CN101545123B - Method for non-cyanide copper electroplating of steel parts - Google Patents
Method for non-cyanide copper electroplating of steel parts Download PDFInfo
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- CN101545123B CN101545123B CN2009100716716A CN200910071671A CN101545123B CN 101545123 B CN101545123 B CN 101545123B CN 2009100716716 A CN2009100716716 A CN 2009100716716A CN 200910071671 A CN200910071671 A CN 200910071671A CN 101545123 B CN101545123 B CN 101545123B
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Abstract
The invention discloses a method for non-cyanide copper electroplating of steel parts, which relates to a method for copper electroplating of the steel parts. The method solves the problems that cyanide is easy to pollute air and water sources, can be naturally oxidized in plating baths, is oxidized on electrodes and has quick consumption and high cost. The method for the non-cyanide copper electroplating of the steel parts is realized according to the following steps of oil removal, non-cyanide copper leaching and copper electroplating, and thus the steel parts with electroplated copper are obtained. The steel parts with the electroplated copper prepared by the method have unpeeled plating layers, do not blister, and have good bonding force after high-temperature treatment. The method has simple process and convenient operation.
Description
Technical field
The present invention relates to a kind of method of steel part electro-coppering.
Background technology
Copper-nickel-chromium, copper-nickel-imitative gold or copper-MULTI-LAYER NICKEL-chrome electroplating technology are application surface electroplating technology combinations very widely.Hydrosulphate copper facing has developed quite ripely now, but it is not suitable for electro-coppering on iron-based, and reason is that in a single day steel part enters acidic bath moment replacement(metathesis)reaction just takes place, and produces that hole is many, the displacement copper layer of tissue looseness.Bottom copper in the above-mentioned treatment process combination of steel part generally adopts cyanide electroplating to obtain, and electroplating technology uses the history in existing more than 100 year of prussiate electrolytic solution.Cyanide copper plating process, this is because cyanide electroplating liquid has some good performances, as direct plating on iron-based or zinc-base workpiece, and can obtain the electric deposited copper floor of good combination power; The thickness distribution of coating is even; The dispersive ability of plating bath is better etc.But also have important disadvantages, maximum problem is the toxicity of prussiate, and cuprous cyanide wherein, sodium cyanide and potassium cyanide all are highly toxic substances, needs carefully to use, in case air and water source are polluted.Therefore, the direct labor will have holidays by turns, and waste water and gas is wanted strict and handled, so cause the increase of production cost.And prussiate also can natural oxidation and oxidation on electrode in plating bath, consume fast, cost is high.Therefore be necessary the technological innovation of cyanide electroplating as bottom.
Summary of the invention
The objective of the invention is to consume the problem fast, that cost is high, and a kind of method of non-cyanide copper electroplating of steel parts is provided in order to solve prussiate easily to air with the water source pollutes and prussiate can natural oxidation in plating bath and oxidation on electrode.
The method of non-cyanide copper electroplating of steel parts realizes according to the following steps: one, steel part is immersed temperature and be 50～80 ℃, concentration and be in 40～60 milliliters/liter the electrochemical deoiling liquid, soak time is 5～15min, taking out the back, to insert temperature as negative electrode be that 40～60 ℃, concentration are in the electrolytic degreasing liquid of 40～60 grams per liters, with the stainless steel is anode, is 1.0～3.0A/dm in current density
2Condition under anticathode carry out electrolytic degreasing 1～5min, immerse volume percent behind clear Xian of deionized water more at ambient temperature and be in 5%～10% the hydrochloric acid, soak time is 10～60s; Two, will behind clear Xian, be 15～35 ℃ conditions under to immerse in no cyanogen copper leaching liquid 20～1200s in temperature with deionized water through the steel part that step 1 was handled, regulating the pH value be 2.5～8.0; Three, will insert in the acid copper sulfate electroplate liquid as negative electrode behind clear Xian with deionized water through steel part that step 2 was handled, as anode, be that 20～30 ℃, cathode current density be 2.0～4.0A/dm in temperature with phosphor-copper
2Condition under anticathode carry out electro-coppering 10～50min, promptly get the steel part of electro-coppering; Wherein no cyanogen copper leaching liquid is made into by complexing agent, cupric ion and water in the step 2, and the concentration of complexing agent is that the concentration of 10～200 grams per liters, bivalent cupric ion is 0.5～30 grams per liter; The acid copper sulfate electroplate liquid is made into by copper sulfate, sulfuric acid, chlorion, additive and water in the step 3, the concentration of copper sulfate is that 210 grams per liters, vitriolic concentration are that the concentration of 50 grams per liters, chlorion is that the concentration of 50 mg/litre, additive is 2.0 milliliters/liter, and complexing agent is mixing more than two kinds in ethylenediamine tetraacetic acid (EDTA), triethyl tetramine six acetate, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid, ethylene diamine tetra methylene phosphonic acid, Amino Trimethylene Phosphonic Acid, tetra-sodium, tartrate, citric acid, gluconic acid and sodium salt, sylvite or amine salt, the thiocarbamide in the step 2.
The product that the inventive method makes is heated to 250 ℃ at baking oven or High Temperature Furnaces Heating Apparatus, is incubated 1 hour, take out then in the cold water of room temperature and cool off, with the naked eye or 4N times of magnifying glass observe, coating does not peel off, and is non-foaming, bonding force is good.
Solute in the electroplate liquid that the inventive method is used is difficult for oxidation, consumes to reduce, thereby reduces cost, and compared with prior art cost reduces by 20%～30%.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the method for present embodiment non-cyanide copper electroplating of steel parts realizes according to the following steps: one, steel part is immersed temperature and be 50～80 ℃, concentration and be in 40～60 milliliters/liter the electrochemical deoiling liquid, soak time is 5～15min, taking out the back, to insert temperature as negative electrode be that 40～60 ℃, concentration are in the electrolytic degreasing liquid of 40～60 grams per liters, with the stainless steel is anode, is 1.0～3.0A/dm in current density
2Condition under anticathode carry out electrolytic degreasing 1～5min, immerse volume percent behind clear Xian of deionized water more at ambient temperature and be in 5%～10% the hydrochloric acid, soak time is 10～60s; Two, will behind clear Xian, be 15～35 ℃ conditions under to immerse in no cyanogen copper leaching liquid 20～1200s in temperature with deionized water through the steel part that step 1 was handled, regulating the pH value be 2.5～8.0; Three, will insert in the acid copper sulfate electroplate liquid as negative electrode behind clear Xian with deionized water through steel part that step 2 was handled, as anode, be that 20～30 ℃, cathode current density be 2.0～4.0A/dm in temperature with phosphor-copper
2Condition under anticathode carry out electro-coppering 10～50min, promptly get the steel part of electro-coppering; Wherein no cyanogen copper leaching liquid is made into by complexing agent, cupric ion and water in the step 2, and the concentration of complexing agent is that the concentration of 10～200 grams per liters, bivalent cupric ion is 0.5～30 grams per liter; The acid copper sulfate electroplate liquid is made into by copper sulfate, sulfuric acid, chlorion, additive and water in the step 3, and the concentration of copper sulfate is that 210 grams per liters, vitriolic concentration are that the concentration of 50 grams per liters, chlorion is that the concentration of 50 mg/litre, additive is 2.0 milliliters/liter.
Electrochemical deoiling liquid adopts the PROCLEANER BR1# of star chemical industry company limited electrochemical deoiling liquid forever in the present embodiment step 1; Electrolytic degreasing liquid adopts the MP5000 of star chemical industry company limited electrolytic degreasing liquid forever in the step 1; Adopt sulfuric acid and sodium hydroxide to regulate pH in the step 2; Additive adopts star chemical industry company limited forever in the step 3
The AM additive.
The product that present embodiment makes is heated to 250 ℃ at baking oven or High Temperature Furnaces Heating Apparatus, is incubated 1 hour, take out then in the cold water of room temperature and cool off, with the naked eye or 4N times of magnifying glass observe, coating does not peel off, and is non-foaming, bonding force is good.
Embodiment two: what present embodiment and embodiment one were different is that current density is 1.5～2.5A/dm in the step 1
2Other is identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is that current density is 2.0A/dm in the step 1
2Other is identical with embodiment one.
Embodiment four: what present embodiment and embodiment one were different is that current density is 1.0A/dm in the step 1
2Other is identical with embodiment one.
Embodiment five: what present embodiment and embodiment one were different is that current density is 3.0A/dm in the step 1
2Other is identical with embodiment one.
Embodiment six: present embodiment is different with embodiment one or two be in the step 1 electrolytic degreasing time be 2～4min.Other is identical with embodiment one or two.
Embodiment seven: present embodiment is different with embodiment one or two be in the step 1 electrolytic degreasing time be 3min.Other is identical with embodiment one or two.
Embodiment eight: present embodiment is different with embodiment one or two be in the step 1 electrolytic degreasing time be 1min.Other is identical with embodiment one or two.
Embodiment nine: present embodiment is different with embodiment one or two be in the step 1 electrolytic degreasing time be 5min.Other is identical with embodiment one or two.
Embodiment ten: what present embodiment and embodiment six were different is to immerse 100～1000s in the no cyanogen copper leaching liquid in the step 2.Other is identical with embodiment six.
Embodiment 11: what present embodiment and embodiment six were different is to immerse 600s in the no cyanogen copper leaching liquid in the step 2.Other is identical with embodiment six.
Embodiment 12: what present embodiment and embodiment six were different is to immerse 20s in the no cyanogen copper leaching liquid in the step 2.Other is identical with embodiment six.
Embodiment 13: what present embodiment and embodiment six were different is to immerse 1200s in the no cyanogen copper leaching liquid in the step 2.Other is identical with embodiment six.
Embodiment 14: present embodiment and embodiment one, two or ten are different is that to regulate the pH value in the step 2 be 3.0～6.0.Other is identical with embodiment one, two or ten.
Embodiment 15: present embodiment and embodiment one, two or ten are different is that to regulate the pH value in the step 2 be 5.0.Other is identical with embodiment one, two or ten.
Embodiment 16: present embodiment and embodiment one, two or ten are different is that to regulate the pH value in the step 2 be 2.5.Other is identical with embodiment one, two or ten.
Embodiment 17: present embodiment and embodiment one, two or ten are different is that to regulate the pH value in the step 2 be 8.0.Other is identical with embodiment one, two or ten.
Embodiment 18: present embodiment and embodiment 14 are different is that complexing agent is that in ethylenediamine tetraacetic acid (EDTA), triethyl tetramine six acetate, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid, ethylene diamine tetra methylene phosphonic acid, Amino Trimethylene Phosphonic Acid, tetra-sodium, tartrate, citric acid, gluconic acid and sodium salt, sylvite or amine salt, the thiocarbamide two or more mixes in the step 2.Other is identical with embodiment 14.
When the component of complexing agent was two or more in the present embodiment, each component was pressed arbitrary proportion and is mixed.
Embodiment 19: what present embodiment and embodiment one, two, ten or 18 were different is that bivalent cupric ion is provided by copper sulfate, copper carbonate, neutralized verdigris or cupric nitrate in the step 2.Other is identical with embodiment one, two, ten or 18.
Embodiment 20: present embodiment and embodiment 19 are different be in the step 3 in the phosphor-copper mass percent of phosphorus be 0.03%～0.06%.Other is identical with embodiment 19.
Embodiment 21: what present embodiment and embodiment one, two, ten, 18 or 20 were different is that cathode current density is 2.5～3.5A/dm in the step 3
2Other is identical with embodiment one, two, ten, 18 or 20.
Embodiment 22: present embodiment and embodiment 21 are different be in the step 3 electro-coppering time be 20～40min.Other is identical with embodiment 21.
Embodiment 23: the method for present embodiment non-cyanide copper electroplating of steel parts realizes according to the following steps: one, steel part is immersed temperature and be 60 ℃, concentration and be in 50 milliliters/liter the electrochemical deoiling liquid, soak time is 10min, taking out the back, to insert temperature as negative electrode be that 50 ℃, concentration are in the electrolytic degreasing liquid of 50 grams per liters, with the stainless steel is anode, is 2.0A/dm in current density
2Condition under anticathode carry out electrolytic degreasing 2min, immerse volume percent behind clear Xian of deionized water more at ambient temperature and be in 7% the hydrochloric acid, soak time is 30s; Two, will behind clear Xian, be 25 ℃ conditions under to immerse in no cyanogen copper leaching liquid 120s in temperature with deionized water through the steel part that step 1 was handled, regulating the pH value be 5.0; Three, will insert in the acid copper sulfate electroplate liquid as negative electrode behind clear Xian with deionized water through the steel part that step 2 was handled, as anode, be 25 ℃ in temperature with phosphor-copper, and cathode current density is 3.0A/dm
2Condition under anticathode carry out electro-coppering 30min, promptly get the steel part of electro-coppering; Wherein in every liter of no cyanogen copper leaching liquid 3.5 gram cupric sulfate pentahydrates, 30 gram triethyl tetramine six sodium acetates and 20 gram thiocarbamides are arranged in the step 2; Be dissolved with 210 gram copper sulfate, 50 gram sulfuric acid, 50 milligrams of chlorions and 2.0 milliliters of additives in every liter of acid copper sulfate electroplate liquid in the step 3; In the step 2 in no cyanogen copper leaching liquid and the step 3 solvent of acid copper sulfate electroplate liquid be water.
The product that present embodiment makes is heated to 250 ℃ at baking oven or High Temperature Furnaces Heating Apparatus, is incubated 1 hour, take out then in the cold water of room temperature and cool off, with the naked eye or 4N times of magnifying glass observe, coating does not peel off, and is non-foaming, bonding force is good.
Embodiment 24: the method for present embodiment non-cyanide copper electroplating of steel parts realizes according to the following steps: one, steel part is immersed temperature and be 60 ℃, concentration and be in 50 milliliters/liter the electrochemical deoiling liquid, soak time is 5min, taking out the back, to insert temperature as negative electrode be that 50 ℃, concentration are in the electrolytic degreasing liquid of 50 grams per liters, with the stainless steel is anode, is 2.0A/dm in current density
2Condition under anticathode carry out electrolytic degreasing 2min, immerse volume percent behind clear Xian of deionized water more at ambient temperature and be in 7% the hydrochloric acid, soak time is 20s; Two, will behind clear Xian, be 25 ℃ conditions under to immerse in no cyanogen copper leaching liquid 180s in temperature with deionized water through the steel part that step 1 was handled, regulating the pH value be 5.0; Three, will insert in the acid copper sulfate electroplate liquid as negative electrode behind clear Xian with deionized water through the steel part that step 2 was handled, as anode, be 25 ℃ in temperature with phosphor-copper, and cathode current density is 3.0A/dm
2Condition under anticathode carry out electro-coppering 30min, promptly get the steel part of electro-coppering; Wherein in every liter of no cyanogen copper leaching liquid 4 gram cupric sulfate pentahydrates, 35 gram triethyl tetramines, six sodium acetates, 20 gram thiosinamines are arranged in the step 2; Be dissolved with 210 gram copper sulfate, 50 gram sulfuric acid, 50 milligrams of chlorions and 2.0 milliliters of additives in every liter of acid copper sulfate electroplate liquid in the step 3; In the step 2 in no cyanogen copper leaching liquid and the step 3 solvent of acid copper sulfate electroplate liquid be water.
The product that present embodiment makes is heated to 250 ℃ at baking oven or High Temperature Furnaces Heating Apparatus, is incubated 1 hour, take out then in the cold water of room temperature and cool off, with the naked eye or 4N times of magnifying glass observe, coating does not peel off, and is non-foaming, bonding force is good.
Embodiment 25: the method for present embodiment non-cyanide copper electroplating of steel parts realizes according to the following steps: one, steel part is immersed temperature and be 60 ℃, concentration and be in 50 milliliters/liter the electrochemical deoiling liquid, soak time is 7min, taking out the back, to insert temperature as negative electrode be that 50 ℃, concentration are in the electrolytic degreasing liquid of 50 grams per liters, with the stainless steel is anode, is 2.0A/dm in current density
2Condition under anticathode carry out electrolytic degreasing 4min, immerse volume percent behind clear Xian of deionized water more at ambient temperature and be in 7% the hydrochloric acid, soak time is 10s; Two, will behind clear Xian, be 25 ℃ conditions under to immerse in no cyanogen copper leaching liquid 300s in temperature with deionized water through the steel part that step 1 was handled, regulating the pH value be 4.5; Three, will insert in the acid copper sulfate electroplate liquid as negative electrode behind clear Xian with deionized water through the steel part that step 2 was handled, as anode, be 25 ℃ in temperature with phosphor-copper, and cathode current density is 3.0A/dm
2Condition under anticathode carry out electro-coppering 30min, promptly get the steel part of electro-coppering; Wherein in every liter of no cyanogen copper leaching liquid 6 gram cupric sulfate pentahydrates, 35 gram/ethylenediamine tetraacetic acid (EDTA)s, 20 gram 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid and 10 gram tartrate are arranged in the step 2; Be dissolved with 210 gram copper sulfate, 50 gram sulfuric acid, 50 milligrams of chlorions and 2.0 milliliters of additives in every liter of acid copper sulfate electroplate liquid in the step 3; In the step 2 in no cyanogen copper leaching liquid and the step 3 solvent of acid copper sulfate electroplate liquid be water.
The product that present embodiment makes is heated to 250 ℃ at baking oven or High Temperature Furnaces Heating Apparatus, is incubated 1 hour, take out then in the cold water of room temperature and cool off, with the naked eye or 4N times of magnifying glass observe, coating does not peel off, and is non-foaming, bonding force is good.
Claims (9)
1. the method for non-cyanide copper electroplating of steel parts, the method that it is characterized in that non-cyanide copper electroplating of steel parts realizes according to the following steps: one, steel part is immersed temperature and be 50～80 ℃, concentration and be in 40～60 milliliters/liter the electrochemical deoiling liquid, soak time is 5～15min, taking out the back, to insert temperature as negative electrode be that 40～60 ℃, concentration are in the electrolytic degreasing liquid of 40～60 grams per liters, with the stainless steel is anode, is 1.0～3.0A/dm in current density
2Condition under anticathode carry out electrolytic degreasing 1～5min, immerse volume percent behind clear Xian of deionized water more at ambient temperature and be in 5%～10% the hydrochloric acid, soak time is 10～60s; Two, will behind clear Xian, be 15～35 ℃ conditions under to immerse in no cyanogen copper leaching liquid 20～1200s in temperature with deionized water through the steel part that step 1 was handled, regulating the pH value be 2.5～8.0; Three, will insert in the acid copper sulfate electroplate liquid as negative electrode behind clear Xian with deionized water through steel part that step 2 was handled, as anode, be that 20～30 ℃, cathode current density be 2.0～4.0A/dm in temperature with phosphor-copper
2Condition under anticathode carry out electro-coppering 10～50min, promptly get the steel part of electro-coppering; Wherein no cyanogen copper leaching liquid is made into by complexing agent, cupric ion and water in the step 2, and the concentration of complexing agent is that the concentration of 10～200 grams per liters, bivalent cupric ion is 0.5～30 grams per liter; The acid copper sulfate electroplate liquid is made into by copper sulfate, sulfuric acid, chlorion, additive and water in the step 3, the concentration of copper sulfate is that 210 grams per liters, vitriolic concentration are that the concentration of 50 grams per liters, chlorion is that the concentration of 50 mg/litre, additive is 2.0 milliliters/liter, and complexing agent is mixing more than two kinds in ethylenediamine tetraacetic acid (EDTA), triethyl tetramine six acetate, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid, ethylene diamine tetra methylene phosphonic acid, Amino Trimethylene Phosphonic Acid, tetra-sodium, tartrate, citric acid, gluconic acid and sodium salt, sylvite or amine salt, the thiocarbamide in the step 2.
2. the method for non-cyanide copper electroplating of steel parts according to claim 1 is characterized in that current density is 1.5～2.5A/dm in the step 1
2
3. the method for non-cyanide copper electroplating of steel parts according to claim 1 and 2 is characterized in that the electrolytic degreasing time is 2～4min in the step 1.
4. the method for non-cyanide copper electroplating of steel parts according to claim 3 is characterized in that immersing in the step 2 100～1000s in the no cyanogen copper leaching liquid.
5. according to the method for claim 1,2 or 4 described non-cyanide copper electroplating of steel parts, it is characterized in that regulating the pH value in the step 2 is 3.0～6.0.
6. according to the method for claim 1,2 or 4 described non-cyanide copper electroplating of steel parts, it is characterized in that bivalent cupric ion is provided by copper sulfate, copper carbonate, neutralized verdigris or cupric nitrate in the step 2.
7. the method for non-cyanide copper electroplating of steel parts according to claim 6 is characterized in that in the step 3 that the mass percent of phosphorus is 0.03%～0.06% in the phosphor-copper.
8. according to the method for claim 1,2,4 or 7 described non-cyanide copper electroplating of steel parts, it is characterized in that cathode current density is 2.5～3.5A/dm in the step 3
2
9. the method for non-cyanide copper electroplating of steel parts according to claim 8 is characterized in that the electro-coppering time is 20～40min in the step 3.
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| CN107502928A (en) * | 2017-07-18 | 2017-12-22 | 山西运城制版集团（上海）企业发展有限公司 | It is a kind of that the method for setting copper prime coat is plated on steel rider |
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