Formation of component coating by chemical conversion (versions)

FIELD: chemistry.

SUBSTANCE: invention refers to methods formation of component coating by chemical conversion for dielectrics, semiconductors and electronegative metals (iron, aluminium, titanium and their alloys), as well as combined ceramic-metal materials and can be used in radio engineering industry, in instrument engineering and for manufacturing of printed-circuit boards and decoration of wax, plastisol and other products. The first version of the method involves component surface processing in sorption stabilising solution in ratio as follows, g/l: SiO2 - (35-45)×10-3, Al2O3 - (0.5-10)×10-3, MgO - (0.5-10)×10-3, HF - (0.5-1)×10-3, water - the rest. It is followed with sensitisation, activation in solution containing palladium chloride and hydrochloric acid, and metal plating. The second version of the method involves sensitisation of component surface in sorption stabilising solution in ratio as follows, g/l: SiO2 - (35-45)×10-3, Al2O3 - (0.5-10)×10-3, MgO - (0.5-10)×10-3, HF - (0.5-1)×10-3, water - the rest.

EFFECT: improved plating quality ensured with higher catalytic activity of processed surface and reduced palladium content in solution for activation.

2 cl, 8 tbl, 8 ex

 

The invention relates to methods of chemical metallization of dielectrics, semiconductors and electronegative metals (iron, aluminium, titanium and their alloys), and composite metal-ceramic materials and can be used in the radio industry and instrument-making, including in the manufacture of printed circuit boards and art handling products made of wax, plastisol and other materials.

The known method of chemical metallization of the combined surface copper-polyimide comprising a surface treatment solution containing sodium hydroxide, Ethylenediamine, monoethanolamine and triatanolamine in the following ratio of components, g/l: sodium hydroxide 200-400; Ethylenediamine 79-80; monoethanolamine 60-70; triethanolamine 40-50; water - the rest, at a temperature of 50-60°C for 5...7 minutes sensitization in solutions of salts of tin and activation solution containing palladium chloride, hydrochloric acid, glycine and water in the following ratio of components, g/l: palladium chloride 0,1-0,01; hydrochloric acid 0,0004-0,0006; glycine 1,5-2,0; water - the rest, at pH of 3.2 to 3.5 at a temperature of 20-25°C for 9-10 minutes and metal coating (see RF patent №2041575, CL IPC6NC 3/18).

However, this method of chemical metallization does not provide high-quality coating of the workpiece surface, p is because used for sensitization metal system on the basis of salts of tin unstable because of its autoxidation in daylight.

Sn2+spontaneously goes into Sn4+the reaction Sn2+→Sn4++2e, resulting colloidal system on the tin Sn2+formed in solution and not on the surface of the workpiece. As a result, the part surface is not formed a sufficient activation of the metal centers, which leads to deterioration of the quality of the coating by chemical metallization.

Colloidal film formed on the surface of the workpiece, also largely depends on the subsequent rinsing, which makes it impossible to obtain the same quality coatings on different batches of parts in the chemical metallization process.

The instability of the metal system, based on the salts of tin, lead to the necessity of frequent replacement of the solution of tin for the operation of sensitization, which complicates the technology and lead to its appreciation.

In addition, this method does not provide a sufficient thickness of the metal coating due to low autocatalysis.

This method is also harmful production, because the surface treatment of parts prior to sensitization carried out in a solution containing substances of the group of amines in combination with sodium hydroxide at elevated temperature.

Application of the above method may cause the same to the pollution of the environment, in particular waters because the wastewater from the substances of the group of amines is not provided.

In addition, the processing solution of the following composition promotes formation on the surfaces of sufficient activation of the metal centers, since the film formed on the surface of the parts is purely organic composition. Organic film increases the wettability of the workpiece, but at the same time serves as a barrier between the workpiece surface and metal ions.

Insufficient activation centers leads to deterioration of the quality of the coating by chemical metallization, and in some cases to mediocrity individual sections of the workpiece.

Finally, this method is only applicable for machining combined cermet surface.

The known method of chemical metallization parts of ferrites, ceramics and ferrite-ceramic, including sensitization in solutions of salts of tin, rinsing, activation in solution composition: palladium chloride 1,0-2,0 g/l; hydrochloric acid (ρ=1.19 g/cm3) - 1,0-2,0 ml/l at a temperature of 15-20°C for 5...7 min, drying at a temperature of 30...50°drying and subsequent metallization (see RF patent №2219284, CL IPC7SS 18/31, NC 3/18).

In the above method is superior adhesion between the treated surface and the metal due to the removal of water during the drying process after activation.

In addition, significantly reduced the harmful metallization process by eliminating machining before sensitization in the solution containing the substances of the group of amines.

However, the high content of palladium in the solution for activation leads to a significant appreciation of the metallization process.

All the other disadvantages of the previous method is inherent in him.

The way, the latest, is the closest technical solution to the technical nature for both versions.

Challenge, which is aimed by the invention, is to improve the quality of the coating by increasing the catalytic activity of the treated surface and reduce the content of palladium in the solution for activation.

The task in the first embodiment, the method is solved in such a way that in the known method of chemical metallization of surfaces, including sensitization, activation solution containing palladium chloride and hydrochloric acid, and the metal coating, before sensitization surface processes in adsorption stabilization solution based on compounds of silicon, aluminum, magnesium and fluoride (in terms of SiO2, Al2O3, MgO, HF) in the following ratio of components, g/l: SiO2- (35...45)×10sup> -3; Al2O3is (0.5...10)×10-3; MgO - (0,5...10)×10-3; HF - (0,5...1)×10-3; water - the rest.

In the first variant of the method of chemical metallization of the surface of the parts prior to operation sensitization details in sorption process stabilization solution based on compounds of silicon, aluminum, magnesium and fluoride (in terms of SiO2, Al2About3, MgO, HF) in the following ratio of components, g/l: SiO2- (35...45)×10-3; Al2O3is (0.5...10)×10-3; MgO - (0,5...10)×10-3; HF - (0,5...1)×10-3; water - the rest.

Machining of parts in sorptive stabilization solution based on compounds of silicon, aluminum, magnesium and fluoride promotes the formation of the surface film with ion exchange and recovery properties, ensuring a constant sorption of metals forming the activation centers.

Thus the resilience of the activation centers and direction of the reaction of chemical metallization towards formation on the surface of the workpiece metal rather than the oxide of the metal.

Formation on the surface of the workpiece a large number of activation centers, possessing regenerative ability, promotes the formation of uniform quality coating in the process the chemical metallization.

Fixing sorption activation centers on the surface of the workpiece can significantly reduce the concentration of expensive metal catalyst is palladium.

The increased metal content in the coating leads to an increase in the conductivity of the deposited coating.

The task in the second embodiment, the method is solved in such a way that in the known method of chemical metallization of surfaces, including sensitization, activation solution containing palladium chloride and hydrochloric acid, and the metal coating, as a solution for sensitization using sorptive stabilization solution based on compounds of silicon, aluminum, magnesium and fluoride (in terms of SiO2, Al2O3, MgO, HF) in the following ratio of components, g/l: SiO2(35...45)×10-3; Al2About3is (0.5...10)×10-3; MgO - (0,5...10)×10-3; HF - (0,5...1)×10-3; water - the rest.

All the advantages of the first variant of the method, and the second.

In addition, the creation of a large number of activation centers on the surface of the workpiece after processing its sorption solution allows to exclude from the solution for sensitization precariously employed salts of tin.

The method of chemical metallization surface, and parts in the first embodiment is as follows.

The party details in a quantity of 50 pieces with a surface of 5 cm2plastic ABS and 50 of printed circuit boards from foil fiberglass FS-35 with the surface 1 DM2and 70 holes from 1 to 2 mm was subjected to chemical magnesiu according to the method described in the patent of Russian Federation №2219284, and method for option 1 with the processing before the operation sensitization in sorptive stabilization solution based on compounds of silicon, aluminum, magnesium and fluoride (in terms of SiO2, Al2O3, MgO, HF).

The results of the processing of the workpiece surface after the chemical copper plating are shown in table 1.

Party details waveguides in quantities of 50 pieces with a surface area of 2 cm of titanium was subjected to chemical magnesiu according to the method described in the patent of Russian Federation №2219284, and method for option 1 with the processing before the operation sensitization in sorptive stabilization solution based on compounds of silicon, aluminum, magnesium and fluoride (in terms of SiO2, Al2About3, MgO, HF).

The results of the processing of the workpiece surface after the chemical copper plating are shown in table 2.

The party details in a quantity of 50 pieces with a surface of 5 cm2plastic ABS and 50 of printed circuit boards from foil fiberglass FS-35 with poverhnosti DM 2and 70 holes from 1 to 2 mm was subjected to chemical plating and chemical plating according to the method described in the patent of Russian Federation №2219284, and method for option 1 with the processing before the operation sensitization in sorptive stabilization solution composition: SiO2- 35×10-3g/l Al2About3- 0,5×10-3g/l MgO is 0.5×10-3g/l, HF - 0,5×10-3g/l, water - the rest.

Activation was carried out in solution composition: palladium chloride 10 mg/l and hydrochloric acid (ρ=1.19 g/cm3) 2 ml/l at 20°C for 3-4 minutes

The results of the processing of the workpiece surface after chemical Nickel plating and chemical silver plating are shown in table 3.

Party details waveguides in quantities of 50 pieces with a surface area of 2 cm2titanium was subjected to chemical plating and chemical plating according to the method described in the patent of Russian Federation №2219284, and method for option 1 with the processing before the operation sensitization in sorptive stabilization solution composition: SiO2- 35×10-3g/l Al2About3- 0,5×10-3g/l MgO is 0.5×10-3g/l, HF - 0,5×10-3g/l, water - the rest.

Activation was carried out in solution composition: palladium chloride 10 mg/l and hydrochloric acid (ρ=1.19 g/cm3) 2 ml/l at 120°C for 34 minutes

The results of the processing of the workpiece surface after chemical Nickel plating and chemical silver plating are shown in table 4.

Table 4
MaterialChemical Nickel platingChemical plating
the placeholderofferthe placeholderoffer
titaniumweak adhesionsufficient adhesion

floor 6 microns
weak adhesionsufficient adhesion

floor 4-5 microns

Thus, the details that are processed before sensitization in sorptive stabilization solution based on compounds of silicon, aluminum, magnesium and fluoride after metallization had a uniform thick coating. The quality of coverage has not changed after processing the 12th batch of parts in chemical madnani, 10 parts by chemical plating and 12 parts by chemical plating.

Significantly reduced in the operation of activating concentration of expensive metal catalyst is palladium.

The method of chemical metallization of the surfaces in the second embodiment is as follows.

Party on the hoist in the amount of 50 pieces with a surface of 5 cm 2plastic ABS and 50 of printed circuit boards from foil fiberglass FS-35 with the surface 1 DM2and 70 holes from 1 to 2 mm was subjected to chemical magnesiu according to the method described in the patent of Russian Federation №2219284, and the method according to option 2 with sensitization in sorptive stabilization solution based on compounds of silicon, aluminum, magnesium and fluoride (in terms of SiO2, Al2O3, MgQ, HF).

The results of the processing of the workpiece surface after the chemical copper plating are given in table 5.

Party details waveguides in quantities of 50 pieces with a surface area of 2 cm2titanium was subjected to chemical magnesiu according to the method described in the patent of Russian Federation №2219284, and the method according to option 2 with sensitization in sorptive stabilization solution based on compounds of silicon, aluminum, magnesium and fluoride (in terms of SiO2, Al2O3, MgO, HF).

The results of the processing of the workpiece surface after the chemical copper plating are shown in table 6.

Table 6
Material - titanium
prototype methodoffer
sensitization in the solution Sn2+- Sn4+sensitization in a solution of SiO2- 40×0 -3g/l Al2About3- 3×10-3g/l MgO - 4×10-3g/l, HF - 0,7×10-3g/l, water - the rest
rinse in cold running waterrinse in warm water
rinsing in distilled waterrinsing in distilled water
the activating solution consisting of: palladium chloride 1 g/l and hydrochloric acid (ρ=1.19 g/cm3) 1.5 ml/l at 117°C for 5...7 min, drying at 140°C until drythe activating solution consisting of: palladium chloride 10 mg/l and hydrochloric acid (ρ=1.19 g/cm3) 2 ml/l at 20°C for 3-4 min)
chemical copper platingchemical copper plating
there is no adhesionfloor pink (%Cu>CuO)
the thickness of the coating to 6 microns

The party details in a quantity of 50 pieces with a surface of 5 cm2plastic ABS and 50 of printed circuit boards from foil fiberglass FS-35 with the surface 1 DM2and 70 holes from 1 to 2 mm was subjected to chemical plating and chemical plating according to the method described in the patent of Russian Federation №2219284, and the method according to option 2 with sensitization in sorptive stabilization solution composition: SiO2- 40×10-3g/l Al2About3- 3&x000D7; 10-3g/l MgO - 4×10-3g/l, HF - 0,7×10-3g/l, water - the rest.

Activation was carried out in solution composition: palladium chloride 10 mg/l and hydrochloric acid (ρ=1.19 g/cm3) 2 ml/l at 20°C for 3-4 minutes

The results of the processing of the workpiece surface after chemical Nickel plating and chemical plating are shown in table 7.

Party details waveguides in quantities of 50 pieces with a surface area of 2 cm2titanium was subjected to chemical plating according to the method described in the patent of Russian Federation №2219284, and the method according to option 2 with sensitization in sorptive stabilization solution composition: SiO2- 40×10-3g/l Al2About3- 3×10-3g/l MgO - 4×10-3g/l, HF - 0,7×10-3g/l, water - the rest.

Activation was carried out in solution composition: palladium chloride 10 mg/l and hydrochloric acid (R=1.19 g/cm3) 2 ml/l at 20°C for 3-4 minutes

The results of the processing of the workpiece surface after chemical Nickel plating and chemical silver plating are shown in table 8.

Table 8
MaterialChemical Nickel platingChemical plating
prototip The inventive methodthe placeholderThe inventive method
titaniumweak adhesionsufficient adhesion

floor 6-9 microns
weak adhesionsufficient adhesion

floor - 3-4 microns

The details that are processed before activating in sorption solution based on compounds of silicon, aluminum, magnesium and fluoride, after metallization had a uniform thick coating. The quality of coverage has not changed after processing the 12th batch of parts in chemical madnani, 9th party details with chemical Nickel plating and after the 10th of parts for chemical plating.

Significantly reduced (up to 10 mg/l) concentration of expensive metal catalyst of palladium in the operation of the activation.

Machining of parts in a solution of the following composition allows to exclude from the solution for sensitization precariously employed salts of tin and a drying operation after activation, which leads to simplification of the process of metallization and to reduce its duration.

The proposed method also enables chemical metallizing the surface of electronegative metals, improving their technological properties.

The proposed method of chemical metallization of the surfaces allow you to plug the et to increase the efficiency of the systems sensitization and activation and to obtain high-quality thick coating by chemical means.

1. The method of chemical metallization of surfaces, including sensitization, activation solution containing palladium chloride and hydrochloric acid, and the metal coating, characterized in that prior sensitization of the workpiece surface processes in adsorption stabilization solution based on compounds of silicon, aluminum, magnesium and fluorine in terms of SiO2, Al2About3, MgO, HF in the following ratio of components, g/l: SiO2- (35-45)·10-3, Al2About3is (0.5-10)·10-3, MgO - (0.5 to 10)·10-3, HF - (0.5 to 1)·10-3water - the rest.

2. The method of chemical metallization of surfaces, including sensitization, activation solution containing palladium chloride and hydrochloric acid, and the metal coating, characterized in that as a solution for sensitization using sorptive stabilization solution based on compounds of silicon, aluminum, magnesium and fluorine in terms of SiO2, Al2About3, MgO, HF in the following ratio of components, g/l: SiO2- (35-45)·10-3, Al2About3is (0.5-10)·10-3, MgO - (0.5 to 10)·10-3, HF - (0.5 to 1)·10-3water - the rest.



 

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EFFECT: improved plating quality ensured with higher catalytic activity of processed surface and reduced palladium content in solution for activation.

2 cl, 8 tbl, 8 ex

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