CN101314848B - Non-ammonia type plating solution for chemical nickel plating - Google Patents
Non-ammonia type plating solution for chemical nickel plating Download PDFInfo
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- CN101314848B CN101314848B CN200810029520XA CN200810029520A CN101314848B CN 101314848 B CN101314848 B CN 101314848B CN 200810029520X A CN200810029520X A CN 200810029520XA CN 200810029520 A CN200810029520 A CN 200810029520A CN 101314848 B CN101314848 B CN 101314848B
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Abstract
The invention discloses an ammonia-free chemical nickel plating bath which adopts an ammonia-free pH modifying agent to regulate the pH value of the bath. Each liter of the bath contains the components that nickel salt is 24 to 30g, reducing agent is 24 to 33g, buffering agent is 10 to 18g, complexing agent is 20 to 30g, stabilizing agent is 0.5 to 1.5mL, brightener is 1.5 to 3.0mL, and others arewater. In the ammonia-free chemical nickel plating bath, the ammonia-free pH modifying agent is selected from one or the mixture of sodium hydroxide, and potassium hydroxide or potassium carbonate. All materials in the ammonia-free chemical nickel plating bath do not contain heavy metal, ammonia water is not utilized to regulate the pH value, the problems of environment pollution, invalidation caused by overlong storing time of the bath, etc. are not caused, and the obtained chemical plating bath is friendly to the environment, in addition, the luminance brightness of the made plating layer can be full-bright. The bath has wide application prospect.
Description
Technical field
The present invention relates to a kind of chemical plating bath, specifically a kind of non-ammonia type plating solution for chemical nickel plating.
Background technology
Common chemical plating fluid is to adopt ammoniacal liquor to provide alkalescence to regulate the pH value of plating bath and provide complexing action with the nickel ion in the complexing plating bath.The complex ability of ammoniacal liquor can make plating bath more stable, and the alkalescence that ammoniacal liquor provides makes the plating speed energy high maintenance of plating bath a relative higher level with more weak complex ability.But the ammoniacal liquor highly volatile that uses in the coating preparation process causes environmental pollution, does not meet the requirement of cleaner production; The content of ammoniacal liquor a large amount of minimizings along with the growth of time in the plating bath simultaneously produce certain influence to plating solution performance, must constantly add ammoniacal liquor for this reason.The chemical plating bath that uses ammoniacal liquor through four MTO (loop cycle) after, the decay of plating speed is comparatively serious, can below 10 μ m/h production efficiency greatly be descended usually, has increased the production cost of factory.
Summary of the invention
The present invention is directed to prior art problems, purpose is to provide a kind of non-ammonia type plating solution for chemical nickel plating.
The present invention is achieved through the following technical solutions above-mentioned purpose:
Main contribution of the present invention is to provide the agent of a kind of no ammonia type pH regulator, and it is one or both the mixture in sodium hydroxide, potassium hydroxide, salt of wormwood, yellow soda ash, saleratus or the sodium bicarbonate.
The screening formulation of non-ammonia type plating solution for chemical nickel plating of the present invention is that per 1 liter of plating bath contains following component:
Nickel salt 24～30g,
Reductive agent 24～33g,
Buffer reagent 10～18g,
Complexing agent 20～30g,
Stablizer 0.5～1.5mL,
Brightening agent 1.5～3.0mL,
Water surplus;
Regulating plating bath pH with the pH regulator agent is 4.8～6.0.
Described nickel salt is single nickel salt, nickelous chloride or nickel acetate preferably.
Described reductive agent is Hypophosporous Acid, 50 and salt, boron hydrohalogenic acid salt or hydrazine hydrate preferably; Described hypophosphite is sodium hypophosphite or potassium hypophosphite preferably, and described boron hydrohalogenic acid salt is sodium borohydride or POTASSIUM BOROHYDRIDE preferably.
Described buffer reagent is acetic acid, sodium-acetate, ammonium acetate or ammonium sulfate preferably.
Described complexing agent is the mixture of two or more in Succinic Acid, tartrate, citric acid, lactic acid, propionic acid, oxysuccinic acid or the glycine etc. preferably.
Described stablizer is preferably and comprises sodium wolframate 4～9g in every liter of stabiliser solution, imidazoles 0.2～9g and ethylenediamine tetraacetic acid (EDTA) or its salt 5～20g.
Described brightening agent is preferably in every liter of brightening agent solution and contains copper sulfate 2～10g, zinc sulfate 2～10g or tin protochloride 2～10g, Bismuth trinitrate 3～10g, tartrate 5～20g.
It is 4.8～6.0 that described conditioning agent is regulated plating bath pH, preferably the mixture of one or both in sodium hydroxide, potassium hydroxide or salt of wormwood.
The present invention is by adding highly basic and an amount of complexing agent in ammonia Ni-P chemical plating fluid is arranged, thereby the alkalescence and the complexing action that replace ammoniacal liquor, the plating bath environmentally safe that obtains, and can make the luminance brightness of coating reach full light, still can maintain more than the 16 μ m/h through plating speed behind 4 MTO.
The preparation method of non-ammonia type plating solution for chemical nickel plating of the present invention is nickel salt, reductive agent, buffer reagent, complexing agent, stablizer and brightening agent to be mixed obtain, and is heated to and can uses after assigned temperature is stablized 10min.The plating temperature of chemical plating fluid is 90～97 ℃.
Compared with prior art, the present invention has following beneficial effect:
(1) all raw materials of the present invention all do not contain heavy metal, and do not use ammoniacal liquor to regulate the pH value, can not cause environmental pollution and plating bath because of problems such as long inefficacies storage period, the chemical plating bath that obtains is not only environmentally friendly, and the luminance brightness of the coating of making reaches full light, maintains more than the 16 μ m/h in plating speed behind 4 MTO, plating bath does not produce white precipitate, do not have nickel in the aqueduct and separate out, phosphorus content reaches more than 11% (wt%), and stronger corrosion resistance nature is arranged;
(2) all to plate performance strong for plating bath provided by the invention, and coating is not subjected to the influence of the complex configuration of body material, all keeps original shape of material after the plating, bonding force is strong, incrust, than the bonding force height of durionise and ion plating, saved the follow-up polishing program of electroplating preparation;
(3) plating bath all the components provided by the invention all can adopt domestic raw material, makes the plating bath cost reduce significantly.
(4) plating bath provided by the invention can be widely used in industrial sectors such as machinery, electronics, plastics, mould, metallurgy, petrochemical complex, pottery, waterpower, aerospace, does not contain the electroless plating workpiece processing needs that lead and cadmium heavy metal ion can satisfy outlet European Union, the U.S. and Japan.
Embodiment
Comparative Examples 1
3.5g copper sulfate and 13g tartrate are added the less water dissolving, then with 4.0g Bismuth trinitrate and 4.5g zinc sulfate sulfuric acid dissolution, at last both are mixed, adding packs into behind the ammoniacal liquor fills in the beaker of 1L deionized water, until clarification, obtain brightening agent solution 1L with magnetic stirrer.
With sodium wolframate 5g, imidazoles 2g, EDTA2Na 15g, packing into fills in the beaker of deionized water, and the high speed magnetic agitation is settled to 1L to all dissolvings with the deionized water volume, obtains stabiliser solution.
With six hydration nickel sulfate 28g, a hydration inferior sodium phosphate 24g, sodium acetate trihydrate 10g, glycine 2g, lactic acid 10mL (12g), propionic acid 5mL (6g), stabiliser solution 1.0mL, brightening agent 1.5mL, packing into fills in the beaker of deionized water, and the high speed magnetic agitation is to all dissolvings, with the pH value modulation about 5.4 of 25mL ammoniacal liquor with solution, be settled to 1L with the deionized water volume, obtain preparing the plating bath 1L of high bright Electroless Ni-P Plating.
To beaker preheating 15min in 90 ℃ of water-baths of above-mentioned plating bath be housed, common iron plate is gone out rolled tin in 10% dilute hydrochloric acid and 5% vitriolic mixed solution, the hydrochloric acid of putting into then 1: 1 is put into plating bath after activating 3～5min, plating 1 hour.By titration Ni
2+Content, determine to add the volume of A liquid and C liquid, by the calculating plating speed of poor quality before and after the weighing plating, put into new test piece then, until covering four circulations.
This method is for there being the ammonia bath system, and the first seven hour of plating speed of the coating that makes is respectively: 17.4 μ m/h, 19.9 μ m/h, 16.0 μ m/h, 16.3 μ m/h, 13.4 μ m/h, 13.1 μ m/h, 12.5 μ m/h; The average plating speed in first three cycle is respectively: 17.8 μ m/h, 13.7 μ m/h, 10.6 μ m/h.Phosphorus content average out to 9%～12% in the coating.
Embodiment 1
3.5g copper sulfate and 13g tartrate are added the less water dissolving, then with 4.0g Bismuth trinitrate and 4.5g zinc sulfate sulfuric acid dissolution, at last both are mixed, adding packs into behind the ammoniacal liquor fills in the beaker of 1L deionized water, until clarification, obtain brightening agent solution 1L with magnetic stirrer.
With sodium wolframate 4g, imidazoles 3g, EDTA2Na 17g, packing into fills in the beaker of deionized water, and the high speed magnetic agitation is settled to 1L to all dissolvings with the deionized water volume, obtains stabiliser solution.
With six hydration nickel sulfate 28g, ortho phosphorous acid 24g, ammonium acetate 10g, tartrate 3g, lactic acid 10mL, propionic acid 5mL, stabiliser solution 1.0mL, brightening agent 1.5mL, packing into fills in the beaker of deionized water, and the high speed magnetic agitation is to all dissolvings, with the pH value modulation 5.3 of sodium hydroxide with solution, be settled to 1L with the deionized water volume, obtain the height that the present invention prepares complete bright Electroless Ni-P Plating and plate fast no ammonia type environmental protection plating bath 1L.
To beaker preheating 15min in 90 ℃ of water-baths of above-mentioned plating bath be housed, common iron plate is gone out rolled tin in 10% dilute hydrochloric acid and 5% vitriolic mixed solution, the hydrochloric acid of putting into then 1: 1 is put into plating bath after activating 3～5min, plating 1 hour.By titration Ni
2+Content, determine to add the volume of A liquid and C liquid, by the calculating plating speed of poor quality before and after the weighing plating, put into new test piece then, until covering four circulations.
Embodiment 2
4.5g cupric chloride and 15g tartrate are added the less water dissolving, then with 4g tin protochloride and 3g Bismuth trinitrate sulfuric acid dissolution, at last both are mixed, adding packs into behind the ammoniacal liquor fills in the beaker of 1L deionized water, until clarification, obtain brightening agent solution 1L with magnetic stirrer.
With sodium wolframate 5g, imidazoles 3g, EDTA2Na 15g, packing into fills in the beaker of deionized water, and the high speed magnetic agitation is settled to 1L to all dissolvings with the deionized water volume, obtains stabiliser solution.
With nickelous chloride 25g, inferior sodium phosphate 27g, ammonium acetate 12g, oxysuccinic acid 1.8g, lactic acid 11mL (12g), propionic acid 4mL (6g), stabiliser solution 1.2mL, brightening agent 1.8mL, packing into fills in the beaker of deionized water, and the high speed magnetic agitation is to all dissolvings, with the pH value modulation 5.5 of potassium hydroxide with solution, be settled to 1L with the deionized water volume, obtain the height that the present invention prepares complete bright Electroless Ni-P Plating and plate fast no ammonia type environmental protection plating bath 1L.
To beaker preheating 15min in 92 ℃ of water-baths of above-mentioned plating bath be housed, common iron plate is gone out rolled tin in 10% dilute hydrochloric acid and 5% vitriolic mixed solution, the hydrochloric acid of putting into then 1: 1 is put into plating bath after activating 3～5min, plating 1 hour.By titration Ni
2+Content, determine to add the volume of A liquid and C liquid, by the calculating plating speed of poor quality before and after the weighing plating, put into new test piece then, until covering four circulations.
Embodiment 3
3.5g copper sulfate and 20g tartrate are added the less water dissolving, then with 4.0g Bismuth trinitrate and 4.5g zinc sulfate sulfuric acid dissolution, at last both are mixed, adding packs into behind the ammoniacal liquor fills in the beaker of 1L deionized water, until clarification, obtain brightening agent solution 1L with magnetic stirrer.
With sodium wolframate 7g, imidazoles 2g, EDTA 18g, packing into fills in the beaker of deionized water, and the high speed magnetic agitation is settled to 1L to all dissolvings with the deionized water volume, obtains stabiliser solution.
With six hydration nickel sulfate 29g, sodium borohydride 23g, Glacial acetic acid 5.5mL, citric acid 4g, lactic acid 13mL, propionic acid 4mL, stabiliser solution 1.4mL, brightening agent 2.2mL, packing into fills in the beaker of deionized water, and the high speed magnetic agitation modulates 5.6 with sodium hydroxide and salt of wormwood with the pH value of solution to all dissolvings, be settled to 1L with the deionized water volume, obtain the height that the present invention prepares complete bright Electroless Ni-P Plating and plate fast no ammonia type environmental protection plating bath 1L.
To beaker preheating 15min in 90 ℃ of water-baths of above-mentioned plating bath be housed, common iron plate is gone out rolled tin in 10% dilute hydrochloric acid and 5% vitriolic mixed solution, the hydrochloric acid of putting into then 1: 1 is put into plating bath after activating 3～5min, plating 1 hour.By titration Ni
2+Content, determine to add the volume of A liquid and C liquid, by the calculating plating speed of poor quality before and after the weighing plating, put into new test piece then, until covering four circulations.
Embodiment 4
2g copper sulfate and 19g tartrate are added the less ammonia dissolving, then with 5.0g Bismuth trinitrate sulfuric acid dissolution, at last both are mixed, adding packs into behind the ammoniacal liquor fills in the beaker of 1L deionized water, and the usefulness magnetic stirrer obtains brightening agent solution 1L until clarification.
With sodium wolframate 6g, imidazoles 2g, EDTA 16g, packing into fills in the beaker of deionized water, and the high speed magnetic agitation is settled to 1L to all dissolvings with the deionized water volume, obtains stabiliser solution.
With nickel acetate 24g, POTASSIUM BOROHYDRIDE 23g, Potassium ethanoate 7g, citric acid 4g, lactic acid 13mL, propionic acid 4mL, Succinic Acid 3g, stabiliser solution 1.3mL, brightening agent 2.4mL, packing into fills in the beaker of deionized water, the high speed magnetic agitation is to all dissolvings, with the pH value of solution modulation 5.6, be settled to 1L with salt of wormwood, obtain the height that the present invention prepares complete bright Electroless Ni-P Plating and plate fast no ammonia type environmental protection plating bath 1L with the deionized water volume.
To beaker preheating 15min in 90 ℃ of water-baths of above-mentioned plating bath be housed, common iron plate is gone out rolled tin in 10% dilute hydrochloric acid and 5% vitriolic mixed solution, the hydrochloric acid of putting into then 1: 1 is put into plating bath after activating 3～5min, plating 1 hour.By titration Ni
2+Content, determine to add the volume of A liquid and C liquid, by the calculating plating speed of poor quality before and after the weighing plating, put into new test piece then, until covering four circulations.
The comparison of Comparative Examples 1 and embodiment 1-4
Calculate the plating speed that embodiment 1 arrives under the no ammono-system of embodiment 4, calculation result is respectively, average plating speed of the first seven hour: 27.4 μ m/h, 23.2 μ m/h, 21.7 μ m/h, 20.2 μ m/h, 19.5 μ m/h, 18.1 μ m/h, 17.6 μ m/h; The average plating speed in first three cycle is respectively: 25.1 μ m/h, 20.6 μ m/h and 18.4 μ m/h.The phosphorus content average out to 10%～13% of coating.
Comparative Examples 1 is for there being the ammonia bath system, and the first seven hour of plating speed of the coating that makes is respectively: 17.4 μ m/h, 19.9 μ m/h, 16.0 μ m/h, 16.3 μ m/h, 13.4 μ m/h, 13.1 μ m/h, 12.5 μ m/h; The average plating speed in first three cycle is respectively: 17.8 μ m/h, 13.7 μ m/h, 10.6 μ m/h.Phosphorus content average out to 9%～12% in the coating.
The result shows that plating bath of the present invention obviously is better than traditional ammono-system that has on plating speed, work-ing life and phosphorus content, can improve the efficient of plant produced, reduces cost, and making erosion resistance simultaneously can better coating.
Claims (6)
1. non-ammonia type plating solution for chemical nickel plating is characterized in that per 1 liter of plating bath contains following component:
Nickel salt 24～30g,
Reductive agent 24～33g,
Buffer reagent 10～18g,
Complexing agent 20～30g,
Stablizer 0.5～1.5mL,
Brightening agent 1.5～3.0mL,
Water surplus;
Regulating plating bath pH with the pH regulator agent is 4.8～6.0;
Wherein, described pH regulator agent is one or both the mixture in sodium hydroxide, potassium hydroxide, salt of wormwood, yellow soda ash, saleratus or the sodium bicarbonate;
Described stablizer is to comprise sodium wolframate 4～9g in every liter of stabiliser solution, imidazoles 0.2～9g and ethylenediamine tetraacetic acid (EDTA) or its salt 5～20g;
Described brightening agent is to contain copper sulfate 2～10g in every liter of brightening agent solution, zinc sulfate 2～10g or tin protochloride 2～10g, Bismuth trinitrate 2～10g, tartrate 5～20g.
2. plating bath as claimed in claim 1 is characterized in that described nickel salt is single nickel salt, nickelous chloride or nickel acetate.
3. plating bath as claimed in claim 1 is characterized in that described reductive agent is Hypophosporous Acid, 50 or its salt, boron hydrohalogenic acid salt or hydrazine hydrate.
4. plating bath as claimed in claim 3 is characterized in that described hypophosphite is sodium hypophosphite or potassium hypophosphite, and described boron hydrohalogenic acid salt is sodium borohydride or POTASSIUM BOROHYDRIDE.
5. plating bath as claimed in claim 1 is characterized in that described buffer reagent is acetic acid, sodium-acetate, ammonium acetate or ammonium sulfate.
6. plating bath as claimed in claim 1 is characterized in that described complexing agent is two or more the mixture in Succinic Acid, tartrate, citric acid, lactic acid, propionic acid, oxysuccinic acid or the glycine.
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| CN200810029520XA CN101314848B (en) | 2008-07-16 | 2008-07-16 | Non-ammonia type plating solution for chemical nickel plating |
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