WO2008004315A1 - procédé de production d'objets plaqués de manière décorative en communiquant une électroconductivité à la résine par pulvérisation cathodique - Google Patents

procédé de production d'objets plaqués de manière décorative en communiquant une électroconductivité à la résine par pulvérisation cathodique Download PDF

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Publication number
WO2008004315A1
WO2008004315A1 PCT/JP2006/313968 JP2006313968W WO2008004315A1 WO 2008004315 A1 WO2008004315 A1 WO 2008004315A1 JP 2006313968 W JP2006313968 W JP 2006313968W WO 2008004315 A1 WO2008004315 A1 WO 2008004315A1
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WIPO (PCT)
Prior art keywords
resin
plating
sputtering
decorative
metal
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Application number
PCT/JP2006/313968
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English (en)
Japanese (ja)
Inventor
Kunihiro Kakihara
Yoshinori Noda
Takashi Ouro
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Kakihara Kogyo Co., Ltd.
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Publication date
Application filed by Kakihara Kogyo Co., Ltd. filed Critical Kakihara Kogyo Co., Ltd.
Publication of WO2008004315A1 publication Critical patent/WO2008004315A1/fr

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    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/20—Metallic material, boron or silicon on organic substrates
    • 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
    • C25D5/56—Electroplating of non-metallic surfaces of plastics

Definitions

  • the present invention relates to a resin plating technique for applying metal plating to a resin molded product, and in particular, before the resin plating until the surface adjustment process of the resin resin plating, the etching process power, and the conductive metal treatment process.
  • the present invention relates to a method for producing a decorative adhesive product using a resin conductive material by sputtering, which is carried out by sputtering treatment without using hexavalent chromic acid.
  • a conventional general resin plating film forming method includes: an etching process for roughening the surface of the resin molded article, an etching neutralization process, Direct plating pretreatment process such as catalyst application process, conductive process (or electroless plating), etc.
  • This is a plating method in which bright nickel plating and MP nickel plating (microporous nickel plating) are used for each plating treatment, and finally chromium plating is applied to finish.
  • a conductive step direct plating pretreatment or electroless plating is required to impart conductivity to the resin as a pretreatment for electroplating.
  • the conductive process (or electroless plating) of a resin molded product that uses a general wet method for resin plating is performed with high concentrations of chromic acid (hexavalent chromium) and sulfuric acid.
  • a catalyst such as PdZSn
  • a pretreatment technique for plating when electroless plating is applied to a resin molded product for example, as disclosed in Japanese Patent Application Laid-Open No. 5-132785, “Electroless plating pretreatment method”, a glass fiber is used.
  • the surface of the insulating material is treated with chromic anhydride and sulfuric acid in the etching treatment of the insulating material, which is performed as a pretreatment when the surface of the insulating material made of polyimide resin containing
  • An electroless plating pretreatment method has been proposed in which a two-stage etching process is performed in which etching is performed using a solution containing hydrazine and then etching is performed using a solution containing hydrazine.
  • Patent Document 1 Japanese Patent Laid-Open No. 5-132785
  • the resin etching process that roughens the resin surface which is the basis of this resin plating, still uses a mixed acid of high-concentration chromic acid (hexavalent chromium) and sulfuric acid.
  • This etching process using chromic acid has the potential to adversely affect the human body even during work in the process that requires only waste liquid treatment.
  • various technologies have been proposed to eliminate the etching process using chromic acid.
  • a pretreatment has been proposed that satisfies the stringent adhesion standards that are the basic performance of resin plating, such as automotive parts standards! I did not hesitate.
  • a PA resin polyamide resin, 6-nylon
  • POM resin polyacetal
  • LC P resin liquid crystal polymer
  • some resin materials can be etched without using a chromic acid-based etching solution.
  • a resin molded product of a resin that is relatively weak in acidity such as PPE resin (polyphenyl ether) can be surface-roughened using a permanganic acid-based etching solution.
  • PPE resin polyphenyl ether
  • a resin molded product of a general-purpose resin such as ABS resin (acrylonitrile Z butadiene Z styrene resin) can be etched using a manganic acid-based etchant. Etching can be performed with a weak etchant such as permanganate etching by adding a solvent pre-etching process. Disclosure of the invention
  • PCZABS resin is mainly used for plating automotive door handles.
  • PC for the same type of resin
  • PCZ polyester-based materials such as ZPBT and PCZPET are used. This is because PCZ polyester-based materials are more suitable as a resin material for door handles, but it is not possible to make resin-handled door handles that can meet automotive specifications that are difficult to plate.
  • the present invention has been devised in order to solve the problem. That is, the object of the present invention is to provide a resin surface roughening to a resin molded product by a processing method that does not use chemicals such as a mixed acid of chromic acid and sulfuric acid in the conventional etching process and conductive process, that is, a dry method.
  • a processing method that does not use chemicals such as a mixed acid of chromic acid and sulfuric acid in the conventional etching process and conductive process, that is, a dry method.
  • the surface layer of the resin does not deteriorate due to such chemicals, and it is possible to prevent cracking due to peeling between the oils and prevent cracking, and the safety of the resin-plated product Is to provide a method for producing a decorative product using a resin conductive material by sputtering.
  • the object of the present invention is to suppress the deformation of the resin molded product and to sputter By using a sputtering device that has been improved so that it can be coated, by imparting conductivity to the resin molded product by the dry method, it is possible to plate a strong resin material that is difficult to fit by the wet method, Another object of the present invention is to provide a method for producing a decorative plated product, which can easily carry out a pretreatment process for various types of resin molded products.
  • the surface of the resin molded product is cleaned with a gas by sputtering and the surface modification activity is performed in a vacuum atmosphere state.
  • a metal thin film forming step (S2) for forming a metal film on the surface of the resin molded product to ensure adhesion to the resin by sputtering
  • a conductive film forming step (S4) for forming a conductive film on the metal thin film formed on the resin molded product by the metal thin film forming step (S2) by sputtering, and the conductive Production of decorative plating products using resin conductive material by sputtering, which is characterized by the fact that it has an electric plating process for electroplating the resin molded product after the chemical film formation process (S4) is completed.
  • a method is provided.
  • an active treatment step (S3) in which the metal thin film formed on the resin molded product is activated by an argon ion source treatment.
  • 'It is preferable to irradiate argon gas with a small amount of air remaining on the surface of the resin molded product by sputtering.
  • the resin surface cleaning 'activation step (S1) it is preferable to irradiate ion source by injecting argon and trace oxygen into the surface of the resin molded product by a magnetron sputtering method in a vacuum atmosphere. ,.
  • a single metal having a strong binding force with oxygen or a strong binding force with oxygen is formed on the surface of the resin molded product in a vacuum atmosphere.
  • An alloy containing a metal, or a magnetic metal or an alloy containing a magnetic metal can be formed by sputtering.
  • a magnetic metal ionized to 0.01 to 50% can be formed on the surface of the resin molded article in a vacuum atmosphere.
  • the film is formed so as to have a film thickness of about 0. O / zm.
  • the conductive film forming step (S4) it is preferable to form nickel or copper.
  • the film is formed so that the film thickness is about 0.1 ⁇ m to 5.0 m.
  • the electroplating process is performed in the order of bright copper sulfate plating (S6), semi-bright nickel plating (S7), Mitsuzawa-Neckel plating (S8), MP nickel plating (microporous nickel plating) (S9). It is preferable that each plating process is performed in step (b), and the plating process is completed by applying a decorative finish plating (S10).
  • a plating process such as trivalent chromium plating, tin Z nickel alloy plating, ruthenium or gold plating is performed.
  • the surface of the resin molded product is cleaned with gas by sputtering and the surface modification activity in the sputtering apparatus in the resin surface cleaning 'activity process (S1).
  • the metal thin film deposition step (S2) in the same sputtering apparatus, a single metal having a strong binding force with oxygen or an alloy containing a metal having a strong binding force with oxygen, or a magnetic metal Alternatively, an alloy containing a magnetic metal is formed, and then a conductive film is formed by sputtering a predetermined metal on the metal thin film formed on the resin molded product in the conductive film forming step (S4).
  • Conductive film processing step (S4) is performed by adding an activation processing step (S3) after the metal thin film deposition step (S2), which is processed for the purpose of obtaining adhesion to the resin.
  • the adhesion of the chemical film becomes stronger.
  • the final resin-plated product can be produced simply by applying the same electrical plating as in normal resin-plating.
  • the pretreatment of the resin plating that is, the conductive treatment of the resin molded product!
  • the resin plating is performed. Because it is not a wet conductive process that uses chemicals that have a large environmental impact in production, environmental impact substances can be drastically reduced. As before, waste liquid treatment such as hexavalent chromium can be unnecessary or drastically reduced.
  • FIG. 1 is a process diagram showing a method for producing a decorative garnish using a resin conductive material obtained by sputtering in Example 1.
  • FIG. 2 A bright nickel plating method is shown, (a) is a process diagram of a resin conductive treatment, and (b) is a wet electroplating process diagram.
  • FIG. 3 is a cross-sectional view of a plating film attached by the method for producing a decorative garment using the resin conductive material obtained by sputtering in Example 1.
  • FIG. 4 A table showing "Table 1. Plate adhesion measurement results”.
  • FIG. 5 is a table showing “Table 2. Sputtering experimental conditions”.
  • FIG. 8 is a table showing “Table 5. Actual Product Adhesion Measurement Results (Cr)”.
  • FIG. 9 is a process diagram showing a conventional bright nickel plating method.
  • FIG. 10 is a process chart showing a conventional method for conducting a resin.
  • the method for producing a decorative garnish using a resin conductive material by sputtering according to the present invention is a pretreatment method in which the wet conductive method of the resin plating is changed to the dry conductive method. After the electrification, wet electroplating is performed as usual.
  • FIG. 1 is a process diagram showing a method for producing a decorative garment using the resin conductive material by sputtering in Example 1.
  • FIG. 2 shows an example of the bright nickel plating method.
  • (A) is a process diagram of a resin conductive treatment, and (b) is a wet electroplating process diagram.
  • FIG. 3 is a cross-sectional view of the plating film attached by the method for producing a decorative garment using the resin conductive material obtained by sputtering in Example 1.
  • the resin molded product is set in a jig, and the resin surface cleaning 'active process step S1 is performed. Inside the sputtering device, the surface of the resin molded product is cleaned with gas and activated by surface modification in a vacuum atmosphere, and then in the metal thin film formation step S2, the resin molding is performed in the same sputtering device.
  • a single metal having a strong binding force with oxygen, or an alloy containing a metal having a strong binding force with oxygen, or a magnetic metal or an alloy containing a magnetic metal is deposited by sputtering,
  • a conductive metal film is formed by sputtering a predetermined metal on the metal thin film formed on the resin molded product.
  • the surface of the resin molded product is roughened and a metal film is formed by a dry-type magnetron sputtering method or the like to impart conductivity.
  • the resin molded product subjected to the resin conductive treatment is a method for producing a decorative swaged product, in which the jig force is also removed and the electric galling process S5 to S10 is performed as described later.
  • Sputtering equipment used in magnetron sputtering is a vacuum atmosphere. This is an apparatus that ionizes the target metal and deposits it on the resin molded product by argon gas ion irradiation. This sputtering process forms a target metal film on the resin molded product or irradiates the resin molded product with gas.
  • the resin molded product to be used as a decorative product of the present invention is a so-called "appearance product” such as a resin-coated component for automobiles, a housing-related resin-plated component such as a shower or faucet component.
  • an adhesive product such as a resin-coated component for automobiles, a housing-related resin-plated component such as a shower or faucet component.
  • the plating film floats due to the separation of the resin-molded products, which may cause personal injury such as cutting hands. is important.
  • it is a “functional product” such as a printed circuit board, it is not necessary to apply such decoration.
  • a vacuum atmosphere such as a vacuum chamber one' ⁇ surface cleaning by sputtering, Clean and activate the surface of the resin in vacuum.
  • it is irradiated with argon gas with a small amount of air remaining.
  • ion source irradiation with argon and trace oxygen is performed.
  • This resin surface cleaning 'active step S1 can use a plasma treatment method by an arc plasma deposition method in addition to the magnetron' sputtering method.
  • the metal thin film forming step S2 is a step for securing the adhesion between the resin and the plating film by the magnetron-sutter method in a vacuum atmosphere such as a vacuum chamber.
  • Vacuum for example 10 _2 ⁇ 3 (10 - 2-3 square) pulled about Pa, chromium ionized to 0.01 to 50% by the plasma, molybdenum, tungsten, titanium, zirconium, aluminum - ⁇ beam, indium
  • a single metal of a metal having a strong binding force with oxygen, such as nickel, noradium (an oxyphilic metal) or an alloy containing these metals is formed on a resin molded article.
  • the metal thin film for ensuring the adhesion between the resin and the plating film is not only a good adhesion with the resin but also a conductive film for smoothly treating the electric plating in the next process. It is necessary to use a metal with good adhesion.
  • a film-forming metal material with good adhesion is selected according to the type of resin and molding conditions. For example, metallic copper can be used. There is no limit on the film thickness to ensure the adhesion of plating. Considering plating stress, 0.05 / ⁇ ⁇ to 0.5 / zm was appropriate.
  • the resin molded product that has undergone the metal thin film formation step S2 is further subjected to an activation treatment in an activation treatment step S3.
  • an activation treatment step S3 a metal thin film formed on a resin molded product at a ratio of 0.01 / ⁇ ⁇ to 2. O / z m is activated by an argon ion source treatment. This increases the adhesion between the resin molded product and the metal thin film.
  • Conductive film forming step S4 is a step of forming a conductive film for electroplating the resin molded article.
  • the conductive film for electroplating is a conductive film for electroplating, but the plating film formed by the dry plating method and the film deposited by the electroplating method are closely attached. It is necessary to be a metal film that can withstand acid treatment for ensuring the property, soft etching with a dilute oxidizing agent, or electrolytic activation treatment. Therefore, the appropriate film thickness by the conductive film forming step S4 is, for example, 0. force and 2. O / zm in the case of metallic copper.
  • This conductive film formation process S4 film formation is a pre-process (activation process) of wet electroplating (electrocopper plating and electronickel plating), which is a subsequent process that has good adhesion to the underlying metal.
  • a metal other than metallic copper can be deposited if S5 is simple and has high adhesion.
  • a dry squeeze film is activated in the activation step S5 on a resin molded product that has been subjected to a resin conductivity treatment by magnetron sputtering.
  • This activation process S5 is a process for ensuring close contact with the electric plating. For example, when copper was used as the final conductive metal for dry plating, it was performed in a soft etching process that was immersed for 30 seconds in a 20 gZL sodium persulfate solution.
  • This active process S5 depending on the type of conductive metal used in the dry plating. As long as the adhesion between the dry plating film and the electric plating film can be secured, the method is not limited.
  • Electrical plating process S6 to S10 are normal resin plating such as bright copper sulfate plating or metal plating
  • the electric mesh used in the can be adapted.
  • bright copper sulfate plating S6, semi-bright nickel plating S7, bright nickel plating S8, MP nickel plating (microporous nickel plating) S9 are applied in this order.
  • plating finish S10 with trivalent chromium plating, tin Z nickel alloy plating, ruthenium or gold plating, and finish the plating process.
  • This electric plating process S6 to S10 is an example, and it is needless to say that other metals can be bonded.
  • Fig. 4 is a table showing "Table 1. Plate adhesion measurement results”.
  • Figure 5 is a table showing “Table 2.
  • Fig. 6 is a table showing "Table 3. Results of actual product adhesion measurement (Ni-Cr) Nol”.
  • Fig. 7 is a table showing "Table 4. Actual product adhesion measurement results (Ni-Cr) No2”.
  • Fig. 8 is a table showing "Table 5. Actual product adhesion measurement results (Cr)”.
  • Figures 6 to 8 show the results for nickel and chromium alloys in Table 3. Actual product adhesion measurement results (Ni—Cr) Nol and Table 4. Actual product adhesion measurement results (Ni—Cr) No2. Table 5. Actual product adhesion measurement results (Cr) ”shows the results for chromium.
  • PCZABS resin plating prototype product of NiZCr experimental condition 10
  • PA / ABS resin plating prototype standard condition 30 ° C / 0.5Hr ⁇ 80 ° C / 0.5Hr, 120 cycles
  • the thermal shock test was conducted, but the buoyancy phenomenon due to the peeling of the thin resin layer film at the part was not confirmed. Therefore, it has been proved that the use of the method of the present invention makes it possible to mass-produce safe resin-plated parts.
  • the method for producing a decorative garnish using the resin conductive material by sputtering according to the present invention uses the dry galvanization method for the pretreatment of the resin plating, and thus, using conventional chromic acid. Unlike the conductive wrinkle treatment method, various types of resin can be targeted.
  • AB S resin acrylonitrile / butadiene / styrene
  • PCZABS resin polycarbonate Z acrylonitrile / butadiene / styrene
  • PC / PET resin polycarbonate / polyethylene terephthalate
  • PCZPBT resin polycarbonate Z polybutylene terephthalate
  • LCP resin liquid crystal polymer
  • PA resin polyamide
  • PA / ABS polyamide Z atari port-tolyl / butadiene / styrene
  • PPE resin polyphenylene ether
  • PP resin polypropylene
  • PPS resin polyphenylene sulfide
  • SPS resin crystalline polystyrene
  • PS resin polystyrene
  • MMA resin methyl methacrylate
  • epoxy resin urethane resin
  • PET resin polyethylene terephthalate
  • PBT oil polybutylene terephthalate
  • the adhesion between the nylon-based resin and the dry-type adhesive film is good.
  • Nylon-based resin is difficult to obtain a beautiful plating appearance due to etching treatment with hydrochloric acid or the like when wet-coated, and it is difficult to obtain a beautiful plating appearance. A beautiful appearance like a messy product can be obtained.
  • ABS resin generally used for resin plating a plating adhesion strength of 1 kgfZcm (9.8 N / cm) or more was obtained.
  • the test was conducted with a plating adhesion strength of 0.5 kgf / cm (4.9 NZcm) as a passing target value. I did it.
  • 1. OKgf / cm (9.8 NZcm) is set as an effort target value, but it can be used at 0.5 kgf / cm (4.9 NZcm) in actual use.
  • Adhesion can be improved by performing oxygen plasma treatment (including plasma treatment with air) together with resin cleaning prior to dry plating.
  • oxygen plasma treatment including plasma treatment with air
  • the conditions need to be changed depending on the resin and molding conditions.
  • the present invention provides a resin surface on a resin molded article by a processing method that does not use chemicals such as a mixed acid of chromic acid and sulfuric acid in a conventional etching process and a conductive plating process, that is, a dry method.
  • a processing method that does not use chemicals such as a mixed acid of chromic acid and sulfuric acid in a conventional etching process and a conductive plating process, that is, a dry method.
  • chemicals such as a mixed acid of chromic acid and sulfuric acid in a conventional etching process and a conductive plating process, that is, a dry method.
  • the present invention provides a conductive process by a dry method, thereby enabling the plating of a resin material that has been difficult to fit by a wet process, and a pretreatment process for various types of resin molded products. If it can carry out easily, it will not be limited to the above-mentioned fat.
  • a method for producing a decorative garment using the resin conductive material by sputtering according to the present invention includes: High-corrosion and heat-cycle resistant parts such as radiator grille, door regulator handle, knock door gauze, molding parts, etc., oil-resisting parts for automobiles such as handles and knobs that do not require high corrosion resistance It can be used for various applications such as metal fittings, products such as laptop casings, camera casings, and mobile phone casings that require high corrosion resistance.
  • the method for producing a decorative garnish using a resin conductive material by sputtering is a method for producing an automobile greaves component such as an automobile interior door handle, an exterior door handle, an exterior handle cover part, etc. It is suitable for products such as shower heads, faucet parts, etc. that are directly touched by people such as housing-related grease plated parts and mobile phone parts.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Mechanical Engineering (AREA)
  • Physical Vapour Deposition (AREA)
  • Electroplating Methods And Accessories (AREA)

Abstract

Dans le procédé de la présente invention, la surface d'un objet en résine moulée est rendue rugueuse et une électroconductivité est communiquée à l'objet par un procédé à sec sans produits chimiques classiques tels que l'acide chromique, ce qui entraîne une protection de l'objet vis-à-vis de la dégradation de surface par les produits chimiques, une réduction de la charge environnementale due à la non-utilisation de produits chimiques ayant un impact important sur l'environnement, l'inhibition du décollement des objets en résine plaquée, et une innocuité des objets. Le procédé comprend l'étape de nettoyage/activation de la surface (S1) consistant à réaliser le nettoyage de la surface et la modification/l'activation de la surface d'un objet en résine moulée par pulvérisation cathodique gazeuse, l'étape de formation d'une couche mince métallique (S2) consistant à former une couche mince métallique sur la surface de l'objet en résine résultant par pulvérisation cathodique métallique, l'étape de formation d'un film électroconducteur (S4) consistant à former un film électroconducteur de nickel, de cuivre ou analogue sur la couche mince métallique par pulvérisation cathodique, et l'étape finale de dépôt électrolytique consistant à réaliser le dépôt électrolytique de l'objet résultant en résine.
PCT/JP2006/313968 2006-07-05 2006-07-13 procédé de production d'objets plaqués de manière décorative en communiquant une électroconductivité à la résine par pulvérisation cathodique WO2008004315A1 (fr)

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PCT/JP2007/063324 WO2008004558A1 (fr) 2006-07-05 2007-07-03 Procédé de production un objet ornemental plaqué en convertissant une résine en une résine conductrice par métallisation sous vide et gabarit suspendu pour la fixation du moulage de résine

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JP2014524977A (ja) * 2011-06-29 2014-09-25 ヴァレオ セキュリテ アビタクル 選択的に金属化されたプラスチック部品および対応する製造プロセス
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US20100161359A1 (en) * 2008-12-18 2010-06-24 At&T Intellectual Property I, L.P. Risk Management for Cable Protection Via Dynamic Buffering
JP2014524977A (ja) * 2011-06-29 2014-09-25 ヴァレオ セキュリテ アビタクル 選択的に金属化されたプラスチック部品および対応する製造プロセス
CN107326414A (zh) * 2017-05-11 2017-11-07 厦门建霖工业有限公司 一种塑料基材无铬金属化方法
CN107326414B (zh) * 2017-05-11 2020-05-15 厦门建霖健康家居股份有限公司 一种塑料基材无铬金属化方法

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