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Single dye type bright acidic copper plating additive and preparation method and application thereof

An acidic copper plating and additive technology, applied in the field of copper plating additives, can solve the problems of insufficient fineness of the high and middle areas of the coating, the influence of the polarization of the plating solution, and increase the production cost, etc., and achieve excellent deep plating ability and good filling and leveling performance of the coating , easy to manage the effect

Inactive Publication Date: 2010-12-01
济南德锡科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing additives in the market are generally composed of three components. The addition process is complicated and requires workers to have certain technical skills. Once the additive is out of balance, it is difficult to adjust. In many cases, it is re-added after treatment with activated carbon. increased production costs
We have also tried to mix the three agents of 610 or 630 or Atotech Ultra in proportion to make a single agent additive, but the fineness of the high and middle areas of the coating is not enough, the crystallization is rough, and the polarization is poor. The analysis is EO-PO copolymerization The substance will react in the presence of other substances, which will affect the polarization of the bath

Method used

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  • Single dye type bright acidic copper plating additive and preparation method and application thereof
  • Single dye type bright acidic copper plating additive and preparation method and application thereof
  • Single dye type bright acidic copper plating additive and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Synthesis of self-made polymerized phenazine dyes: add 20ml of concentrated hydrochloric acid or concentrated sulfuric acid to a four-necked flask, and 1g of 3-amino-7-(N,N dimethylamino)-2-methyl-5-phenyl-phenazine Add the monomer and 300mg cupric chloride or nickel chloride powder into the flask, stir to suspend it in the acid, heat to 60-65°C, slowly add saturated sodium nitrite aqueous solution dropwise, continue stirring for 1- Cool to room temperature after 1.5h. 15 ml of 50% (wt%) sodium hydroxide solution was added dropwise at room temperature, and the reaction solution was cooled with an ice-water bath. The resulting reaction solution was filtered to obtain a dark purple solid, which was dried.

[0047] Through high-performance liquid chromatography and mass spectrometry, it is found that the yield of the desired polymerization product is 80-85% (wt%), and the rest is unreacted monomers.

Embodiment 2

[0049] 1) Preparation of additives (1L)

[0050] Azophenazine polymer hydrochloride (Guangzhou Chaorun Chemical) 3g

[0051] Gentian violet 2g

[0052] Methylene blue 1g

[0053] Polypropylene Glycol 1000 5g

[0054] Macrogol 2000 5g

[0055] Sodium polydithiobutane sulfonate 2.5g;

[0056] Preparation method: Add about 300ml of water into a large beaker, add 2g of sulfuric acid and stir evenly, add polypropylene glycol, polyethylene glycol and sodium polydithiobisbutane sulfonate, stir for at least 1 hour to completely dissolve, and then add azo Phenazine polymer hydrochloride (super-moisturizing), gentian violet and methylene blue, stir for more than 3 hours until completely dissolved, and dilute to 1L.

[0057] 2) Preparation and use of bright acidic copper plating solution (1L)

[0058] CuSO 4 ·6H 2 O 210g

[0059] h 2 SO 4 33ml

[0060] Cl - 100mg

[0061] Additive 2.5ml

[0062] Preparation meth...

Embodiment 3

[0066] 1) Preparation of additives (1L)

[0067] Azophenazine Polymer Sulfate (Keyu Chemical) 5g

[0068] Gentian violet 1.5g

[0069] Lowe's Violet 0.8g

[0070] Polypropylene glycol 600 7g

[0071] Macrogol 1000 8g

[0072] Sodium polydithiodipropane sulfonate 3g;

[0073] Preparation method is with embodiment 2.

[0074] 2) bright acidic copper plating solution preparation (1L) and use are the same as embodiment 2

[0075] Plating piece (Hull cell test piece) as an example: take 250ml of the prepared plating solution and put it into the Hull cell, keep room temperature, under the condition of strong air bubbling, use phosphor copper plate as the anode, conduct electroplating, current 2A, time 10min . The whole plated sheet is bright, without fogging, and there is no pitting and pitting on the surface.

[0076] Pilot test: Prepare 25L of plating solution, add it to the pilot test plating tank, and under strong bubbling, carry out rack plating on the degreasing and ac...

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Abstract

The invention discloses a single dye type bright acidic copper plating additive and a preparation method and application thereof. The additive is prepared from a polymeric phenazine dye, a triphenylmethane dye, a thiazine dye, a surfactant and polysulfide serving as main raw materials; when the additive is applied to copper plating solution for copper plating, the using effect can reach that of a three-dose additive; the entire plated sheet is bright; the additive is simple to manage and the maladjustment of the plating solution additive is not caused; and even if the concentration of the additive is over-high, the plating solution can be continuously used after the plating solution is slightly diluted.

Description

technical field [0001] The invention relates to a copper plating additive, in particular to a single-dose dye type bright acidic copper plating additive. Background technique [0002] Due to the good toughness of the coating, the plating solution has good bright leveling and fast deposition speed. It is used in plastic electroplating, metal copper-nickel-chromium decorative electroplating, metallization electroplating of printing plate holes and electroforming. occupies an important position. [0003] Research on acidic copper plating additives by major companies around the world began in the 1950s, and foreign research has successfully added sulfur- and nitrogen-containing compounds, such as thiourea and its derivatives, 2-mercaptobenzothiazole, 2-mercaptobenzothiazole Some dyes such as imidazole and basic saffron, thiazapine, triphenylmethane, etc., may have a brighter coating; in the 1960s, some additives such as polyether were added to make the brightness, leveling abil...

Claims

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Application Information

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IPC IPC(8): C25D3/38
Inventor 罗祖文曾凡亮王凯铭
Owner 济南德锡科技有限公司
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