CN100494497C - Nickel pre-coating process and nickel pre-coating solution for magnesium alloy surface - Google Patents

Nickel pre-coating process and nickel pre-coating solution for magnesium alloy surface Download PDF

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CN100494497C
CN100494497C CNB2007100345134A CN200710034513A CN100494497C CN 100494497 C CN100494497 C CN 100494497C CN B2007100345134 A CNB2007100345134 A CN B2007100345134A CN 200710034513 A CN200710034513 A CN 200710034513A CN 100494497 C CN100494497 C CN 100494497C
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nickel
magnesium alloy
coating
plating
plating bath
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CN101021009A (en
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余刚
肖耀坤
易祥榕
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Hunan University
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Hunan University
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Abstract

The present invention is nickel pre-coating process and nickel pre-coating solution for the surface of magnesium alloy. The technological process features that magnesium alloy is pre-treated through immersion coating of zinc and then nickel pre-coated, and may be used to replace traditional cyaniding copper pre-coating. The pre-treatment may be any of available zinc immersing processes. The pre-coating solution has nickel sulfate as main component and citrate as accessory ingredient. The present invention has great cathode current range and high current efficiency, and the obtained coating has compact structure, high adhesion and excellent anticorrosive performance.

Description

Mg alloy surface nickel preplating technology and pre-plating bath
Technical field
The present invention relates to a kind of on magnesium alloy the method for nickel preplating, this invention can replace cyanide pre-plating copper, belongs to metallic corrosion and protection field.
Technical background
Magnesium alloy has the advantage of many uniquenesses, and density is low, specific tenacity and specific rigidity height and damping and amortization, machinability, castability are superior, has obtained increasingly extensive application on automotive industry, space flight and aviation industry, electronic industry.Magnesium raw material is abundant, is in the 8th in natural resources, but as structured material, and its solidity to corrosion difference has restricted the major cause that it uses widely.
The Standard Electrode Potentials of magnesium is-2.37V, has very high reactive behavior, in air or solution, magnesium alloy can very fast generation one deck passive film as thin as a wafer, thereby cause electroplating or during electroless plating metal plating not strong with the magnesium substrate adhesion, do not reach service requirements, thus electroplate and electroless plating before must elder generation's process special pre-treatment to remove surperficial passive film, obtain even, a clean surface, to obtain metal plating with good combination power.
The ASTM of American Society for testing and materials-88 has provided the magnesium alloy direct chemical nickel-plating of DOW company and has soaked two kinds of pre-treating technologies of zinc.Its main direct chemical nickel plating is to carry out the alkali cleaning oil removing earlier, corrodes the hydrofluoric acid activation by chromic acid then, carries out chemical nickel plating at last.Because the chemical nickel-plating liquid instability on the magnesium alloy is so the plating cost of direct chemical nickel plating is very high.The main technique flow process of soaking the zinc method is: alkali cleaning oil removing → chromic acid erosion → hydrogen fluoride activates → soaks zinc → cyanide pre-plating copper → plating or electroless plating, it.These two technologies have all been used highly toxic substance, are unfavorable for health of human body and environment protection.
The Norsk Hydro technology and the WCM technology in addition of zinc method is soaked in employing.They are the same with the dip galvanizing technique that DOW company proposes, and all need just can electroplate and electroless plating through cyanide pre-plating copper after soaking zinc, exist the problem of not environmental protection.
Summary of the invention
Purpose of the present invention is intended to the defective at prior art, provide a kind of new when Mg alloy surface can obtain having the pre-plating layer of good combination power and high anti-corrosion, the more important thing is the Mg alloy surface nickel preplating technology and the pre-plating bath that can effectively reduce environmental pollution.
The objective of the invention is to realize by following manner:
Technology of the present invention is: magnesium alloy carried out soaking zinc after the pre-treatment, and then nickel preplating.
Employed pre-plating bath is that main salt is that single nickel salt, Synergist S-421 95 are that Citrate trianion, inhibiter are fluorochemical in the described nickel preplating, the concentration ratio of main salt and Synergist S-421 95 is 10:1～20:1, service temperature is 45～55 ℃, and pH is 4.0～5.5, and cathode current density is 0.5～10Adm -2
Pre-plating bath of the present invention comprises: main salt is single nickel salt 20～250gdm -3, Synergist S-421 95 is Citrate trianion 2.5～15gdm -3, inhibiter fluorochemical 10～55gdm -3, pH:4.0 ~ 5.5, the concentration ratio of main salt and Synergist S-421 95 is 10:1～20:1.
Described pre-plating bath also can add the anode activator, can be halogenide etc.
Described pre-plating bath also can comprise existing commercial nickel plating additive, or asccharin and 1, the 4-butynediol.
Pre-plating bath adopts ammoniacal liquor as the pH regulator agent.
The present inventor has proposed a new Mg alloy surface and has carried out the method that preplating is handled, change the technical thought of original technology,, adopt the mode of nickel preplating at pre-treating technology and after soaking zinc, make the technical process of whole technology that a new change take place, avoided deleterious technological process.Plating can pre-treatment → soaking zinc → nickel preplating → conventional electroplating technique flow process carries out electroplating parts according to plating.
The present invention when obtaining having the pre-plating layer of good combination power and high anti-corrosion, can effectively reduce environmental pollution owing to adopted nontoxic nickel preplating to replace the cyanide pre-plating copper of severe toxicity.
Pre-plating bath composition of the present invention is simple, easy and simple to handle, plating bath is easy to safeguard to have lower plating cost.
Nickel preplating technology of the present invention does not increase extra step and equipment than cyanide pre-plating copper, can replace existing cyanide pre-plating copper very easily, has favorable industrial application prospect.
The concrete technical process of the present invention is as follows:
1. mechanical grinding and polishing
The handled magnesium alloy parts of the present invention can be die casting, sand mold casting part or plastic shaping part, also can be the part after the machining.For non-machining part, carry out mechanical grinding or polishing earlier, polishing also can adopt the mode of electrochemistry or chemistry to carry out.
2. degreasing
May there be greases such as releasing agent, rubbing paste in pending part, adopts the ultrasonic wave Solvent degreasing to clean, and organic solvent can be acetone or gasoline, kerosene, trieline etc.
3. oil removing
Adopt basic solution to do further skimming treatment.Basic solution is exemplified below: sodium hydroxide (NaOH) 50gdm -3, sodium phosphate (Na 3PO 412H 2O) 10gdm -3, temperature: 60 ± 5 ℃, the time: 8 ~ 10min.Oil removing also can be by cloudy
The mode of utmost point electrolytic degreasing is carried out, and cathodic current is 8～10Adm -2
4. pickling
Adopt pickle solution to remove the passive film and the intermetallic segregation compound of Mg alloy surface, thereby obtain clean Mg alloy surface uniformly.Being exemplified below of pickle solution: oxalic acid (C 2H 4O 2) 10gdm -3, sodium lauryl sulphate (C 12H 25SO 3Na), 0.1gdm -3, room temperature.Pickle solution gives an example 2: chromium trioxide (CrO 3) 120gdm -3, nitric acid (HNO 3) 110cm 3Dm -1
5. activation
Passivation more very easily takes place in the magnesium alloy behind removal passive film and the intermetallic segregation compound in air and plating bath; protect magnesium alloy so need to generate one deck activation film by activation; the activation film that generates can be dissolved in thereafter the zincate solution, has good bonding force so can guarantee the zinc-impregnating layer of generation.Activating recipe is exemplified below: potassium pyrophosphate (K 4P 2O 7) 40gdm -3, Potassium monofluoride (KF) 5gdm -3, 75 ℃, 1min.The activation solution 2:HF 220m that gives an example 3Dm -3
6. soak zinc
Soak zinc and can on magnesium alloy, form one deck displacement zinc layer.Zinc-impregnating layer has reduced the potential difference between nickel dam and magnesium alloy as the middle layer, thereby has weakened replacement(metathesis)reaction, has strengthened the bonding force of coating.It is as follows to soak the zinc formula examples: zinc sulfate ZnSO 450gdm -3, potassium pyrophosphate (K 4P 2O 7) 150gdm -3, yellow soda ash (Na 2CO 3) 5gdm -3, lithium fluoride (LiF) 3gdm -3Or Potassium monofluoride (KF) 5gdm -3, pH10.2～10.4,65 ℃, time: 2min.
7. nickel preplating
Magnesium alloy after soaking zinc and finishing can carry out nickel preplating, single nickel salt (NiSO in the nickel preplating of the present invention 4) be main salt, content is low, and solution dispersibility is good, and the coating crystallization is careful, but cathode efficiency and limit current density are low, and sedimentation velocity is slow, the nickel sulfate content height, limit current density is big, but the corrosion resistance of coating that obtains is bad.Ammonium citrate ((NH 4) 3C 6H 5O 7) as Synergist S-421 95, can follow Ni 2+Generate the citric acid nickel complex, be adsorbed on the cathode sample.The concentration ratio of main salt and Synergist S-421 95 is between 10:1 ~ 20:1, and ratio is too high, the coating porosity height that obtains, and solidity to corrosion is bad, and ratio is too low, and cathode efficiency is low, and low district can not get coating.Ammonium bifluoride (NH 4HF 2) as inhibiter, its effect is that the magnesium alloy that protection is soaked behind the zinc is not corroded in weakly acidic plating bath, concentration is too low, does not reach corrosion mitigating effect, and is too high, then easily and Ni 2+Generate NiF 2Precipitate, not only influence the stability of plating bath, also have a strong impact on the quality of coating, the pH value of regulating plating bath with ammoniacal liquor.According to job requirements, also can add an amount of additive, to obtain to have the nickel coating of good glossy surface.Additive can use existing commercial nickel plating additive, also can use asccharin and 1, the 4-butynediol, but need the strict ratio of controlling the primary and secondary brightening agent, in order to avoid generate coating with big internal stress.
Carrying out routine on the basis of resulting pre-plating layer electroplates or electroless plating.
Magnesium alloy behind the nickel preplating can directly carry out routine to be electroplated or electroless plating, as electroplating bright nickel/chromium, and electro-coppering/three layer nickel/chromium, chemical nickel plating etc.
The present invention also can adopt other pre-treating technology, as long as can make the good zinc-impregnating layer of one deck bonding force, carries out nickel preplating with regard to adopting pre-plating bath of the present invention.
Embodiment
The invention will be further described below in conjunction with embodiment, but the present invention is not limited to these embodiment.
Embodiment 1
Test materials is the AZ91D magnesium alloy
1. polishing
Adopt the mechanical polishing mode that magnesium alloy work-piece surface is treated to glossy surface.
2. Solvent degreasing
With acetone solvent washing 10 minutes, service temperature was a room temperature under the ultrasonic wave effect.
3. alkali cleaning oil removing
Sodium hydroxide (NaOH) 50gdm -3, sodium phosphate (Na 3PO 412H 2O) 10gdm -3, temperature: 60 ± 5 ℃, the time: 8-10min;
4. acid erosion
Oxalic acid (C 2H 4O 2) 10gdm -3, sodium lauryl sulphate (C 12H 25SO 3Na), 0.1gdm -3, room temperature.
5. alkaline activation
Potassium pyrophosphate (K 4P 2O 7) 40gdm -3, Potassium monofluoride (KF) 5gdm -3,75 ℃, 1min.
6. soak zinc
Zinc sulfate ZnSO 450gdm -3, potassium pyrophosphate (K 4P 2O 7) 150gdm -3, yellow soda ash (Na 2CO 3) gdm -3, fluoridize (LiF) 3gdm -3, pH10.2～10.4,65 ℃, time: 2min.
7. nickel preplating
Single nickel salt (NiSO 46H 2O) 100gdm -3, ammonium citrate ((NH 4) 3C 6H 5O 7) 5gdm -3, ammonium bifluoride (NH 4HF 2) 25dm -3, ammoniacal liquor (NH 3H 2O) 35mldm -3, pH:4.5 ~ 5.5, temperature: 45 ~ 55 ℃, time: 10min, cathode current density: 5Adm -2, pneumatic blending, continuous filtration.
The sample that obtains adopts following method to carry out Performance Detection, and the result is as shown in table 1.
Solidity to corrosion is estimated with neutral salt spray test.Salt air corrosion experimental standard by GB/T10125-97 carries out neutral salt spray test, and be 24h experimental period, evaluates the protection class of coating then according to GB/T6461-85.
Scratch method and thermal shock experiment that the bonding strength of coating adopts GB/T5270-85 to recommend, scratch experiment uses the steel knife that has ground 30 ° of acute angle of layer, on sample, draw 5 rows, length and width are the square lattice of 1mm, observe the coating peeling or come off whether between line, and, observe the coating peeling situation of gluing after drawing, relatively the power of bonding force with the coating in mightiness belt employing vertical mode glug; Thermal shock experiment is that plating piece is heated to 250 ℃, be incubated 1 hour, rapidly it is put in the cold water then, so repeats 20 times, and whether observation coating peeling or come off.
Embodiment 2
Test materials is the AZ91D magnesium alloy
Testing sequence is identical with embodiment 1, and nickel preplating prescription and processing condition are: single nickel salt 25gdm -3, ammonium citrate ((NH 4) 3C 6H 5O 7) 2.5gdm -3, ammonium bifluoride (NH 4HF 2) 35gdm -3, ammoniacal liquor (NH 3H 2O) 45cm 3Dm -3, pH:4.5-5.5, temperature: 45-55 ℃, time: 30min, cathode current density: 2Adm -2, pneumatic blending, continuous filtration.
Embodiment 3
Test materials is the AZ91D magnesium alloy
Testing sequence is identical with embodiment 1, and nickel preplating prescription and processing condition are: its prescription and processing condition are: single nickel salt (NiSO 46H 2O) 200gdm -3, ammonium citrate ((NH 4) 3C 6H 5O 7) 15g.dm -3, ammonium bifluoride (NH 4HF 2) 25gdm -3, ammoniacal liquor (NH 3H 2O) 35cm 3Dm -3, pH:4.5-5.5, temperature: 45-55 ℃, time: 6min, cathode current density: 10Adm -2, pneumatic blending, continuous filtration.
Embodiment 4
Test materials is the AZ91D magnesium alloy
Testing sequence is identical with embodiment 1, has just added brightening agent in the nickel preplating, and its prescription and processing condition are: single nickel salt (NiSO 46H 2O) 100gdm -3, ammonium citrate ((NH 4) 3C 6H 5O 7) 5gdm -3, ammonium bifluoride (NH 4HF 2) 25gdm -3, ammoniacal liquor (NH 3H 2O) 35cm 3Dm -3, 1,4-butynediol 0.3gdm -3, asccharin 2gdm -3, pH:4.5 ~ 5.5, temperature: 45-55 ℃, time: 10min, cathode current density: 5Adm -2, pneumatic blending, continuous filtration.
Embodiment 5
Test materials is the AZ91D magnesium alloy
Testing sequence is identical with embodiment 1, has just added nickel plating additive (company provides by Atotech, and compositions such as every additive hereinafter also provide by Atotech company) in the nickel preplating, and its prescription and processing condition are: single nickel salt (NiSO 46H 2O) 100gdm -3, ammonium citrate ((NH 4) 3C 6H 5O 7) 5gdm -3, ammonium bifluoride (NH 4HF 2) 25gdm -3, ammoniacal liquor (NH 3H 2O) 35mldm -3, open cylinder agent 8cm 3Dm -3, fill and lead up agent 5cmm 3Dm -3, wetting agent 1cm 3Dm -3, pH:4.5-5.5, temperature: 45 ~ 55 ℃, time: 10min, cathode current density: 5Adm -2, pneumatic blending, continuous filtration.
Embodiment 6
Test materials is the AZ91D magnesium alloy
Step 1-7 is with example 1.
8. electroplating bright nickel
Single nickel salt (NiSO 4.6H 2O) 250～325gdm -3, nickelous chloride (NiCl 2.6H 2O) 50～70gdm -3, boric acid (H 3BO 3) 40～55gdm -3, key light agent 1cm 3Dm -3, softening agent 10cm 3Dm -3, auxiliary 4cm 3Dm -3, wetting agent (Y-19) 1.5cm 3Dm -3, total nickel amount 75gdm -3, chlorion 15gdm -3, 55 ℃ of temperature, pH4.5, cathode current density 5Adm -2, time: 8min, pneumatic blending, continuous filtration.
9. electrodeposited chromium
Chromic anhydride 220～260gdm -3, sulfuric acid 1.0～1.2gdm -3, trivalent chromium 1.5～3.0gdm -3, additive A 1cm 3Dm -3, additive B 5cm 3Dm -3, 40 ℃ of temperature, time: 10min, cathode current density 15Adm -2The result is as shown in table 1.
Embodiment 7
Experiment material is the AZ91D magnesium alloy.
Step 1-7 is with example 1
8. electroplating acid copper
Copper sulfate (CuSO 4.5H 2O) 200 ~ 220gdm -3, sulfuric acid (H 2SO 4) (30-the 40cm of ρ=1.84g/1) 3Dm -3, chlorion (Cl -) 80-150mgdm -3, open cylinder agent 5～10cm 3Dm -3, fill and lead up agent 0.4～0.6cm 3Dm -3, brightening agent 0.4～0.6cm 3Dm -3, 20～30 ℃ of temperature, cathode current density 1～6Adm -2, anodic current density 0.5～2.5Adm -2, anodic phosphorous copper angle (0.03-0.06%), pneumatic blending, continuous filtration.
9. electroplate half light nickel
Half light nickel (NiSO 4.6H 2O) 265～375gdm -3, NiCl 2.6H 2O 38～53gdm -3, H 3BO 338～50gdm -3Open cylinder agent 3～6cm 3Dm -3, fill and lead up agent 0.25～1.0cm 3Dm -3, auxiliary is according to coating current potential needs, wetting agent (NP-A) 1～3cm 3Dm -3, temperature: 50～70 ℃, pH:3.6～4.0, cathode current density: 5.4Adm -2, time: 5min inflates stirring, continuous filtration.
10. electroplate high-sulfur nickel
Single nickel salt (NiSO 4.6H 2O) 240-360gdm -3, nickelous chloride (NiCl 2.6H 2O) 60～120gdm -3, boric acid (H 3BO 3) 35～40gdm -3, additive 3.5～7.5cm 3Dm -3, wetting agent 1～5cm 3Dm -3, 50 ℃ of temperature, pH2.5, cathode current density 3Adm -2, time: 3min, mechanical stirring, continuous filtration.
11. electroplating bright nickel
Single nickel salt (NiSO 4.6H 2O) 250～325gdm -3, nickelous chloride (NiCl 2.6H 2O) 50～70gdm -3, boric acid (H 3BO 3) 40～55gdm -3, key light agent 1cm 3Dm -3, softening agent 10cm 3Dm -3, auxiliary 4cm 3Dm -3, wetting agent (Y-19) 1.5cm 3Dm -3, total nickel amount 75gdm -3, chlorion 15gdm -3, 55 ℃ of temperature, pH4.5, cathode current density 5Adm -2, time: 8min, pneumatic blending, continuous filtration.
12. electrodeposited chromium
With step 9 among the embodiment 4, the result is as shown in table 1.
Embodiment 8
Test materials is the AZ91D magnesium alloy
Step 1-7 is with example 1
8. chemical nickel plating
Single nickel salt (NiSO 4) 20～25gdm -3, sodium hypophosphite (NaH 2PO 2) 20～25gdm -3, sodium-acetate (CH 3COONa) 12gdm -3, Trisodium Citrate (Na 3C 6H 5O 7) 12gdm -3, pH value 4.1-4.5,80-90 ℃ of temperature, the time is 1 hour, the result is as shown in table 1.
Embodiment 9
Test materials is the AZ31B magnesium alloy
Experimental procedure is with embodiment 1, and the result is as shown in table 1.
Embodiment 10
Test materials is the AM60 magnesium alloy
Experimental procedure is with embodiment 1, and the result is as shown in table 1.
Embodiment 11
Test materials is the AZ91D magnesium alloy
Step 1-3 is with embodiment 1.
4. acid erosion
Chromium trioxide 180 (CrO 3) gdm -3, iron nitrate (Fe (NO 3) 39H 2O) 40gdm -3, Potassium monofluoride (KF) 3.5gdm -3, 15～35 ℃ of temperature, the time is 15 seconds to 3 minutes.
5. activation
Phosphoric acid (H 3PO 4) 200mldm -3, ammonium bifluoride (NH 4HF 2) 105gdm -3, 16～38 ℃ of temperature, the time is 15 seconds to 2 minutes.
6. soak zinc
Zincate solution composition and operational condition are with embodiment 1, and just time lengthening is 10 minutes.
7. with embodiment 1.The result is as shown in table 1.
The performance test result of table 1 embodiment (zero non-scale, * peeling)

Claims (5)

1, Mg alloy surface nickel preplating technology is characterized in that: magnesium alloy carried out soaking zinc after the pre-treatment, and then nickel preplating; Employed pre-plating bath is that main salt is that single nickel salt, Synergist S-421 95 are that Citrate trianion, inhibiter are fluorochemical in the described nickel preplating, the concentration ratio of main salt and Synergist S-421 95 is 10:1～20:1, service temperature is 45～55 ℃, and pH is 4.0～5.5, and cathode current density is 0.5～10Adm -2
2, magnesium alloy nickel preplating technology according to claim 1 is characterized in that, the nickel preplating treatment time is 3～30 minutes.
3, the employed pre-plating bath of Mg alloy surface nickel preplating technology, it is characterized in that it comprises: main salt is single nickel salt 20～250gdm -3, Synergist S-421 95 is Citrate trianion 2.5～15gdm -3, inhibiter fluorochemical 10～55gdm -3, pH:4.0～5.5, the concentration ratio of main salt and Synergist S-421 95 is 10:1～20:1.
4, the employed pre-plating bath of Mg alloy surface nickel preplating technology according to claim 3 is characterized in that described pre-plating bath also adds the anode activator.
5, the employed pre-plating bath of Mg alloy surface nickel preplating technology according to claim 3 is characterized in that described pre-plating bath also is added with the nickel plating additive.
CNB2007100345134A 2007-03-09 2007-03-09 Nickel pre-coating process and nickel pre-coating solution for magnesium alloy surface Expired - Fee Related CN100494497C (en)

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