CN101012569A - Method for direct copper non-cyanide plating of zinc alloy casting die - Google Patents
Method for direct copper non-cyanide plating of zinc alloy casting die Download PDFInfo
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- CN101012569A CN101012569A CN 200610151222 CN200610151222A CN101012569A CN 101012569 A CN101012569 A CN 101012569A CN 200610151222 CN200610151222 CN 200610151222 CN 200610151222 A CN200610151222 A CN 200610151222A CN 101012569 A CN101012569 A CN 101012569A
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Abstract
The invention discloses a copper plating method of zinc alloy casting piece, which comprises the following steps: a. electrolyzing cathode to remove oil; b. activating through washing by organic acid; c. immersing in the organic acid; d. plating copper directly with bivalent copper ion density at 10-25g/L and complexing agent density at 120-350 g/L, potassium carbonate density at 10-50g/L and hydroperoxide density at 1-15mL/L; maintaining pH value between 9 and 12; adjusting pH value through 50% potassium hydroxide solution; setting the current density of cathode 0.5-2.5A/dm2 at 20-50 deg.c.
Description
Technical field
The present invention relates to a kind of method of electro-coppering.Be specifically related to the method for direct non-cyanide copper electroplating on a kind of zinc alloy diecasting, both can be used for the directly pre-copper facing of zinc alloy diecasting, also can be used for the copper electroplating layer thickening.
Background technology
Zinc alloy has advantages of good casting, is good casting alloy, has more superiority when being used to cast complex-shaped, high-precision workpiece, and zinc alloy diecasting is applied to fields such as automobile, electronics, aerospace more and more.But cast zinc alloy is not wear-resistant, is vulnerable to the corrosion of moist atmosphere, in order to overcome above-mentioned shortcoming, improves its performance at enterprising electroplating monometallic of zinc alloy or alloy usually.Advantages such as electro-coppering coating has densification, light, and ductility is good generally are used as the plating bottom, proceed to electroplate wear-resisting, corrosion-resistant coating on electro-coppering coating.
Because the standard potential lower (0.76 volt) of zinc is electroplated, the replacement(metathesis)reaction of main salt metal ion and zinc in the solution easily takes place, and the displacement layer short texture causes problems such as the electrolytic coating bonding force is poor, coating is coarse thus on zinc alloy.And in the zinc alloy diecasting process, workpiece surface temperature is inconsistent during owing to cooling, zinc alloy surface easily produces the component segregation phenomenon, rich zinc of surface local or rich aluminium, this has caused very big difficulty also for the pre-treatment of zinc alloy diecasting, deals with the quality that can directly influence electrolytic coating improperly.
The pre-copper facing of prussiate is to use more method, but prussiate has very big toxic action to environment and operator, the investigator attempted a lot of cyanide-free copper electroplating technology for a long time, but when being applied in the zinc alloy diecasting plating, often effect is undesirable, roughly show four aspects: (1) cupric ion can produce tangible chemical replacement effect at zinc alloy surface, and pre-copper facing bonding force is bad; (2) anode dissolves undesirable in electroplating process; (3) covering power is undesirable; (4) complex process, pre-treatment step is long.
Summary of the invention
The objective of the invention is that the copper coating bonding force is poor, the problem of complex process in order to solve, a kind of method of direct copper non-cyanide plating of zinc alloy casting die is provided, and method flow of the present invention is as follows: the organic acid-wash activation of a. catholyte oil removing → b. → c. organic acid dipping → d. Direct Electroplating copper; The composition and the processing condition of described " oil removing of a. catholyte " degreasing fluid are: tertiary sodium phosphate 10～40g/L, vitriolate of tartar 5～15g/L, yellow soda ash 10～30g/L, OS-10 (peregal series) 0.5～5g/L, pH value≤12, cathode current density D
k=3～8A/dm
2, 2～5 minutes time, temperature is a room temperature; The composition and the processing condition of described " the organic acid-wash activation of b. " pickle solution are: hydrochloric acid 10～40g/L, and organic acid 5～40g/L, temperature is a room temperature, soak time 3～30 seconds; The composition and the processing condition of described " c. organic acid dipping " solution are: organic acid 30～80g/L, and temperature is a room temperature, dipping time 1～10 second; The composition and the processing condition of described " d. Direct Electroplating copper " solution are: bivalent cupric ion concentration 10～25g/L, complexing agent 120～350g/L, salt of wormwood 10～50g/L, hydrogen peroxide 1～15mL/L, the pH value remains between 9～12, use 50% potassium hydroxide solution adjusting pH value, cathode current density D
k=0.5～2.5A/dm
2, 20～50 ℃ of temperature.
The present invention both can be used for the directly pre-copper facing of zinc alloy diecasting, also can be used for the copper electroplating layer thickening.
The present invention has copper coating outward appearance light, bonding force is good, porosity is low, and technology is simple, easy to maintenance, the advantage that covering power and covering power are good.
Embodiment
Embodiment one: the technical process of present embodiment is as follows: the organic acid-wash activation of a. catholyte oil removing → b. → c. organic acid dipping → d. Direct Electroplating copper; The composition and the processing condition of described " oil removing of a. catholyte " degreasing fluid are: tertiary sodium phosphate 10～40g/L, vitriolate of tartar 5～15g/L, yellow soda ash 10～30g/L, OS-10 (peregal series) 0.5～5g/L, pH value≤12, cathode current density D
k=3～8A/dm
2, 2～5 minutes time, temperature is a room temperature; The composition and the processing condition of described " the organic acid-wash activation of b. " pickle solution are: hydrochloric acid 10～40g/L, and organic acid 5～40g/L, temperature is a room temperature, soak time 3～30 seconds; The composition and the processing condition of described " c. organic acid dipping " solution are: organic acid 30～80g/L, and temperature is a room temperature, dipping time 1～10 second; Described " d. Direct Electroplating copper " solution composition and processing condition are: bivalent cupric ion concentration 10～25g/L, complexing agent 120～350g/L, salt of wormwood 10～50g/L, hydrogen peroxide 1～15mL/L, the pH value remains between 9～12, use 50% potassium hydroxide solution adjusting pH value, cathode current density D
k=0.5～2.5A/dm
2, 20～50 ℃ of temperature.
Embodiment two: the organic acid of present embodiment in " the organic acid-wash activation of b. " is one or more the combination in oxalic acid, citric acid, tartrate, organic phosphoric acid and the organophosphate.Other is identical with embodiment one.
Embodiment three: present embodiment organic phosphoric acid in " the organic acid-wash activation of b. " is 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid (abbreviating HEDP as), ethylene diamine tetra methylene phosphonic acid (abbreviating EDTMP as) or Amino Trimethylene Phosphonic Acid (abbreviating ATMP as); Organophosphate is 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid sodium (abbreviating HEDPS as) or ethylene diamine tetra methylene phosphonic acid sodium (abbreviating EDTMPS as).Other is identical with embodiment two.
Embodiment four: the organic acid of present embodiment in " c. organic acid dipping " is oxalic acid, citric acid, tartrate, organic phosphoric acid or organophosphate.Other is identical with embodiment one.
Embodiment five: the organic phosphoric acid of present embodiment in " c. organic acid dipping " is HEDP, EDTMP or ATMP; Organophosphate is HEDPS or EDTMPS.Other is identical with embodiment four.
Embodiment six: present embodiment in " d. Direct Electroplating copper " bivalent cupric ion by one or more the combination in cupric chloride, copper sulfate, ventilation breather, the cupric nitrate.Other is identical with embodiment one.
Embodiment seven: present embodiment complexing agent in " d. Direct Electroplating copper " is one or more the combination in citric acid, tartrate, organic phosphoric acid and the organophosphate.Other is identical with embodiment one.
Embodiment eight: present embodiment organic phosphoric acid in " d. Direct Electroplating copper " is HEDP, EDTMP or ATMP; Organophosphate is HEDPS or EDTMPS.Other is identical with embodiment seven.
Embodiment nine: the copper electroplating solution layoutprocedure is as follows in the present embodiment: one, the weighing complexing agent injects groove, with 50% potassium hydroxide solution dissolved dilution, adds water and stirs to 2/3 volume dilution; Two, add oxygenant, constantly adding in the groove under the stirring condition behind 5 times of the dilute with waters; Three, adjust pH to 8 with 50% potassium hydroxide aqueous solution, add while hot in batches and dissolved good cupric salt, make it dissolving; Four, add salt of wormwood, while stirring dissolving; Five, adjust pH between 9～12 with 50% potassium hydroxide solution; Six, add water to capacity, remove impurity and can filter earlier, get final product plating after adopting low current density electrolysis a few hours then.Other is identical with embodiment one.
Embodiment ten: the zinc alloy diecasting trade mark of present embodiment is ZZnAl4Y or ZZnAl4Cu1Y.
Embodiment 11: the technical process of direct copper non-cyanide plating of zinc alloy casting die is as follows in the present embodiment: the organic acid-wash activation of a. catholyte oil removing → b. → c. organic acid dipping → d. Direct Electroplating copper; The composition and the processing condition of the degreasing fluid of described " oil removing of a. catholyte " are: tertiary sodium phosphate 20g/L, vitriolate of tartar 10g/L, yellow soda ash 10g/L, OS-10 (peregal series) 1g/L, pH value≤12, cathode current density D
k=5A/dm
2, 5 minutes time, temperature is a room temperature; The composition and the processing condition of the pickle solution of described " the organic acid-wash activation of b. " are: hydrochloric acid 15g/L, and oxalic acid 15g/L, temperature is a room temperature, soak time 10 seconds; The composition and the processing condition of the solution of described " c. organic acid dipping " are: citric acid 30g/L, and temperature is a room temperature, dipping time 3 seconds; The composition and the processing condition of the solution of described " d. Direct Electroplating copper " are: cupric chloride 45g/L, HEDP150g/L, EDTMP80g/L, salt of wormwood 30g/L, hydrogen peroxide 8mL/L, the pH value remains between 10～12, use 50% potassium hydroxide solution adjusting pH value, cathode current density D
k=0.5A/dm
2, 25 ℃ of temperature.
The zinc alloy diecasting trade mark is ZZnAl4Y in the present embodiment, carries out pre-copper facing bottoming and handles.Zinc alloy diecasting is made of by mass percentage following ingredients: Al3.5～4.3%, and Cu0.25%, Mg0.02～0.06%, Fe)≤0.1%, Pb≤0.005%, Zn surplus.
The precaution of present embodiment: organic acid dipping back does not stop the long time directly into groove.
The electro-coppering coating outward appearance light, the porosity that obtain with the technology of present embodiment are low, and file test test bonding force is good.
Embodiment 12: present embodiment and embodiment 11 are different is that the composition and the processing condition of the pickle solution of described " the organic acid-wash activation of b. " are: hydrochloric acid 20g/L, and tartrate 25g/L, temperature is a room temperature, soak time 10 seconds; The composition and the processing condition of the solution of described " c. organic acid dipping " are: HEDP45g/L, and temperature is a room temperature, dipping time 3 seconds; The composition and the processing condition of the solution of described " d. Direct Electroplating copper " are: ventilation breather 55g/L, HEDP180g/L, citric acid 75g/L, salt of wormwood 30g/L, hydrogen peroxide 10mL/L, the pH value remains between 9～11, use 50% potassium hydroxide solution adjusting pH value, cathode current density D
k=0.5A/dm
2, 25 ℃ of temperature.Other is identical with embodiment 11.
The zinc alloy diecasting trade mark is ZZnAl4Cu1Y in the present embodiment, carries out pre-copper facing bottoming and handles.Zinc alloy diecasting is made of by mass percentage following ingredients: Al3.5～4.3%, and Cu0.75～1.25%, Mg0.03～0.08%, Fe≤0.1%, Pb)≤0.005%, the Zn surplus.
The precaution of present embodiment: organic acid dipping back does not stop the long time directly into groove.
The electro-coppering coating outward appearance light, the porosity that obtain with the technology of present embodiment are low, and file test test bonding force is good.
Embodiment 13: present embodiment and embodiment 11 are different is that the composition and the processing condition of the solution of described " d. Direct Electroplating copper " are: copper sulfate 75g/L, HEDP120g/L, tartrate 50g/L, salt of wormwood 30g/L, hydrogen peroxide 12mL/L.Processing condition are: the pH value remains between 9～10, uses 50% potassium hydroxide solution adjusting pH value, cathode current density D
k=1.5A/dm
2, 45 ℃ of temperature.Other is identical with embodiment 11.
Zinc alloy zinc alloy diecasting trade mark ZZnAl4Y in the present embodiment carries out the electro-coppering thickening and handles.
The precaution of present embodiment: organic acid dipping back does not stop the long time directly into groove.
Electro-coppering coating outward appearance light, porosity that the technology of present embodiment obtains are low, and file test test bonding force is good, and coating fragility is low, ductility is good.
Claims (9)
1, a kind of method of direct copper non-cyanide plating of zinc alloy casting die is characterized in that its method flow is as follows: the organic acid-wash activation of a. catholyte oil removing → b. → c. organic acid dipping → d. Direct Electroplating copper; The composition and the processing condition of described " oil removing of a. catholyte " degreasing fluid are: tertiary sodium phosphate 10～40g/L, vitriolate of tartar 5～15g/L, yellow soda ash 10～30g/L, OS-10 (peregal series) 0.5～5g/L, pH value≤12, cathode current density D
k=3～8A/dm
2, 2～5 minutes time, temperature is a room temperature; The composition and the processing condition of described " the organic acid-wash activation of b. " pickle solution are: hydrochloric acid 10～40g/L, and organic acid 5～40g/L, temperature is a room temperature, soak time 3～30 seconds; The composition and the processing condition of described " c. organic acid dipping " solution are: organic acid 30～80g/L, and temperature is a room temperature, dipping time 1～10 second; The composition and the processing condition of described " d. Direct Electroplating copper " solution are: bivalent cupric ion concentration 10～25g/L, complexing agent 120～350g/L, salt of wormwood 10～50g/L, hydrogen peroxide 1～15mL/L, the pH value remains between 9～12, use 50% potassium hydroxide solution adjusting pH value, cathode current density D
k=0.5～2.5A/dm
2, 20～50 ℃ of temperature.
2, the method for a kind of direct copper non-cyanide plating of zinc alloy casting die according to claim 1 is characterized in that organic acid in " the organic acid-wash activation of b. " is the one or more combination in oxalic acid, citric acid, tartrate, organic phosphoric acid and the organophosphate.
3, the method for a kind of direct copper non-cyanide plating of zinc alloy casting die according to claim 2 is characterized in that organic phosphoric acid is 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid, ethylene diamine tetra methylene phosphonic acid or Amino Trimethylene Phosphonic Acid in " the organic acid-wash activation of b. "; Organophosphate is 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid sodium or ethylene diamine tetra methylene phosphonic acid sodium.
4, the method for a kind of direct copper non-cyanide plating of zinc alloy casting die according to claim 1 is characterized in that the organic acid in " c. organic acid dipping " is oxalic acid, citric acid, tartrate, organic phosphoric acid or organophosphate.
5, the method for a kind of direct copper non-cyanide plating of zinc alloy casting die according to claim 4 is characterized in that the organic phosphoric acid in " c. organic acid dipping " is HEDP, EDTMP or ATMP; Organophosphate is HEDPS or EDTMPS.
6, the method for a kind of direct copper non-cyanide plating of zinc alloy casting die according to claim 1 is characterized in that bivalent cupric ion is by the one or more combination in cupric chloride, copper sulfate, ventilation breather, the cupric nitrate in " d. Direct Electroplating copper ".
7, the method for a kind of direct copper non-cyanide plating of zinc alloy casting die according to claim 1 is characterized in that in " d. Direct Electroplating copper " complexing agent is one or more the combination in citric acid, tartrate, organic phosphoric acid and the organophosphate.
8, the method for a kind of direct copper non-cyanide plating of zinc alloy casting die according to claim 7 is characterized in that organic phosphoric acid is HEDP, EDTMP or ATMP in " d. Direct Electroplating copper "; Organophosphate is HEDPS or EDTMPS.
9, the method for a kind of direct copper non-cyanide plating of zinc alloy casting die according to claim 1, the solution allocation process that it is characterized in that " d. Direct Electroplating copper " is as follows: one, the weighing complexing agent injects groove, with 50% potassium hydroxide solution dissolved dilution, add water and stir to 2/3 volume dilution; Two, add oxygenant, constantly adding in the groove under the stirring condition behind 5 times of the dilute with waters; Three, adjust pH to 8 with 50% potassium hydroxide aqueous solution, add while hot in batches and dissolved good cupric salt, make it dissolving; Four, add salt of wormwood, while stirring dissolving; Five, adjust pH between 9～12 with 50% potassium hydroxide solution; Six, add water to capacity, remove impurity and can filter earlier, get final product plating after adopting low current density electrolysis a few hours then.
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| CN 200610151222 CN101012569A (en) | 2006-12-29 | 2006-12-29 | Method for direct copper non-cyanide plating of zinc alloy casting die |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101914789A (en) * | 2010-08-12 | 2010-12-15 | 河南平原光电有限公司 | Cyanide-free copper electroplating method |
| CN102242381A (en) * | 2011-06-29 | 2011-11-16 | 杭州阿玛尔科技有限公司 | Alkaline non-cyanide copper plating solution with main coordination agent of methylenediphosphonate |
| CN104087985A (en) * | 2014-06-25 | 2014-10-08 | 安徽长青电子机械（集团）有限公司 | Copper coating method of metal part |
| CN104264194A (en) * | 2014-10-13 | 2015-01-07 | 无锡长辉机电科技有限公司 | Preparation method of acid copper plating bath |
| CN105112898A (en) * | 2015-08-27 | 2015-12-02 | 无锡贺邦金属制品有限公司 | Surface treatment method for zinc alloy die casting |
| CN106757195A (en) * | 2016-12-05 | 2017-05-31 | 浙江工业大学 | A kind of process for protecting surface of high activity concrete dynamic modulus class material |
| CN107142502A (en) * | 2017-05-15 | 2017-09-08 | 佛山市兴中达化工实业有限公司 | A kind of replacement has the direct plating of cyanogen alkali copper in the non-cyanogen electro-plating method of kirsite matrix |
| CN108977860A (en) * | 2018-06-19 | 2018-12-11 | 南开大学 | A method of by electrodeposition process on Mo substrate depositing high-quality Cu film |
| CN110062820A (en) * | 2016-12-16 | 2019-07-26 | 柯尼卡美能达株式会社 | The forming method and plating plating solution of transparent conductive film |
| CN110344079A (en) * | 2019-08-16 | 2019-10-18 | 广东超华科技股份有限公司 | A kind of device and method reducing iron concentration in electrolytic copper foil electrolyte |
| CN110453246A (en) * | 2019-08-28 | 2019-11-15 | 中南大学 | A method of the fabricated in situ copper arsenic alloy from copper electrolyte |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914789A (en) * | 2010-08-12 | 2010-12-15 | 河南平原光电有限公司 | Cyanide-free copper electroplating method |
| CN102242381A (en) * | 2011-06-29 | 2011-11-16 | 杭州阿玛尔科技有限公司 | Alkaline non-cyanide copper plating solution with main coordination agent of methylenediphosphonate |
| CN104087985A (en) * | 2014-06-25 | 2014-10-08 | 安徽长青电子机械（集团）有限公司 | Copper coating method of metal part |
| CN104264194A (en) * | 2014-10-13 | 2015-01-07 | 无锡长辉机电科技有限公司 | Preparation method of acid copper plating bath |
| CN105112898A (en) * | 2015-08-27 | 2015-12-02 | 无锡贺邦金属制品有限公司 | Surface treatment method for zinc alloy die casting |
| CN106757195B (en) * | 2016-12-05 | 2019-05-03 | 浙江工业大学 | A kind of process for protecting surface of the porous class material of high activity |
| CN106757195A (en) * | 2016-12-05 | 2017-05-31 | 浙江工业大学 | A kind of process for protecting surface of high activity concrete dynamic modulus class material |
| CN110062820A (en) * | 2016-12-16 | 2019-07-26 | 柯尼卡美能达株式会社 | The forming method and plating plating solution of transparent conductive film |
| CN110062820B (en) * | 2016-12-16 | 2021-07-20 | 柯尼卡美能达株式会社 | Method for forming transparent conductive film and plating solution for electroplating |
| CN107142502A (en) * | 2017-05-15 | 2017-09-08 | 佛山市兴中达化工实业有限公司 | A kind of replacement has the direct plating of cyanogen alkali copper in the non-cyanogen electro-plating method of kirsite matrix |
| CN108977860A (en) * | 2018-06-19 | 2018-12-11 | 南开大学 | A method of by electrodeposition process on Mo substrate depositing high-quality Cu film |
| CN110344079A (en) * | 2019-08-16 | 2019-10-18 | 广东超华科技股份有限公司 | A kind of device and method reducing iron concentration in electrolytic copper foil electrolyte |
| CN110344079B (en) * | 2019-08-16 | 2021-06-08 | 广东超华科技股份有限公司 | Device and method for reducing concentration of iron ions in electrolytic copper foil electrolyte |
| CN110453246A (en) * | 2019-08-28 | 2019-11-15 | 中南大学 | A method of the fabricated in situ copper arsenic alloy from copper electrolyte |
| CN110453246B (en) * | 2019-08-28 | 2021-03-23 | 中南大学 | Method for in-situ synthesis of copper-arsenic alloy from copper electrolyte |
| CN110616448A (en) * | 2019-10-14 | 2019-12-27 | 南京航空航天大学 | Electrochemical pretreatment-in-situ electrodeposition method |
| CN110616448B (en) * | 2019-10-14 | 2021-02-05 | 南京航空航天大学 | Electrochemical pretreatment-in-situ electrodeposition method |
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