WO2020000942A1 - Film mince de blindage électromagnétique transparent, flexible et étirable et son procédé de préparation - Google Patents

Film mince de blindage électromagnétique transparent, flexible et étirable et son procédé de préparation Download PDF

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Publication number
WO2020000942A1
WO2020000942A1 PCT/CN2018/123384 CN2018123384W WO2020000942A1 WO 2020000942 A1 WO2020000942 A1 WO 2020000942A1 CN 2018123384 W CN2018123384 W CN 2018123384W WO 2020000942 A1 WO2020000942 A1 WO 2020000942A1
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Prior art keywords
layer
transparent
colloidal particles
stretchable
flexible
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PCT/CN2018/123384
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English (en)
Chinese (zh)
Inventor
胡友根
赵涛
张馨予
梁先文
朱朋莉
孙蓉
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中国科学院深圳先进技术研究院
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Publication of WO2020000942A1 publication Critical patent/WO2020000942A1/fr

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    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00—Screening of apparatus or components against electric or magnetic fields
    • 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
    • B32B15/02—Layer formed of wires, e.g. mesh
    • 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
    • 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
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/10—Interconnection of layers at least one layer having inter-reactive properties

Definitions

  • the invention relates to an electromagnetic shielding material, particularly a transparent flexible stretchable electromagnetic shielding film and a preparation method thereof.
  • Electromagnetic shielding material is an effective means to protect against electromagnetic radiation pollution, and has received wide attention and application in recent years.
  • Chinese invention patent CN 102063951B proposes a transparent conductive film based on nano-imprint and nano-coating methods. Trenches are formed by nano-imprint, and nano-conductive materials are filled in the trenches, and then sintered to form high-performance conductive films. For making electromagnetic shielding films. During the sintering process of the nano-conductive material, the organic solvent is volatilized, and the metal particles in the conductive material are aggregated to form a conductive grid structure. In this solution, the conductive material is sintered at low temperature, and the contact resistance between metal particles is large, which affects the conductivity of the grid structure, thereby affecting the electromagnetic shielding performance of the thin film produced by this solution.
  • Invention patent CN106061218A discloses a method for manufacturing a transparent electromagnetic shielding film based on photolithography, electrodeposition process and embossing process. It has the advantages of high transparency, good temperature resistance, and can realize flexible bending and complex structure surface bonding. Claim.
  • the photolithography process often requires complex process technology and expensive equipment to support, and the production cost is high, which is not suitable for the low cost requirements of large-scale production.
  • transparent electromagnetic shielding films are based on polyester (PET) or polyimide (PI) materials, and often have only flexible flexibility, but not stretchability. This is suitable for flexible wearable electronics.
  • PET polyester
  • PI polyimide
  • the present invention provides a stretchable flexible transparent electromagnetic shielding film with low cost, simple structure, and convenient manufacture, and a preparation method thereof.
  • the invention first prepares a transparent elastic substrate, and then self-assembles colloidal particles on its surface.
  • a metal layer is prepared by etching and magnetron sputtering techniques. After removing the colloidal particles, a grid-like metal layer is obtained.
  • a transparent elastomer encapsulation layer is prepared, and the structure and performance of the mesh metal layer during mechanical deformation such as bending and stretching are further stabilized by firmly bonding the substrate layer and the encapsulation layer without an interface.
  • the stretchable flexible transparent electromagnetic shielding film provided by the present invention comprises a transparent flexible stretchable substrate layer; a hole grid metal shielding layer and a transparent flexible stretchable encapsulation layer;
  • the grid-like metal shielding layer is between a transparent flexible stretchable substrate layer and a transparent flexible stretchable encapsulation layer.
  • the transparent flexible stretchable substrate layer or transparent flexible stretchable encapsulation layer is made of one or more materials selected from silicone, thermoplastic polyurethane, and polyolefin elastomer transparent elastomer.
  • the silica gel is selected from the group consisting of polydimethylsiloxane, polydimethyldiphenylsiloxane, polyvinyltriisopropoxysilane, and polymethylvinylsiloxane.
  • the transparent flexible stretchable substrate layer and the transparent flexible stretchable packaging layer are made of the same material or different materials.
  • the transparent flexible stretchable substrate layer and the transparent flexible stretchable packaging layer are made of the same material, and the transparent flexible stretchable substrate layer and the transparent flexible stretchable packaging layer are made of the same material. The materials are fused with each other and there is no obvious interface.
  • the grid-shaped metal shielding layer is made of one or more magnetic shielding materials of gold, silver, copper, nickel, aluminum, iron, and carbon, and has a hole-like grid shape.
  • the hole grid metal shielding layer is made of one or more magnetic shielding materials of gold, silver, copper, nickel, aluminum, iron, and carbon by a physical vapor deposition or chemical vapor deposition method. Deposited in a transparent flexible stretchable substrate layer.
  • the minimum value of the grid line width of the grid-shaped metal shielding layer is 10 nm-100 ⁇ m, and preferably 100 nm-10 ⁇ m.
  • the maximum value of the grid line voids of the grid-shaped metal shielding layer is 100 nm-100 ⁇ m, and preferably 500 nm-50 ⁇ m.
  • the light transmittance of the stretchable flexible transparent electromagnetic shielding film is 50% or more, preferably 60% or more or 70% or more.
  • the stretchable flexible transparent electromagnetic shielding effectiveness is 30 dB or more, preferably 35 dB or more, or 50 dB or more.
  • the hole grid metal shielding layer is prepared by the following method:
  • the colloidal particles are removed by solvent dissolution and etching methods to obtain a grid-like metal shielding layer deposited on a transparent flexible stretchable substrate layer.
  • the diameter of the colloidal particles is higher than the highest value of the grid line voids of the grid-like metal shielding layer.
  • step ii) the distance between the non-closely arranged colloidal particles is higher than or equal to the minimum value of the grid line width of the grid-like metal shielding layer.
  • the etching method includes a plasma etching method and a reactive ion etching method.
  • the colloid particles used are selected from the group consisting of polystyrene microspheres, silica microspheres, polymethyl methacrylate microspheres, polyacrylic microspheres, polyphenolic resin microspheres, and polyurea resin microspheres.
  • Spheres poly (propylene methacrylate) microspheres.
  • the colloidal particles used are selected from 10 nm to 100 ⁇ m, preferably 100 nm to 50 ⁇ m.
  • the thickness of the transparent flexible stretchable substrate layer is 20-500 ⁇ m.
  • the thickness of the transparent flexible stretchable encapsulation layer is 20-500 ⁇ m.
  • the present invention also provides a method for preparing a stretchable flexible transparent electromagnetic shielding film, including the following steps:
  • the magnetic shielding material is sputtered on the non-tightly arranged single-layer colloidal particles and the transparent flexible stretchable substrate layer by physical vapor deposition and chemical vapor deposition methods;
  • the colloidal particles are removed by solvent dissolution and etching methods to obtain a grid-like metal shielding layer deposited on a transparent flexible stretchable substrate.
  • the preparation method includes the following steps:
  • the silicone prepolymer and its curing agent are mixed and heat-cured through casting, spin coating and other processes to obtain a transparent and flexible stretchable silicone substrate; or transparent thermoplastic polyurethane and polyolefin elastomer are used as raw materials and dissolved in a solvent
  • a transparent flexible stretchable polyurethane or polyolefin substrate is obtained through thermal curing treatment through processes such as injection molding, blow molding, extrusion, and spin coating.
  • Plasma etching, reactive ion etching and other methods are used to etch the close-packed single-layer colloidal particles into a non-close-packed shape
  • magnetic shielding materials such as gold, silver, copper, nickel, aluminum, iron, and carbon are sputtered onto non-tightly arranged single-layer colloidal particles and a transparent flexible stretchable substrate ;
  • the colloidal particles are removed by solvent dissolution and etching to obtain a grid-like metal shielding layer deposited on a transparent flexible stretchable substrate.
  • the transparent flexible stretchable substrate, the grid-like metal shielding layer, and the transparent flexible stretchable encapsulation layer together form a flexible transparent stretchable electromagnetic shielding film, in which the grid-like metal shielding layer is on a transparent flexible stretchable liner. Between the bottom and the transparent flexible stretchable encapsulation layer.
  • the structure of the present invention is simple and stable. It is a sandwich sandwich structure of a stretchable transparent film on the upper and lower layers and a grid-like metal layer in the middle layer. The upper and lower materials are firmly bonded through the gap area of the metal grid, thereby making the middle The structure of the metal grid layer can maintain good stability even in the state of bending and stretching.
  • the preparation process of the present invention is simple.
  • the grid-like metal layer adopts colloidal particle self-assembly and etching methods to achieve non-close contact arrangement.
  • the grid-like metal layer can be formed on a transparent elastic substrate through a magnetron sputtering process.
  • the invention has high light transmittance and electromagnetic shielding effectiveness, and it is easy to realize performance regulation.
  • the size of the metal grid line width (tens of nanometers to tens of micrometers) and the grid gap (hundreds of nanometers to tens of micrometers) can be easily realized. , And then control its light transmittance and electromagnetic shielding performance.
  • FIG. 1 is a schematic structural diagram (a plan view) of a stretchable flexible transparent electromagnetic shielding film.
  • FIG. 2 is a schematic structural diagram (section) of a stretchable flexible transparent electromagnetic shielding film.
  • FIG. 3 is a schematic structural view of a stretchable flexible transparent electromagnetic shielding film in a stretched state (plan view).
  • 1 is a transparent flexible stretchable substrate
  • 2 is a transparent flexible stretchable encapsulation layer
  • 3 is a grid-like metal shielding layer.
  • FIG. 4 is a SEM image of a hole-shaped gold film shielding layer vapor-deposited on the surface of the PDMS film without an encapsulation layer.
  • FIG. 5 is a SEM image of a hole-shaped gold film shielding layer vapor-deposited on the surface of the PDMS film without an encapsulation layer.
  • Polydimethylsiloxane (PDMS) precursor and its curing agent were mixed at a mass ratio of 10: 1, and the mixed solution was spin-coated on a glass substrate by a spin coating process, and then heated and cured at 60 ° C for 30 minutes to form a half. Cured PDMS film.
  • the thickness of the final PDMS film (20-500 ⁇ m) can be adjusted by controlling the spin speed (400-2000 rpm) and time (5-30 seconds).
  • the PS microsphere colloid single layer was self-assembled on the surface of the PDMS film by a gas-liquid interface self-assembly method to form a close-packed PS colloid array .
  • the plasma is used to etch the closely arranged PS colloidal particles into a non-closely arranged structure.
  • the degree of etching (the distance between adjacent PS colloidal particles) can be determined by the etching power and the etching time. Regulate and control, in this case, the pitch is controlled to about 1 ⁇ m.
  • Metal silver was deposited on the above-not-closely arranged PS colloidal particles and their PDMS substrate (the front surface of the PS colloidal particles and the PDMS surface between the colloidal particles) by the magnetron sputtering method. Due to the low elastic modulus of semi-cured PDMS, the magnetron sputtered silver will be embedded into the inner surface layer of the PDMS film to some extent, forming a more stable conductive silver layer. Solvents such as N, N-dimethylformamide, toluene, and tetrahydrofuran are used to dissolve and remove the PS colloid particles. In this process, the silver deposited on the surface of the PS colloid particles will be removed by the disappearance of the PS carrier, leaving only the deposition.
  • Solvents such as N, N-dimethylformamide, toluene, and tetrahydrofuran are used to dissolve and remove the PS colloid particles. In this process, the silver deposited on the surface of the PS colloid particles will be removed by
  • the grid-like metallic silver on the PDMS film that is, the electromagnetic shielding metal layer.
  • a PDMS encapsulation layer was prepared on the surface of the grid-like metallic silver PDMS film by spin coating again, and the film formation conditions were 80 ° C and 2 hours. Since the PDMS in the first step is a semi-cured body, during the curing process of the re-encapsulation layer, the two will continue to undergo chemical cross-linking reactions at the interface, thereby forming a strong bond without an obvious interface layer, and further stabilizing the grid-like metallic silver. It is fixed between the PDMS substrate layer and the encapsulation layer.
  • both the PDMS substrate and the encapsulation layer are transparent, and the line width of the grid-like silver conductive network in the middle is only about 1 ⁇ m, which has good light transmittance, the PDMS film can be pulled off from the glass substrate to obtain a pull.
  • Flexible transparent electromagnetic shielding film its light transmittance is 85%, and its electromagnetic shielding effectiveness is 35dB.
  • thermoplastic polyurethane TPU
  • DMF dimethylformamide
  • TPU thermoplastic polyurethane
  • silica (SiO 2 ) microsphere dispersion with an average particle diameter of 500 nm as a colloid a single layer of SiO 2 microsphere colloid was self-assembled on the surface of the TPU film by a self-assembly method to form a closely-aligned SiO 2 colloid array.
  • Re-reactive ion etching etches closely-aligned PS colloidal particles into a non-close-packed structure.
  • the degree of etching (the distance between adjacent SiO 2 colloidal particles) can be measured by gas flow, temperature, and gas pressure. The etching process is controlled, and the shortest distance between SiO 2 colloidal particles is controlled at about 200 nm in this case.
  • Gold was deposited onto the above-not-closely arranged SiO 2 colloidal particles and its TPU substrate (the front surface of the SiO 2 colloidal particles and the surface of the gap TPU between the colloidal particles) by a magnetron sputtering method.
  • the magnetron sputtered gold will be embedded into the inner surface layer of the TPU film to some extent, forming a more stable conductive gold layer.
  • hydrofluoric acid is used to dissolve and remove the SiO 2 colloidal particles.
  • the gold deposited on the surface of the SiO 2 colloidal particles will be removed due to the disappearance of the SiO 2 carrier, leaving only the grid-like metal gold deposited on the TPU film. , That is, the electromagnetic shielding metal layer.
  • a TPU encapsulation layer was prepared on the surface of the TPU film of the grid-like gold layer by spin coating, blade coating, and casting.
  • the solvent contained in the TPU solution of the encapsulation layer can dissolve the TPU of the substrate layer to a certain extent at the interface, the TPU substrate layer and the TPU encapsulation layer can form a strong bond without obvious interface during the film formation process of the encapsulation layer.
  • the grid-like gold layer is stably fixed between the TPU substrate layer and the encapsulation layer. Because the TPU substrate and the encapsulation layer are both transparent, and the line width of the grid-like gold conductive network in the middle is only about 200 nm, which has good light transmittance, a stretchable flexible transparent electromagnetic shielding film is prepared. The optical efficiency is 70% and the electromagnetic shielding effectiveness is 50dB.

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  • Engineering & Computer Science (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
  • Laminated Bodies (AREA)

Abstract

Film mince de blindage électromagnétique transparent, flexible et étirable et son procédé de préparation. Le film mince de blindage électromagnétique comprend : un substrat transparent, flexible et étirable ; une couche de blindage métallique en forme de grille ; et une couche d'encapsulation transparente, flexible et étirable. La couche de blindage métallique en forme de grille se trouve entre le substrat transparent, flexible et étirable et la couche d'encapsulation transparente, flexible et étirable. La couche de blindage métallique en forme de grille est préparée au moyen d'une combinaison d'un procédé de gravure colloïdale et d'un procédé de dépôt de métal, et les étapes principales de ceux-ci sont : 1) l'agencement étroit d'une seule couche de particules colloïdales sur le substrat transparent, flexible et étirable ; 2) la gravure de la couche unique de particules colloïdales étroitement agencées pour qu'elles soient dans un agencement non étroit ; 3) le dépôt d'une couche de nano-métal sur le substrat transparent, flexible et étirable pour la couche unique de particules colloïdales non étroitement agencées ; et 4) l'élimination des particules colloïdales pour obtenir la couche de blindage métallique en forme de grille déposée sur le substrat transparent, flexible et étirable. Le film mince de blindage électromagnétique flexible et étirable préparé selon la présente invention est de structure simple et facile à fabriquer, et présente une bonne aptitude à l'étirage et une bonne performance de blindage électromagnétique.
PCT/CN2018/123384 2018-06-25 2018-12-25 Film mince de blindage électromagnétique transparent, flexible et étirable et son procédé de préparation WO2020000942A1 (fr)

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CN201810660647.5A CN108882661B (zh) 2018-06-25 2018-06-25 一种透明柔性可拉伸的电磁屏蔽薄膜及其制备方法
CN201810660647.5 2018-06-25

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CN108882661B (zh) * 2018-06-25 2020-05-01 中国科学院深圳先进技术研究院 一种透明柔性可拉伸的电磁屏蔽薄膜及其制备方法
CN110003514B (zh) * 2019-04-16 2020-07-21 电子科技大学 一种高介电复合膜的制备方法和应用
CN110430741B (zh) * 2019-08-09 2021-09-07 北京航空航天大学 一种电磁屏蔽材料及其制备装置和制备方法
CN110767736A (zh) * 2019-11-06 2020-02-07 武汉华星光电半导体显示技术有限公司 显示面板及其制备方法、显示装置
CN111511181B (zh) * 2020-05-18 2022-08-12 深圳先进技术研究院 一种图案化电磁屏蔽材料及其制备方法和应用
CN114472915B (zh) * 2022-01-19 2023-07-28 东南大学 一种可拉伸仿生簇状金纳米线薄膜及制备方法与应用

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