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Citrate-tartrate dual-complexing non-cyanide alkaline copper-plating electrolyte on steel substrate

A technology of citrate and tartrate, which is applied in the field of cyanide-free copper plating, can solve the problems of short plating time, high chemical oxygen consumption, and narrow current density, and achieves convenient control, simple process operation, and wide working current density range Effect

Inactive Publication Date: 2013-09-18
HUBEI HENGXIN ELECTRO PLATING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Scholars at home and abroad have done a lot of research on the copper plating process. Hydroxyethylidene diphosphonic acid copper plating has been used in mass production reports abroad. The cyanide-free alkaline copper plating produced by Plaschem and Cupral companies uses organic phosphonates as formula; the current domestic pyrophosphate copper plating is used for acid sulfate copper plating on zinc alloy substrates, and has been widely used in copper plating thickening processes for tubular and complex workpieces; the invention of Chinese patent publication No. CN101550569A is based on Ethyl diphosphonic acid is the main complexing agent, citrate is the auxiliary complexing agent, and the current density of the formed alkaline copper plating process is in the range of 0.5-3A / dm 2 , the temperature control range is wide, the coating crystallization is fine, and the electrolyte is stable, but these processes are prone to phosphorus pollution in wastewater
And the reported EDTA can also be used for cyanide-free alkaline copper plating process as the main complexing agent, but because the boiling action of EDTA and copper ion is too strong, it is not convenient for waste water treatment
The invention of Chinese patent publication number CN101665962A uses citrate, tartaric acid and organic amine as complexing agent, and the brightener is preferably selected from antimony trichloride, antimony nitrate, antimony sulfate, selenium dioxide, nitrate, nitrite At least one of the above, the obtained test piece is bright, but the cathode current density is in the range of 0.5-2A / dm 2 , the current density is narrow, and it is not easy to handle more complex parts
However, there are too many organic substances, and the chemical oxygen demand is too high, which is not convenient for wastewater treatment.
[0004] Judging from the existing reported research and basic work carried out, the citrate system alkaline copper plating is most likely to be used as a substitute for cyanide-free environmental protection electroplating, such as the patent 201010164782.4 applied by our company in April 2010—lemon on steel substrate The industrialized method of salt alkaline cyanide-free copper plating provides a plating solution formula with good stability, economy and environmental protection, and a long service life. The copper plating layer has problems such as short plating time, poor bonding force of the plating layer, and limited dispersion of the plating solution.

Method used

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  • Citrate-tartrate dual-complexing non-cyanide alkaline copper-plating electrolyte on steel substrate
  • Citrate-tartrate dual-complexing non-cyanide alkaline copper-plating electrolyte on steel substrate
  • Citrate-tartrate dual-complexing non-cyanide alkaline copper-plating electrolyte on steel substrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Prepare 250ml containing copper sulfate 30 g / L, sodium citrate 147 g / L, potassium sodium tartrate 45 g / L, potassium nitrate 8 g / L, sodium bicarbonate 10 g / L, niacin 1 g / L, polyethylene glycol Electrolyte of amine 1 ml / L, polyethylene glycol 0.1 g / L, 2-mercaptobenzimidazole 1.2 mg / L: weigh 7.5 g of copper sulfate, 36.75 g of sodium citrate, 11.25 g of potassium sodium tartrate, and potassium nitrate Add 2g, 2.5g of sodium bicarbonate, 0.25g of niacin, 0.25ml of polyethyleneimine, 0.0250g of polyethylene glycol, and 0.3mg of 2-mercaptobenzimidazole into 160ml of tap water, stir to dissolve, and adjust the pH value to 7-8 , and then add tap water until the volume of the solution is 250ml, and adjust the pH value to 9. The electrolyte solution was heated to 50°C for later use.

[0054] Preparation of chemical degreasing liquid: prepare sodium hydroxide 20-40g / L, sodium carbonate 20-30 g / L, trisodium phosphate 5-10g / L, sodium silicate 5-15 g / L, OP emulsification according t...

Embodiment 2

[0059] According to the method described in Example 1, 250ml of copper sulfate 30 g / L, sodium citrate 147 g / L, potassium sodium tartrate 45 g / L, potassium nitrate 8 g / L, sodium bicarbonate 10 g / L, tobacco An electrolyte solution of 1 g / L acid, 1 ml / L polyethyleneimine, 0.2 g / L polyethylene glycol, and 0.9 mg / L 2-mercaptobenzimidazole was preheated to 50°C.

[0060] According to the scheme of Example 1, after the steel test piece is pickled, degreased and washed with water, it is placed in the Hull cell equipped with the above electrolyte, and the cathode current density is set to be 4A / dm 2 , under bubbling and stirring, electroplating for 10 minutes, using a scanning electron microscope to observe the microscopic morphology of the coating, the copper crystals are relatively uniform in size, and the distribution in rows is relatively uniform, see Image 6 .

[0061] In this embodiment, the content of other components in the electrolyte is kept constant, the content of 2-merc...

Embodiment 3

[0063] According to the method described in Example 1, 250ml of copper sulfate 30 g / L, sodium citrate 147 g / L, potassium sodium tartrate 45 g / L, potassium nitrate 8 g / L, sodium bicarbonate 10 g / L, tobacco Electrolyte with 0.5 g / L acid, 1 ml / L polyethyleneimine, 0.2 g / L polyethylene glycol, and 1.2 mg / L 2-mercaptobenzimidazole, preheated to 50°C.

[0064] According to the scheme of Example 1, after the steel test piece is pickled, degreased and washed with water, it is placed in the Hull cell equipped with the above electrolyte, and the cathode current density is set to be 4A / dm 2 , under bubbling and stirring, electroplating for 10 minutes, using a scanning electron microscope to observe the microscopic morphology of the coating, the copper crystals are relatively uniform in size, and the distribution in rows is relatively uniform, see Figure 7 .

[0065] In this example, keep the content of other components in the electrolyte constant, adjust the content of nicotinic acid ...

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Abstract

The invention discloses a citrate-tartrate dual-complexing non-cyanide alkaline copper-plating electrolyte on a steel substrate. The electrolyte per liter is prepared from the following raw materials by weight: 29-32g of copper sulfate, 110-147g of sodium citrate, 40-50g of sodium potassium tartrate, 6-8g of potassium nitrate, 8-12g of sodium bicarbonate, 0.5-1.5g of nicotinic acid, 0.1-0.2g of polyethylene glycol, 1-1.5ml of polyethyleneimine, 0.84-1.32mg of 2-mercapto benzimidazole and the balance of water. The electrolyte disclosed by the invention is good in dispersion capability, strong in coverage capability, high in stability, clean and environmentally-friendly in formula and suitable for wide working current density range; a plating coat of a plated part electroplated by the electrolyte is excellent in binding force, uniform in distribution and suitable for preparing a basic layer or a copper-plating layer in a medium thickness on a complex steel part.

Description

technical field [0001] The invention relates to a cyanide-free copper plating technology, in particular to a citrate-tartrate double complex alkaline cyanide-free copper plating electrolyte on a steel substrate. Background technique [0002] Cyanide copper plating has good dispersing ability and covering ability, and the composition of the electrolyte is simple and easy to maintain. It is suitable for the primer of steel parts, zinc and aluminum alloy products, etc. , Exhaust gas endangers the health of operators. In recent years, my country has issued regulations to cancel cyanide electroplating, and the European Union and Norway have also formulated RoHS (Regarding the Prohibition of Certain Hazardous Substances in Electronic and Electrical Equipment) and PoHS (Prohibition of Specific Hazardous Substances in Consumer Products) regulations. A further step is to restrict the use of toxic additives in the electrolyte. [0003] The primary task of replacing the cyanide copper...

Claims

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Application Information

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IPC IPC(8): C25D3/38
Inventor 陈小兵
Owner HUBEI HENGXIN ELECTRO PLATING
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