CN102168291B - Palladium plating solution - Google Patents
Palladium plating solution Download PDFInfo
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- CN102168291B CN102168291B CN 201110063665 CN201110063665A CN102168291B CN 102168291 B CN102168291 B CN 102168291B CN 201110063665 CN201110063665 CN 201110063665 CN 201110063665 A CN201110063665 A CN 201110063665A CN 102168291 B CN102168291 B CN 102168291B
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Abstract
The invention discloses a palladium plating solution. The formula of the palladium plating solution includes palladium salt, conductive agent, phosphate and water and pH is 8-10. The palladium plating solution meets the conditions as follows: phosphate refers to ammonium hydrogen phosphate and sodium hydrogen phosphate in mass ratio of 1:1-1:4, and or the palladium plating solution also contains thiourea and/or compounds as shown in formula I, wherein R1, R2, R3 and R4 respectively and independently are -H, -CH3, -CH2OH or -CO-NH2. The palladium plating solution is applicable to conventional plating substrates and Ti substrates; a medium layer is not needed; the plating layer is uniform, compact and glossy; the corrosion resistance of plated products is excellent; and electro-brush plating can be realized and large-area plating application can be rapidly and conveniently finished. Formula I.
Description
Technical field
The present invention relates to a kind of plating palladium liquid.
Background technology
In the prior art, the plating palladium is mainly used in the base protection to stainless steel, corronel or above metal alloy, plates accordingly palladium liquid and also mainly is applicable to above-mentioned several alloy.Patent CN101187044A discloses a kind of stainless steel surface large area brush Pd-electroplating process, and the plating palladium liquid that wherein relates to contains: palladium salt Pd (NH
3)
4Cl
2In Pd quality 5-12g/L, NH
4Cl 50-125g/L, (NH
4)
2PO
450-100g/L, Tween-20 0-0.002mL/L, all the other are water, the pH value is 7-8; The use processing parameter is: voltage 5-10V, and plated pen is made anode, and workpiece is made negative electrode, the relative work speed of plated pen: 8-12cm/s, temperature is normal temperature, but the plating palladium liquid of the document is only applicable to stainless material; Patent CN101285203A discloses a kind of Pd-containing plating solution and application thereof, the Pd-containing plating solution that wherein relates to contains: palladous sulfate is in palladium 2-200g/L, active conduction salt 10-200g/L, misfit agent 10-150g/L, buffer reagent make the pH value be 9-12, and the applicable base material of this Pd-containing plating solution is the alloy of iron, copper, nickel and above metal, belonging to conventional electroplates, and need to plate first one deck medium layer and could plate again palladium, and plating bath alkalescence is stronger, large to environmental influence.
By contrast, less for the research of plating palladium at the titanium base material in the prior art.Titanium or titanium alloy density is little, intensity is high, chemical stability is good in air and general acid-alkali medium, can be used on and to have resisted in larger corrosive chemical environment, but titanium or titanium alloy also exists the surface to scratch easily, lack the shortcoming of high-temperature corrosion resistance performance, thereby in some strong corrosive environment, also can be corroded, the titanium electrode base material processed that for example immerses electrolytic solution in the chlorine industry still can be corroded, and at this moment just need to overcome above shortcoming by palladium coating on its plated surface; But, not having a kind of special plating palladium liquid for titanium base material in the prior art, this present situation needs to be resolved hurrily.
Summary of the invention
Technical problem to be solved by this invention is to have overcome in the prior art plating palladium liquid to exist the applicable base materials object single as be only applicable to stainless steel, perhaps be applicable to iron, copper, the alloy of nickel and above metal but need to plate first one deck medium layer and could plate again palladium, and plating bath alkalescence is stronger, large to environmental influence, do not have a kind of defective that can be applicable to the titanium base material, a kind of conventional plating substrate that is applicable to is provided, also be applicable to the titanium base material, do not need medium layer, the coating even compact is glossy, plated item is corrosion-resistant good, can realize Brush Plating and can finish easily rapidly the plating palladium liquid of big area plating.
Limitation in view of plating palladium liquid in the prior art, the contriver constantly attempts through lot of experiments, finally finds to select the specific phosphoric acid salt proportioning of the present invention can effectively realize plating palladium liquid in conjunction with other conditions and can not cause again palladium too much to deposit and improve the even smoothness of coating when guaranteeing the rapid large-area brush plating; Simultaneously, also contain at plating palladium liquid and also contain thiocarbamide and/or can also effectively realize plating coating even compact that palladium liquid electroplates and glossy in conjunction with other conditions during suc as formula the compound shown in the I.
Plating palladium liquid formula of the present invention contains palladium salt, conductive agent, phosphoric acid salt and water, and pH is 8~10; Described plating palladium liquid also satisfies following condition: described phosphoric acid salt is ammonium hydrogen phosphate and the sodium hydrogen phosphate of mass ratio 1: 1~1: 4, and/or described plating palladium liquid also contains thiocarbamide and/or suc as formula the compound shown in the I, wherein, and R
1, R
2, R
3And R
4Independently be separately-H-CH
3,-CH
2OH or-CO-NH
2
Formula I
Among the present invention, the kind of described palladium salt and content can be selected by this area normal condition.Described palladium salt better for containing the palladium inorganic salt, better for containing palladium ammonium complex ion inorganic salt, further that better is dichloro four ammonia palladium (Pd (NH
3)
4Cl
2).The content of described palladium salt is haggled over good for 5~200g/L take palladium, that better is 10~50g/L, and further that better is 10~20g/L.
Among the present invention, described conductive agent has another name called active transduction agent, and its kind and content can be selected by this area normal condition.What described conductive agent was better is ammonium salt, and better is inorganic ammonium salt, and further better is ammonium chloride and/or ammonium sulfate.That the content of described conductive agent is better is 1.0~100g/L, and that better is 1.0~50g/L, and further that better is 5.0~20g/L.
Among the present invention, described phosphatic content can be selected by this area normal condition, and that better is 10~100g/L.
Among the present invention, what described pH value was better is 8~9, and better is 8.5~9.The adjusting of described pH value is generally regulated by the conventional pH adjusting agent (also claiming buffer reagent) of using in this area.Described pH adjusting agent kind and content can be selected by this area normal condition.What described pH adjusting agent was better is oxyhydroxide, one or more that better is in sodium hydroxide, potassium hydroxide and the ammoniacal liquor (ammonium hydroxide).The content of described buffer reagent is adjusted to target pH value by this area routine and gets final product.
Among the present invention, described suc as formula the compound shown in the I better be urea, biuret, tetramethyl-urea, dimethyl urea, one or more in monomethylolurea and the dimethylolurea.Described thiocarbamide and/or suc as formula the content of the compound shown in the I better be greater than 0 and≤10g/L, better is greater than 0 and≤5g/L, further better be greater than 0 and≤2g/L.
Among the present invention, described water is the conventional water that uses in this area, is generally deionized water.
Plating palladium liquid of the present invention can also contain various other additives of conventional interpolation in this area routine plating palladium liquid and pyridine compounds and their or multi-carboxylic acid's material of other active substances such as routine use, as long as it does not have antagonistic action or not remarkably influenced the present invention to plate palladium liquid effect.
What plating palladium liquid formula of the present invention was better forms by containing palladium salt, conductive agent, phosphoric acid salt and water, and pH is 8~10; And described plating palladium liquid also satisfies following condition: described phosphoric acid salt is ammonium hydrogen phosphate and the sodium hydrogen phosphate of mass ratio 1: 1~1: 4, and/or described plating palladium liquid also contains thiocarbamide and/or suc as formula the compound shown in the I, wherein, and R
1, R
2, R
3And R
4Independently be separately-H-CH
3,-CH
2OH or-CO-NH
2
Wherein, described palladium salt, conductive agent, phosphoric acid salt, water, pH value and suc as formula each optimum condition of the compound shown in the I all as previously mentioned.
Plating palladium liquid one preferred embodiments prescription of the present invention contains palladium salt Pd (NH
3)
4Cl
2In Pd 10~50g/L, NH
4Cl 5~20g/L; (NH
4)
2HPO
410~100g/L, Na
2HPO
410~100g/L, monomethylolurea 0~2g/L, and water, the pH value is 8.5~9.0, wherein, the mass ratio of ammonium hydrogen phosphate and sodium hydrogen phosphate is 1: 1~1: 4.
Plating palladium liquid of the present invention makes by this area ordinary method, and is better for by aforementioned formula each composition except buffer reagent is dissolved in deionized water, adds afterwards pH adjusting agent and adjust system pH and get final product.What wherein, described dissolving was better dissolves for stirring low-grade fever.
The use of plating palladium liquid of the present invention gets final product by this area routine operation.
Agents useful for same of the present invention and raw material be commercially available getting all.
On the basis that meets this area general knowledge, each above-mentioned among the present invention technical characterictic optimum condition can arbitrary combination obtain preferred embodiments.
Positive progressive effect of the present invention is: plating palladium liquid of the present invention is applicable to conventional plating substrate, also be applicable to the titanium base material, do not need medium layer, can realize Brush Plating and can finish easily rapidly the big area plating, brush plating is effective and can not cause palladium too much to deposit, the coating even compact is glossy, plated item is corrosion-resistant good, and cost is lower, and plating palladium liquid alkalescence itself is little, little to environmental influence, have very big economic worth.
Embodiment
Mode below by embodiment further specifies the present invention, but does not therefore limit the present invention among the described scope of embodiments.
Embodiment 1
Plating palladium liquid formula: palladium salt Pd (NH
3)
4Cl
2In Pd 10.0g/L, (NH
4)
2SO
45.0g/L; (NH
4)
2HPO
410g/L, (NH
4)
2HPO
440g/L, monomethylolurea 1.0g/L, thiocarbamide 0.5g/L; All the other are deionized water, and the pH value is 8.5, and pH adjusting agent is ammoniacal liquor.
The preparation method: by prescription each composition except buffer reagent is dissolved in deionized water, the low-grade fever stirring and dissolving adds afterwards buffer reagent adjustment system pH and gets final product.
Embodiment 2
Plating palladium liquid formula: palladium salt Pd (NH
3)
4Cl
2In Pd 20.0g/L, NH
4Cl 20.0g/L; (NH
4)
2HPO
415.0g/L, Na
2HPO
445.0g/L, urea 0.1g/L, monomethylolurea 0.6g/L; All the other are deionized water, and the pH value is 8.5, and pH adjusting agent is ammoniacal liquor.
The preparation method: by prescription each composition except buffer reagent is dissolved in deionized water, the low-grade fever stirring and dissolving adds afterwards buffer reagent adjustment system pH and gets final product.
Embodiment 3
Plating palladium liquid formula: palladium salt Pd (NH
3)
4Cl
2In Pd 50.0g/L, NH
4Cl 20.0g/L; (NH
4)
2HPO
450g/L, Na
2HPO
450g/L, all the other are deionized water, and the pH value is 8.5, and pH adjusting agent is ammoniacal liquor.
The preparation method: by prescription each composition except buffer reagent is dissolved in deionized water, the low-grade fever stirring and dissolving adds afterwards buffer reagent adjustment system pH and gets final product.
Embodiment 4
Plating palladium liquid formula: palladium salt Pd (NH
3)
4Cl
2In Pd 5.0g/L, (NH
4)
2SO
41.0g/L; (NH
4)
2HPO
45g/L, (NH
4)
2HPO
45g/L, biuret 2.0g/L, tetramethyl-urea 3.0g/L; All the other are deionized water, and the pH value is 9, and pH adjusting agent is sodium hydroxide.
The preparation method: by prescription each composition except buffer reagent is dissolved in deionized water, the low-grade fever stirring and dissolving adds afterwards buffer reagent adjustment system pH and gets final product.
Embodiment 5
Plating palladium liquid formula: palladium salt Pd (NH
3)
4Cl
2In Pd 200.0g/L, (NH
4)
2SO
450.0g/L; (NH
4)
2HPO
410g/L, (NH
4)
2HPO
440g/L, dimethyl urea 1.0g/L, dimethylolurea 1.0g/L; All the other are deionized water, and the pH value is 8, and pH adjusting agent is potassium hydroxide.
The preparation method: by prescription each composition except buffer reagent is dissolved in deionized water, the low-grade fever stirring and dissolving adds afterwards buffer reagent adjustment system pH and gets final product.
Embodiment 6
Plating palladium liquid formula: palladium salt Pd (NH
3)
4Cl
2In Pd 40.0g/L, (NH
4)
2SO
43.0g/L; (NH
4)
2HPO
410g/L, (NH
4)
2HPO
440g/L, monomethylolurea 5.0g/L, thiocarbamide 5.0g/L; All the other are deionized water, and the pH value is 10, and pH adjusting agent is ammoniacal liquor.
The preparation method: by prescription each composition except buffer reagent is dissolved in deionized water, the low-grade fever stirring and dissolving adds afterwards buffer reagent adjustment system pH and gets final product.
Embodiment 7
Plating palladium liquid formula: palladium salt Pd (NH
3)
4Cl
2In Pd 10.0g/L, (NH
4)
2SO
45.0g/L; (NH
4)
2HPO
410g/L, Na
2HPO
440g/L; All the other are deionized water, and the pH value is 8.5, and pH adjusting agent is ammoniacal liquor.
The preparation method: by prescription each composition except buffer reagent is dissolved in deionized water, the low-grade fever stirring and dissolving adds afterwards buffer reagent adjustment system pH and gets final product.
Embodiment 8
Plating palladium liquid formula: palladium salt Pd (NH
3)
4Cl
2In Pd 20.0g/L, NH
4Cl 20.0g/L; (NH
4)
2HPO
415.0g/L, Na
2HPO
445.0g/L; All the other are deionized water, and the pH value is 8.5, and pH adjusting agent is ammoniacal liquor.
The preparation method: by prescription each composition except buffer reagent is dissolved in deionized water, the low-grade fever stirring and dissolving adds afterwards buffer reagent adjustment system pH and gets final product.
Embodiment 9
Plating palladium liquid formula: palladium salt Pd (NH
3)
4Cl
2In Pd 10.0g/L, (NH
4)
2SO
45.0g/L; (NH
4)
2HPO
410g/L, (NH
4)
2HPO
445g/L, monomethylolurea 2.0g/L, thiocarbamide 0.1g/L; All the other are deionized water, and the pH value is 8.5, and pH adjusting agent is ammoniacal liquor.
The preparation method: by prescription each composition except buffer reagent is dissolved in deionized water, the low-grade fever stirring and dissolving adds afterwards buffer reagent adjustment system pH and gets final product.
Embodiment 10
Plating palladium liquid formula: palladium salt Pd (NH
3)
4Cl
2In Pd 20.0g/L, NH
4Cl 20.0g/L; (NH
4)
2HPO
410.0g/L, Na
2HPO
445g/L, urea 0.2g/L, biuret 0.1g/L; All the other are deionized water, and the pH value is 8.5, and pH adjusting agent is ammoniacal liquor.
The preparation method is with embodiment 1.
Embodiment 11
Plating palladium liquid formula: palladium salt Pd (NH
3)
4Cl
2In Pd 20.0g/L, (NH
4)
2SO
410.0g/L; (NH
4)
2HPO
410g/L, Na
2HPO
445g/L, tetramethyl-urea 5.0g/L, dimethyl urea 2.0g/L, dimethylolurea 3.0g/L; All the other are deionized water, and the pH value is 10, and pH adjusting agent is ammoniacal liquor.
The preparation method is with embodiment 1.
Embodiment 12
Plating palladium liquid formula: palladium salt Pd (NH
3)
4Cl
2In Pd 10.0g/L, (NH
4)
2SO
45.0g/L; (NH
4)
2HPO
410g/L, (NH
4)
2HPO
440g/L, monomethylolurea 1.0g/L, dipyridyl 0.2g/L; All the other are deionized water, and the pH value is 8.5, and pH adjusting agent is ammoniacal liquor.
The preparation method: by prescription each composition except buffer reagent is dissolved in deionized water, the low-grade fever stirring and dissolving adds afterwards buffer reagent adjustment system pH and gets final product.
Comparative Examples 1
Plating palladium liquid formula: palladium salt Pd (NH
3)
4Cl
2In Pd 20.0g/L, NH
4Cl 20.0g/L; (NH
4)
2HPO
415.0g/L, Na
2HPO
4(10.0g/L both ratios are less than 1: 1 herein), urea 0.5g/L, methylolurea 1.0g/L; All the other are deionized water, and the pH value is 8.5.
The preparation method: by prescription each composition except buffer reagent is dissolved in deionized water, the low-grade fever stirring and dissolving adds afterwards buffer reagent adjustment system pH and gets final product.
Effect embodiment
With the plating palladium liquid of embodiment 1~3 and Comparative Examples in the same way brush plating on titanium-base, wherein processing parameter is: voltage 8-10V, plated pen is made anode, workpiece is made negative electrode, the relative work speed of plated pen: 3-4cm/s, and temperature is normal temperature, then use respectively appearance luster, outward appearance uniformity coefficient and coating palladium content are weighed electroplating effect, and wherein appearance luster and outward appearance uniformity coefficient adopt naked-eye observation, and coating palladium content adopts the XRF detector to detect.
In general, the palladium content of plating palladium layer, if palladium content is very little, coating too thin being not enough to plays a protective role; If palladium content is too high, crackle appears in the too thick liberation of hydrogen that in use produces easily of coating, reduce on the contrary result of use, such as above-mentioned experimental data as can be known, the effect of the embodiment of the invention 3 brush platings is better, the palladium coating better effects if of embodiment 1 and 2 brush platings, and the effect of Comparative Examples 1 is unsatisfactory.
Claims (12)
1. one kind is plated palladium liquid, and it is characterized in that: its prescription contains palladium salt, conductive agent, phosphoric acid salt and water, and pH is 8~10; Described plating palladium liquid also satisfies following condition: described phosphoric acid salt is the (NH of mass ratio 1: 1~1: 4
4)
2HPO
4And Na
2HPO
4, described plating palladium liquid also contains or does not contain suc as formula the compound shown in the I,
Wherein, R
1, R
2, R
3And R
4Independently be separately-H-CH
3,-CH
2OH or-CO-NH
2The content of described palladium salt is counted 5~200g/L with palladium, and the content of described conductive agent is 1.0~100g/L, and described phosphatic content is 10~100g/L; Described content suc as formula the compound shown in the I be greater than 0 and≤10g/L.
2. plating palladium liquid as claimed in claim 1, it is characterized in that: described palladium salt is for containing the palladium inorganic salt; The content of described palladium salt is counted 10~50g/L with palladium.
3. plating palladium liquid as claimed in claim 2, it is characterized in that: described palladium salt is for containing palladium ammonium complex ion inorganic salt, and the content of described palladium salt is counted 10~20g/L with palladium.
4. plating palladium liquid as claimed in claim 2, it is characterized in that: described palladium salt is Pd (NH
3)
4Cl
2
5. plating palladium liquid as claimed in claim 1, it is characterized in that: described conductive agent is ammonium salt; The content of described conductive agent is 1.0~50g/L.
6. plating palladium liquid as claimed in claim 5, it is characterized in that: described conductive agent is inorganic ammonium salt; The content of described conductive agent is 5.0~20g/L.
7. plating palladium liquid as claimed in claim 5, it is characterized in that: described conductive agent is ammonium chloride and/or ammonium sulfate.
8. plating palladium liquid as claimed in claim 1, it is characterized in that: described pH value is 8~9; The pH adjusting agent of described pH value is one or more in sodium hydroxide, potassium hydroxide and the ammoniacal liquor.
9. plating palladium liquid as claimed in claim 8, it is characterized in that: described pH value is 8.5~9.
10. plating palladium liquid as claimed in claim 1, it is characterized in that: described is urea, biuret, tetramethyl-urea, dimethyl urea suc as formula the compound shown in the I, one or more in monomethylolurea and the dimethylolurea; Described content suc as formula the compound shown in the I be greater than 0 and≤5g/L.
11. plating palladium liquid as claimed in claim 10 is characterized in that: described content suc as formula the compound shown in the I for greater than 0 and≤2g/L.
12. plating palladium liquid as claimed in claim 1 is characterized in that: described plating palladium liquid formula contains palladium salt Pd (NH
3)
4Cl
2In Pd 10~50g/L, NH
4Cl5~20g/L; (NH
4)
2HPO
410~100g/L, Na
2HPO
410~100g/L, monomethylolurea 0~2g/L, and deionized water, the pH value is 8.5~9.0, wherein, (NH
4)
2HPO
4And Na
2HPO
4Mass ratio be 1: 1~1: 4.
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CN 201110063665 CN102168291B (en) | 2011-03-16 | 2011-03-16 | Palladium plating solution |
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CN 201110063665 CN102168291B (en) | 2011-03-16 | 2011-03-16 | Palladium plating solution |
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CN102168291A CN102168291A (en) | 2011-08-31 |
CN102168291B true CN102168291B (en) | 2013-05-01 |
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JP6031319B2 (en) * | 2012-10-04 | 2016-11-24 | ローム・アンド・ハース電子材料株式会社 | Electrolytic copper plating solution and electrolytic copper plating method |
CN105401182B (en) * | 2015-10-14 | 2017-06-23 | 佛山科学技术学院 | A kind of electroplate liquid formulation and its electro-plating method of the palladium of plating thick on stainless steel |
CN106521576A (en) * | 2016-11-29 | 2017-03-22 | 江苏澳光电子有限公司 | Plating solution for copper alloy surface palladium plating and application of plating solution |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3376206A (en) * | 1964-06-30 | 1968-04-02 | Ibm | Electrolyte for the electrodeposition of palladium |
EP0149029A1 (en) * | 1983-12-29 | 1985-07-24 | INOVAN-Stroebe GmbH & Co. KG | Palladium bath |
CN101285203A (en) * | 2007-04-13 | 2008-10-15 | 碧氢科技开发股份有限公司 | Pd-containing plating solution and uses thereof |
-
2011
- 2011-03-16 CN CN 201110063665 patent/CN102168291B/en not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3376206A (en) * | 1964-06-30 | 1968-04-02 | Ibm | Electrolyte for the electrodeposition of palladium |
EP0149029A1 (en) * | 1983-12-29 | 1985-07-24 | INOVAN-Stroebe GmbH & Co. KG | Palladium bath |
CN101285203A (en) * | 2007-04-13 | 2008-10-15 | 碧氢科技开发股份有限公司 | Pd-containing plating solution and uses thereof |
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