CN101851752A - Long-service-life high-speed acid environment protection bright chemical nickel plating additive and use method thereof - Google Patents
Long-service-life high-speed acid environment protection bright chemical nickel plating additive and use method thereof Download PDFInfo
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Abstract
The invention relates to a long-service-life high-speed acid environment protection bright chemical nickel plating additive and a use method thereof. A complexing agent in the additive is a mixture of three kinds or more than three kinds of materials in lactic acid, malic acid, citric acid, glycine, glycollic acid and salicylic acid through being mixed according to any proportion. A stabilizing agent is a composite stabilizing agent prepared from thiosemicarbazone derivatives and oxygenated chemicals according to a mass ratio of 1/10 to 30, and the oxygenated chemicals are iodate or molybdate or bromate, an accelerating agent is one kind of materials in glutaric acid or adipic acid. A buffering agent is prepared from either boric acid or sodium tetraborate and either acetic acid or sodium acetate according to a mass ratio of 1/2 to 5. The chemical nickel plating additive of the invention can realize the mass production. When being used, the chemical nickel plating additive is directly added into water to be diluted according to the proportion for use, and the operation is simple. After the use for 8 to 10 periods, the plating layer performance and the speed are still stable, the stability of plating liquid is good, nickel is not separated out from the wall of a tank, the phosphorus content of the plating layer is stabilized ranged from 5 to 8 percent, and the plating layer is bright.
Description
Technical field
The present invention relates to the technical field that the metallic surface chemical nickel plating is handled, particularly a kind of longevity, high speed acid environment protection bright chemical nickel plating additive and using method thereof.
Background technology
Chemical nickel plating is called electroless nickel plating again, is the film technique that has deposited metal plating in the common solution that exists of metal-salt and reductive agent by the chemical reaction of autocatalysis in the metallic surface.
Electroless Plating of Ni-P Alloy coating has comprehensive physical and chemical performances such as outstanding all plating property, higher hardness, good wear resistance and corrosion resisting property, almost is difficult to find an industrial circle not adopt chemical plating nickel technology at present.It is reported that the ratio that chemical nickel plating is used is roughly as follows: aerospace industry in each industry: 9%, automotive industry: 5%, electronic computer industry: 15%, foodstuffs industry: 5%, mechanical industry: 15%, nuclear industry: 2%, petroleum industry: 10%, plastics industry: 5%, power transmission industry: 3%, Printing industry: 3%, the pump production: 5%, the valve production: 17%, other: 6%.In economy flourish East Asia and southeast, comprise China, electroless plating is used just at ascent stage, expection will keep unprecedented high speed development, aspect electronic industry, light metal (magnesium, the aluminium) protection important growth will arranged, in the oil field, it is stable that mining and chemical engineering industry keep, and very big in the automobile industry development potentiality.
Current chemical nickel plating product is numerous, and village's rising sun light, Atotech, U.S. heavily fortified point, wheat dolantin etc. are thought, go up by bigger abroad electroplating additive producer as finding pleasure in all have sophisticated product to come out, but equal price is higher, and the demestic user is difficult to accept.At present, manufacturer is autogamy chemical nickel-plating additives all generally, general is exactly direct soluble in water the getting final product of raw material, need the raw material of preparation too many, and because the different qualities of raw material batch also have very big-difference, add especially rule of thumb, daily administration needs certain state of the art, otherwise makes the solution composition imbalance easily; Life cycle is few, and three or four cycles that have have just scrapped, and use five or six cycles at most only, cause the waste of raw material and a large amount of factory effluents; Domestic manufacturer generally uses plumbous cadmium and thiocarbamide to cooperate as stablizer and brightening agent, and entering environment can pollute, and coating fragility is bigger; The bad control of the amount of bath stability agent, the amount of stablizer adds too much, and bath stability is too strong, and plating speed is slack-off even can not go up plating, otherwise bath stability deficiency then very little is easily at position precipitating metals such as cell wall, heating tubes, reduce the life-span of plating bath, cause waste, increase cost; Coating causes coating performance inconsistent because the continuous consumption of plating bath and add untimelyly can not be stablized the phosphorus content of coating.
More than the variety of issue of Cun Zaiing has limited chemical nickel plating application at home, therefore, needs a kind of use of research and development simple, the bright chemical nickel additive of life-span length, good stability, coating nickel stable content, environmental protection.Application number is that 200410036014.5 Chinese patent discloses a kind of chemical nickel composite additive, this kind chemical nickel plating composite additive, every liter of composite additive comprises: one or both sums 100-400g in citric acid and the tartrate, one or both sums 100-300g in oxysuccinic acid and the lactic acid; Sodium acetate 200-400g; One or both sums 200-400g of sodium hydroxide and sodium bicarbonate; One or both sums 20-100mg in one or both sums 50-200g in propionic acid and the Succinic Acid and molybdenum oxide, thiocarbamide, the potassiumiodide.Directly add composite additive, nickel salt and hypophosphite during production in water, dissolving back is adjusted plating bath and is carried out chemical nickel plating and get final product fully, and be 6-8 cycle work-ing life, but stability is not really high.
Summary of the invention
The purpose of this invention is to provide a kind of longevity, high speed acid environment protection bright chemical nickel plating additive and preparation method thereof, this kind additive is prepared, is added simply, the life-span is long, good, the coating nickel stable content of bath stability.
General commercially available chemical nickel-plating additive is all formed by three doses, and A, B open cylinder A, C and then be used to add, and prepares easyly, is easy to management, and plating bath is difficult for imbalance.Therefore, the present invention also adopts this method, the nickel ion, complexing agent, buffer reagent and the stablizer that provide required in the plating bath mainly is responsible in the A agent, provides reductive agent, complexing agent, buffer reagent, accelerator etc. in B agent and the C agent, during production A agent and B agent directly added to be diluted to desired concn in the entry and to get final product.
A kind of longevity, high speed acid environment protection bright chemical nickel plating additive, the content of its composition in every liter of chemical nickel plating aqueous solution is: complexing agent 30-35g, stablizer 25-50mg, buffer reagent 10-20g, accelerator 0-5g; Wherein complexing agent be in lactic acid, oxysuccinic acid, citric acid, glycine, oxyacetic acid, the Whitfield's ointment more than three kinds or three kinds with arbitrary proportion blended mixture; Stablizer is that thiourea derivative (its preparation method is seen (1)) fits in one package stabilizer with oxygenatedchemicals by mass ratio 1: 10～30, and described oxygenatedchemicals is iodate or molybdate or bromate; Accelerator is a kind of in pentanedioic acid or the hexanodioic acid; Buffer reagent is a kind of and acetate in boric acid or the sodium tetraborate or forms a kind of the cooperation by mass ratio 1: 2～5 in the sodium acetate.
The screening formulation of above-mentioned longevity, high speed acid environment protection bright chemical nickel plating additive is: the content of its composition in every liter of chemical nickel plating aqueous solution is lactic acid 17.7g, oxysuccinic acid 7.5g, oxyacetic acid 5.25g, Whitfield's ointment 2.25g, acetate 9g, boric acid 3g, one package stabilizer thiourea derivative and Potassium Iodate press mass ratio and are total to 34.5mg at 1: 20, and pentanedioic acid 1.1g cooperation forms.
The using method of above-mentioned longevity, high speed acid environment protection bright chemical nickel plating additive comprises the steps:
(1) preparation of thiourea derivative,
The PEG of 200g (molecular weight is from 400～2000) is joined the four-hole bottle, behind the acetone of adding 500ml, add the thiocarbamide of 15g then, N
2Under the protection, after slowly refluxing 5 hours, cool to room temperature; With saturated salt washing organic phase; Removal of solvent under reduced pressure gets solid, obtains white solid.
(2) preparation of A agent,
A agent main component is main salt single nickel salt, buffer reagent and stablizer, and it mainly consists of (being example with 1L):
NiSO
2·6H
2O???????????????????420-450g
Complexing agent 0-50
Buffer reagent 0-40g
Stablizer 0.4-0.5g
A. add the water that accounts for institute's water requirement 1/2, heat to about 70 ℃;
B. add single nickel salt, be stirred to dissolving fully;
C. the gac that adds 6-8g leaves standstill 1-2h after stirring, and filters out the deactivation charcoal;
D. add buffer reagent and complexing agent, be stirred to dissolving fully;
E. use hot water dissolving's stablizer, pour into then in the solution of steps d preparation, make up water stirs to required scale, the A agent is standby.
(3) preparation of B agent and C agent,
The B agent mainly consists of (1L is an example):
Inferior sodium phosphate 170-210g
Complexing agent 180-220g
Buffer reagent 60-100g
Sodium hydroxide 40-60g
Stablizer 0.04-0.1g
C agent (1L is an example) mainly composed as follows
Inferior sodium phosphate 470-570g
Complexing agent 70-130g
Buffer reagent 40-70g
Sodium hydroxide 25-50g
Stablizer 0.25-0.3g
Accelerator 15-20g
B agent and C agent all can be prepared as follows:
A. in groove, add the water that accounts for institute's water requirement 1/2, add sodium hydroxide, stir;
B. add inferior sodium phosphate while hot, be stirred to dissolving fully;
C. add complexing agent, buffer reagent, accelerator successively, stir;
D. hot water dissolving's stablizer is poured in the groove;
E. make up water stirs to requirement, B agent or C agent are standby.
(4) preparation chemical nickel plating bath
A. after coating bath carries out the passivation pre-treatment, clean coating bath, guarantee that nitric acid gets rid of fully and neutralize, add about 1/2 water;
B. measure accurate volume by A agent 60ml/L, B agent 150ml/L, join in the coating bath, make up water stirs to volume required;
C. plating bath is heated to 88-90 ℃, adjusts about plating bath to 4.7, promptly can begin the examination plating with pH meter;
D. plating bath uses for some time to add, and titration is nickel content wherein, adds the A agent by nickel content in the maintenance plating bath at 5.8-6.0g/L, and C agent add-on is identical with the A agent, can guarantee plating bath in span of control, can not lack of proper care.
(5) plating piece; Chemical nickel plating does not need electric current, only needs that workpiece is immersed in the plating bath that heat required time and obtains desired thickness and get final product.
Longevity of the present invention, high speed acid environment protection bright chemical nickel plating additive can quantize to produce, directly add in proportion during use and dilute in the entry and can use, simple to operate, use 8-10 all after date, coating performance and speed are still very stable, and the bath stability performance is good, do not separate out nickel at cell wall, the coating phosphorus content is stabilized in 5-8%, the coating light.
Embodiment
Embodiment 1:
The preparation of thiourea derivative
A. the PEG600 of 200g is joined in three four-hole bottles, add the acetone of 500ml separately after, add the thiocarbamide of 15g, N then
2Under the protection, after slowly refluxing 5 hours, cool to room temperature; With saturated salt washing organic phase; Removal of solvent under reduced pressure gets solid, obtains white solid.
B. the PEG100 of 200g is joined in three four-hole bottles, add the acetone of 500ml separately after, add the thiocarbamide of 15g, N then
2Under the protection, after slowly refluxing 5 hours, cool to room temperature; With saturated salt washing organic phase; Removal of solvent under reduced pressure gets solid, obtains white solid.
C. the PEG2000 of 200g is joined in three four-hole bottles, add the acetone of 500ml separately after, add the thiocarbamide of 15g, N then
2Under the protection, after slowly refluxing 5 hours, cool to room temperature; With saturated salt washing organic phase; Removal of solvent under reduced pressure gets solid, obtains white solid.
Embodiment 2
The present embodiment stablizer selects the thiourea derivative of preparation among the embodiment 1 (a) and Potassium Iodate to be made into one package stabilizer by weight 1: 20.
(1) A agent (1L is an example):
NiSO
2·6H
2O????????????????430g
Lactic acid 45g
One package stabilizer 0.4g,
Preparation:
A. add the water that accounts for institute's water requirement 1/2, heat to about 70 ℃;
B. add single nickel salt, be stirred to dissolving fully;
C. the gac that adds 6g leaves standstill 2h after stirring, and filters out the deactivation charcoal;
D. add buffer reagent and complexing agent, be stirred to dissolving fully;
E. use hot water dissolving's stablizer, pour into then in the solution of steps d preparation, make up water stirs to required scale, the A agent is standby.
(2) B agent (1L is an example):
Inferior sodium phosphate 180g
Lactic acid 100g
Oxysuccinic acid 50g
Oxyacetic acid 35g
Whitfield's ointment 15g
Acetate 60g
Boric acid 20g
Sodium hydroxide 90g
One package stabilizer 0.07g;
C agent (1L is an example):
Inferior sodium phosphate 500g
Oxysuccinic acid 80g
Acetate 30g
Boric acid 15g
Sodium hydroxide 45g
One package stabilizer 0.25g
Pentanedioic acid 18g;
B agent and C agent all can be prepared as follows:
A. in groove, add the water that accounts for institute's water requirement 1/2, add sodium hydroxide, stir;
B. add inferior sodium phosphate while hot, be stirred to dissolving fully;
C. add complexing agent, buffer reagent, accelerator successively, stir;
D. hot water dissolving's stablizer is poured in the groove;
E. make up water stirs to requirement, B agent or C agent are standby.
(3) preparation chemical nickel plating bath, plating piece
A. after coating bath carries out the passivation pre-treatment, clean coating bath, guarantee that nitric acid gets rid of fully and neutralize, add about 1/2 water;
B. measure accurate volume by A agent 60ml/L, B agent 150ml/L, join in the coating bath, make up water stirs to volume required;
C. plating bath is heated to 88-90 ℃, adjusts about plating bath to 4.7, promptly can begin the examination plating with pH meter;
D. plating bath uses for some time to add, and titration is nickel content wherein, adds the A agent by nickel content in the maintenance plating bath at 5.8-6.0g/L, and C agent add-on is identical with the A agent, can guarantee plating bath in span of control, can not lack of proper care.
Embodiment 3:
The present embodiment stablizer selects the thiourea derivative of preparation among the embodiment 1 (b) and potassium bromate to be made into one package stabilizer by weight 1: 15.
(1) A agent (1L is an example):
NiSO
2·6H
2O?????????????435g
Sodium acetate 20g
Sodium tetraborate 15g
One package stabilizer 0.5g,
A. add the water that accounts for institute's water requirement 1/2, heat to about 70 ℃;
B. add single nickel salt, be stirred to dissolving fully;
C. the gac that adds 8g leaves standstill 1h after stirring, and filters out the deactivation charcoal;
D. add buffer reagent and complexing agent, be stirred to dissolving fully;
E. use hot water dissolving's stablizer, pour into then in the solution of steps d preparation, make up water stirs to required scale, the A agent is standby.
B agent (1L is an example):
Inferior sodium phosphate 190g
Lactic acid 115g
Oxysuccinic acid 40g
Glycine 25g
Sodium acetate 75g
Sodium tetraborate 15g
Sodium hydroxide 75g
One package stabilizer 0.06g;
C agent (1L is an example):
Inferior sodium phosphate 530g
Lactic acid 60g
Oxysuccinic acid 50g
Sodium acetate 28g
Sodium tetraborate 17g
Sodium hydroxide 38g
One package stabilizer 0.3g
Hexanodioic acid 20g;
B agent and C agent preparation are as embodiment 2.
(3) preparation chemical nickel plating bath, plating piece step such as embodiment 2.
Embodiment 4:
The present embodiment stablizer selects the thiourea derivative of preparation among the embodiment 1 (c) and potassium molybdate to be made into one package stabilizer by weight 1: 10.
A agent (1L is an example):
NiSO
2·6H
2O?????????435g
Sodium acetate 28g
Sodium tetraborate 10g
One package stabilizer 0.45g;
B agent (1L is an example):
Inferior sodium phosphate 200g
Lactic acid 130g
Oxysuccinic acid 50g
Whitfield's ointment 30g
Sodium acetate 60g
Sodium tetraborate 15g
Sodium hydroxide 80g
One package stabilizer 0.09g;
C agent (1L is an example):
Inferior sodium phosphate 550g
Lactic acid 70g
Oxysuccinic acid 35g
Sodium acetate 32g
Sodium tetraborate 23g
Sodium hydroxide 45g
One package stabilizer 0.4g
Pentanedioic acid 15g.
A agent, B agent and C agent preparation are as embodiment 2.
(3) preparation chemical nickel plating bath, plating piece step such as embodiment 2.
Embodiment 5
Performance test:
Detection method mainly is prescription and my the existing product Nispirit of company that this patent is related to
TM706 and conventional formulation carry out the various aspects of performance contrast test.Nispirit
TM706 for my company's one light, at a high speed in phosphorus chemistry nickel product, it selects heavy metal and thiocarbamide to cooperate as stablizer, the life-span is long, can reach 12-15 cycle, plating is soon fast and stablize, minute surface light, but because of containing heavy metal stabilizer, do not meet environmental requirement.The contrast test performance is as follows:
A. plating speed check
Latten(-tin) is removed greasy dirt with removing oil-bound distemper, uses sand papering then, the H with 5%
2SO
4Activation, chemical nickel plating was taken out the back with the tap water flushing every 5 minutes, dry up with hair dryer then, tested some points with thickness tester, the record mean thickness.And take by weighing and gain in weight (the plating sheet is must size consistent, and the result that plating sheet not of uniform size draws is wrong, and little bubbling makes the plating bath homogeneity relatively good).
B. stability experiment
Respectively get the plating bath 50ml for preparing, add the palladium chloride aqueous solution of 1ml 100ppm, begin slowly to heat plating bath, observe plating bath and muddy temperature occurs from room temperature.(traditional method is to keep plating bath at 60 ℃, observes plating bath and muddy second number occurs, but for Nispirit
TM706 and the prescription that relates to of this patent, good stability even muddiness can not occur in several days, therefore adopts and observes temperature and can degree of being subjected to carry out Detection of Stability).
C. cycle experiment promptly consumes experiment, plates sheet behind the preparation 1L plating bath, and replenishes the A agent according to titration results, and C agent magnitude of recruitment is then identical with the A agent, and the A agent that whenever replenishes 60ml/L is an one-period, is low to moderate to plating bath plating prompt drop to begin to plate 1/3 of speed and finish.
D. antiseptic property check
(1) hydrochloric acid experiment ground is a steel, chemical nickel plating thickness 25.4 μ m, and 50%HCl, soaking at room temperature 3 minutes, coating does not have the serious discoloration explanation by test.
(2) concentrated nitric acid test ground is a steel, and the chemical nickel plating layer thickness is 25.4 μ m, and concentrated nitric acid, soaking at room temperature 30S, coating do not have the serious discoloration explanation by test.
(3) salt mist experiment is 35 ℃, 5%NaCl, and steel plate, thickness of coating 25.4 μ m, the hours of first hot spot appears in test.
E. the phosphorus content test utilizes chemical Ni-plating layer component metering method mensuration phosphorus content among the GB/T 13913-92.
F. other coating performances.Mainly comprise hardness, polishing machine etc.
Contrast test embodiment 2 prescriptions, embodiment 3 prescriptions, embodiment 4 prescriptions, Nispirit
TM706 and electroplate the plating speed of a conventional formulation on the handbook, it is 1 as follows that test result sees Table:
Table 1
By above take off data as can be seen, the 12-17 μ of conventional formulation m/ hour, 706 plating speed are plated speed and are then reached 19-21m/ hour, phosphorus chemistry nickel product Nispirit in the prescription that this patent relates to and our company 16-20 μ m/ hour when PEG and thiourea derivative are made stablizer
TM706 plating speed all are higher than conventional formulation.And this patent prescription and the Nispirit that relate to
TMPlating in 706 early stages speed is similar, and after consumption for some time, the prescription that this patent relates to still can keep certain plating speed, but Nispirit
TM706 are slowly descending.Three embodiment can find in the contrast this patent, because complexing agent content is inconsistent in the plating bath, therefore plating speed has difference slightly, and complexing agent plates speed then because complexing action is slow more.
The stability test, test result is as follows:
Table 2
| ??1 | ??2 | ??3 | |
| Embodiment 2 | ??83℃ | ??85℃ | ??79℃ |
| Embodiment 3 | ??87℃ | ??89℃ | ??83℃ |
| Embodiment 4 | ??92℃ | ??90℃ | ??88℃ |
| ??Nispirit TM706 | ??77℃ | ??79℃ | ??73℃ |
| Conventional formulation | ??53℃ | ??54℃ | ??56℃ |
By above data as can be seen, the prescription and the Nispirit that relate to of this patent
TM706 stability all are higher than conventional formulation far away, and the recipe ratio Nispirit that this patent relates to
TM706 is high slightly.Comparing embodiment 2, embodiment 3 and embodiment 4 find to adopt the molecular weight of PEG high more, and the synthetic thiourea derivative is good more as the stability of stablizer.
The corrosive nature test, above-mentioned four prescriptions all can be tested by hydrochloric acid, but all can not test by nitric acid.The salt mist experiment variable color with hot spot time such as following table appear:
Table 3
| Embodiment 2 | Embodiment 3 | Embodiment 4 | ??NispiritTM?706 | Conventional formulation | |
| 24 hours | ??- | ??- | ??- | ??- | ??- |
| 48 hours | ??- | ??- | ??- | ??- | ??- |
| 96 hours | ??- | ??- | ??- | ??- | Variable color |
| 120 hours | Variable color | Variable color | Variable color | Occur | Occur |
| Embodiment 2 | Embodiment 3 | Embodiment 4 | ??NispiritTM?706 | Conventional formulation | |
| 132 hours | Occur | Occur | Occur |
The prescription solidity to corrosion experiment that this patent relates to is greater than Nispirit
TM706 and conventional formulation.
The cycle experiment:
Through consuming experiment, the prescription that embodiment 2, embodiment 3 and embodiment 4 relate to all can reach 10 cycle requests, and Nispirit
TM706 to reach 14 prescription plating speed still more stable, and four cycle platings of conventional formulation speed is promptly very low, can not use.
The phosphorus content test:
Embodiment 2 coating phosphorus contents are 8.21%, embodiment 3 plating sheet phosphorus contents 8.54%, and embodiment 4 prescription plating sheet nickel contents are 8.72%, Nispirit
TM706 coating phosphorus contents 8.07%, the conventional formulation phosphorus content has only 7.2%, and this also is prescription corrosion resistance of coating that why this patent an is mentioned major cause preferably.Simultaneously, the prescription and the Nispirit that relate to of this patent
TM706 all select oxysuccinic acid as coating phosphorus content stablizer, and phosphorus content can guarantee that also phosphorus content is in certain limit in the coating in the coating after plating bath begins to wear out even make.
Coating hardness, wear resisting property test:
With embodiment 2, embodiment 3 and embodiment 4 prescriptions copper sheet is carried out plating, coating 76 μ m, 400 ℃ of thermal treatment one hour, load 50g, knoop hardness can reach 900kg/mm
2, wearing and tearing mass loss 4-6mg/1000 changes, and all can reach the quality of coating requirement.
In a word, the chemical nickel plating formula for a product that this patent relates to has at a high speed, stability is good, the cycle is long, phosphorus content is stablized and eco-friendly advantage, can adapt to the requirement of current manufacturer to chemical nickel plating, is worth promoting.
Claims (3)
1. a longevity, high speed acid environment protection bright chemical nickel plating additive is characterized in that the content of its composition in every liter of chemical nickel plating aqueous solution is: complexing agent 30-35g, stablizer 25-50mg, buffer reagent 10-20g and accelerator 0-5g; Wherein complexing agent be in lactic acid, oxysuccinic acid, citric acid, glycine, oxyacetic acid, the Whitfield's ointment more than three kinds or three kinds with arbitrary proportion blended mixture; Stablizer is that thiourea derivative and oxygenatedchemicals fit in one package stabilizer by mass ratio 1: 10～30, and described oxygenatedchemicals is iodate or molybdate or bromate; Accelerator is a kind of in pentanedioic acid or the hexanodioic acid; Buffer reagent is a kind of and acetate in boric acid or the sodium tetraborate or forms a kind of the cooperation by mass ratio 1: 2～5 in the sodium acetate.
2. a longevity, high speed acid environment protection bright chemical nickel plating additive, it is characterized in that, the content of its composition in every liter of chemical nickel plating aqueous solution is: lactic acid 17.7g, oxysuccinic acid 7.5g, oxyacetic acid 5.25g, Whitfield's ointment 2.25g, acetate 9g, boric acid 3g, one package stabilizer thiourea derivative and Potassium Iodate press 1: 20 mixture 34.5mg of mass ratio and pentanedioic acid 1.1g.
3. according to the using method of claim 1 or 2 described longevities, high speed acid environment protection bright chemical nickel plating additive, comprise the steps:
(1) preparation of stablizer
The PEG of the molecular weight 400～2000 of 200g is joined in the four-hole bottle, behind the acetone of adding 500ml, add the thiocarbamide of 15g then, N
2Under the protection, after slowly refluxing 5 hours, cool to room temperature; With saturated salt washing organic phase; Removal of solvent under reduced pressure gets solid, obtains white solid;
(2) preparation of A agent
It mainly consists of 1L A agent:
NiSO
2·6H
2O?????????????????420-450g
Complexing agent 0-50
Buffer reagent 0-40g
Stablizer 0.4-0.5g
Step:
A. add the water that accounts for institute's water requirement 1/2, heat to about 70 ℃;
B. add single nickel salt, be stirred to dissolving fully;
C. the gac that adds 6-8g leaves standstill 1-2h after stirring, and filters out the deactivation charcoal;
D. add buffer reagent, be stirred to dissolving fully;
E. use hot water dissolving's stablizer, pour into then in the solution of steps d preparation, make up water stirs to required scale, the A agent is standby;
(3) preparation of B agent and C agent,
1L B agent mainly consists of:
Inferior sodium phosphate 170-210g
Complexing agent 180-220g
Buffer reagent 60-100g
Sodium hydroxide 40-60g
Stablizer 0.04-0.1g,
1L C agent is mainly composed as follows:
Inferior sodium phosphate 470-570g
Complexing agent 70-130g
Buffer reagent 40-70g
Sodium hydroxide 25-50g
Stablizer 0.25-0.3g
Accelerator 15-20g,
B agent and C agent be preparation as follows all:
A. in groove, add the water that accounts for institute's water requirement 1/2, add sodium hydroxide, stir;
B. the temperature of taking advantage of after the dissolving of sodium hydroxide adds inferior sodium phosphate, is stirred to dissolving fully;
C. add complexing agent, buffer reagent, accelerator successively, stir;
D. hot water dissolving's stablizer is poured in the groove;
E. make up water stirs to requirement, B agent or C agent are standby;
(4) preparation chemical nickel plating bath
A. after coating bath carries out the passivation pre-treatment, clean coating bath, guarantee that nitric acid gets rid of fully and neutralize the water of adding institute water requirement 1/2;
B. measure accurate volume by A agent 60ml/L, B agent 150ml/L, join in the coating bath, make up water stirs to volume required;
C. plating bath is heated to 88-90 ℃, adjusts plating bath to 4.7 ± 0.5, promptly can begin the examination plating with pH meter;
D. plating bath uses for some time to add, and titration is nickel content wherein, adds the A agent by nickel content in the maintenance plating bath at 5.8-6.0g/L, and C agent add-on is identical with the A agent, can guarantee plating bath in span of control, can not lack of proper care.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102021543A (en) * | 2010-12-10 | 2011-04-20 | 广州晋惠化工科技有限公司 | Composite complexing agent and chemical nickel-plating solution containing same |
| CN103352213A (en) * | 2013-06-18 | 2013-10-16 | 陕西巨基实业有限公司 | Environment-friendly type high hydrogen sulfide resistant and high wear-resistant Ni-P-W-Mo quaternary alloy plating solution and its preparation method |
| CN104357812A (en) * | 2014-10-17 | 2015-02-18 | 金川集团股份有限公司 | Low-phosphorous chemical nickel-plating concentrated solution and plating process |
| CN106011802A (en) * | 2015-03-30 | 2016-10-12 | 上村工业株式会社 | Chemical nickel plating bath and chemical plating method using same |
| CN106048568A (en) * | 2016-08-21 | 2016-10-26 | 贵州大学 | Environment-friendly chemical nickel plating method |
| CN106048567A (en) * | 2016-08-21 | 2016-10-26 | 贵州大学 | Method for chemically plating high-phosphorus nickel-phosphorus alloy |
| CN107502877A (en) * | 2017-07-11 | 2017-12-22 | 李文军 | It is a kind of to cross the high steel bead wire processing method of liquid utilization rate |
| CN114411129A (en) * | 2021-12-29 | 2022-04-29 | 广东利尔化学有限公司 | Environment-friendly high-phosphorus nickel plating additive |
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| CN104561948B (en) * | 2015-01-28 | 2015-08-05 | 哈尔滨三泳金属表面技术有限公司 | A kind of environment-friendly type aluminium alloy rapid chemical nickel plating-phosphorus additive |
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| CN102021543B (en) * | 2010-12-10 | 2013-04-17 | 广州晋惠化工科技有限公司 | Chemical nickel-plating solution containing composite complexing agent |
| CN102021543A (en) * | 2010-12-10 | 2011-04-20 | 广州晋惠化工科技有限公司 | Composite complexing agent and chemical nickel-plating solution containing same |
| CN103352213A (en) * | 2013-06-18 | 2013-10-16 | 陕西巨基实业有限公司 | Environment-friendly type high hydrogen sulfide resistant and high wear-resistant Ni-P-W-Mo quaternary alloy plating solution and its preparation method |
| CN103352213B (en) * | 2013-06-18 | 2016-08-10 | 宝鸡多元合金科技有限公司 | Environment-friendly type height anti-H 2 S and high abrasion Ni-P-W-Mo quaternary alloy plating solution and compound method thereof |
| CN104357812B (en) * | 2014-10-17 | 2017-02-15 | 金川集团股份有限公司 | Low-phosphorous chemical nickel-plating concentrated solution and plating process |
| CN104357812A (en) * | 2014-10-17 | 2015-02-18 | 金川集团股份有限公司 | Low-phosphorous chemical nickel-plating concentrated solution and plating process |
| CN106011802A (en) * | 2015-03-30 | 2016-10-12 | 上村工业株式会社 | Chemical nickel plating bath and chemical plating method using same |
| CN106011802B (en) * | 2015-03-30 | 2019-12-13 | 上村工业株式会社 | Electroless nickel plating bath and electroless nickel plating method using the same |
| CN106048568A (en) * | 2016-08-21 | 2016-10-26 | 贵州大学 | Environment-friendly chemical nickel plating method |
| CN106048568B (en) * | 2016-08-21 | 2018-07-24 | 贵州大学 | The method of environmentally friendly chemical nickel plating |
| CN106048567A (en) * | 2016-08-21 | 2016-10-26 | 贵州大学 | Method for chemically plating high-phosphorus nickel-phosphorus alloy |
| CN107502877A (en) * | 2017-07-11 | 2017-12-22 | 李文军 | It is a kind of to cross the high steel bead wire processing method of liquid utilization rate |
| CN114411129A (en) * | 2021-12-29 | 2022-04-29 | 广东利尔化学有限公司 | Environment-friendly high-phosphorus nickel plating additive |
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