mL or quadrol 25～40mL or diethylenetriamine 3～20mL or more than the TEPA 3mL or among Seignette salt 15～25g or EDTA 8～15g or the ammoniacal liquor 10～20mL two kinds or two or more.
Described additive is the reaction product of any one and epoxy chloropropane and amine among phytic acid or sodium phytate or the CTAB.Preferably, the binder component of required interpolation is (containing in every liter of plating bath) at content in plating bath: the reaction product 1.5～15mL of phytic acid 0.05～15mL or sodium phytate 0.1～5g or CTAB 0.1～5g, epoxy chloropropane and amine.
Described brightening agent is combined by in ZB, vanillin food grade,1000.000000ine mesh, thiocarbamide, the asccharin one or more.Preferably, the brightening agent content that needs in every liter of plating bath to add is (containing in every liter of plating bath): one or more among ZB 1～10mL or vanillin food grade,1000.000000ine mesh 0.2～2g or thiocarbamide 1～2g or the asccharin 1～5g.
The reaction product of said epoxy chloropropane and amine is DE.
In second step, mechanical grinding is cleaned plating piece.
With plating piece successively 100
#, 200
#, 400
#, 600
#, 800
#, 1000
#Carry out mechanical grinding on the aluminum oxide sandpaper, clean with organic solvent or aqueous cleaning agent then.Described organic solvent or aqueous cleaning agent are used to remove the greasy dirt of matrix surface, and organic solvent can be chosen trichloroethane, gasoline, and acetone, ethanol, trieline, a kind of arbitrarily in the tetracol phenixin, and adopt more than the ultrasonic cleaning matrix surface 10min.
The 3rd step, alkali cleaning.
The alkaline wash that plating piece after second step cleaned immerses the first step preparation carries out alkali cleaning, and the temperature of alkali cleaning is 70～90 ℃, behind time 10～20min with plating piece successively via mobile hot water wash, mobile cold wash;
The 4th step, pickling.
To carry out pickling through the plating piece after the 3rd step alkali cleaning, 15～30 ℃ of pickle solution temperature, scavenging period 0.5～1.0min takes out after the via flow cold wash.
In the 5th step, electroplate.
To be immersed in the Alkaline Zinc boron-tungsten-iron-nickel alloy electroplating for preparing in the first step through the plating piece after the 4th step pickling and electroplate current density 1～6A/dm
2, 10～35 ℃ of temperature according to needed thickness of coating, are regulated solution composition and technology, and under identical solution composition and processing condition, the thick more needed electroplating time of coating is long more.For example, thickness of coating can reach 6 μ m behind the plating 20min, and thickness of coating is less than 3.5 μ m behind the 10min.
The zn-ni alloy deposits that obtains after electroplating is carried out pattern with performance analysis shows, the alloy layer surfacing is bright, and nickel content is 10%～15%, and coating is single γ phase; The current efficiency of negative electrode is high, reaches 80～90%; Coating has good corrosion resisting property, in the neutral salt spray test not the Zinc-Nickel coating layer of passivation red rust appears later at 1500h.
The invention has the advantages that:
(1) adopts the alkali zinc nickel alloy plating process, solved in the acid technology with current density change coating interalloy composition variation problem greatly;
(2) coating smooth, nickel content are 10%～15%, and coating is single γ phase;
(3) compare with general alkali plating solution, the current efficiency of negative electrode is high, reaches 80～90%;
(4) solidity to corrosion of coating is good, in the neutral salt spray test not the Zinc-Nickel coating layer of passivation red rust appears later at 1500h;
(5) electroplating technology is simple to operate, and the plating bath cost is low, stable performance.
Description of drawings
Fig. 1 adopts zn-ni alloy deposits that the inventive method the prepares metallograph at 500 times of following microscopic appearances;
Fig. 2 is the EDX figure that adopts the zn-ni alloy deposits that the inventive method prepares;
Fig. 3 is the XRD figure that adopts the zn-ni alloy deposits that the inventive method prepares;
Fig. 4 is the influence of current density change to zn-ni alloy deposits nickel content.
Embodiment
Below in conjunction with accompanying drawing and embodiment to of the present invention a kind of in alkali plating solution the method for electroplated zinc nickel alloy be elaborated.
The present invention provide a kind of in alkali plating solution the method for electroplated zinc nickel alloy, specifically comprise the steps:
The first step, preparation alkaline wash, pickle solution and electroplate liquid.
Alkaline wash is to contain NaOH, Na
3PO
412H
2O, Na
2CO
31OH
2O, Na
2SiO
3NH
2The aqueous solution liquid of O wherein contains NaOH 60～80g, Na in every liter of alkaline wash
3PO
412H
2O 20～40g, Na
2CO
31OH
2O20～40g, Na
2SiO
3NH
2 O 20～40g, all the other are water.
Pickle solution adopts HCl solution, and to contain HCl in every liter of pickle solution be 4～8mL.
The Alkaline Zinc boron-tungsten-iron-nickel alloy electroplating is for containing ZnO, NiSO
4, NaOH, complexing agent, additive and brightening agent the aqueous solution, in every liter of plating bath, contain ZnO 10～30g, NiSO
45～13g, NaOH 100～140g contains an amount of complexing agent, additive and brightening agent and water in addition.
Described complexing agent is made up of two or more the material in lemon acid amide, trolamine, quadrol, diethylenetriamine, TEPA, Seignette salt, EDTA and the ammoniacal liquor.The complexing agent components contents of required interpolation in plating bath is (containing in every liter of plating bath): lemon acid amide 5～40g or trolamine 38～80mL or quadrol 25～40mL or diethylenetriamine 3～20mL or more than the TEPA 3mL or among Seignette salt 15～25g or EDTA 8～15g or the ammoniacal liquor 10～20mL two kinds or two or more.
Described additive is the mixture of any one and DE among phytic acid or sodium phytate or the CTAB.The binder component of required interpolation is (containing in every liter of plating bath) at content in plating bath: phytic acid 0.05～15mL or sodium phytate 0.1～5g or CTAB 0.1～5g and DE 1.5～15mL.
Described brightening agent is one or more in ZB, vanillin food grade,1000.000000ine mesh, thiocarbamide, three kinds of materials of asccharin.Needing the brightening agent content of interpolation in every liter of plating bath is (containing in every liter of plating bath): one or more among ZB 1～10mL or vanillin food grade,1000.000000ine mesh 0.2～2g or thiocarbamide 1～2g or the asccharin 1～5g.
In second step, mechanical grinding is cleaned plating piece.
With plating piece successively 100
#, 200
#, 400
#, 600
#, 800
#, 1000
#Carry out mechanical grinding on the aluminum oxide sandpaper, clean with organic solvent or aqueous cleaning agent then.Described organic solvent or aqueous cleaning agent are used to remove the greasy dirt of matrix surface, and organic solvent can be chosen trichloroethane, gasoline, and acetone, ethanol, trieline, a kind of arbitrarily in the tetracol phenixin, and adopt more than the ultrasonic cleaning matrix surface 10min.
The 3rd step, alkali cleaning.
The alkaline wash that plating piece after second step cleaned immerses the first step preparation carries out alkali cleaning, and the temperature of alkali cleaning is 70～90 ℃, behind time 10～20min with plating piece successively via mobile hot water wash, mobile cold wash;
The 4th step, pickling.
To carry out pickling through the plating piece after the 3rd step alkali cleaning, 15～30 ℃ of pickle solution temperature, scavenging period 0.5～1.0min takes out after the via flow cold wash.
In the 5th step, electroplate.
To be immersed in the Alkaline Zinc boron-tungsten-iron-nickel alloy electroplating for preparing in the first step through the plating piece after the 4th step pickling and electroplate current density 1～6A/dm
2, 10～35 ℃ of temperature, under the constant condition of other processing condition, electroplating time is long more, and thickness of coating is thick more.
The zn-ni alloy deposits that obtains after electroplating is carried out pattern with performance analysis shows, the alloy layer surfacing is bright, and nickel content is 10%～15%, and coating is single γ phase; The current efficiency of negative electrode is high, reaches 80～90%; Coating has good corrosion resisting property, in the neutral salt spray test not the Zinc-Nickel coating layer of passivation red rust appears later at 1500h.
Neutral salt spray test adopts 5% the sodium chloride salt aqueous solution, and the solution pH value is transferred at the solution of neutral range (6～7) as spraying usefulness, and test temperature is all got 35 ℃, and the rate of descent that requires salt fog is between 1～2mL.
Embodiment one:Electroplated zinc nickel alloy coating on the 30CrMnSiA steel matrix.
The first step, preparation alkaline wash, pickle solution and electroplate liquid.
Contain in every liter of alkaline wash: NaOH 70g, Na
3PO
412H
2O 30g, Na
2CO
310H
2O 30g, Na
2SiO
3NH
2O 30g.All the other are water.
Contain HCl 6mL in every liter of pickle solution.
Every liter of Alkaline Zinc boron-tungsten-iron-nickel alloy electroplating contains: ZnO 10g, NiSO
45g, NaOH 120g, complexing agent TEPA 3mL, trolamine 38mL, ammoniacal liquor 10mL, additive DE 1.5mL, CTAB 2g, brightening agent ZB 3mL, vanillin food grade,1000.000000ine mesh 0.2g, all the other are water.
In second step, mechanical grinding is cleaned plating piece.
With aluminum oxide sandpaper polishing plating piece matrix to 1000
#Sand paper selects for use organic solution ethanol to carry out ultrasonic cleaning matrix surface 10min, removes the greasy dirt of matrix surface.
The 3rd step, alkali cleaning.
Plating piece after second step cleaned immerses alkaline wash and carries out alkali cleaning, and the temperature of alkali cleaning is 80 ℃, behind the time 15min with plating piece successively via mobile hot water wash, mobile cold wash.
The 4th step, pickling.
Plating piece after the alkali cleaning is immersed pickle solution carry out pickling, 20 ℃ of pickle solution temperature, scavenging period 0.5min takes out after the via flow cold wash.
In the 5th step, electroplate.
With electroplating in the Alkaline Zinc boron-tungsten-iron-nickel alloy electroplating for preparing in the immersion of the plating piece after the pickling the first step, get 1,2,3,4,5 in current density, 6A/dm
2In time, electroplate respectively, and each current density value carries out three plating and measures nickel content in the coating respectively, gets the MV of nickel content and analyzes the relation between nickel content and the current density.10 ℃ of bath temperatures, electroplating time are 20min.
At 2A/dm
2Under the current condition coating is carried out pattern and performance analysis, from metallograph shown in Figure 1, can see, alloy layer has the surface topography of smooth densification.
Zn-ni alloy deposits is carried out power spectrum and phase composition analysis, can know, coating is mainly elementary composition by zinc and two kinds in nickel, in addition, also contains a spot of oxygen and iron matrix element, and is as shown in Figure 2.Coating power spectrum display result is: O-0.24%; Fe-2.98%; Ni-12.88%; Zn-83.90%.XRD phase composition analytical results shows and only has γ-phase in the coating that Coating composition is single, like Fig. 3.Through under different current densities, electroplating, can draw the influence curve of current density change to nickel content in the zn-ni alloy deposits, as shown in Figure 4, can find out that current density is at 1～6A/dm
2Scope in when changing, the nickel content is mild in the coating.
In addition, adopt the weighting method binding constituents to measure and calculate, at 2A/dm
2Under the condition, the current efficiency of coating is 88.3%.The solidity to corrosion of coating can know through neutral salt spray test, and to go out the time of red rust be not 1500h to the zn-ni alloy deposits of passivation; Can know that through scratch test the bonding force of coating is good.
Embodiment two:Electroplated zinc nickel alloy coating on stainless steel base.
The first step, preparation alkaline wash, pickle solution and electroplate liquid.
The preparation of alkaline wash and pickle solution is with embodiment one.
Electroplate liquid is ZnO, NiSO
4, the aqueous solution formed of NaOH, lemon acid amide, TEPA, trolamine, EDTA, phytic acid, DE, thiocarbamide, and contain in every liter of Alkaline Zinc boron-tungsten-iron-nickel alloy electroplating: ZnO 20g, NiSO
410g, NaOH 100g, complexing agent lemon acid amide 15g, TEPA 20mL, trolamine 40mL, EDTA15g, additive phytic acid 0.15mL, DE 9mL, brightening agent thiocarbamide 1g, all the other are water.
In second step, mechanical grinding is cleaned plating piece.
With sand papering plating piece surface to 1000
#, select for use organic solution acetone to carry out ultrasonic cleaning matrix surface 10min.
The 3rd step, alkali cleaning.
Plating piece after second step cleaned immerses alkaline wash and carries out alkali cleaning, and the temperature of alkali cleaning is 70 ℃, behind the time 20min with plating piece successively via mobile hot water wash, mobile cold wash.
The 4th step, pickling.
Plating piece after the alkali cleaning is immersed pickle solution carry out pickling, 15 ℃ of pickle solution temperature, scavenging period 1min takes out after the via flow cold wash.
In the 5th step, electroplate.
With electroplating in the Alkaline Zinc boron-tungsten-iron-nickel alloy electroplating for preparing in the immersion of the plating piece after the pickling the first step, current density is got 2A/dm
2, 20 ℃ of bath temperatures, electroplating time are 20min.
The alkali zinc nickel alloy layer that adopts electro-plating method of the present invention to prepare is observed the coating smooth under 500 times of metaloscopes; The content that EDX detects Ni in the coating is 14.45%; Can find out that from the XRD figure that records only there is single γ-phase in coating; Adopting the weighting method binding constituents to measure calculates at 2A/dm
2Current efficiency under the condition is 85.3%; The solidity to corrosion of coating can know through salt-fog test, and to go out the time of red rust be not 1500h to the zn-ni alloy deposits of passivation; Can know that through scratch test the bonding force of coating is good.
Embodiment three:Electroplated zinc nickel alloy coating on the copper matrix.
The first step, preparation alkaline wash, pickle solution and electroplate liquid.
Preparation alkaline wash, pickle solution are with embodiment one.
The Alkaline Zinc boron-tungsten-iron-nickel alloy electroplating is ZnO, NiSO
4, the aqueous solution formed of NaOH, Seignette salt, TEPA, trolamine, sodium phytate, DE, asccharin, and in every liter of basic plating admiro plating bath, contain ZnO 30g, NiSO
413g, NaOH 140g, complexing agent Seignette salt 20g, TEPA 20mL, trolamine 80mL, additive sodium phytate 0.15g and DE 15mL, brightening agent asccharin 1g, all the other are water.
In second step, mechanical grinding is cleaned plating piece.
With aluminum oxide sandpaper polishing plating piece matrix to 1000
#, select for use organic solution acetone to carry out ultrasonic cleaning matrix surface 15min, remove the greasy dirt of matrix surface.
The 3rd step, alkali cleaning.
Plating piece after second step cleaned immerses alkaline wash and carries out alkali cleaning, and the temperature of alkali cleaning is 90 ℃, behind the time 10min with plating piece successively via mobile hot water wash, mobile cold wash.
The 4th step, pickling.
Plating piece after the alkali cleaning is immersed pickle solution carry out pickling, 30 ℃ of pickle solution temperature, scavenging period 0.1min takes out after the via flow cold wash.
In the 5th step, electroplate.
With electroplating in the Alkaline Zinc boron-tungsten-iron-nickel alloy electroplating for preparing in the immersion of the plating piece after the pickling the first step, current density is got 2A/dm
2, 35 ℃ of bath temperatures, electroplating time are 20min.
The zn-ni alloy deposits that adopts the inventive method to prepare is observed the coating smooth under 500 times of metaloscopes; Detect through EDX, wherein the content of Ni is 14.76%; From the XRD figure that records, draw and only have single phase γ-phase in the coating;
Adopting the weighting method binding constituents to measure calculates at 2A/dm
2Current efficiency under the condition is 87.1%; The solidity to corrosion of coating can know through salt-fog test, and to go out the time of red rust be not 1500h to the zn-ni alloy deposits of passivation; Can know that through scratch test the bonding force of coating is good.
Claims (6)
1. the method for an electroplated zinc nickel alloy in alkali plating solution is characterized in that comprising the steps to electroplate:
Step 1, preparation alkaline wash, pickle solution and electroplate liquid; Described electroplate liquid contains ZnO, NiSO
4, NaOH and an amount of complexing agent, additive, brightening agent;
Described complexing agent is two or more lemon acid amide, trolamine, quadrol, diethylenetriamine, TEPA, Seignette salt, EDTA, ammoniacal liquor;
Described additive is two kinds of materials, i.e. the reaction product of any one material, epoxy chloropropane and the amine among phytic acid or sodium phytate or the CTAB;
Described brightening agent is one or more in ZB, vanillin food grade,1000.000000ine mesh, thiocarbamide, the asccharin;
Described electroplating bath components is to contain ZnO 10～30g, NiSO in every liter of plating bath
45～13g; NaOH 100～140g; The lemon acid amide 5～40g, trolamine 38～80mL, quadrol 25～40mL, diethylenetriamine 3～20mL, TEPA 3mL that contains two or more is above, Seignette salt 15～25g, EDTA 8～15g, ammoniacal liquor 10～20mL; Contain any one and DE 1.5～15mL among phytic acid 0.05～15mL or sodium phytate 0.1～5g or the CTAB 0.1～5g; Contain one or more of ZB 1～10mL or vanillin food grade,1000.000000ine mesh 0.2～2g or thiocarbamide 1～2g or asccharin 1～5g, all the other are water; DE wherein is the reaction product of epoxy chloropropane and amine;
Step 2, mechanical grinding are cleaned plating piece;
Step 3, alkali cleaning;
Step 4, pickling;
Step 5, plating.
2. according to claim 1 a kind of in alkali plating solution the method for electroplated zinc nickel alloy, it is characterized in that: the alkaline wash in the step 1 is for containing NaOH, Na
3PO
412H
2O, Na
2CO
310H
2O, Na
2SiO
3NH
2The aqueous solution of O, and contain NaOH 60～80g, Na in every liter of alkaline wash
3PO
412H
2O 20～40g, Na
2CO
310H
2O 20～40g, Na
2SiO
3NH
2O 20～40g, all the other are water;
Described pickle solution is a HCl solution, contains HCl 4～8mL in every liter of pickle solution.
3. according to claim 1 a kind of in alkali plating solution the method for electroplated zinc nickel alloy, it is characterized in that: the cleaning plating piece described in the step 2 is selected organic solvent or aqueous cleaning agent for use, chooses trichloroethane; Gasoline, acetone, ethanol; Trieline, a kind of arbitrarily in the tetracol phenixin.
4. according to claim 1 a kind of in alkali plating solution the method for electroplated zinc nickel alloy, it is characterized in that: the temperature of the said alkali cleaning of step 3 is 70～90 ℃, time 10min～20min, plating piece is successively via mobile hot water wash, the cold wash of flowing afterwards.
5. according to claim 1 a kind of in alkali plating solution the method for electroplated zinc nickel alloy, it is characterized in that: the said pickling of step 4 is that the plating piece after the alkali cleaning is immersed pickle solution, 15～30 ℃ of temperature, time 0.5～1.0min is afterwards through the via flow cold wash.
6. according to claim 1 a kind of in alkali plating solution the method for electroplated zinc nickel alloy, it is characterized in that: the said plating of step 5 is the plating piece after the pickling to be immersed in the alkali zinc nickel alloy electroplating bath for preparing electroplate current density 1～6A/dm
2, 10～35 ℃ of temperature according to needed thickness of coating, are regulated solution composition and technology, and under identical solution composition and processing condition, the thick more needed electroplating time of coating is long more.
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2008
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