CN100371497C - Acidic chemical nickel plating composite brightening agent and its use method - Google Patents
Acidic chemical nickel plating composite brightening agent and its use method Download PDFInfo
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- CN100371497C CN100371497C CNB2005100506122A CN200510050612A CN100371497C CN 100371497 C CN100371497 C CN 100371497C CN B2005100506122 A CNB2005100506122 A CN B2005100506122A CN 200510050612 A CN200510050612 A CN 200510050612A CN 100371497 C CN100371497 C CN 100371497C
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- plating
- brightening agent
- composite
- brightener
- composite brightening
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Abstract
The present invention discloses an acidic chemical nickel plating composite brightening agent and a use method thereof. The composite brightening agent is composed of primary brightening agents, secondary brightening agents and auxiliary brightening agents. The use method: the composite brightening agent is slowly added into chemical plating liquid, and the pH value is regulated to 4.5 to 7.0 by 5% to 10% of dilute sulphuric acid solution; the temperature for plating is from 70 to 95 DEG C; clean and oilless parts are dipped in the plating liquid for 10 to 150 min after the parts are in activating treatment by 3% to 6% of dilute sulphuric acid solution to obtain bright nickel plating layers on the surfaces of the parts. The present invention not only can obviously enhance the brightness of plating layers, but also can not obviously reduce the placing speed. The present invention has the advantages of fast light emission, good dispersing performance, enhanced stability of the plating liquid, prolonged service life of the plating liquid, no affection to components of the plating liquid and the quality of the plating parts by the decomposition of the brightening agents, compact plating layers, low surface stress, good toughness, high microhardness, good corrosion resistance and high activity of the plating layers. The film has an amorphous structure.
Description
Technical field
The present invention relates to the chemically treated technical field of metal material surface, relate in particular to a kind of acidic compound brightener of electroless plating nickel and application method.
Technical background
Electroless Plating of Ni-P Alloy becomes the emphasis of domestic and international R﹠D institution, manufacturing enterprise's research and development as a kind of novel excellent engineering material.It is to utilize a kind of emerging process for treating surface of oxidation-reduction reaction at catalysis specific surface deposition one deck alloy layer, the chemical nickeling phosphorus alloy film of gained has good solidity to corrosion and wear resistance, thickness of coating is even, hardness is high and following an example property is good, thereby is widely used in fields such as chemical machinery, universe aviation.
For a long time, chemical nickel plating all is to use as a kind of functional coating, and its surface brightness is not high, does not use so generally do not do to decorate, but, how to develop the brightener for chemical nickel plating that makes new advances and caused the very big interest of people along with more and more higher in producing to the requirement of functional and decorative coating.Because the chemical plating bath complicated component, influence factor is many, and its mechanism of action is different with plating, so the brightening agent of introducing from electroplate liquid is not fairly obvious to the electroless plating action effect.Present existing brightener for chemical nickel plating or use deleterious heavy metal cadmium and plumbous divalent ion; Or the plating bath instability, degradation production harm plating bath; Or cost an arm and a leg, limited its widespread use.
Summary of the invention
The purpose of this invention is to provide a kind of brightening and leveling good, go out ray velocity fast and to solution composition and plating quality be safe from harm, the acidic compound brightener of electroless plating nickel and application method of not obvious reduction plating speed.
The composite brightening agent that acidic chemical nickel plating composite brightening agent of the present invention is made up of elementary brightening agent, second-class brightener and auxiliary brightener; In 1 liter, elementary brightening agent is made up of a kind of in Phenylsulfonic acid, benzene sulfinic acid sodium salt or the asccharin or two kinds, and its content is 1-15g; Second-class brightener is formed with thiocarbamide is composite by at least a in tonka bean camphor, the pyridine, and wherein, tonka bean camphor or pyridine content are 1-10g, and thiocarbamide content is 0.1g; Auxiliary brightener is a sodium allyl sulfonate, and its content is 10-150g; All the other are water.
The using method of acidic chemical nickel plating composite brightening agent is that composite brightening agent is slowly added in the chemical plating fluid, and regulates the pH value to 4.5-7.0 (4.5-6.0 is preferable) with the dilution heat of sulfuric acid of 5%-10%; Plating temperature is 70-95 ℃ (80-90 ℃ preferable); The part that does not totally have oil is immersed 10-150min in the plating bath after the dilution heat of sulfuric acid activation treatment of 3%-6%, can obtain the nickel layer of light at piece surface.
Compared with prior art, the present invention has following advantage:
1. can not only significantly improve the light of coating, and can obviously not reduce plating speed;
2. bright dipping is fast, and dispersive ability is good, can improve bath stability, prolongs bath life, and the brightening agent degradation production does not influence solution composition and plating quality;
3. coating densification, low, the good toughness of surface stress, the microhardness height has amorphous structure, and solidity to corrosion is good, and coating is active high.
Embodiment
It is basic components that the present invention adopts acid chemical plating nickel liquid, adds the composite brightening agent that is formed by several electronickelling brightening agents and other additive compound, formed non-crystalline state coating minute surface light, surface born of the same parents' shape thing is tiny, binding force of cladding material is good, and solidity to corrosion is good, the microhardness height.Bath stability is good.
Acidic chemical nickel plating composite brightening agent of the present invention forms by elementary brightening agent, second-class brightener and auxiliary brightener are composite.In 1 liter, elementary brightening agent is by Phenylsulfonic acid (C
6H
5SO
3H), benzene sulfinic acid sodium salt (C
6H
5NaO
2S) or asccharin (C
7H
5NO
3S) a kind of or two kinds of compositions in, its content is 1-15g; Second-class brightener is by tonka bean camphor (C
9H
6O
2), pyridine (C
5H
5N) at least a and thiocarbamide ((NH in
2)
2CS) composite forming, wherein, tonka bean camphor or pyridine content are 1-10g, thiocarbamide content is 0.1g; Auxiliary brightener is sodium allyl sulfonate (CH
2CHCH
2SO
3Na), its content is 10-150g, and all the other are water.After being made into composite brightening agent, slowly add according to quantity in the chemical plating fluid, can obtain the chemical Ni-plating layer of light.
In the mentioned component, the main effect of elementary brightening agent is to make grain refining, reduces coating fragility, and with the increase of addition, the coating tensile stress reduces and shifts gradually is stress; Elementary brightening agent can also reduce the effect of plating bath to metallic impurity susceptibility.The elementary brightening agent mechanism of action be it the adding refinement metallic crystal and changed the orientation of crystal plane, and can improve the dispersive ability of plating bath, these organic molecules or micropartical are mingled with in crystallization, can produce stress.
Second-class brightener can make coating produce tangible gloss, but brings the tension stress of coating and fragility simultaneously and to the susceptibility of impurity, by cooperating with the reasonable of elementary brightening agent, can produce bright full coating.Thiocarbamide can prevent or reduce plating leakage in the second-class brightener, improves the tolerance to beavy metal impurity, and thiocarbamide has function of stabilizer concurrently, make bath stability within the specific limits, but surpass certain consumption, make the plating prompt drop low, so content is no more than 0.001g/l in chemical nickel-plating liquid.Second-class brightener changes condition of surface by being adsorbed on the micro cathode district of catalytic surface, makes hydrogen be easy to separate out, and it is careful to help crystallization.
Auxiliary brightener only helps out to the coating light, has good dissemination, and to improving the covering power of coating, it is favourable to the susceptibility of metallic impurity to reduce plating bath.
The using method of above-mentioned brightening agent: the brightening agent that will prepare on request slowly adds in the chemical plating fluid, and regulates the pH value to 4.5-6.0 with the dilution heat of sulfuric acid of 5%-10%; Heat to 75-90 ℃; The part that does not totally have oil is immersed 10-150min in the plating bath after the dilution heat of sulfuric acid activation treatment of 3%-6%, can obtain the non-crystalline state nickel layer of minute surface light at piece surface.
For cooperating enforcement of the present invention, the chemical nickel-plating liquid that adopts industrial widespread use is basic plating bath, and concrete prescription and plating condition are as follows:
Six hydration nickel sulfate (NiSO
46H
2O) 30g/l
Inferior sodium phosphate (NaH
2PO
2H
2O) 28g/l
Lactic acid (CH
3CHOHCOOH) 11g/l
Sodium acetate (NaAc) 40g/l
Regulate the pH value of plating bath with the dilution heat of sulfuric acid of 5%-10%.
By above-mentioned formulated 250ml plating bath, use 45# steel and the A of 30mm * 30mm * 3mm respectively
3Steel is tested as matrix, and sample is put into the plating bath plating after steps such as rust cleaning, corase grind, fine grinding, oil removing, acid-wash activation.
According to brightening agent kind of the present invention and composition range, prepare the chemical nickel plating composite brightening agent of the present invention of heterogeneity respectively, add in the above-mentioned basic plating bath and mix plating under these conditions then.
Specific embodiment is as follows:
Embodiment 1:
Elementary brightening agent: benzene sulfinic acid sodium salt 1g
Second-class brightener: tonka bean camphor 1g
Thiocarbamide 0.1g
Auxiliary brightener: sodium allyl sulfonate 10g
Be made into 1 liter of composite brightening agent solution, get 2.5ml and add in the basic plating bath, adjust pH to 7.0 is heated to 70 ℃ plating then.
Embodiment 2:
Elementary brightening agent: benzene sulfinic acid sodium salt 15g
Second-class brightener: tonka bean camphor 10g
Thiocarbamide 0.1g
Auxiliary brightener: sodium allyl sulfonate 150g
Be made into 1 liter of composite brightening agent solution, get 5ml and add in the basic plating bath, adjust pH to 7.0 is heated to 70 ℃ plating then.
Embodiment 3:
Elementary brightening agent: Phenylsulfonic acid 1g
Second-class brightener: tonka bean camphor 1g
Thiocarbamide 0.1g
Auxiliary brightener: sodium allyl sulfonate 10g
Be made into 1 liter of composite brightening agent solution, get 2.5ml and add in the basic plating bath, adjust pH to 5.20 is heated to 80 ℃ plating then.
Embodiment 4:
Elementary brightening agent: Phenylsulfonic acid 15g
Second-class brightener: tonka bean camphor 10g
Thiocarbamide 0.1g
Auxiliary brightener: sodium allyl sulfonate 150g
Be made into 1 liter of composite brightening agent solution, get 5ml and add in the basic plating bath, adjust pH to 5.20 is heated to 80 ℃ plating then.
Embodiment 5:
Elementary brightening agent: asccharin 1g
Second-class brightener: tonka bean camphor 1g
Thiocarbamide 0.1g
Auxiliary brightener: sodium allyl sulfonate 10g
Be made into 1 liter of composite brightening agent solution, get 2.5ml and add in the basic plating bath, adjust pH to 5.12 is heated to 90 ℃ plating then.
Embodiment 6:
Elementary brightening agent: asccharin 15g
Second-class brightener: tonka bean camphor 10g
Thiocarbamide 0.1g
Auxiliary brightener: sodium allyl sulfonate 150g
Be made into 1 liter of composite brightening agent solution, get 5ml and add in the basic plating bath, adjust pH to 5.12 is heated to 90 ℃ plating then.
Embodiment 7:
Elementary brightening agent: benzene sulfinic acid sodium salt 1g
Second-class brightener: pyridine 1g
Thiocarbamide 0.1g
Auxiliary brightener: sodium allyl sulfonate 10g
Be made into 1 liter of composite brightening agent solution, get 2.5ml and add in the basic plating bath adjust pH to 4.5, plating then.
Embodiment 8:
Elementary brightening agent: benzene sulfinic acid sodium salt 15g
Second-class brightener: pyridine 10g
Thiocarbamide 0.1g
Auxiliary brightener: sodium allyl sulfonate 150g
Be made into 1 liter of composite brightening agent solution, get 5ml and add in the basic plating bath, adjust pH to 4.5 is heated to 95 ℃ plating then.
Embodiment 9:
Elementary brightening agent: Phenylsulfonic acid 1g
Second-class brightener: pyridine 1g
Thiocarbamide 0.1g
Auxiliary brightener: sodium allyl sulfonate 10g
Be made into 1 liter of composite brightening agent solution, get 2.5ml and add in the basic plating bath adjust pH to 5.20, plating then.
Embodiment 10:
Elementary brightening agent: Phenylsulfonic acid 15g
Second-class brightener: pyridine 10g
Thiocarbamide 0.1g
Auxiliary brightener: sodium allyl sulfonate 150g
Be made into 1 liter of composite brightening agent solution, get 5ml and add in the basic plating bath, adjust pH to 5.20 is heated to 95 ℃ plating then.
Embodiment 11:
Elementary brightening agent: asccharin 1g
Second-class brightener: pyridine 1g
Thiocarbamide 0.1g
Auxiliary brightener: sodium allyl sulfonate 10g
Be made into 1 liter of composite brightening agent solution, get 2.5ml and add in the basic plating bath, adjust pH to 6.0 is heated to 89 ℃ plating then.
Embodiment 12:
Elementary brightening agent: asccharin 15g
Second-class brightener: pyridine 10g
Thiocarbamide 0.1g
Auxiliary brightener: sodium allyl sulfonate 150g
Be made into 1 liter of composite brightening agent solution, get 5ml and add in the basic plating bath, adjust pH to 6.0 is heated to 89 ℃ plating then.
Embodiment 13:
Elementary brightening agent: asccharin 4g
Benzene sulfinic acid sodium salt 4g
Second-class brightener: pyridine 6g
Thiocarbamide 0.1g
Auxiliary brightener: sodium allyl sulfonate 20g
Be made into 1 liter of composite brightening agent solution, get 2.5ml and add in the basic plating bath, adjust pH to 5.20 is heated to 89 ℃ plating then.
Embodiment 14:
Elementary brightening agent: asccharin 6g
Benzene sulfinic acid sodium salt 4g
Second-class brightener: pyridine 6g
Tonka bean camphor 3g
Thiocarbamide 0.1g
Auxiliary brightener: sodium allyl sulfonate 20g
Be made into 1 liter of composite brightening agent solution, get 2.5ml and add in the basic plating bath, adjust pH to 5.20 is heated to 89 ℃ plating then.
Embodiment 15:
Elementary brightening agent: benzene sulfinic acid sodium salt 5g
Second-class brightener: pyridine 8g
Thiocarbamide 0.1g
Auxiliary brightener: sodium allyl sulfonate 20g
Be made into 1 liter of composite brightening agent solution, get 2.5ml and add in the basic plating bath, adjust pH to 5.20 is heated to 89 ℃ plating then.
Plating postevaluation coating luminance brightness and test plating speed and surface microhardness are as shown in the table.
| Embodiment and matrix | The coating outward appearance | Plating speed (um/h) | Surface microhardness (HV) | |
| Do not add brightening agent | The 45# steel | Canescence is more coarse | 19.28 | 718 |
| A 3Steel | Canescence is more coarse | 19.32 | 720 | |
| Embodiment 1 | The 45# steel | The minute surface light, smooth | 17.46 | 715 |
| A 3Steel | The minute surface light, smooth | 17.50 | 710 | |
| Embodiment 2 | The 45# steel | Light, evenly | 16.52 | 744 |
| A 3Steel | Light, evenly | 16.46 | 732 | |
| Embodiment 3 | The 45# steel | The minute surface light, smooth | 18.72 | 736 |
| A 3Steel | The minute surface light, smooth | 18.76 | 728 | |
| Embodiment 4 | The 45# steel | Light, evenly | 16.82 | 722 |
| A 3Steel | Light, evenly | 16.86 | 719 | |
| Embodiment 5 | The 45# steel | The minute surface light, smooth | 17.74 | 735 |
| A 3Steel | The minute surface light, smooth | 17.66 | 730 | |
| Embodiment 6 | The 45# steel | Light, evenly | 16.56 | 712 |
| A 3Steel | Light, evenly | 16.55 | 722 | |
| Embodiment 7 | The 45# steel | The minute surface light, smooth | 16.52 | 728 |
| A 3Steel | The minute surface light, smooth | 16.58 | 722 | |
| Embodiment 8 | The 45# steel | Light, evenly | 16.21 | 732 |
| A 3Steel | Light, evenly | 16.28 | 727 | |
| Embodiment 9 | The 45# steel | The minute surface light, smooth | 18.76 | 736 |
| A 3Steel | The minute surface light, smooth | 18.76 | 724 | |
| Embodiment 10 | The 45# steel | Light, evenly | 16.94 | 718 |
| A 3Steel | Light, evenly | 16.89 | 729 | |
| Embodiment 11 | The 45# steel | The minute surface light, smooth | 19.16 | 730 |
| A 3Steel | The minute surface light, smooth | 19.20 | 704 | |
| Embodiment 12 | The 45# steel | Light, evenly | 17.16 | 734 |
| The A3 steel | Light, evenly | 17.22 | 722 | |
| Embodiment 13 | The 45# steel | The minute surface light, smooth | 18.89 | 725 |
| A 3Steel | The minute surface light, smooth | 18.92 | 731 | |
| Embodiment 14 | The 45# steel | The minute surface light, smooth | 18.96 | 739 |
| A 3Steel | The minute surface light, smooth | 19.04 | 726 | |
| Embodiment 15 | The 45# steel | The minute surface light, smooth | 19.12 | 733 |
| A 3Steel | The minute surface light, smooth | 19.17 | 716 | |
By table as seen, adds brightening agent of the present invention after, specimen surface light when not adding brightening agent is smooth, uniform hue, and very little to plating fast influence, to surface microhardness almost less than influencing.
Claims (4)
1. an acidic chemical nickel plating composite brightening agent is characterized in that, the composite brightening agent that it is made up of elementary brightening agent, second-class brightener and auxiliary brightener; Elementary brightening agent is made up of a kind of in Phenylsulfonic acid, benzene sulfinic acid sodium salt or the asccharin or two kinds, second-class brightener is formed with thiocarbamide is composite by at least a in tonka bean camphor, the pyridine, auxiliary brightener is a sodium allyl sulfonate, and in 1 liter of composite brightening agent, the content of elementary brightening agent is 1-15g; Tonka bean camphor in the second-class brightener or pyridine content are 1-10g, and thiocarbamide content is 0.1g; The content of auxiliary brightener is 10-150g; All the other are water.
2. the using method of an acidic chemical nickel plating composite brightening agent as claimed in claim 1 is characterized in that, composite brightening agent is slowly added in the chemical plating bath, and regulate the pH value to 4.5-7.0 with the dilution heat of sulfuric acid of 5%-10%; Plating temperature is 70-95 ℃; The part that does not totally have oil is immersed 10-150min in the plating bath after the dilution heat of sulfuric acid activation treatment of 3%-6%, can obtain the nickel layer of light at piece surface.
3. the using method of a kind of acidic chemical nickel plating composite brightening agent according to claim 2 is characterized in that, described pH value is 4.5-6.0.
4. the using method of a kind of acidic chemical nickel plating composite brightening agent according to claim 2 is characterized in that, described plating temperature is 80-90 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100506122A CN100371497C (en) | 2005-07-07 | 2005-07-07 | Acidic chemical nickel plating composite brightening agent and its use method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100506122A CN100371497C (en) | 2005-07-07 | 2005-07-07 | Acidic chemical nickel plating composite brightening agent and its use method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1718859A CN1718859A (en) | 2006-01-11 |
| CN100371497C true CN100371497C (en) | 2008-02-27 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100506122A Expired - Fee Related CN100371497C (en) | 2005-07-07 | 2005-07-07 | Acidic chemical nickel plating composite brightening agent and its use method |
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|---|---|
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100462485C (en) * | 2006-04-07 | 2009-02-18 | 浙江大学 | Alkali compound brightening agent for chemical plating of nickel and use method thereof |
| CN105177585A (en) * | 2015-10-19 | 2015-12-23 | 大连海事大学 | High-smoothness metal surface preparation method based on chemical plating and polishing technology |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3528894A (en) * | 1966-08-25 | 1970-09-15 | M & T Chemicals Inc | Method of electrodepositing corrosion resistant coating |
| US3697392A (en) * | 1970-07-02 | 1972-10-10 | Allied Res Prod Inc | Electrodeposition of nickel |
| US3804726A (en) * | 1973-04-23 | 1974-04-16 | M & T Chemicals Inc | Electroplating processes and compositions |
| CN85100385A (en) * | 1985-04-01 | 1986-08-27 | 湘潭大学 | The electroplate liquid and the method for quick barrel nickel plating iron alloy |
| CN1477236A (en) * | 2003-07-10 | 2004-02-25 | 上海交通大学 | Additive component of alkaline solution for electroplating zinc-nickel alloy and brass and its preparation method |
-
2005
- 2005-07-07 CN CNB2005100506122A patent/CN100371497C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3528894A (en) * | 1966-08-25 | 1970-09-15 | M & T Chemicals Inc | Method of electrodepositing corrosion resistant coating |
| US3697392A (en) * | 1970-07-02 | 1972-10-10 | Allied Res Prod Inc | Electrodeposition of nickel |
| US3804726A (en) * | 1973-04-23 | 1974-04-16 | M & T Chemicals Inc | Electroplating processes and compositions |
| CN85100385A (en) * | 1985-04-01 | 1986-08-27 | 湘潭大学 | The electroplate liquid and the method for quick barrel nickel plating iron alloy |
| CN1477236A (en) * | 2003-07-10 | 2004-02-25 | 上海交通大学 | Additive component of alkaline solution for electroplating zinc-nickel alloy and brass and its preparation method |
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| CN1718859A (en) | 2006-01-11 |
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Assignee: Deqing County Sanxing Plastics Chemical Co., Ltd. Assignor: Zhejiang University Contract fulfillment period: 2008.12.31 to 2013.12.30 contract change Contract record no.: 2009330002627 Denomination of invention: Acidic chemical nickel plating composite brightening agent and its use method Granted publication date: 20080227 License type: Exclusive license Record date: 20091026 |
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