SU1010157A1 - Solution for activating surface of materials before chemical metallization (modifications) - Google Patents

Abstract

1. A solution for activating the surface of materials prior to chemical metallization, containing sodium borohydride and a solvent, characterized in that, for the purpose of washing. In addition, it contains phthalamide, which enhances the catalytic effect of sodium borohydride, and dimethylformamide as a solvent in the following ratio of components: Borohydride4-15. Phthalamide, g 0.05-1.5 Dimethylformamide, l Up to 1 2. Solution for activating the surface of materials before chemical metallization, containing sodium borohydride and solvent, about 1 and 2; y and so that, in order to increase its stability, the solution additionally contains hexachloroethane which enhances the catalytic action of sodium borohydride, and the solvent is a monohydric alcohol selected from the group comprising ethyl, propyl, butyl, isopropyl alcohol, isobutyl alcohol or their mixture , in the following ratio of components: Sodium borohydride, g 0.5-5.0. Hexachloroethane, f 0.1-1.0 A monohydric alcohol selected from the group consisting of ethyl, propyl, butyl, CO isoproyl, isobutyl alcohols or their mixture, l. Up to 1 3. Solution for activation of surface materials prior to chemical metallization, containing sodium borohydride, alkali metal hydroxide and water as a solvent, in that, to increase its stability, the solution additionally contains phenolphthalein, which enhances the catalytic effect of borohydride sodium, and diQ1 methylformamide as an additional solvent at the following ratio of components:. Sodium borohydride, g; 4-15 Alkali metal hydroxide, g 4-8 Phenolphthalein, g0.25-1.5 Dimethylformamide, ml400-700 Water, lUd 1 4. Solution for surface activation of materials before chemical metallization, containing sodium borohydride, alkali metal hydroxide and solvent

Description

water, characterized in that, in order to increase its stability, the solution additionally contains diacetyl, enhancing the catalytic action of sodium borohydride, and a monohydric alcohol selected from the group including ethyl, propyl, butyl, isopropyl, isobutyl alcohols or their mixture, as an additional solvent in the following ratio of components:

Sodium borohydride Alkali metal hydroxide, g Diacetyl, g. Monohydric alcohol selected from the group including ethyl propyl, butyl, isopropyl, isobutyl alcohols or their mixture, ml Water, l

The invention relates to the metallization of materials, in particular to races. It can be used for chemical copper plating or nickel plating of plastic ceramic and graphite products, polymer films and fibrous materials, catalytic inactive metals. Solutions are known for preparing the surface of materials containing ions of catalytically active metals (Hell, Pd, Au, Pt, etc.) or their complex compounds with S (I) 1. However, the use of these solutions due to the use of scarce and expensive precious metals is not economically feasible. Known solutions containing io base metals (Cu, Ni, Co, Fe) and other components, as well. namely, promoter catalysts (compounds, Ca, Cr, Sr, etc.) 2. These solutions are complex in composition, some of them do not exclude preliminary sensitization in tin solutions. Processing in such solutions requires further processing in solutions of reducing agents. Disposal of used solvents is difficult. In industry, such preparation solutions are not widely used, since they are not acceptable for various non-metallic materials and give unstable results. It is known to use solutions of strong reducing agents for initiating the autocatalytic reaction of chemical reduction of metals. For this purpose, a solution of the product of the reaction of white phosphorus with a nucleophilic compound or with an organometallic compound H is used. Such preparation solutions are not widely used due to the fact that white phosphorus is highly poisonous and self-ignites. The closest in composition and technical essence to the invention is an aqueous solution of sodium borohydride and alkali metal hydroxide 4. The disadvantages of the prototype are the low stability of the activation solution, since the solution decomposes within a few hours. The aim of the invention is to increase the stability of the solution for activating the surface of materials prior to chemical metallization. This goal is achieved in that the solution is to activate the surface of the materials before the chemical. metallization, containing sodium borohydride and water as a solvent, additionally contains phthalimide, which enhances the catalytic action of sodium borohydride, and dimethylformamide as a solvent in the following ratio of sodium borohydride components, 4-15 phthalamide, g, 0.05-1.5 dimethylformamide, l To 1 According to the second variant of the solution as a substance that enhances. the catalytic effect of sodium borohydride contains hexachloroethane, and the solvent is a monohydric alcohol selected from the group consisting of ethyl, propyl, butyl, isopropyl, isobutyl alcohols or their mixture, with the following ratio of components: Sodium borohydride, g 0.5-5.0 Hexachloroethane, g. O, Monohydric alcohol selected from the group including propyl alcohol, butyl alcohol, isopropyl alcohol, isobutyl alcohol or their mixture, l Up to 1

According to the third variant, the solvent contains phenolphthalein as a substance that enhances the catalytic action of sodium borohydride, and the solvent is a mixture of water and dimethylformamide, which, as usual, the solvent containing water stabilizes with alkali metal oxide in the following ratio components: Sodium borohydride, g 4.0-15.0 Alkali metal hydroxide, 4.0-8.0 g Phenolphthalein, g 0.25-1.5 Dimethylformamide, ml400.0-700.0

Water ldo 1

According to the fourth variant, the solution contains diacetyl as a substance that enhances the catalytic action of sodium borohydride, and a mixture of water and a monohydric alcohol selected from the group consisting of ethyl, propyl, butyl, isopropyl, isobutyl alcohols or their mixture, and usually, the solvent containing water is stabilized with alkali metal hydroxide in the following ratio of components:

Sodium borohydride, g 2.5-10.0 Alkali metal hydroxide, g. 4.0-8.0 Diacetyl, g0.01-0.1

Monohydroxy alcohol selected from the group comprising ethyl, propyl,. butyl, isopropyl, isobutyl alcohols or

their mixture, ml 500.0-900, Water, ldo 1

The first version of the proposed solution for the activation of the surface of the materials before chemical metallization is intended for the treatment of copper, graphite, glass cloth, glass, alkali-resistant paper. The induction period during metallization is 10–30 s, the stability of the solution, the operating time before decomposition is 31 days.

The second variant of the proposed solution for the activation of the surface of the materials before chemical metallization is intended for the treatment of copper, graphite, fiberglass, impact polystyrene, ABC plastic. 2020, sitalla, alkali-resistant paper. Induction period with metallization 10-60 s, solution stability 10 days. When the solution is cooled to 10-13 ° C after hours, its service life increases to 16–20 days.

The third variant of the invented solution for activating the surface of materials before chemical metallization is intended for the treatment of copper, graphite, fiberglass, plastic ABC 2020, and cellars. Induction period with metallization 10-70 s, solution stability 10 days. When the solution is cooled to 10–13 s after hours, its service life increases to 20 days.

The fourth variant of the invented 0 solution for the activation of the surface of materials before chemical metallization is intended for the treatment of copper, graphite, glass cloth, sitall, plastic ABC 2020, alkali resistant 5 bamagi.

Induction period with metallization 5-60 s, solution stability 10 days. When the solution is cooled to J.O-13 ° C after hours, its service life increases to 20 days.

The efficiency of the variants of the proposed solution can be illustrated by the data presented in the table.

5 in 1 liter of solution for the activation process a batch of powder of Taiga graphite. After all batches of graphite are nickel-plated, nickel is uniformly coated with all the particles of the powder.

0

All solutions can be adjusted as far as the production and ablation of sodium borohydride and a substance that enhances its catalytic action is selected, selected from the group phthalimide, hexachloroethane, phenolphthalein and diacetyl. In this case, both components are introduced directly into the solution.

Analysis of the content of the main components of the solution is carried out according to known methods.

Waste solutions can be regenerated by distillation. Purified alcohols or dimethylformamide can be reused for preparing the working solution.

It is recommended to periodically (once a day) filter the working solution to separate foreign particles introduced into the detail solution. Q The lower limits of the concentrations of the components of the solution variants for the activation of the surface of materials before chemical metallization ensure high quality of the metallization. depending on the composition of the solution variant and the material to be coated, and exceeding the upper limits of the concentrations of the components of the solution variants is not economically feasible. . The working temperature of the solution for activation is room temperature. The practical application of the solution for the activation of the surface of materials before chemical metallization of its variants can be illustrated by the following 5 examples in which the preparation of the surface of the activated material does not differ from the generally accepted technology. Option 1. Example. A sample of copper foil is treated with 10 s in 1 liter of dimethylformamide containing 4, O g / l of MaHlc and 0.05 g / l of phthalamide, and then immersed in a solution of chemical nickel plating. Nickel coating results in a solid, compact glitter sh. PRI mme R 2. A degreased and dried sample of glass cloth T 40-KEP is processed for 45 s in 1 liter of drmethylformamide containing 5.5 g / l of NpBH and 0.05 g / l of phthalamide, and then metallized in an ammonia solution nickel plating. The precipitate of nickel is solid, bright, brilliant. Froze Sitallov plastics is processed 30 s in 1, l dimethyl formamide containing 8.0 g / l Hi 1.5 g / l phthalimide. Then the sample is placed in a glycerin H1eni honey solution. The copper precipitate on the plate is single-colored, semi-bright Rome. 4. A sample of alkali resistant paper is placed for 15 seconds in 1 liter of dimethylformamide containing 1; 5 g / liter of 1 g / l phthalamide, and then metallized in triethanolamine solution nickel plating. The sample is covered with a semi-bright solid layer of nickel, all the fibers are alkali: the epoxy of paper is covered with metal. Option I. Example. A sample of glass cloth is degreased, washed with water, dried and processed for 30 seconds with sodium borohydride solution (1.5 g / l in 1 liter of propyl alcohol with 0.1 g / l of hexachloroethane added and immersed in the nickel plating solution. After 15 minutes, the sample covered with a compact, bright, shiny nickel deposit. EXAMPLE 2 Samples of high impact polystyrene after degreasing, pickling and drying are processed for 45 seconds in a solution of sodium hydride (1.5 g / l) in ethyl alcohol with 0.5 g / l of hexachloroethane and is metallized in ammonium triethano a Nickel plating. Solid nickel precipitate, light, lubly-blue I. Example 3. The products from ABC 2020, after degreasing, pickling and drying, are processed with sodium borohydride solution (4.0 g / l) in isopropyl alcohol with hexachloroethane (0.3 g / l) and metalized in a glycerol mediating solution. Copper is deposited as a compact semi-glossy coating. EXAMPLE 4 Alkali-resistant paper sample is degreased, washed, dried and processed in 46 seconds ethyl isopropyl alcohol (1: 1) containing 0.5 g / l of borohydride per three and g / l of hexachloroethane, and then placed in an ammoniacal nickel plating solution. The coating is of high quality: all paper fibers are covered with a continuous sediment of light, semi-glossy nickel. Example 5. A sitallov plate is treated for 30 s in 1 liter of a mixture of propyl-isopropyl (l: l) alcohols containing 5.0 g / l of sodium borohydride and 0.5 g / l of hexachloroethane and placed in a copper plating solution. The copper precipitate on the plate is compact, semi-glossy, pink in color. Example b. A sample of copper foil is processed 15 s in 1 liter of isobutyl alcohol containing 1.5 g / l sodium borohydride and 0.5 g / l hexachloroethane, and then immersed in a solution of chemical nickel plating. The sample is coated with a compact, bright, bright nickel. Option. Example. A defatted glass fiber sample is processed at room temperature for 40 seconds in a solution containing 4 g / l NaBH4, 0.25 g / l phenolphthalein, 8 g / l NaOH and 400 ml / l dimethylformamide and water to l, and then placed in an ammonia solution chemical nickel plating. After 15 minutes, the fiberglass sample is covered with a solid, compact, bright, shiny nickel deposit. EXAMPLE 2. A plate from ABC 2020, after degreasing and etching, is placed for 45 seconds in a solution containing 8 g / l NaBH4, 0.5 g / l phenolphthalein, 4 g / l NaOH, 500 ml / l dimethylformamide and water up to 1 l. The treatment is carried out at room temperature. After treatment in the injected solution, the sample is chemically nickelized. Nickel precipitate is compact, light, semi-bright. EXAMPLE 3 A sample of a sieve after degreasing and pickling is processed at room temperature for 60 seconds in a solution containing 15 g / l of NaBH4, 1.0 g / l of phenolphthalein, 6 g / l of KOH, 700 ml / l dimethylformamide and water up to 1 l, and then placed in a solution of chemical copper. The precipitate of copper on the sitall sample is obtained in a compact, light, semi-glossy, pink color. EXAMPLE 4 A sample of copper foil is treated for 10 s in a solution containing 5 g / l NaOH, 600 ml / l dimethylformamide, 4 g / l NaBH /, IfEf g / l phenolphthalein and water to 1 l. Then the sample. immersed in a chemical nickel plating solution. A compact, bright, shiny nickel is deposited on the sample. Option l3. Example 1. A sample of glass T-40-ZOP after degreasing is processed 45 seconds in 1 liter of a mixture of water and isopropyl alcohol (1: 1) containing 4.0 g / l of NaOH, 2.5 g / l of NaBH and 1 g / l diacetyl. The sample is then nickel plated with an alkaline solution. After 10 minutes, the sample is covered with a continuous layer of semi-bright nickel. Example 2. A sample of a sieve after degreasing and etching is treated for 1.5 minutes in 1 liter of a mixture of ethyl alcohol and water (1: 1), in which 7.5 g / l of NaBH, 8 g / l of NaOH and 0.01 are dissolved g / l diacetyl. The sample is then coated with copper in a glycerin solution. The copper precipitate is compact, glossy, pink in color. Example 3. Fat-free and pickled products from ABS 2020 are placed 60 v in 1 liter of a mixture of water - isopropyl alcohol - propyl alcohol (1: 5: 4, containing 6 g / l KOH, 10 g / l NaBH and 0.5 g / After this, the samples are coated with nickel in an ammonia solution. The precipitates of nickel on ABS plastic are compact, light, semi-bright. Example 4. A sample of alkali resistant paper is degreased for 3 minutes in 1 liter of water-isobutyl alcohol (1: 4) with 4 g / l NaBH4 5.5 g / l NaOH and 0.03 g /

1. Sodium borohydride, g 6 Phthalamide, g 0.75 Dimethylformamide, l To 1

Sodium borohydride, g 2,5 Hexachloroethane, g Oh, 5

Isopropyl blend

and ethyl alcohol (1: 1),

l to 1

7,000

7500 diacetyl, and then coated with copper in a glycerol solution of copper. After 10 minutes, the sample is covered with an even layer of compact copper. Example 5. A sample of copper foil is treated 15 seconds in 1 liter, a solution containing 2.5 g / l NaBH, 0.02 g / l diacetyl, 7.0 g / l KOH, the rest is a mixture of isobutyl alcohol and water (ratio: 9: 1), but for--, he is immersed in a solution of chemical nickel plating. Nickel plating is continuous, compact, sterile and shiny. The adhesion strength of metallized materials with pre-activation of the surface in the proposed solution variants is evaluated by the methods of multiple bending. a MIRP machine, peeling off a strip of coating on a PM-30-1 tensile machine, thermal shock (3 cycles of abrupt temperature change) and manually bending it several times at an angle of leo. The test shows that the coupling of copper and nickel with the substrate activated by the proposed invention is not inferior to the adhesion of copper and nickel to the substrate, processed according to the traditional technology, which includes sensitization and activation operations in known solutions. The proposed solutions can be driven at enterprises of all industries using the metallization of dielectrics and other catalytic inactive materials. The annual economic effect is 349394 r. (I solution), 353157 p. (17 option), 346882 p. (iTj option), 351335 p. ( (Option 2).

Sodium borohydride, g 4 Hydroxide.cali, g 6 Phenolphthalein, g 0.75 Dimethylformamide, ml 500 Water, l Up to 1

Sodium borohydride, g 2.5 Potassium hydroxide, g 8 Diacetyl, g 0.07

Isopropyl alcohol, 700 ml

Water, l To 1

101015710

Table continuation

8,000

1000

Claims (4)

1. A solution for activating the surface of materials before chemical metallization, containing sodium borohydride and a solvent, characterized in that, in order to increase its stability, the solution additionally contains phthalamide, enhancing the catalytic effect of sodium borohydride, and dimethylformamide as a solvent in the following ratio of components : Borohydride 4-15 Phthalamide, g 0.05-1.5 Dimethylformamide, l To 1 2.5-10.0 2. A solution for activating the surface of materials before chemical metallization, containing sodium borohydride and a solvent, characterized in that, in order to increase its stability, the solution additionally contains hexachloroethane, enhancing the catalytic effect of sodium borohydride, and as a solvent is a monoatomic ', an alcohol selected from the group comprising ethyl, propyl, butyl, isopropyl, isobutyl alcohols or their mixture, in the following ratio of components: Sodium borohydride, g 0.5-5.0 Hexachloroethane, g 0.1-1.0 Monohydric alcohol selected from the group consisting of ethyl, propyl, butyl, isopropyl, isobutyl alcohols or a mixture thereof, l Up to 1 3. A solution for activating the surface of materials before chemical metallization, containing sodium borohydride, alkali metal hydroxide and water as a solvent, characterized in that, in order to increase its stability, the solution additionally contains phenolphthalein, enhancing the catalytic effect of sodium borohydride, and dimethylformamide as additional solvent in the following ratio of components: SU,.,. 1010157 Sodium borohydride, Alkali metal hydroxide, g Phenolphthalein, g Dimethylformamide, ml Water, l I) 4-15 4-8 0.25-1.5 400-700 Up to 1 _; 4. A solution for activating the surface of materials before chemical metallization, containing sodium borohydride, an alkali metal hydroxide and water as a solvent, characterized in that, in order to increase its stability, the solution further comprises diacetyl, enhancing the catalytic effect of sodium borohydride, and monohydric alcohol, selected from the group including ethyl, propyl, butyl, isopropyl, isobutyl alcohols or a mixture thereof, as an additional solvent in the following ratio of components : Sodium borohydride, Alkali metal hydroxide, g Diacetyl, g. Monohydric alcohol selected from the group consisting of ethyl, propyl, butyl, and zopropyl, isobutyl alcohols or a mixture thereof, ml Water, l 4-8 0.01-0.1 .500-900 Up to 1