The solution for the contact copper coating of refractory metals

 

(57) Abstract:

The invention relates to the field of applying metal coatings, in particular, compositions of the solutions for the contact copper coating of refractory metals such as zirconium and its alloys, and can be used for applying technological Podlaski during wire drawing. The solution contains copper sulfate 100 to 220 g/l hydrofluoric acid 5-20 g/l as corrosion inhibitor of toluylenediamine and/or the condensation products of urotropine of 0.01-0.05 g/l and surfactant nonionic type 0.1-0.4 g/L. the Invention improves the adhesion of the copper coating, the quality of the finished product and to increase the life of the copper plating solution. 1 C.p. f-crystals, 3 tables.

The invention relates to the field of applying metal coatings, in particular, compositions of the solutions for the contact copper coating of refractory metals such as zirconium and its alloys, and can be used for applying technological Podlaski when being drawn.

Known solutions for the contact copper coating of refractory metals such as tantalum and niobium [1, 2, 3].

A disadvantage of the known solutions is that when madnani zirconium and its alloys, the coating is formed when the group [4], containing the following components, wt.%:

copper sulfate and 1.5 - 2.5

sulfuric acid - 2,0-4,0

the condensation products of urotropine with aniline in the presence of melamine and chloride benzyl - 0,05-0,15

water - the rest

The disadvantage of the solution is the inability to use the solution of this composition for copper plating zirconium products as metallic zirconium does not react with sulfuric acid.

Closest to the proposed composition and effect is achieved is the solution [5] , containing copper sulphate (20-100 g), hydrofluoric acid (0.3 to 1.5%) and surfactant nonionic type (1-10 g) in 1 l of solution.

The disadvantage of this solution is the low adhesion of the coating to the surface of the products.

Given the fact that the coating is used as podmazochnaja layer when the pressure treatment, it must be firmly linked with the product and should have a reliable shielding, anti-friction and wear-resistant properties. Poor adhesion of the coating to the surface of zirconium products due to the fact that when processing them in solutions of known composition on the surface instantly formed a characteristic of the metal layer of loose cuttings is to eliminate the above drawback, you must use a corrosion inhibitor.

The invention solves the problem of increasing the adhesion of the copper coating, the quality of the finished product and increase endurance for the copper plating solution.

According to the invention the problem is solved by supplemental solution containing copper sulphate, hydrofluoric acid and a surface-active substance (surfactant), as corrosion inhibitor of toluenediamine (TDA) and/or condensation products of urotropine (PKU) in the following ratio of components, g/l:

copper sulphate - 100 to 220

hydrofluoric acid - 5-20

Nonionic surfactants of type (OP-7(10) neonol or sintimid-5) - 0,1-0,4

TDA and/or PKU - 0,01-0,05

Total for the prototype and the proposed method is the presence in the composition of the solution for the contact copper plating the surface of the refractory metal, copper sulphate, hydrofluoric acid and surfactant.

Distinguishing features:

the ratio of components in the solution;

- additional introduction into the solution of toluenediamine (TDA) and/or condensation products of urotropine (PKU).

Known sources of technical solutions that solve the task and having the whole set of features of restrictive and distinctive parts of the formula claimed Liski level of the proposed technical solution stems from the fact that despite the popularity of some significant signs of finding their combinations and intervals used components requires significant time and costs.

Introduction to the known composition of the solution components TDA and/or PKU gives it a new, previously unknown properties. Coating on zirconium products with the use of the solutions proposed composition, high adhesion, wear resistance and ductility.

Examples

To study the optimal concentrations additionally introduced in a known solution components TDA and/or PKU was preparing the compositions, each containing, g/l: copper sulphate 100, hydrofluoric acid 8, surfactant 0.2 and differ from each other by the content of the TDA and PKU. Mortar compositions are shown in table 1.

The coating quality was evaluated by the method of meshing of the incision with subsequent assessment of the degree of coupling according to table 2, and results of the cold-rolled billets mills HPT and hptr directly in an industrial environment.

The results are given in table 3.

As can be seen from the table, the greatest effect on the stabilization of the quality of the coating and the degree of coupling is achieved PS 0.01 g/l to 0.005 g/l, the degree of coupling decreases, deformation takes place with the local detachment of copper and point the build-up of metal on the instrument.

The increase in the number of TDA (PKU) in solution more than 0.05 g/l does not change the degree of adhesion of the coating and improve its shielding and corrosion properties. Therefore, the content of inhibiting additive is more than 0.05 g/l is not economically feasible.

The process of copper plating in the proposed solution and cold rolling billets of zirconium and its alloys E110, A and E635, C-2, C-4, titanium tubes of alloy VT-1-0, PT-7M, tantalum, niobium and hafnium successfully carried out in industrial conditions at JSC "Bank". The use of a new structure helped to stabilize the process of copper plating, to improve adhesion of the copper layer with a basis to improve the quality of the finished product and to increase the endurance of the solution more than 3 times.

Implementation of the solution proposed structure is scheduled for JSC "CHMP" in 1999.

Sources of information

1. The solution for the contact copper plating the surface of the refractory metal. Auth.mon. The USSR 360402, 28.09.70.

2. The solution for the contact copper plating the surface of the refractory metal. Auth.mon. The USSR 360403, 28.09.70.

3. The solution for the contact copper plating surfaces that is before inclusion. Auth.mon. The USSR 595423, 28.02.78.

5. Solution for contact deposition of copper on refractory metals. Auth. mon. The USSR 241881, 16.12.68.

1. The solution for the contact copper coating of refractory metals containing copper sulphate, hydrofluoric acid, surfactant nonionic type, characterized in that it further comprises a corrosion inhibitor of toluylenediamine and/or the condensation products of urotropine in the following ratio of components, g/l:

Copper sulphate - 100 - 220

Hydrofluoric acid - 5 - 20

Surfactant nonionic type - 0,1 - 0,4

Toluylenediamine and/or the condensation products of urotropine - 0,01 - 0,05

2. The solution on p. 1, characterized in that as surfactants nonionic type it contains OP 7, OP-10, neonol or sintimid-5.

 

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