CN100535199C - Dispersion method for nanometer particles in electroplating solution - Google Patents
Dispersion method for nanometer particles in electroplating solution Download PDFInfo
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- CN100535199C CN100535199C CNB2005100120428A CN200510012042A CN100535199C CN 100535199 C CN100535199 C CN 100535199C CN B2005100120428 A CNB2005100120428 A CN B2005100120428A CN 200510012042 A CN200510012042 A CN 200510012042A CN 100535199 C CN100535199 C CN 100535199C
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- nanoparticle
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- cats product
- nanometre
- dispersing method
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Abstract
The invention relates to a nanometre-sized particle scattering method in electric plating dissolvent, which comprises the following steps: adding mixture of cationic surfactant and anionic surfactant into water and boiling it for 15 minutes; cooling it down to 40-50Deg C; adding nanometre-sized particle; and stirring for 24h. The invention can not only realize stable dispersion of single and mixture of multiple nanometre-sized particles to make composite deposite carry on multiple functions, but also have no affect on adhesive force and mechanical property of coating.
Description
Technical field
The invention belongs to the composite plating technology field.
Background technology
Compound plating claims again to disperse plating, dispersion plating, is the technological process that makes metal and particulate codeposition acquisition coating with the method for galvanic deposit or electroless plating.The heterogeneous composite material that composite deposite is made up of matrix metal and disperse particles, can give composite deposite high rigidity, wear-resisting, self-lubricating, corrosion-resistant and other specific function according to the difference of disperse particles, therefore be subject to people's attention, especially with the nanoparticle Development of Preparation Technology, the nanoparticle composite plating technology also receives publicity day by day.But nanoparticle is because himself specific surface area is big, and the surface energy height makes nanoparticle reunite easily in electroplating dispersion liquid and grows up, and the nanoparticle that enters coating simultaneously also can take place to reunite and that coating is formed is inhomogeneous.Solving nanoparticle main method of stable dispersion in plating bath is that nanoparticle is carried out surface modification.CN 1552952A " a kind of raising metallic surface is high temperature resistant and anti abrasive galvanic deposit composite plating method " uses asccharin, 1 in watt type nickel plating solution, the 4-butynediol is to Al
2O
3, nanoparticles such as WC, SiC disperse, the nanoparticle consumption is big, dispersion effect is poor, even also can produce the reunion precipitation of a large amount of nanoparticles under the ultra-sonic oscillation stirring state.CN 1414144A " a kind of nano compound electroplating slurry and preparation and electro-plating method " is earlier with Al
2O
3Carrying out the surface with metal oxide coats; add quaternary ammonium salt again, complexing agent carries out dispersion suspension; a large amount of other metal oxides influence the mechanical property of composite deposite to this dispersion suspension method owing to nano-particle surface coats, and the metal oxide of nano-particle surface can dissolve and loses provide protection in acid electroplating liquid.
Summary of the invention
Technical problem to be solved by this invention is that the reunion that reduces nanoparticle in the nano compound electroplating electroplate liquid deposits, and the invention provides a kind of stable dispersion method of nanoparticle.
The step of dispersing method of the present invention is:
Step 1 is that 10: 1~30: 1 mixtures are put into water with cats product and anion surfactant mol ratio, heated and boiled 15 minutes;
Step 2, be cooled to 40~50 ℃ after, add nanoparticle, stirred 24 hours, promptly get the dispersion liquid of nanoparticle;
The per minute 1g nanoparticle of loosing needs water 50~200mL, surfactant mixture 0.0167~0.0250g.
Above-mentioned said nanoparticle is the Al of particle diameter less than 100nm
2O
3Perhaps SiC or WC, or two or three mixture in them.
Quadrol, trolamine or this several mixing that can form ammonium ion under quaternary ammonium salt that above-mentioned said cats product is the 6-18 carbochain or the solutions of weak acidity are used; Anion surfactant is sodium lauryl sulphate, sodium laurylsulfonate or Sodium dodecylbenzene sulfonate.
The stirring means of above-mentioned said nanoparticle dispersion treatment and plating bath stirring means can adopt electric mixer to stir, perhaps adopt pneumatic blending, perhaps stir, perhaps adopt ultra-sonic oscillation to carry out ultrasonic agitation, and the combination of above-mentioned several alr modes is stirred with the mechanical pump circulation.
The present invention compares the beneficial effect that is had with prior art, has realized in electroplate liquid single the kind and the stable dispersion of multiple nanoparticle mixture, thereby can make composite deposite show multiple function.
The tensio-active agent of selecting for use not only can guarantee the nanoparticle stable dispersion, and does not influence the sticking power and the mechanical property of coating, and the consumption of nanoparticle in plating bath is few.
Embodiment
According to cats product and anion surfactant mol ratio is 10: 1~30: 1, calculates the needed cats product of nanoparticle of dispersion certain mass and the quality of anion surfactant.
Embodiment one: the preparation of SiC nanoparticle dispersion liquid.
Take by weighing cats product dodecyl bromination ammonium 0.0846g, anionic surfactant sodium dodecylbenzene sulfonate 0.0060g was dissolved in 50 ml waters heated and boiled 15 minutes;
After being cooled to 40~50 ℃, add SiC nanoparticle 1g, stirred 24 hours, promptly get SiC nanoparticle dispersion liquid with electric mixer.
Embodiment two: Al
2O
3The preparation of nanoparticle dispersion liquid.
Take by weighing cats product trolamine 0.0409g (transferring the pH to 7 following with 20%HCl), anionic 0.0050g was dissolved in 200 ml waters heated and boiled 15 minutes;
Add Al after being cooled to 40~50 ℃
2O
3Nanoparticle 1g stirred 24 hours with ultra-sonic oscillation, promptly got Al
2O
3The nanoparticle dispersion liquid.
Embodiment three: WC and Al
2O
3The preparation of mixture dispersion liquid.
Take by weighing cats product quadrol 0.0082g (transferring below the pH to 7) with 20%HCl, dodecyl bromination ammonium 0.0423g, anionic 0.0025g, Sodium dodecylbenzene sulfonate 0.0030g was dissolved in 200 ml waters heated and boiled 15 minutes;
Add WC and Al after being cooled to 40~50 ℃
2O
3Nanoparticle mixture 1g, electronic stirring 24 hours promptly gets WC and Al
2O
3Mixture nanoparticle dispersion liquid.
When implementing composite plating, according to the concentration requirement preparation plating bath of nanoparticle in the electroplate liquid.
For example, when implementing the high-frequency impulse composite plating, be that cats product and anionic surfactant mixture dispersive SiC (seeing embodiment one) are made an addition in watt type nickel plating bath NiSO
47H
2O250g/L; NiCl
26H
2O 30g/L; H
3BO
335g/L, SiC 2g/L, electric mixer stirs, 200 rev/mins of rotating speeds, 50 ℃ of temperature are made anode with nickel, are subjected to plating piece to make negative electrode, apply pulsed current, frequency 100MHz, dutycycle 42%, average current density 1A/dm
2Coating plated state microhardness is greater than 1000Hv.
Claims (2)
1. a dispersing method that is used for the electroplate liquid nanoparticle is characterized in that, the step of this dispersing method is:
Step 1 is that 10: 1~30: 1 mixtures are put into water with cats product and anion surfactant mol ratio, heated and boiled 15 minutes;
Step 2, be cooled to 40~50 ℃ after, add nanoparticle, stirred 24 hours, promptly get the dispersion liquid of nanoparticle;
The per minute 1g nanoparticle of loosing needs water 50~200mL, surfactant mixture 0.0167~0.0250g.
2. a kind of dispersing method that is used for the electroplate liquid nanoparticle according to claim 1, it is characterized in that cats product is that the quadrol that can form ammonium ion under the quaternary ammonium salt of 6-18 carbochain or the solutions of weak acidity, trolamine or these two kinds mix and use; Anion surfactant is sodium lauryl sulphate, sodium laurylsulfonate or Sodium dodecylbenzene sulfonate.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CNB2005100120428A CN100535199C (en) | 2005-06-30 | 2005-06-30 | Dispersion method for nanometer particles in electroplating solution |
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Application Number | Priority Date | Filing Date | Title |
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CNB2005100120428A CN100535199C (en) | 2005-06-30 | 2005-06-30 | Dispersion method for nanometer particles in electroplating solution |
Publications (2)
Publication Number | Publication Date |
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CN1737213A CN1737213A (en) | 2006-02-22 |
CN100535199C true CN100535199C (en) | 2009-09-02 |
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ID=36080147
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CNB2005100120428A Expired - Fee Related CN100535199C (en) | 2005-06-30 | 2005-06-30 | Dispersion method for nanometer particles in electroplating solution |
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CN (1) | CN100535199C (en) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9217205B2 (en) * | 2007-12-11 | 2015-12-22 | Enthone Inc. | Electrolytic deposition of metal-based composite coatings comprising nano-particles |
CN106676613B (en) * | 2016-12-28 | 2019-01-11 | 北京有色金属研究总院 | The dispersing method of ceramic particle during a kind of metal material surface Composite Coatings |
CN111575686A (en) * | 2020-06-11 | 2020-08-25 | 青田永拓金属表面技术处理有限公司 | Wear-resistant corrosion-resistant high-phosphorus plating solution for surface of stainless steel ball valve and wear-resistant corrosion-resistant preparation method |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1414144A (en) * | 2002-06-29 | 2003-04-30 | 重庆阿波罗机电技术开发公司 | Nano composite plating paste material and its preparation and electroplating method |
-
2005
- 2005-06-30 CN CNB2005100120428A patent/CN100535199C/en not_active Expired - Fee Related
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1414144A (en) * | 2002-06-29 | 2003-04-30 | 重庆阿波罗机电技术开发公司 | Nano composite plating paste material and its preparation and electroplating method |
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