KR20030026470A - preprocessing method for plating non conducting material with gold - Google Patents

preprocessing method for plating non conducting material with gold Download PDF

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Publication number
KR20030026470A
KR20030026470A KR1020010059316A KR20010059316A KR20030026470A KR 20030026470 A KR20030026470 A KR 20030026470A KR 1020010059316 A KR1020010059316 A KR 1020010059316A KR 20010059316 A KR20010059316 A KR 20010059316A KR 20030026470 A KR20030026470 A KR 20030026470A
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South Korea
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conductive material
plating
copper
solution
gold
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KR1020010059316A
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Korean (ko)
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이경회
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전정식
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/54—Electroplating of non-metallic surfaces
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1646—Characteristics of the product obtained
    • C23C18/165—Multilayered product
    • C23C18/1653—Two or more layers with at least one layer obtained by electroless plating and one layer obtained by electroplating
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
    • C23C18/28—Sensitising or activating
    • C23C18/285—Sensitising or activating with tin based compound or composition
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
    • C23C18/28—Sensitising or activating
    • C23C18/30—Activating or accelerating or sensitising with palladium or other noble metal
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31—Coating with metals
    • C23C18/38—Coating with copper
    • C23C18/40—Coating with copper using reducing agents
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/48—Electroplating: Baths therefor from solutions of gold

Abstract

PURPOSE: A pretreatment method for plating non-conductive material with gold is provided which not only forms a coating film of even thickness, but also forms a gold plating layer to a desired thickness when plating gold on the non-conductive material. CONSTITUTION: The pretreatment method for plating non-conductive material with gold comprises a power drop line process of exposing the copper wire coiled non-conductive material to the outside by coiling copper wire on a specific part of the non-conductive material; a sensitizing process of adsorbing tin ions on the surface of the non-conductive material by dipping the non-conductive material into an aqueous solution of tin chloride shortly; an activation process of adhering palladium onto the surface of the non-conductive material by dipping the tin ion adsorbed non-conductive material into a mixed solution of palladium chloride and acid; a copper sulfate chemical plating process of adhering copper onto the surface of the palladium adhered non-conductive material by dipping the palladium adhered non-conductive material into a nonelectrolytic copper plating solution shortly; and a copper sulfate electroplating process, wherein the pretreatment method further comprises a heating process of arranging unnecessary parts of the non-conductive material by dipping a non-conductive material into an aqueous solution of sodium hydroxide heated to a boiling point or more; a formation process of removing the unnecessary parts of the non-conductive material passing the heating process using a supersonic cleaner; and a drying process of removing moisture of the non-conductive material passing the formation process before performing the power drop line process.

Description

비전도성 물질의 금 도금을 위한 전처리 방법{preprocessing method for plating non conducting material with gold}Preprocessing method for plating non conducting material with gold}

본 발명은 도금 방법에 관한 것으로, 보다 상세하게는 비전도성 물질의 금 도금을 위하여 일정한 사전 처리 후에 파라듐 도금과 동 도금을 시행하여 금 도금을 보다 확고하게 할 수 있도록 하는 비전도성 물질의 금 도금을 위한 전처리 방법에 관한 것이다.The present invention relates to a plating method, and more particularly, gold plating of a non-conductive material to make gold plating more firm by performing palladium plating and copper plating after a predetermined pretreatment for gold plating of a non-conductive material. It relates to a pretreatment method for.

일반적으로 금속 또는 비금속 물질의 방식(防蝕), 내마모성이나 내열성의 향상은 물론 표면의 색채와 광택의 향상을 목적으로 표면처리법을 시행하고 있다.이과 같은 표면처리법 중 도금(palting)은 금속이나 비금속의 표면에 다른 금속을 사용하여 피막을 입히는 처리방법으로서, 전기도금, 화학도금, 용융도금, 진공도금, 침투도금, 이온도금 등이 있다.In general, surface treatment is carried out for the purpose of improving the anti-corrosion, abrasion resistance and heat resistance of metals or nonmetallic materials, as well as the color and gloss of the surface. As a treatment method for coating a film using another metal on the surface, there are electroplating, chemical plating, hot-dip plating, vacuum plating, penetration plating, ion plating and the like.

금 도금은 전기에너지를 이용하여 금속 또는 비금속 소지에 금(Au)의 피막을 만들어 주는 표면처리법 중 하나인 전기도금의 한 종류로서, 전도성 물질의 경우에는 간단한 전기도금 장치에 의하여 쉽게 금 도금을 시행할 수 있으나, 비전도성 물질인 경우에는 일정한 전처리를 필요로 한다.Gold plating is a type of electroplating, which is one of the surface treatment methods to make gold (Au) film on metal or nonmetallic material by using electric energy. In the case of conductive material, gold plating is easily performed by simple electroplating device. Non-conductive materials can be used, but require some pretreatment.

비전도성 물질에 대한 금 도금 시행을 위한 전처리에 관한 종래 기술에 의하면, 비전도성 물질에 대하여 화학도금이나 전기도금 등을 통하여 동 등의 전도성 물질의 피막을 형성시킨 후, 통상적인 금 도금을 시행하였으나, 상기한 전처리 과정에서의 동 등의 피막 형성이 미비하거나 불균일하게 됨으로써 후에 시행하는 금 도금층의 두께에 영향을 미침은 물론 전체적인 두께의 균일성에 대해서도 문제가 있었다.According to the related art of pretreatment for gold plating on non-conductive materials, conventional gold plating was performed after forming a film of a conductive material such as copper on the non-conductive material through chemical plating or electroplating. In the above pretreatment process, the formation of the film such as copper is insufficient or uneven, which affects the thickness of the gold plating layer to be carried out later, as well as the uniformity of the overall thickness.

본 발명는 상기한 바와 같은 문제점을 해결하기 위하여 안출된 것으로서, 비전도성 물질의 금 도금시 균일한 피막 두께를 형성함은 물론 원하는 두께로 금 도금층을 형성할 수 있도록 하는 비전도성 물질의 금 도금을 위한 전처리 방법을 제공하는데 그 목적이 있다.The present invention has been made to solve the problems as described above, for the gold plating of the non-conductive material to form a gold coating layer of the desired thickness as well as to form a uniform film thickness when gold plating of the non-conductive material. The purpose is to provide a pretreatment method.

도 1은 본 발명에 의한 비전도성 물질의 금 도금을 위한 전처리 방법을 나타내는 순서도,1 is a flow chart showing a pretreatment method for gold plating of a non-conductive material according to the present invention,

도 2는 본 발명에 의한 비전도성 물질의 전원인입선 설치 방법을 나타내는 사시도.Figure 2 is a perspective view showing a power lead wire installation method of a non-conductive material according to the present invention.

본 발명은 상기한 바와 같은 목적을 달성하기 위하여, 비전도성 물질의 금 도금 시행을 위한 전처리 방법에 있어서, 상기 비전도성 물질의 특정 부분에 구리철사를 감아 외부로 노출되도록 하는 전원인입선 공정과, 염화제1주석수용액에 단시간 침지시켜 상기 비전도성 물질의 표면에 주석이온을 흡착시키는 감수성 부여 공정과, 염화파라듐과 산의 혼합 용액에 단시간 침지하여 상기 비전도성 물질의 표면에 파라듐을 부착시키는 활성화 공정과, 무전해 동 도금액에 단시간 침지하여 상기 비전도성 물질의 표면에 동을 부착시키는 황산동 화학도금 공정과, 황산동 전기도금 공정으로 구성되는 것을 특징으로 한다.The present invention, in order to achieve the above object, in the pre-treatment method for gold plating of the non-conductive material, the power lead-in process for winding the copper wire around a specific portion of the non-conductive material to be exposed to the outside, chloride A process of providing sensitivity to adsorb tin ions on the surface of the non-conductive material by immersing in a first tin aqueous solution for a short time, and activating to attach paradium to the surface of the non-conductive material by immersing in a mixed solution of palladium chloride and acid for a short time. And a copper sulfate chemical plating step of adhering copper to the surface of the non-conductive material by immersing the electroless copper plating solution for a short time, and a copper sulfate electroplating step.

이하, 첨부된 도면을 참조하면서, 본 발명의 구성에 대하여 상세히 설명한다.EMBODIMENT OF THE INVENTION Hereinafter, the structure of this invention is described in detail, referring an accompanying drawing.

본 발명에 있어서, 바람직한 일 실시예로서 나뭇잎을 비전도성 물질로 상정한 후, 이에 대한 금 도금 시행을 위한 전처리 방법을 기술한다. 본 실시예에서는 나뭇잎을 그 예로 들었으나, 일정한 외형을 이루고 있는 비전도성 물질 어느 것에도 적용될 수 있다.In the present invention, as a preferred embodiment, after the leaf is assumed to be a non-conductive material, it describes a pretreatment method for gold plating. In the present embodiment, the leaf is taken as an example, but may be applied to any non-conductive material having a certain appearance.

도 1은 본 발명에 의한 비전도성 물질의 금 도금을 위한 전처리 방법을 나타내는 순서도이다.1 is a flow chart showing a pretreatment method for gold plating of a nonconductive material according to the present invention.

도면에서 도시하고 있는 바와 같이, 우선 나뭇잎을 채취하여 일정 온도 이상, 예컨대 끓는점 이상으로 가열된 상태에 있는 수산화나트륨수용액에 침지하여 온도와 시간을 조절하면서 나뭇잎을 삶는 가열 공정(100)을 시행한다. 상기 가열공정(100)은 나뭇잎의 잎맥을 제외한 부분이 쉽게 제거될 수 있는 정도까지 시행한다.As shown in the figure, the leaves are first collected and immersed in a sodium hydroxide aqueous solution heated at a predetermined temperature or more, for example, at a boiling point or more, and then a heating step (100) is performed to boil the leaves while controlling the temperature and time. The heating step 100 is carried out to the extent that the parts except the leaf veins of the leaves can be easily removed.

다음으로, 상기 가열공정(100)을 거친 나뭇잎을 초음파 세척기를 통하여 잎맥만 남기고 나머지 부분을 제거하는 형상화 공정(130)이 이행된다. 상기 형상화 공정(130)을 통하여 나뭇잎은 잎맥을 통하여 일정한 외형만을 가지고 잎맥 사이에는 공동이 형성되는 형태, 즉 섬유질만이 남는 상태가 된다.Next, the shaping process 130 is performed to remove the remaining portions of the leaves after the heating step 100 leaves only the leaf vein through the ultrasonic cleaner. Through the shaping process 130, the leaves have only a certain shape through the leaf vein, the cavity is formed between the leaf veins, that is, the fiber remains.

상기 형상화 공정(130)에서 초음파 세척기를 이용하는 것은 교반과 진동을 통하여 효과적인 탈지와 떨어지기 힘든 고형물이나 구석에 있는 더러움의 제거를 효과적으로 하기 위함이다.Using the ultrasonic cleaner in the shaping process 130 is to effectively remove the degreasing and dirt in the corner or hard to fall through the effective degreasing and vibration.

형상화 공정(130)를 거친 나뭇잎은 일정한 함량 이상의 수분을 함유하고 있으므로, 수분의 제거를 위한 건조 공정(160)이 필요하다. 또한 추후 전기도금의 시행을 위하여 특정 부분에 전원인입선의 설치가 필요하다. 따라서 상기 형상화 공정(130)을 거친 나뭇잎을 일정한 형틀에 장입하여 수분을 건조시킴은 물론 특정 부분, 예컨대 나뭇잎의 꼭지부분을 상기 형틀의 외부로 돌출시킨 후, 구리철사를 감아 구리철사가 외부로 노출되도록 구성하여 전원인입선을 완성한다. 이 공정이 건조 공정(160) 및 전원인입선 공정(200)이다.Since the leaves undergoing the shaping process 130 contain more than a certain amount of water, a drying process 160 for removing water is required. In addition, it is necessary to install power lead-in wires in a specific part in order to carry out electroplating later. Therefore, the leaves that have passed through the shaping process 130 are charged into a predetermined mold to dry moisture, and protrude a specific portion, for example, a leaf of the leaf to the outside of the mold, and then wind the copper wire to expose the copper wire to the outside. It is configured to complete the power lead-in wire. This step is a drying step 160 and a power lead-in step 200.

상기 전원인입선 공정(200)에 있어서, 전원인입선의 총 길이는 약 5∼6㎝이며, 후술하는 도금시의 도금액 면을 기준으로 하여 도금액 내부에 장입되는 부분이 1.5∼2㎝, 도금액 외부에 위치되는 부분이 약 3.5∼4㎝ 정도가 되도록 한다.In the power lead-in process 200, the total length of the power lead-in wire is about 5 to 6 cm, and the portion to be charged inside the plating liquid is 1.5 to 2 cm based on the surface of the plating liquid at the time of plating, which will be described later. It should be about 3.5 to 4 cm.

상기 건조 및 전원인입선 공정(160, 200)을 위한 형틀은 나뭇잎 등을 적층하여 장입할 수 있는 형태, 예컨대 책과 같이 다수개의 세로 구획공간을 갖는 형태로서, 일부분이 외부와 개방된 구조로 함이 바람직하다. 도 2는 본 발명에 의한 비전도성 물질의 전원인입선 설치 방법을 나타내는 사시도이다.The mold for the drying and power supply process (160, 200) is a form that can be charged by stacking leaves, such as a form having a plurality of vertical partition space, such as a book, part of the structure is open to the outside desirable. Figure 2 is a perspective view showing a power lead wire installation method of a non-conductive material according to the present invention.

다음으로 염화제1주석수용액에 단시간 침지시켜 나뭇잎의 표면에 주석이온을 흡착시키는 감수성 부여(sensitizing) 공정(300)을 시행한다. 본 실시예에서는 염화제1주석수용액(SnCl2·2H2O) 30∼40g/l, 35% HCl 30ml/l의 조성을 가진 액에 약 10초간 침지하여 나뭇잎의 표면에 Sn2+을 흡착시킨 후, 물 속에 단시간 침지시켜 미소하게 요동시킨 후 물에서 이탈시킨다. 상기 염화상기 감수성 부여 공정(300)의 원활한 수행을 보조하기 위하여 나뭇잎의 표면에 친수성을 부여할 필요가 있는 바, 나뭇잎의 표면에 약 10초 정도 초음파를 부가할 수 있다.Next, a sensitizing process 300 is performed in which the tin ions are immersed in the tin chloride solution for a short time to adsorb tin ions to the surface of the leaves. In this embodiment, immersion in a tin tin aqueous solution (SnCl 2 · 2H 2 O) 30 ~ 40g / l, 35% HCl 30ml / l for about 10 seconds to adsorb Sn 2 + to the surface of the leaves After soaking in water for a short time, make small shaking and then remove it from water. In order to aid in the smooth performance of the chloride-sensitive sensitivity providing process 300, it is necessary to give hydrophilicity to the surface of the leaf, so that ultrasonic waves may be added to the surface of the leaf for about 10 seconds.

상기 감수성 부여 공정(300)은 후술하는 파라듐(Pd)의 부착을 용이하도록 하기 위한 공정으로서, Sn2+의 흡착 이후 물에 침지하여 요동하는 것은 Sn2+의 균일 부착을 위해 불순물과 불형상 부착물의 제거를 위함이다.The sensitivity applying process 300, is it to swing by immersion in a process to facilitate the adhesion to the palladium (Pd), which will be described later, after the adsorption of Sn 2+ water for uniform deposition of Sn 2+ impurities and fire shapes To remove deposits.

상기 감수성 부여 공정(300) 후에는 활성화 공정(350)을 하는 바, 활성화액( activator)인 PdCl 2∼5g/l, 35% HCl 40∼50ml/l 액에 약 5∼10초간 침지시켜, Sn2++ Pd2+→ Pd0+ Sn4+의 반응을 일으키고, 다음에 수세(水洗)를 통하여 Sn4+을 제거하고 표면의 Pd의 핵만을 부착시키도록 한다. 묽은 염산에 침지하고 수세하여 Sn4+을 제거하는 상기 활성화 공정(350)은 후 진행하는 황산동 화학도금 공정(400)에서 불필요한 화학반응을 야기시켜 동 도금액의 상태를 불량하게 만드는 것을 방지하기 위함이다.After the susceptibility imparting step 300, the activation step 350 is performed, and immersed for about 5 to 10 seconds in PdCl 2 to 5 g / l and 35% HCl 40 to 50 ml / l as an activator for about 5 to 10 seconds. The reaction of 2+ + Pd 2+ → Pd 0 + Sn 4+ is caused, followed by washing with water to remove Sn 4+ and attach only the nuclei of Pd on the surface. The activation process 350 to remove Sn 4+ by immersing in dilute hydrochloric acid and washing with water is to prevent unnecessary chemical reaction in the subsequent copper sulfate chemical plating process 400 to prevent the state of the copper plating solution from being poor. .

파라듐(Pd)은 원자번호 46, 원자량 106.4, 비중 12.02 이며, 융점은 1552℃인 금속으로서, 화학적으로 안정되며, 가격은 백금족 중에서 가장 저렴하며, 후술하는 동 도금을 위한 하지 도금으로 활용된다.Palladium (Pd) is an atomic number of 46, atomic weight 106.4, specific gravity 12.02, melting point is 1552 ℃ metal, chemically stable, the cheapest price among the platinum group, it is utilized as a base plating for copper plating described below.

상기 감수성 부여 공정(300)과 활성화 공정(350)은 무전해 도금 때 표면에 잔류된 Sn(OH)4등 때문에 거친 표면이 되기 쉬워서 일정한 표면 가공을 필요로 하는 불편이 있으며, 활성화액이 불안정한 경향이 있다. 따라서 상기 감수성 부여 공정(300)과 활성화 공정(350) 대신에 카탈리스트-액셀러레이터 공정(390)을 시행할 수도 있다.The susceptibility imparting process 300 and the activation process 350 tends to be a rough surface due to Sn (OH) 4 remaining on the surface during electroless plating, which requires a constant surface processing, and the activating liquid tends to be unstable. There is this. Accordingly, the catalyst-accelerator process 390 may be implemented in place of the sensitivity providing process 300 and the activation process 350.

상기 카탈리스트-액셀러레이터 공정(390)은 카탈리스트(catalyst)액인 PdCl20.1∼0.4g/l, SnCl2·2HO 5∼30g/l, 35% HCl 100∼300ml/l 의 안정된 중합액인 PdCl2-SnCl2-Cln액에 침지하여 처리한다. 상기 카탈리스트액은 PdCl2약 2g/l 정도의 농축 Pd7Cl16·ySnCl3 -의 착이온으로 생각되는 액을 조성하여 상기와 같은 묽은 액으로 만들어서 사용하게 된다. 다음 수세 처리에서 흡착된 착염은 가수분해하여 Sn(OH)Cl 인 2가 주석이온과 4가 주석, 파라듐염이 공존하게 된다. 이 침전된 제1 및 제2주석염을 액셀러레이터에서 용해제거하며 이미 착이온에서 이탈된 Pd2+도 Sn2++ Pd2+의 반응으로 Sn4++ Pd0로 되어 표면에 Pd 금속과 소량의 2가 및 4가의 주석염이 남게 된다. 이 잔류주석염도 액셀러레이터 후의 수세 처리에서 대부분 제거된다. 액셀러레이터 처리는 35% HCl 500∼100m/l, 20∼50℃ 액에서 1∼3분간 처리된다. 이때 Sn4+등을 제거하는 것이 목적이므로 잔류하면 거친 도금이 되기 쉽다.The Catalyst-accelerator process 390 Catalyst (catalyst) aekin PdCl 2 0.1~0.4g / l, SnCl 2 · 2HO 5~30g / l, 35% HCl 100~300ml / l stabilized polymer solution of PdCl 2 in -SnCl Treat by dipping in 2 -Cl n liquid. The catalyst solution is prepared by diluting a solution which is considered to be a complex ion of concentrated Pd 7 Cl 16 · ySnCl 3 − of about 2 g / l PdCl 2 to make a thin solution as described above. The complex salt adsorbed in the next washing treatment is hydrolyzed to coexist with divalent tin ions, Sn (OH) Cl, tetravalent tin and palladium salts. The precipitated first and second tin salts were dissolved in the accelerator and Pd 2+ , which had already been released from complex ions, became Sn 4+ + Pd 0 by the reaction of Sn 2+ + Pd 2+ . The divalent and tetravalent tin salts of remain. This residual tin salt is also largely removed by the water washing treatment after the accelerator. Accelerator treatment is performed in 35% HCl 500-100m / l, 20-50 degreeC liquid for 1-3 minutes. At this time, since the purpose is to remove Sn 4+ and the like, coarse plating is likely to occur.

상기한 바와 같은 카탈리스트-액셀러레이터 공정(390)은 파라듐(Pd)의 소모가 많기 때문에 생산비를 증대시키며, 또한 도금 대상체기 생물(生物)인 경우에는 적용할 수 없다.The above-described catalyst-accelerator process 390 increases the production cost because of the high consumption of palladium (Pd), and is not applicable to the case of plating object-based organisms.

상기한 바와 같은 공정을 마친 상태에서 황산동 화학도금 공정(400)을 시행한다. 상기 황산동 화학도금 공정(400)은 구리이온이 있는 용액 중의 환원제에 의하여 대상 물체 위에 금속이 환원석출되는 도금으로서, 환원제가 산화될 때 방출한 전자를 금속이온이 받아들여 환원하면서 도금할 물건 위에 석출하는 원리를 이용한 것이다.The copper sulfate chemical plating process 400 is performed in the state as described above. The copper sulfate chemical plating process 400 is a plating in which metal is reduced and precipitated on a target object by a reducing agent in a solution containing copper ions, and the electrons released when the reducing agent is oxidized are deposited on an object to be plated while the metal ions are received and reduced. The principle is to use.

상기 황산동 화학도금 공정(400)을 위해서 무전해 동 도금액을 구성하여야 하는 바, 본 실시예에서는 황산동 7.5g/l, 롯셀염 85g/l, 37% 포르말린 22ml/l, 안정제로서 탄산칼슘과 수산화나트륨 약간을 첨가하여, 전체의 pH를 12.8 정도로 하고, 액 온도를 약 20∼30℃로 한 상태로 도금 대상 물질을 단시간 침지시킴으로써 화학 동도금을 시행하였다.The electroless copper plating solution should be configured for the copper sulfate chemical plating process 400. In this embodiment, the copper sulfate 7.5g / l, the Rossel salt 85g / l, 37% formalin 22ml / l, calcium carbonate and sodium hydroxide as a stabilizer Chemical copper plating was performed by immersing a plating target material for a short time in the state which made a little addition, the whole pH was about 12.8, and the liquid temperature was about 20-30 degreeC.

화학도금을 위한 동 도금액을 구성함에 있어서, 우선 황산동을 물에 용해시킨 용액과, 탄산칼슘, 수산화나트륨 및 롯셀염을 물에 용해될 때까지 교반시킨 후,상기 황산동 수용액과 혼합시킨다. 이때 혼합의 용이를 위하여 가수(加水)와 교반을 수행한다. 다음으로 상기 수용액에 포르말린은 가한 후, 화학도금 대상 나뭇잎을 약 10분간 침지하였다가 꺼내면 나뭇잎의 표면에 동이 부착된다.In constructing a copper plating solution for chemical plating, first, a solution in which copper sulfate is dissolved in water, and calcium carbonate, sodium hydroxide and loxel salt are stirred until dissolved in water, and then mixed with the copper sulfate aqueous solution. At this time, for easy mixing, stirring and stirring are performed. Next, after formalin is added to the aqueous solution, copper leaves are attached to the surface of the leaves after immersing the leaves to be chemically plated for about 10 minutes.

상기 황산동 화학도금 공정(400)을 시행한 나뭇잎은 물에 단시간 침지하였다가 꺼내는 정도의 세척과정(420)을 거치도록 한다.The leaves subjected to the copper sulfate chemical plating process 400 are immersed in water for a short time to undergo a washing process 420 to the extent that they are taken out.

상기한 공정을 거친 나뭇잎은 마지막으로 황산동 전기도금 공정(500)으로 이행된다. 상기 황산동 화학도금 공정(400)은 본 황산동 전기도금 공정(500)의 원활한 효과 달성을 위한 하지 도금 공정에 해당되며, 본 황산동 전기도금 공정(500)은 후 시행되는 금 도금 공정에서 금의 원활한 부착을 위한 하지 도금 공정에 해당되며, 비전도성 물체의 도금을 가능하게 하는 역할을 수행한다.Leaves passed through the above process is finally transferred to the copper sulfate electroplating process (500). The copper sulfate chemical plating process 400 corresponds to a base plating process for achieving a smooth effect of the copper sulfate electroplating process 500, and the copper sulfate electroplating process 500 may smoothly attach gold in a gold plating process to be performed later. Corresponds to the underlying plating process for, and serves to enable the plating of non-conductive objects.

황산동 전기도금 공정(500)은 일반적인 동 전기도금 공정과 동일하다. 2가 이온인 황산동(CuSO4·5H2O) 70∼100g/l, 황산(H2SO4) 100∼190g/l의 도금액 조성으로 전기도금을 약 20분간 시행하여 나뭇잎의 표면에 동이 일정 두께로 균일하게 전착되도록 한다.Copper sulfate electroplating process 500 is the same as the general copper electroplating process. Copper plating of divalent ions (CuSO 4 · 5H 2 O) 70 ~ 100g / l, sulfuric acid (H 2 SO 4 ) 100 ~ 190g / l in the plating solution is carried out for about 20 minutes to the copper surface constant thickness Ensure uniform electrodeposition.

상기 황산동 전기도금 공정(500)은 피로인산동 전기도금(copper pyrophosphate plating) 공정(550)으로 대체할 수도 있다. 피로인산동 전기도금은 도금 후의 평활성이 우수하고 저전류밀도부까지 광택이 좋은 도금이 가능함은 물론, pH가 8.6∼9.0으로 폐수 처리가 용이하고 도금이 연한 것과 균일전착성이 우수하고 수소취성이 적기 때문에 널리 사용된다.The copper sulfate electroplating process 500 may be replaced with a copper pyrophosphate plating process 550. Pyrophosphate copper electroplating has excellent smoothness after plating and good gloss to low current density. It has a pH of 8.6-9.0, which makes it easy to treat wastewater, has a soft plating, uniform electrodeposition, and hydrogen embrittlement. It is widely used because it is small.

상기 피로인산동 전기도금 공정(550)은 2가 이온인 피로인산동(Cu2P2O7·3H2O) 65∼105g/l, 피로인산칼륨(K4P2O7) 230∼370g/l, 암모니아수와 폴리인산(H6P4O13) 약간의 도금액 조성으로 전기도금을 약 20분간 시행하여 나뭇잎의 표면에 동이 일정 두께로 균일하게 전착되도록 한다.The copper pyrophosphate electroplating process 550 is 65 to 105 g / l of copper pyrophosphate (Cu 2 P 2 O 7 · 3H 2 O), which is a divalent ion, 230 to 370 g of potassium pyrophosphate (K 4 P 2 O 7 ). / l, ammonia water and polyphosphoric acid (H 6 P 4 O 13 ) Electroplating is carried out for about 20 minutes with a slight plating solution composition so that copper is uniformly deposited on the surface of the leaves with a certain thickness.

상기한 과정을 거쳐 비전도성 물질의 금 도금 시행을 위한 전처리 과정이 완료되며, 통상적인 금 도금 공정(600)으로 이행되게 된다.Through the above process, the pretreatment process for gold plating of the non-conductive material is completed, and the process proceeds to the conventional gold plating process 600.

본 발명에 의한 비전도성 물질의 금 도금 시행을 위한 전처리 과정에서, 가열 공정(100), 형상과 공정(130) 및 건조 공정(160)을 시행하지 아니하고 직접 전원인입성 공정(200)부터 시작할 수도 있다. 다만, 이러한 경우에는 비전도 물질의 형태 유지를 위하여 고정액을 살포하여 형태를 고정하여야 하며, 상기 고정액이 코팅된 표면이 친수성을 갖도록 사포 등을 사용하여 표면을 조정할 필요가 있다.In the pretreatment process for the gold plating of the non-conductive material according to the present invention, the heating process 100, the shape and process 130, and the drying process 160 may be started without performing the direct power draw process (200). have. However, in this case, to maintain the shape of the non-conductive material, it is necessary to fix the shape by spraying the fixing solution, and it is necessary to adjust the surface by using sandpaper or the like so that the surface coated with the fixing solution has hydrophilicity.

상기한 바와 같은 구성을 갖는 본 발명은 비전도성 물질의 금 도금 불량을 해소하기 위하여 주석, 파라듐, 동을 화학도금과 전기도금 방법에 의하여 비전도성 물질에 부착시킴으로써 금 도금 시의 전착 불량을 해소함은 물론 균일한 두께로 양호한 표면상태를 유지할 수 있는 금 도금이 가능하게 하는 효과를 거둘 수 있다.The present invention having the above-described configuration eliminates the electrodeposition defects during gold plating by attaching tin, palladium, and copper to the non-conductive materials by chemical plating and electroplating in order to solve the gold plating defects of the non-conductive materials. Of course, it is possible to achieve an effect of allowing gold plating to maintain a good surface state with a uniform thickness.

또한 본 발명에 의하면 비전도성 물질의 금 도금층을 두텁게 구성할 수 있도록 함으로써 나뭇잎이나 기타 일정한 장식적 효과를 갖는 외형을 가진 비전도성 물질에 금 도금을 효과적으로 시행 가능하게 하기 때문에 장신구 등의 제조에 효율적으로 이용될 수 있다.In addition, according to the present invention, the gold plating layer of the non-conductive material can be made thick so that the gold plating can be effectively performed on the non-conductive material having the appearance of leaves or other decorative effects, and thus, the production of jewelry and the like efficiently. Can be used.

Claims (7)

비전도성 물질의 금 도금 시행을 위한 전처리 방법에 있어서,In the pretreatment method for gold plating of non-conductive material, 상기 비전도성 물질의 특정 부분에 구리철사를 감아 외부로 노출되도록 하는 전원인입선 공정과,A power lead wire process of winding copper wire around a specific portion of the non-conductive material to be exposed to the outside; 염화제1주석수용액에 단시간 침지시켜 상기 비전도성 물질의 표면에 주석이온을 흡착시키는 감수성 부여 공정과,A sensitization imparting step of adsorbing tin ions on the surface of the non-conductive material by immersion in a tin tin chloride solution for a short time; 염화파라듐과 산의 혼합 용액에 단시간 침지하여 상기 비전도성 물질의 표면에 파라듐을 부착시키는 활성화 공정과,An activation process of attaching palladium to the surface of the non-conductive material by immersing it in a mixed solution of palladium chloride and an acid for a short time; 무전해 동 도금액에 단시간 침지하여 상기 비전도성 물질의 표면에 동을 부착시키는 황산동 화학도금 공정과,A copper sulfate chemical plating process of immersing copper in the surface of the non-conductive material by immersing it in an electroless copper plating solution for a short time; 황산동 전기도금 공정으로 구성되는 것을 특징으로 하는 비전도성 물질의 금 도금 시행을 위한 전처리 방법.A pretreatment method for conducting gold plating of a non-conductive material, characterized in that the copper sulfate electroplating process. 제1항에 있어서,The method of claim 1, 상기 공정의 시행에 앞서,Prior to the implementation of the process, 끓는점 이상으로 가열된 수산화나트륨수용액에 침지하여 비전도성 물질의 불필요부분을 정리하기 위한 가열 공정과,A heating process for cleaning up unnecessary portions of non-conductive substances by immersing in an aqueous sodium hydroxide solution heated above the boiling point; 상기 가열 공정을 거친 비전도성 물질의 불필요부분을 초음파 세척기를 사용하여 제거하는 형상화 공정과,A shaping process of removing an unnecessary portion of the non-conductive material that has undergone the heating process by using an ultrasonic cleaner; 상기 형상화 공정를 거친 비전도성 물질의 수분을 제거하는 건조 공정을 선시행하는 것을 특징으로 하는 비전도성 물질의 금 도금 시행을 위한 전처리 방법.The pretreatment method for gold plating of the non-conductive material, characterized in that for performing a drying step of removing the moisture of the non-conductive material passed through the shaping process. 제1항에 있어서,The method of claim 1, 상기 전원인입성 공정에서, 전원인인입선의 총 길이는 5∼6㎝이며, 도금시의 도금액 면을 기준으로 도금액 내부에 장입되는 부분이 1.5∼2㎝, 도금액 외부에 위치되는 부분이 약 3.5∼4㎝인 것을 특징으로 하는 비전도성 물질의 금 도금 시행을 위한 전처리 방법.In the power lead-in process, the total length of the power lead-in wire is 5 to 6 cm, and the portion to be charged inside the plating liquid is 1.5 to 2 cm based on the surface of the plating liquid at the time of plating, and the portion located outside the plating liquid is about 3.5 to Pretreatment method for gold plating of the non-conductive material, characterized in that 4cm. 제1항에 있어서,The method of claim 1, 상기 감수성 부여 공정은, 염화제1주석수용액(SnCl2·2H2O) 30∼40g/l, 35% 염산(HCl) 30ml/l의 조성을 가진 액에 약 10초간 침지한 후, 수세하는 것을 특징으로 하는 비전도성 물질의 금 도금 시행을 위한 전처리 방법.The susceptibility imparting step is immersed in a solution having a composition of 1 st tin chloride aqueous solution (SnCl 2 · 2H 2 O) 30-40 g / l, 30 ml / l 35% hydrochloric acid (HCl) for about 10 seconds, and then washed with water. Pre-treatment method for gold plating of non-conductive material. 제1항에 있어서,The method of claim 1, 상기 활성화 공정은, 염화파라듐(PdCl) 2∼5g/l, 35% 염산(HCl) 40∼50ml/l의 조성을 가진 액에 약 5∼10초간 침지한 후, 수세하는 것을 특징으로 하는 것을 특징으로 하는 비전도성 물질의 금 도금 시행을 위한 전처리 방법.The activating step is characterized in that immersion in a liquid having a composition of palladium chloride (PdCl) 2-5g / l, 35% hydrochloric acid (HCl) 40-50ml / l for about 5 to 10 seconds, and then washed with water. Pre-treatment method for gold plating of non-conductive material. 제1항 또는 제2항에 있어서,The method according to claim 1 or 2, 상기 감수성 부여 공정과 활성화 공정 대신에,Instead of the susceptibility imparting process and the activation process, PdCl2-SnCl2-Cln조성의 카탈리스트액에 단시간 침지하여 상기 비전도성 물질의 표면에 2가 주석염과 4가 주석염 및 파라듐염이 공존하게 한 후, 염산수용액에서 침지하는 액셀러레이터 처리와 수세 처리를 통하여 주석염을 제거하고 파라듐만을 잔류 처리하는 카탈리스트-액셀러레이터 공정을 구비하는 것을 특징으로 하는 비전도성 물질의 금 도금 시행을 위한 전처리 방법.After dipping the catalyst solution of PdCl 2 -SnCl 2 -Cl n composition for a short time, the divalent tin salt, tetravalent tin salt, and palladium salt coexist on the surface of the non-conductive material, followed by an accelerator treatment to be immersed in an aqueous hydrochloric acid solution. A pre-treatment method for gold plating of a non-conductive material, characterized in that it comprises a catalyst-accelerator process for removing tin salt and washing only palladium by washing with water. 제1항 또는 제2항에 있어서,The method according to claim 1 or 2, 상기 황산동 전기도금 공정 대신에,Instead of the copper sulfate electroplating process, 피로인산동 전기도금 공정을 구비하는 것을 특징으로 하는 비전도성 물질의 금 도금 시행을 위한 전처리 방법.A pretreatment method for conducting gold plating of a non-conductive material, characterized by comprising a copper pyrophosphate electroplating process.
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KR940021765A (en) * 1993-03-18 1994-10-19 존 이. 맥카스키 Self-accelerated and rechargeable formaldehyde-free impregnated metal plating methods and compositions therefor
JPH10195691A (en) * 1996-12-26 1998-07-28 Merutetsukusu Kk Pre-processing solution for electroplating nonconductor
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