KR101591973B1 - Method for plating electroless of activated carbon - Google Patents

Abstract

The present invention relates to a method of electroless plating of activated carbon, comprising the steps of: (A) filling activated carbon, which is an object to be plated, with a coating liquid; (B) a caustic alkali etching step of corroding the surface of the activated carbon so as to enhance the adhesion of the activated carbon filled with the coating liquid; (C) attaching tin (Sn) to the activated carbon that has been etched through the step (B); (D) attaching palladium (Pd) to the activated carbon to which the first catalyst is applied; (E) an electroless copper (Cu) strike step in which the second catalyst forms a metal coating on the surface of the activated carbon to which the second catalyst is applied; (F) an electroless copper plating thickness adjusting step of forming copper plating on the coating film formed on the surface of activated carbon through the electroless copper (Cu) strike to a uniform thickness; (G) an electroless nickel (Ni) plating step of forming a nickel metal film on the activated carbon through the electroless copper plating thickness control step, and (H) a step of performing a heat treatment for the high strength of the activated carbon subjected to the electroless nickel , The microporosity formed on the activated carbon is coated and the electroless plating is performed so that the manufacturing cost can be remarkably lowered compared with the existing coated activated carbon while maintaining the inherent function of the activated carbon.

Description

METHOD FOR PLATING ELECTROLESS OF ACTIVATED CARBON FIELD OF THE INVENTION [0001]

The present invention relates to a method of electroless plating of activated carbon, and more particularly, to a method of electroless plating of activated carbon, which comprises coating a microporous material formed on a material such as activated carbon and performing electroless plating to maintain the inherent function of the activated carbon, The present invention relates to a method for electroless plating of activated carbon,

In general, activated carbon is composed of carbonaceous, strong adsorption, and is made by coating wood, lignite and peat with chemicals such as zinc chloride or phosphoric acid, which are activators, or by activating charcoal with water vapor.

Since activated carbon has excellent adsorption characteristics due to a microporous structure, it has been widely used for purification, deodorization (deodorization), filtration, dustproofing, food purification, etc., and technology for performing surface treatment of functional materials by using the activated carbon has been developed come.

On the other hand, since microorganisms such as bacteria among pollutants adsorbed on the microporosity of activated carbon can make the activated carbon itself a secondary pollutant source, recently researches that can perform antibacterial treatment by coating activated carbon with a substance such as silver are active .

For example, a coated activated carbon according to the prior art is disclosed in Korean Patent Laid-open Publication No. 10-2010-0086906 (hereinafter referred to as Document 1) and Patent Registration No. 10-1007435 (hereinafter referred to as Document 2) Lt; / RTI >

That is, the above document 1 includes the activated carbon and the activated carbon fixing member coated with the silver nanoparticles, respectively, so that the adsorbing function of the activated carbon and the sterilizing function of the silver nanoparticles enable the decomposition of the source causing the odor and the sterilization of microorganisms such as bacteria and spores And it is possible to prevent secondary contamination.

Also, the above-mentioned document 2 includes activated carbon particles coated with a water-insoluble coating material effective for shielding the color of activated carbon particles, and the coating material includes a water-insoluble binder effective for binding a shielding agent to a shielding agent and activated carbon particles, Wherein the coating is porous and has an additional level of 5% or more relative to the uncoated activated carbon, wherein the coated activated carbon particles are selected from the group comprising ammonia, triethylamine, trimethylamine, dimethyl disulfide, and isovaleric acid Discloses a coated activated carbon having a relative adsorption efficiency of at least 30% for at least one odorous substance.

Document 1: Japanese Patent Application Laid-Open No. 10-2010-0086906 (entitled: Air Filter Using Activated Carbon Coated With Silver Nanoparticles, Published Date: Aug. 02, 2010) Document 2: Patent Registration No. 10-1007435 (name: coated activated carbon, registered on January 04, 2011)

However, in the prior arts such as the above documents 1 and 2, because of the microporous nature of the activated carbon, plating is difficult and the coating is performed on the outside of the activated carbon for antibacterial action. This not only reduces the function of the activated carbon, There is a problem that the manufacturing cost of the semiconductor device increases.

SUMMARY OF THE INVENTION Accordingly, the present invention has been made to solve the above-mentioned problems occurring in the prior art, and it is an object of the present invention to provide a method and apparatus for coating a microporous material such as activated carbon with electroless plating, The present invention provides an electroless plating method for activated carbon which can significantly reduce the manufacturing cost compared to the existing coated activated carbon.

These and other objects of the present invention will be apparent to those skilled in the art without departing from the scope of the present invention by the appended claims.

According to another aspect of the present invention, there is provided an electroless plating method for activated carbon, comprising the steps of: (A) charging activated carbon, which is an object to be plated, with a coating liquid, wherein the coating liquid contains thioacetal compounds 3-5 By weight of a non-ionic surfactant, 5 to 10 parts by weight of a nonionic surfactant, and 85 to 90 parts by weight of pure water, dissolved in distilled water; (B) a caustic alkali etching step of corroding the surface of the activated carbon so as to enhance the adhesion of the activated carbon filled with the coating liquid; (C) attaching tin (Sn) to the activated carbon that has been etched through the step (B); (D) attaching palladium (Pd) to the activated carbon to which the first catalyst is applied; (E) an electroless copper (Cu) strike step of forming a metal coating on the surface of the activated carbon to which the second catalyst is applied; (F) an electroless copper plating thickness adjusting step of forming copper plating on the coating film formed on the surface of activated carbon through the electroless copper (Cu) strike to a uniform thickness; (G) an electroless nickel (Ni) plating step of forming a nickel metal film on the activated carbon through the electroless copper plating thickness control step, and (H) a step of performing a heat treatment for the high strength of the activated carbon subjected to the electroless nickel The drying step.

Preferably, (F2) between the steps (F) and (G), the activated carbon subjected to the electroless copper plating thickness control step is coated with 800 to 900 ml of pure water so that the electroless nickel / L in which 50-100 ml / L of an ion type catalyst-imparting agent is mixed and 50-100 ml / L of hydrochloric acid is mixed with water.

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The activated carbon in the step (C) is added to a solution of 8-12 g / L tin (SnCl ₂ ) and 8-12 ml / L hydrochloric acid (HCl) at 25-30 ° C for 3-5 minutes It is preferable to wash with water after immersion.

In the step (G), 15-30 parts by weight of nickel sulfate, 1-10 parts by weight of a stabilizer, and 10 parts by weight of a stabilizer are added to the activated carbon in the presence of pure water or ion exchange water 750-780 ml / 1 to 10 parts by weight of ammonia, 8 to 15 parts by weight of hypophosphite, 8 to 15 parts by weight of a stabilizer, and 70 to 80 parts by weight of a pure water of 70 to 80 parts by weight of a first electroless nickel plating solution consisting of 55 to 60 ml / By weight of a second electroless nickel plating solution consisting of 140 to 150 ml / L of water.

According to the electroless plating method of the activated carbon according to the present invention, the microporosity formed on the activated carbon is coated and the electroless plating is performed, so that the manufacturing cost is significantly lower than that of the existing coated activated carbon while maintaining the inherent function of the activated carbon .

Additional features and advantages of the present invention will become more apparent from the following description.

1 is a flowchart showing an electroless plating method of activated carbon according to the present invention.
2 is a photograph showing activated carbon produced by the electroless plating method of activated carbon according to the present invention.
FIG. 3 is a photograph showing a cross-section of an activated carbon prepared by an electroless plating method of activated carbon according to the present invention. FIG.

Hereinafter, an electroless plating method of activated carbon according to a preferred embodiment of the present invention will be described in detail with reference to the accompanying drawings.

In the present specification, the following embodiments are to be considered as illustrative and not restrictive, and the invention is not to be limited to the details given herein but is to be construed as being altered and substituted in other equivalents within the scope and equivalents of the appended claims. .

FIG. 2 is a photograph showing the activated carbon produced by the electroless plating method of the activated carbon according to the present invention, FIG. 3 is a graph showing the results of the electroless plating of the activated carbon according to the present invention, 3 is a photograph showing a cross section of activated carbon produced by an electroless plating method.

<First Step>

First, the activated carbon which is the object to be plated having a microporous structure is filled with the coating liquid (S110).

That is, the first step is a coating treatment step for preventing contamination of the post-process plating solution due to the liquid penetrated in the previous step and making the environment so that electroless plating can be easily performed.

At this time, the activated carbon, which is the object to be plated, is dipped in the coating liquid at a temperature of 30 to 40 ° C for about 30 to 60 seconds and then washed. The coating liquid is prepared by dissolving the coating material in a concentration of 8 to 10% by weight in distilled water.

Here, the coating agent is composed of 3 to 5 parts by weight of a thioacetal compound, 5 to 10 parts by weight of a nonionic surfactant, and 85 to 90 parts by weight of pure water.

<Second Step>

Next, caustic alkali etching is performed on the activated carbon filled with the coating liquid through the first step (S120).

That is, in the second step, the surface of the activated carbon is corroded to improve the adhesion of the activated carbon, which is the object to be plated, so that the tannin component sticking to the activated carbon is removed rather than the debris is formed deeper on the microporous surface of the activated carbon Activating the surface of activated carbon so that electroless plating can be performed well.

At this time, the activated carbon filled with the coating liquid is washed with a caustic alkali etchant having a temperature of 50 to 60 ° C for 10 to 20 seconds and then washed with water. The caustic alkaline etchant is prepared by dissolving 50 to 60 g / l of strong alkaline caustic soda in distilled water .

<Step 3>

Next, a first catalyst providing step of uniformly attaching tin (Sn), which is a fine particle of a catalyst metal, to the activated carbon is performed through the second step (S130).

That is, the third step is a step of immobilizing the activated carbon, which is the object to be plated, with tin chloride (SnCl ₂ ) or the like to perform the bridge function of activating the palladium catalyst.

At this time, the activated carbon subjected to the etching is washed with water after immersing in a first catalyst solution having a temperature of 25 to 30 ° C for 3 to 5 minutes, wherein the first catalyst solution contains 8 to 12 g / L of tin (SnCl ₂ ) (HCl) in an amount of 8 to 12 ml / L.

<Step 4>

Next, a second catalyst providing step of attaching palladium (Pd), which is catalyst fine particles, to the activated carbon to which the first catalyst is applied is performed through the third step (S140).

That is, the fourth step is a step of immersing activated carbon, which is an object to be plated, with palladium chloride (PdCl ₂ ) or the like to serve as a growth nucleus of a plating metal to serve as a reaction initiation catalyst. At this time, seeded palladium ).

At this time, the activated carbon to which the first catalyst is applied is washed with water after immersing in a second catalyst solution at a temperature of 30 to 35 ° C for 3 to 5 minutes. The second catalyst solution is 0.3 to 0.5 g / L of palladium chloride (PdCl ₂ ) And 2 to 4 ml / L of hydrochloric acid (HCl).

In the fourth step, if the water washing is inadequate, the electroless copper plating solution is contaminated by the second catalyst solution and causes decomposition due to a chemical reaction. In the case where the water washing is excessive, the activated palladium fine particles are dissolved in water It is necessary to wash it properly.

<Step 5>

Next, an electroless copper (Cu) strike step of forming a metal coating on the surface of the activated carbon to which the second catalyst is applied is performed through the fourth step (S150).

That is, the electroless copper strike step forms a metal coating on the surface of the activated carbon by reducing and precipitating metal ions with a reducing agent in the plating solution by the action of the activated palladium catalyst.

At this time, the activated carbon to which the second catalyst is applied is washed with water after immersion for 10 to 20 minutes in a treatment solution at a temperature of 40 to 45 ° C. The treating solution in the step of electroless dynamical strike is pure water at 750 to 780 ml / L of alkaline supplement, 70 to 90 ml / L of complexing agent, 50 to 80 ml / L of complexing agent and 2 to 4 ml / L of stabilizer.

Herein, the copper-plating bath and the supplements are mixed with 6 to 12 parts by weight of copper sulfate, 5 to 7 parts by weight of formaldehyde (HCHO), 1 to 1.5 parts by weight of polyethylene glycol, 0.01 to 0.02 part by weight of stabilizer, 78 to 80 parts by weight.

The alkali supplement is composed of 35 to 45 parts by weight of sodium hydroxide (NaOH), 0.01 to 0.02 parts by weight of stabilizer, and 50 to 60 parts by weight of pure water.

The complexing agent is composed of 20-25 parts by weight of edetate (EDTA-4Na), 0.01-0.02 parts by weight of stabilizer, and 75-80 parts by weight of pure water.

The stabilizer is composed of 3 to 5 parts by weight of potassium cyanide, 5 to 10 parts by weight of sodium hydroxide (NaOH) and 85 to 90 parts by weight of pure water.

<Step 6>

Next, an electroless copper plating thickness adjusting step of forming a copper plating uniform thickness on a coating film formed on the surface of the activated carbon through the electroless copper (Cu) strike of the fifth step is performed (S160).

At this time, the activated carbon subjected to the electroless copper strike is washed with water after immersion for 10 to 20 minutes at a precipitation rate of 0.5 to 0.7 탆 in a treatment liquid at a temperature of 45 to 55 캜, and the treatment in the electroless copper plating thickness control step L, formaldehyde (HCHO) 8, stabilizers (HCHO) 8 and stabilizers were added to pure water 850-860 ml / L, 55-65 ml / L copper bath and supplements, 55-65 ml / To 10 ml / L in that order.

Here, the co-bathing and supplementing agent is composed of 6 to 12 parts by weight of copper sulfate, 1 to 1.5 parts by weight of polyethylene glycol, 0.01 to 0.02 parts by weight of stabilizer, and 78 to 80 parts by weight of pure water.

The alkali supplement is composed of 35 to 45 parts by weight of sodium hydroxide (NaOH), 0.01 to 0.02 parts by weight of stabilizer, and 50 to 60 parts by weight of pure water.

The complexing agent is composed of 44 to 50 parts by weight of sodium hydroxide (NaOH), 0.01 to 0.02 parts by weight of stabilizer, and 50 to 55 parts by weight of pure water.

The stabilizer is composed of 0.2 to 0.3 parts by weight of potassium selenocyanate and 90 to 95 parts by weight of pure water.

Meanwhile, the step of filling the activated carbon of the first step with the coating liquid, the electrified copper (Cu) strike step of the fifth step, and the electroless copper plating thickness controlling step of the sixth step may be performed by barrel plating It is desirable to perform stirring and filtration in real time through low pressure air and to analyze components every hour for 30 minutes through the analyzer to supplement the components for the insufficient treatment liquid.

<Step 7>

Meanwhile, in order to allow the electroless nickel (Ni) plating to adhere securely and stably between the electroless copper plating thickness control step of the sixth step and the electroless nickel (Ni) plating step described later, In the treatment liquid composed of 50-100 ml / L of hydrochloric acid mixed with 50-100 ml / L of ion-type catalyst additive, 800-300 ml / Followed by immersing in water at 35 DEG C for about 3-5 minutes, followed by washing with water (S170).

That is, in the catalyst activation step of the seventh step, 90 to 95 parts by weight of a mixture of pure water and a catalyst-imparting agent is mixed with 5 to 10 parts by weight of hydrochloric acid. It is preferable to add a catalyst-imparting treatment solution for electroless plating while heating weakly, and to use a hot water or a steam coil for heating the treatment solution.

<Step 8>

Subsequently, an electroless nickel (Ni) plating step for forming a nickel metal film for corrosion resistance on the activated carbon through the electroless copper plating thickness control step of the sixth step or the catalyst activation step of the seventh step is performed (S180).

At this time, the treated solution in the electroless nickel plating step is prepared by mixing the first electroless nickel plating solution 55 to 60 ml / L and the second electroless nickel plating solution 75 to 780 ml / And a plating solution of 140 to 150 ml / L.

The first electroless nickel plating solution is composed of 15-30 parts by weight of nickel sulfate, 1-10 parts by weight of stabilizer, and 70-80 parts by weight of pure water, and the second electroless nickel plating solution is composed of ammonia 1 8 to 15 parts by weight of a hypophosphite, 8 to 15 parts by weight of a stabilizer and 70 to 80 parts by weight of pure water.

Thereafter, the treatment liquid was adjusted to a temperature of 57 to 80 캜 (preferably 65 캜), a pH of 5.5 to 6.0 and a metal nickel concentration of 5.0 to 6.0 g / L (preferably, 5.8 g / L) Followed by washing with water.

At this time, it is preferable to use a tank made of polypropylene, FRP or Teflon, or a metal tank coated with these materials or a tank made of stainless steel, in order to immerse the activated carbon which is the object to be plated.

In addition, the first and second electroless nickel plating solutions are low-temperature liquids suitable for LDS and can be used for a long time by continuous supply, have excellent bath stability, and are easy to manage the bath.

When the electroless nickel plating solution is subjected to a humidifying operation, the precipitation rate is preferably set to 5 to 6 탆 / hr so that smoothness due to low stress is excellent, and the phosphorus flow rate is preferably 3 to 6 parts by weight.

<Step 9>

Thereafter, the active carbon subjected to the electroless nickel (Ni) plating step of the eighth step is subjected to heat treatment in order to increase the strength and improve reliability (S190).

At this time, the activated carbon subjected to the eighth step is dried at a temperature of 60 to 65 ° C for 55 to 65 minutes through a hot air drier, and then packed and shipped.

Therefore, according to the first through ninth steps, the microporous structure formed on the activated carbon, which is the object to be cast, is coated and the electroless plating is performed, the manufacturing cost can be remarkably lowered compared to the conventional coated activated carbon. The activated carbon produced can be supplied at a low cost.

While the present invention has been described in connection with what is presently considered to be practical exemplary embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, Of course.

In other words, various numerical values applied to the preferred embodiments of the present invention described above are merely examples, and variations of various conditions, thicknesses, and contents may be possible.

Claims (8)

1. A method of electroless plating an electroslag having a microporous structure,
(A) an activated carbon powder to be coated is filled with a coating solution, wherein the coating solution contains 3 to 5 parts by weight of a thioacetal compound, 5 to 10 parts by weight of a nonionic surfactant, 85 to 90 parts by weight of a film-forming agent is dissolved in distilled water and used;
(B) a caustic alkali etching step of corroding the surface of the activated carbon so as to enhance the adhesion of the activated carbon filled with the coating liquid;
(C) attaching tin (Sn) to the activated carbon that has been etched through the step (B);
(D) attaching palladium (Pd) to the activated carbon to which the first catalyst is applied;
(E) an electroless copper (Cu) strike step of forming a metal coating on the surface of the activated carbon to which the second catalyst is applied;
(F) an electroless copper plating thickness adjusting step of forming copper plating on the coating film formed on the surface of activated carbon through the electroless copper (Cu) strike to a uniform thickness;
(G) an electroless nickel (Ni) plating step of forming a nickel metal film on the activated carbon through the electroless copper plating thickness control step; And
(H) a step of performing a heat treatment for high strength of the activated carbon subjected to the electroless nickel (Ni) plating step. The method according to claim 1,
(F2) Between the steps (F) and (G), the activated carbon subjected to the electroless copper plating thickness control step is immersed in pure water at 800 to 900 ml / L so that the electroless nickel (Ni) Further comprising a catalytic activation step of immersing the substrate in water after immersing it in a treating solution composed of 50 to 100 ml / L of ionic type catalyst-imparting agent mixed with 50 to 100 ml / L of hydrochloric acid mixed therein, Way. delete 3. The method according to claim 1 or 2,
The activated carbon in step (C) is immersed in a solution of 8-12 g / L tin (SnCl ₂ ) and 8-12 ml / L hydrochloric acid (HCl) at 25-30 ° C. for 3-5 minutes And then washed with water. 3. The method according to claim 1 or 2,
The activated carbon in step (D) is immersed in a solution of 0.3 to 0.5 g / L of palladium chloride (PdCl ₂ ) and 2 to 4 ml / L of hydrochloric acid (HCl) at a temperature of 30 to 35 ° C. for 3 to 5 minutes And then washed with water. 3. The method according to claim 1 or 2,
The activated carbon in the step (F) is added to the purified water at a concentration of 850 to 860 ml / L, 55 to 65 ml / L of the bath bath and the supplement, 55 to 65 ml / L of the alkali supplement, 15 to 20 ml / And 8 to 10 ml / L of formaldehyde (HCHO) are successively mixed, and then water is dipped in water for 10 to 20 minutes at a precipitation speed of 0.5 to 0.7 占 퐉. The method according to claim 6,
The copper-rich bath and supplements are composed of 6 to 12 parts by weight of copper sulfate, 1 to 1.5 parts by weight of polyethylene glycol, 0.01 to 0.02 parts by weight of stabilizer, and 78 to 80 parts by weight of pure water,
The alkali supplement is composed of 35 to 45 parts by weight of sodium hydroxide (NaOH), 0.01 to 0.02 parts by weight of stabilizer, and 50 to 60 parts by weight of pure water,
The complexing agent is composed of 44 to 50 parts by weight of sodium hydroxide (NaOH), 0.01 to 0.02 parts by weight of stabilizer, and 50 to 55 parts by weight of pure water,
Wherein the stabilizer is composed of 0.2 to 0.3 parts by weight of potassium selenocyanate and 90 to 95 parts by weight of pure water. 3. The method according to claim 1 or 2,
In the step (G), 15-30 parts by weight of nickel sulfate, 1-150 parts by weight of stabilizer, and 70 parts by weight of pure water are added to the activated carbon in the course of mechanical stirring or air agitation with 750 to 780 ml / The first electroless nickel plating solution comprising 55 to 60 ml / L of the first electroless nickel plating solution, 80 to 80 parts by weight of the first stabilizer, 1 to 10 parts by weight of ammonia, 8 to 15 parts by weight of hypophosphite, 8 to 15 parts by weight of stabilizer, And a second electroless nickel plating solution consisting of 140-150 ml / L of the second electroless nickel plating solution. The electroless plating method of activated carbon according to claim 1,

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