WO2019187328A1 - Article décoratif transmettant des ondes millimétriques, film de miroir d'argent et son procédé de formation - Google Patents

Article décoratif transmettant des ondes millimétriques, film de miroir d'argent et son procédé de formation Download PDF

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Publication number
WO2019187328A1
WO2019187328A1 PCT/JP2018/043018 JP2018043018W WO2019187328A1 WO 2019187328 A1 WO2019187328 A1 WO 2019187328A1 JP 2018043018 W JP2018043018 W JP 2018043018W WO 2019187328 A1 WO2019187328 A1 WO 2019187328A1
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WIPO (PCT)
Prior art keywords
silver mirror
mirror film
silver
solution
water
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PCT/JP2018/043018
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English (en)
Japanese (ja)
Inventor
宏明 安藤
美貴 北元
新太朗 大川
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豊田合成株式会社
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Publication of WO2019187328A1 publication Critical patent/WO2019187328A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/36—Successively applying liquids or other fluent materials, e.g. without intermediate treatment
    • B05D1/38—Successively applying liquids or other fluent materials, e.g. without intermediate treatment with intermediate treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/10—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by other chemical means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/06—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain multicolour or other optical effects
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • 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
    • C23C18/42—Coating with noble metals
    • C23C18/44—Coating with noble metals using reducing agents

Definitions

  • the present invention relates to a millimeter-wave permeable silver mirror film and a decorative product including the same.
  • a bright (metallic luster) film may be formed on exterior resin parts such as radiator grills, back panels, and side moldings for automobiles due to their design, and the bright film may be a metal plating film, a vacuum deposited film or a metal. Sputtering films are common.
  • a silver mirror film is known as a bright film that can be uniformly formed even on deep three-dimensional shaped products.
  • the silver mirror film consists of innumerable fine silver particles, and the formation method is to apply a silver mirror film-forming solution consisting of a silver mirror solution and a reducing solution immediately after mixing the two solutions, and then the silver mirror reaction (reduction ) To precipitate silver particles (Patent Document 2).
  • Patent Document 3 repeats spraying a silver mirror reaction treatment agent (a metal salt solution containing silver nitrate and a reducing agent solution) and an activation treatment agent (mixed solution of tin chloride and palladium chloride) almost simultaneously several times.
  • a silver mirror reaction treatment agent a metal salt solution containing silver nitrate and a reducing agent solution
  • an activation treatment agent mixed solution of tin chloride and palladium chloride
  • an object of the present invention is to provide a silver mirror film having both luster and millimeter wave permeability and a decorative product including the same.
  • the present inventor initially studied a method for forming a so-called half-gloss silver mirror film by performing a normal silver mirror reaction only for a short time or by making a silver mirror film-forming solution weak in silver mirror reaction. .
  • those with sufficient glitter cannot achieve millimeter wave transmission at all, and those with sufficient millimeter wave transmission do not have sufficient glitter, resulting in difficulty in solving the problem. Met. Therefore, a new method completely different from those methods was sought and the present invention was reached.
  • FIG. 1 is an image diagram of Examples 1 to 4 described later.
  • the process B tin fine particles adhere to the surface of the substrate.
  • silver particles adhere mainly to the surface of the base material starting from tin fine particles, and a part of the silver mirror film is formed. Since it is a part of the silver mirror film, the silver particles are small and often separated from each other. In addition, silver particles may adhere even where there are no tin fine particles.
  • the step ⁇ silver particles having a weak adhesion (particularly, silver particles adhering to a place where there is no tin fine particle) among the silver particles adhering in the step D1 (or D2) are removed, and the density of the silver particles is lowered.
  • step D2 silver adheres so as to cover the silver particles adhered in the process D1, and the silver particles become large. Some silver particles stick to each other, but many are still separated. In addition, silver particles may adhere even where there are no tin fine particles.
  • Millimeter-wave permeable silver mirror membrane L * a * b * color system L * value is 65 or more, and surface resistance is 1 ⁇ 10 11 ⁇ / ⁇ or more (preferably 3 ⁇ 10 11 ⁇ / ⁇ )
  • Millimeter-wave transparent decorative product The L * value of the L * a * b * color system formed on the base material and the surface of the base material is 65 or more, and the surface resistance value is 1 ⁇ 10 11 ⁇
  • FIG. 1 is an image diagram of the first to fourth embodiments.
  • FIG. 2 is an image diagram of Comparative Example 1.
  • 3A is a SEM photograph of the surface of Example 2
  • FIG. 3B is a SEM photograph of a cross section.
  • 4A is a SEM photograph of the surface of Example 3
  • FIG. 4B is a SEM photograph of a cross section.
  • 5A is a SEM photograph of the surface of Comparative Example 1
  • FIG. 5B is a SEM photograph of the cross section.
  • FIG. 6 is an SEM photograph of the surface of Comparative Example 2.
  • 7A is a SEM photograph of the surface of Comparative Example 5
  • FIG. 7B is a SEM photograph of the cross section.
  • FIG. 8 is an SEM photograph of the surface of Comparative Example 6.
  • FIG. 9 is an SEM photograph of the surface of Comparative Example 9.
  • Step B Before Step B, a step (Aa) of forming an undercoat layer for improving cushioning properties, smoothness, adhesion to the substrate, and the like may be performed. Moreover, you may perform the plasma treatment process (Ab) for improving wettability, adhesiveness with a base material, etc. before the process B.
  • FIG. 1 Aa of forming an undercoat layer for improving cushioning properties, smoothness, adhesion to the substrate, and the like may be performed. Moreover, you may perform the plasma treatment process (Ab) for improving wettability, adhesiveness with a base material, etc. before the process B.
  • Process C Between the process B and the process D1, you may perform the process C which apply
  • step B When the tin chloride solution in step B is an acid solution, the tin chloride solution in step B may be used for step ⁇ , or step B may be performed as step ⁇ . In addition, step ⁇ may be performed with an acid solution other than the stannic chloride solution.
  • Process D1 and Process D2 are common in that a part of the silver mirror film is formed, but the content of each process may be the same or may be different in the silver mirror film forming liquid, the coating amount, and the like.
  • step E the silver mirror film is subjected to corrosion prevention treatment for the purpose of removing unreacted silver mirror film and stabilizing silver (preventing discoloration). Also good. Furthermore, after the step E, a step F for forming a topcoat layer may be performed for the purpose of protecting the silver mirror film or the like.
  • Base material The material of the base material is not particularly limited, and examples thereof include resin, glass, ceramics, and wood.
  • Decorative products are not particularly limited, but automotive exterior resin parts with millimeter-wave radar devices inside are suitable. Radiator grille, grill cover, side molding, back panel, bumper, emblem Etc. can be illustrated.
  • Examples 1 to 4 and Comparative Examples 1 to 9 of decorative articles composed of a base material, an undercoat layer, a silver mirror film, and a topcoat layer were prepared by the method described in the following Table 1 and the process described in the process description.
  • the base material a plate-like base material made of ABS resin and having a size of 100 mm ⁇ 100 mm ⁇ thickness 3.0 mm was used.
  • Step D1 shows an image diagram of Examples 1 to 4.
  • Comparative Example 1 a metallic gloss (full gloss) silver mirror film is formed in one step Da.
  • Comparative Examples 2 to 5 a semi-glossy (half gloss) silver mirror film was formed in one step Db.
  • Comparative Examples 6 to 9 a semi-glossy (half gloss) silver mirror film was formed in one step Dc.
  • FIG. 2 shows an image diagram of the comparative example.
  • curing agent diluent: leveling agent
  • diluent leveling agent
  • spray-coated on the surface of the substrate with a spray gun.
  • the film was kept at 65 ° C. for 30 minutes in a thermostatic bath, cured and dried to form an undercoat layer having a film thickness of 15 to 25 ⁇ m. Then, it washed with ion-exchange water.
  • Plasma treatment (only Example 4) The substrate was subjected to plasma treatment under the conditions of RF 100 W ⁇ O 2 process gas 50 sccm ⁇ 60 seconds by a sputtering apparatus i-miller II manufactured by Shibaura Mechatronics.
  • the surface conditioning liquid 1 was sprayed to adjust the surface of the substrate or the undercoat layer.
  • the following surface conditioning agents a and b were used.
  • ⁇ Surface conditioner a Product name “MFS surface conditioner A”, product number “MFS-40A” (aqueous solution of stannous chloride ⁇ 10%, hydrochloric acid ⁇ 5%) by surface chemical research institute with ion-exchanged water It was diluted 15 times (example: surface conditioning agent A 10 mL, ion exchange water 140 mL).
  • surface conditioner a surface conditioner b were mixed at a mass ratio of 1: 1 to prepare surface conditioner No. 1 and sprayed on the surface of the undercoat layer with a spray gun for 5 seconds. Thereafter, the mixture was allowed to stand for 10 seconds for permeation, washed with ion exchange water, air dried, and washed again with ion exchange water.
  • the surface conditioning solution 2 prepared in this way was sprayed on the surface of the undercoat layer for 2 seconds with a spray gun. Thereafter, it was allowed to stand for 10 seconds to allow penetration.
  • Silver mirror film (Examples 1 to 4 only) A silver mirror film-forming solution was applied to the base material (after undercoating or plasma treatment) (silver mirror coating) to form a part of the silver mirror film.
  • the following silver main liquid, silver secondary liquid, and reducing liquid were used as materials for the silver mirror film forming liquid.
  • Silver main liquid Product name “MFS silver main liquid”, product number “MFS-10” (surface solution of silver nitrate 8.4%, ammonium hydroxide to 5%)
  • Silver secondary liquid Product name “MFS silver secondary liquid” of Surface Chemical Laboratory, product number “MFS-20” (caustic soda up to 10%, ammonium hydroxide up to 5% aqueous solution)
  • Reducing solution Product name “MFS reducing agent” of Surface Chemical Laboratory, product number “MFS-30” (polysaccharide 5-15%, hydrochloric acid-5% aqueous solution)
  • the silver main solution is diluted 15 times with ion-exchanged water (eg; silver main solution 5 mL, water 70 mL), and the silver sub-solution is diluted 15 times with ion-exchanged water (eg; silver auxiliary solution 5 mL, water 70 mL).
  • the diluted solution was mixed to prepare a silver mirror solution.
  • the reducing solution was diluted 30 times with ion-exchanged water (eg, reducing solution 5 mL, water 145 mL) to prepare a reducing solution (diluted solution) containing 0.085 to 0.258 mol / L of aldehyde.
  • Step ⁇ is a step of applying an acid solution to the substrate and then washing with water in order to remove silver particles having weak adhesion.
  • the surface conditioner a in Step B was an acid solution, Step B was directly performed as Step ⁇ .
  • Step D2 Silver mirror film (Examples 1 to 4 only) Step D2 having the same contents as step D1 was performed to form a part of the silver mirror film.
  • Step D1 Full gloss silver mirror film (Comparative Example 1 only)
  • the same silver mirror solution and reducing solution as in Step D1 were simultaneously sprayed with a two-head spray gun, mixed in the air, and applied to the surface of the undercoat for 30 seconds.
  • silver particles were precipitated by the silver mirror reaction formula described in the above step D1, and a full-gloss silver mirror film (a general bright silver mirror film) was formed. Then, it washed with ion-exchange water.
  • the silver main solution is diluted 15 times with ion-exchanged water (eg; silver main solution 5 mL, water 70 mL), and the silver sub-solution is diluted 15 times with ion-exchanged water (eg; silver auxiliary solution 5 mL, water 70 mL).
  • the diluted solution was mixed to prepare a silver mirror solution.
  • the reducing solution was diluted 30 times with ion-exchanged water (eg, reducing solution 5 mL, water 145 mL) to prepare a reducing solution (diluted solution) containing 0.085 to 0.258 mol / L of aldehyde.
  • the silver main solution is diluted 15 times with ion-exchanged water (eg; silver main solution 5 mL, water 70 mL), and the silver sub-solution is diluted 15 times with ion-exchanged water (eg; silver auxiliary solution 5 mL, water 70 mL).
  • the diluted solution was mixed to prepare a silver mirror solution.
  • the reducing solution was diluted 30 times with ion-exchanged water (eg, reducing solution 5 mL, water 145 mL) to prepare a reducing solution (diluted solution) containing 0.085 to 0.258 mol / L of aldehyde.
  • Corrosion prevention treatment (all examples) For the purpose of removing unreacted substances from the silver mirror film and stabilizing silver (preventing discoloration), the anticorrosion solution was sprayed to carry out corrosion prevention treatment of the silver mirror film.
  • the following corrosion inhibitors were used as materials for the corrosion prevention liquid.
  • ⁇ Corrosion Inhibitor Product name “Ag Corrosion Inhibitor # 50” of Surface Chemical Laboratory, product number “MFS-50” (mixture of sodium thiosulfate 1-7%, acetic acid ⁇ 1%, aluminum sulfate ⁇ 1% Aqueous solution).
  • This corrosion inhibitor was diluted 50 times with ion-exchanged water (eg; 10 mL of corrosion inhibitor, 490 mL of water) to prepare a corrosion inhibitor, and sprayed onto the surface of the silver mirror film with a spray gun. While wet with the corrosion prevention liquid, it was washed with ion-exchanged water to wash away the excess of the corrosion prevention liquid. It was kept at 70 ° C. for 60 minutes in a constant temperature bath and dried.
  • ion-exchanged water eg. 10 mL of corrosion inhibitor, 490 mL of water
  • Topcoat layer (all examples) A top coat solution was applied to the silver mirror film after the corrosion prevention treatment for the purpose of protecting the silver mirror film and the like, and a top coat was applied. The following main agent, curing agent and diluent were used as the material for the topcoat solution.
  • Main agent Product name of “MFS Topcoat Special Main Agent (Clear)”, product number “MFS-61-2” (acrylic resin 33%, xylene (mixed) 25.1%, ethylbenzene 25.1%) N-butyl alcohol 10-15% and isobutyl alcohol 5-10%).
  • ⁇ Curing agent Product name “MFS Topcoat Special Curing Agent”, product number “MFS-62-2” of Surface Chemical Research Laboratory (xylene 10.7%, ethylbenzene 10.7%, isopropyl alcohol 25-30%, n A mixture of 1 to 5% butyl alcohol).
  • -Diluent Product name “MFS Top Coat Special Diluent” product number "MFS-63-2” (Toluene 30%, Xylene 25%, Ethylbenzene 25%, Methoxybutyl acetate 5-10% A mixture of 10 to 15% propylene glycol monomethyl ether acetate).
  • curing agents diluents were mixed at a mass ratio of 100: 20: 60 to 80 and spray-coated on the surface of the silver mirror film with a spray gun. After the application, it was held at 65 ° C. for 30 minutes in a thermostatic bath, cured and dried to form a topcoat layer having a thickness of 15 to 25 ⁇ m.
  • Millimeter-wave transmission attenuation was measured using an electromagnetic wave absorption measuring device (free space method, owned by Fine Ceramics Center). Specifically, at room temperature, W-band (76.575 GHz) electromagnetic waves are incident on the sample at an incident angle of 0 ° from the transmitter, and the electromagnetic waves are transmitted through the sample by a receiver facing the transmitter across the sample. The millimeter wave transmission attenuation in the round trip path was measured. The millimeter wave transmission attenuation by the silver mirror film was calculated by subtracting the millimeter wave transmission attenuation by the base material as the reference value. The calculation result is shown in 1.
  • W-band (76.575 GHz electromagnetic waves are incident on the sample at an incident angle of 0 ° from the transmitter, and the electromagnetic waves are transmitted through the sample by a receiver facing the transmitter across the sample.
  • the millimeter wave transmission attenuation in the round trip path was measured.
  • the millimeter wave transmission attenuation by the silver mirror film was calculated by subtracting the millimeter wave transmission attenuation
  • the L * value of the L * a * b * color system is 65 or more, the surface resistance value is 1 ⁇ 10 11 ⁇ / ⁇ or more, and millimeter waves
  • the transmission attenuation is 2 dB or less, and it has both glitter and millimeter wave transparency. This is considered to be due to the action described with reference to FIG. FIG. 1 shows the repetition of the process ⁇ and the process D2 only twice for the convenience of space.
  • Comparative Example 1 full gloss
  • Comparative Example 2 full gloss
  • Comparative Example 3 has glitter, but has a low surface resistance and does not have millimeter wave permeability. As shown in FIG. 2, it is considered that the silver particles adhere to each other and are stacked when the process Da is performed once for a long time.
  • Comparative Examples 2 to 9 half gloss
  • this invention is not limited to the said Example, It can change suitably and can be embodied in the range which does not deviate from the meaning of invention.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Chemically Coating (AREA)
  • Laminated Bodies (AREA)

Abstract

Le problème à résoudre par la présente invention est de fournir un film de miroir d'argent étant à la fois photoluminescent et transmettant des ondes millimétriques, et un article décoratif le comprenant. La solution selon l'invention porte sur : une étape B consistant à appliquer une solution de chlorure d'étain à un matériau de base, puis à rincer avec de l'eau ; une étape D1 pour appliquer un liquide de formation de film de miroir d'argent sur le matériau de base, former une partie d'un film de miroir d'argent et ensuite rincer avec de l'eau ; une étape β pour appliquer une solution d'acide sur le matériau de base et ensuite rincer avec de l'eau ; et une étape D2 pour appliquer le liquide de formation de film de miroir d'argent sur le matériau de base, former plus du film de miroir d'argent et ensuite rincer avec de l'eau. Les étapes β à D2 sont répétées une ou plusieurs fois pour terminer le film miroir d'argent.
PCT/JP2018/043018 2018-03-30 2018-11-21 Article décoratif transmettant des ondes millimétriques, film de miroir d'argent et son procédé de formation WO2019187328A1 (fr)

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JP2018066713A JP7106935B2 (ja) 2018-03-30 2018-03-30 ミリ波透過性加飾品、銀鏡膜及びその形成方法
JP2018-066713 2018-03-30

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JP2022044462A (ja) * 2020-09-07 2022-03-17 昭和電工マテリアルズ株式会社 積層構造体及び対象物検知構造
CN116133759A (zh) * 2020-07-17 2023-05-16 昭和电工材料株式会社 层叠体的制造方法

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WO2023243645A1 (fr) * 2022-06-13 2023-12-21 株式会社レゾナック Stratifié

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JPH0638860A (ja) * 1991-12-04 1994-02-15 Tetsuto Nakajima プラスチック鏡及びその製造方法
JPH11335858A (ja) * 1998-05-27 1999-12-07 Yuji Shikamata 銀鏡面の形成方法及びその溶液
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CN116133759A (zh) * 2020-07-17 2023-05-16 昭和电工材料株式会社 层叠体的制造方法
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JP2022044462A (ja) * 2020-09-07 2022-03-17 昭和電工マテリアルズ株式会社 積層構造体及び対象物検知構造
CN116133841A (zh) * 2020-09-07 2023-05-16 株式会社力森诺科 层叠结构体和对象物检测结构
JP7388323B2 (ja) 2020-09-07 2023-11-29 株式会社レゾナック 積層構造体及び対象物検知構造

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