WO2016190259A1 - Graphène à faible réflexion, et graphène à faible réflexion destiné à être utilisé dans un élément optique - Google Patents

Graphène à faible réflexion, et graphène à faible réflexion destiné à être utilisé dans un élément optique Download PDF

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Publication number
WO2016190259A1
WO2016190259A1 PCT/JP2016/065082 JP2016065082W WO2016190259A1 WO 2016190259 A1 WO2016190259 A1 WO 2016190259A1 JP 2016065082 W JP2016065082 W JP 2016065082W WO 2016190259 A1 WO2016190259 A1 WO 2016190259A1
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Prior art keywords
graphene
low
reflection
low reflection
reflection graphene
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PCT/JP2016/065082
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English (en)
Japanese (ja)
Inventor
那由太 嶋田
健児 矢沢
貴壽 山田
雅考 長谷川
和輝 植草
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尾池工業株式会社
国立研究開発法人産業技術総合研究所
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Publication of WO2016190259A1 publication Critical patent/WO2016190259A1/fr

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    • 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
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G02B1/11—Anti-reflection coatings
    • G02B1/113—Anti-reflection coatings using inorganic layer materials only
    • G02B1/115—Multilayers
    • G02B1/116—Multilayers including electrically conducting layers

Definitions

  • the present invention relates to low reflection graphene and low reflection graphene for optical members.
  • the present invention relates to a low reflection graphene having a low light reflection characteristic below a certain level in the visible light region and the infrared region, and an optical member using the low reflection graphene.
  • Low reflection materials are conventionally used for controlling the amount of light reflection in various optical devices.
  • a lens optical system such as an optical microscope, a telescope, or a camera
  • noise can be reduced by using a low reflective material. This is because the stray light phenomenon in which light incident from the lens is confined in a lens barrel or the like and repeatedly reflected inside can be reduced.
  • the above stray light may be detected by a detector, and it may not be possible to determine whether it is an observation target or noise derived from stray light.
  • a material for reducing such a decrease in stray light a material having lower reflection is desired.
  • JP 2002-146533 A Japanese Patent No. 4762945
  • the present invention solves the above-mentioned problem, and particularly, low reflection graphene having a low total light reflectance in a region of a wavelength of 200 nm or more and 2000 nm or less that covers an ultraviolet region and an infrared region, and It is an object to provide a utilized optical member.
  • a low-reflection graphene with a thin film thickness and an optical member using the same are provided.
  • graphene is actively developed as a transparent conductive film or other material or member that transmits light, but the inventors have intensively studied, and have a completely different concept from the conventional low-reflective graphene and an optical member using the same. Found to provide.
  • low reflection graphene having a total light reflectance of 1.5% or less in a wavelength range of 200 nm to 2000 nm.
  • a first graphene layer having a plane substantially parallel to a first direction, and an orientation in a second direction connected to the first graphene layer and intersecting the first direction A low-reflection graphene is provided.
  • low-reflection graphene in the Raman resonance spectroscopy, low-reflection graphene is provided a peak in a wave number range 2550 cm -1 or 2800 cm -1 is observed.
  • an optical member using low-reflection graphene as a cylindrical base material is provided.
  • a noise reduction wall for optical wireless communication using low reflection graphene as a wall surface is provided.
  • a display device using low-reflection graphene as a conductive low-reflection film is provided.
  • a graphene film having a total light reflectance of 1.5% or less in a wavelength range of 200 nm to 2000 nm by introducing methane gas, argon gas, and hydrogen gas into a plasma CVD film forming apparatus. Is provided on a substrate, and a method for forming a low reflection graphene is provided.
  • low-reflectance graphene and a manufacturing method thereof are provided.
  • Patent Document 1 describes a carbon thin body having a structure capable of producing a planar electron source by a simple method.
  • this document is not a material that focuses on reflectivity.
  • Patent Document 2 includes a substrate having no metal catalyst, and a number of wall shapes standing directly on the surface of the substrate.
  • the thickness is 0.05 nm to 30 nm, and the vertical and horizontal lengths of the surface.
  • graphene that exhibits extremely low reflection with a relative total reflectance of 1.5% in the region of 200 nm to 2000 nm that covers the visible light region and the infrared region.
  • a method for producing such low reflection graphene is provided.
  • the low reflection graphene according to the present invention will be described with reference to the drawings.
  • the low reflection graphene of the present invention is not construed as being limited to the description of the embodiments and examples shown below. Note that in the drawings referred to in this embodiment mode and examples, the same portions or portions having similar functions are denoted by the same reference numerals, and repetitive description thereof is omitted.
  • FIG. 1 is a schematic diagram showing a low reflection graphene 1 according to an embodiment of the present invention.
  • the graphene of the present invention has a first graphene layer 13 extending substantially parallel to the base material 10 and a second graphene layer 15 standing on the first graphene layer 13.
  • up, down, left, and right are defined in the direction when the base material direction is down in the drawings.
  • the stacking direction of the surface formed by the first graphene layer 13 is defined as the first direction L1
  • the orientation direction of the surface formed by the second graphene layer 15 is defined as the second direction L2.
  • the base material 10 can use copper foil.
  • a metal having a catalytic function such as nickel, cobalt, or chromium, or a metal such as aluminum, a silicon substrate, a glass substrate, a Ge substrate, a ZnS substrate, a fluoride substrate such as calcium fluoride, sapphire, or the like
  • An inorganic substrate such as an oxide substrate may be used, and a resin substrate such as PET (polyethylene terephthalate), PEN (polyethylene naphthalate), PC (polycarbonate), acrylic, and polyimide may be used as the organic substrate.
  • the present embodiment is characterized in that since it has the first graphene layer 13 extending in the first direction L1, the adhesive surface with the base material 10 is wide and the mechanical strength is high. In addition, since the first graphene layer 13 extending in the first direction L1 as described above has high adhesion to the substrate, the low-reflection graphene 1 of the present embodiment is used as a desired substrate. It is possible to adhere.
  • the low-reflection graphene 1 when used in a lens barrel of a microscope, a telescope, a camera, etc., the low-reflection graphene 1 is laminated on copper foil, polyimide, etc., and this is attached to the inner member of the lens barrel so that the lens barrel can be easily assembled. Can do. Furthermore, in this embodiment, even when directly laminated on the internal member, the adhesive strength is such that it does not peel naturally. Thereby, it is possible to create a lens barrel more easily.
  • the base material 10 is shown as a flat plate structure for simplicity, but the low reflection graphene 1 according to the present invention is not limited to this, and curved surfaces such as a sphere and a lens-type structure are used. It may be a structure having a cylindrical structure, a structure having irregularities, a structure having a rough surface, a structure having a predetermined pattern shape, or the like.
  • the first direction is parallel to the planar direction of the base material for simplicity, but may be substantially parallel.
  • first direction L1 and the second direction L2 are orthogonal to each other.
  • first direction L1 and the second direction L2 do not have to be orthogonal, and may intersect at an angle of, for example, about 60 degrees.
  • the standing second graphene layer 15 does not have to be perfectly aligned in the L2 direction.
  • the low-reflection graphene 1 has the above-described structure and has an extremely low relative total light reflectance in a region of 200 nm to 2000 nm covering the ultraviolet region to the infrared region.
  • the reflectivity realized by the present invention cannot be achieved by a conventional method in which graphene is simply laminated immediately above.
  • the above characteristics are the first graphene layers stacked in the first direction L1. 13 and the second graphene layer 15 oriented in the second direction L2 combine the light confinement effect due to the formation of the recesses and the above-described characteristics of the high light absorptivity of the graphene, and thus a synergistic effect It can be said that it was generated.
  • a recessed part means that the shape which the 2nd adjacent 2nd graphene layer 15 and the 1st graphene layer 13 to which these adhere
  • the low reflection graphene 1 created as described above can be used as a wall surface material of a lens barrel as a countermeasure against stray light in the lens barrel described above.
  • the countermeasure against stray light in the lens barrel it can be used as a noise canceller in the field of optical wireless communication, for example.
  • a display device can be used as a low reflection film in a display device.
  • a display device that suppresses flickering and optical color mixing by suppressing the inflow of light from the outside of the panel by bonding to a substrate opposite to the light emitting surface is provided. Is possible.
  • a base material 10 having a predetermined shape is prepared.
  • the low reflection graphene 1 can be directly laminated on the base material 10, and the low reflection graphene 1 may be formed on another base material and disposed on the substrate 10.
  • the base material 10 the base material having the material and shape described in the first embodiment can be arbitrarily selected.
  • a plasma CVD film forming apparatus is used to install the base material in a quartz glass tube and introduce a carbon-containing gas, an inert gas, and an additive gas at a predetermined gas ratio to generate plasma.
  • the low reflection graphene 1 is formed on the substrate.
  • a low reflection graphene 1 can be formed on the copper foil by winding a heater around the glass tube and heating the copper foil at a high temperature.
  • microwave surface wave plasma chemical vapor deposition method microwave surface wave plasma CVD
  • International Publication No. 2011/115197 exists as a prior art.
  • the low reflection graphene 1 can be manufactured.
  • the substrate temperature is 500 ° C. or less, preferably 200 ° C. or more and 450 ° C. or less.
  • the pressure is 50 Pa or less.
  • the processing time is not particularly limited, but is about 1 second to 1000 seconds. Preferably, it is about 100 seconds or more and 600 seconds or less.
  • the gas ratio of the additive gas and the carbon-containing gas is necessary to make the gas ratio of the additive gas and the carbon-containing gas substantially the same or to increase the additive gas more than the carbon-containing gas.
  • the carbon-containing gas includes methane, ethylene, acetylene, ethanol, acetone, methanol and the like.
  • Inert gases include helium, neon, argon, and the like.
  • hydrogen gas is preferably used as the additive gas.
  • first graphene film 13 and the second graphene layer 15 may be a film of graphene or a film in which a plurality of layers are stacked. In view of handling the low reflection graphene 1, a graphene film in which a plurality of layers are oriented is preferable.
  • the low-reflection graphene including the first graphene layer 13 and the second graphene layer on the base material 10 By laminating the low-reflection graphene including the first graphene layer 13 and the second graphene layer on the base material 10 as described above, extremely low reflection with respect to light in the wavelength range of 200 nm to 2000 nm. It is possible to produce low reflection graphene that exhibits a rate. This is considered to be a combination of the above-described light confinement effect and the above-described characteristics of high light absorption of graphene, and the above manufacturing method is a technique capable of manufacturing unprecedented graphene. . In the present invention, it is also possible to form a film directly on the above-mentioned metal substrate, glass, polyimide film or the like.
  • Example 1 With a plasma CVD film forming device, a rolled copper foil (33 ⁇ m, Fukuda Metal Foil Powder Industry) is placed in a quartz glass tube, and methane gas, argon gas, and hydrogen gas are introduced at a gas ratio of 6: 1: 6, and a pressure valve The pressure was adjusted so that the internal pressure was 10 Pa. Thereafter, plasma was generated in the chamber to form low reflection graphene 1 on the rolled copper foil. The film formation time was 600 seconds.
  • FIG. 2 shows the reflectance of the low-reflection graphene of Example 1 at a wavelength of 200 nm to 2000 nm. From the results of FIG. 2, it can be seen that the low reflection graphene of Example 1 has a reflectance of less than 1.5% for wavelengths of 200 nm to 2000 nm.
  • FIG. 3 shows a Raman spectrum measured using a 532 nm wavelength laser by a RENISYO Raman apparatus. Peaks due to graphene structure 2550 cm -1 or 2800 cm -1 The following regions were observed. In FIG. 3, the peak is marked with an arrow.
  • Comparative Example 1 Comparative Example 1 was obtained by bonding XGSscience carbon powder (C-750) to an adhesive tape to form a sheet.
  • FIG. 4 shows the reflectance of Comparative Example 1 at a wavelength of 200 nm to 2000 nm. From the result of FIG. 4, the comparative example 1 had a reflectance of 1.5% or more from a wavelength of about 1000 nm to 2000 nm.
  • Comparative Example 2 Comparative Example 2 was made using ACTER MetalVelvet, which is a commercially available low-reflection material. The sample is originally a sheet shape.
  • FIG. 6 shows the reflectance of Comparative Example 2 at a wavelength of 200 nm to 2000 nm. From the results of FIG. 6, although the reflectance is 1.5% or less from the wavelength of 200 nm to 990 nm, the reflection from the wavelength of 990 nm to 2000 nm is 1.5% or more.
  • Example 1 has a total light reflectance of 1.5% or less in the wavelength range of 200 nm to 2000 nm. It can also be seen from the resonance Raman scattering measurement that only Example 1 has a graphene structure. Therefore, it has been clarified that low reflection graphene having a low total light reflectivity can be provided in a region with a wavelength of 200 nm to 2000 nm that covers the ultraviolet region to the infrared region.
  • FIGS. 8 is a transmission electron image obtained by observing the upper part of the graphene of Example 1 at a magnification of 3 million times
  • FIG. 9 is a transmission electron image obtained by observing the lower part of the graphene of Example 1 at a magnification of 3 million times.
  • FIG. 12 reveals that the second graphene layer 15 extends in the second direction and is stacked in the first direction (left-right direction).
  • Example 1 the graphene layer 13 stacked in the first direction L1 and the second graphene layer 15 stacked in the second direction L2 form the above-described recess. I understand.
  • FIG. 10 shows a secondary electron image obtained by observing Example 1 with a scanning electron microscope. Thereby, it can be seen that the second graphene layer 15 extends in the second direction L2 of the first embodiment.
  • it is a low-reflection graphene that synergistically satisfies the relative total light reflectance of 1.5% or less in the wavelength range of 200 nm to 2000 nm. I understood that.
  • the low reflection graphene in the present invention is an effect of not reflecting infrared lasers other than using the low reflection graphene material for stray light countermeasures in the optical member described above, a noise canceller in the field of optical wireless communication, a conductive low reflection film in a display device, etc. It is also possible to use as a low-infrared reflecting member (stealth) using

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Abstract

La présente invention concerne un graphène à faible réflexion dont la réflectance totale est de 1,5 % ou moins dans la gamme de longueurs d'onde de 200 à 2 000 nm inclus. En outre, le graphène à faible réflexion comprend une première couche de graphène qui a une surface à peu près parallèle à une première direction, ainsi qu'une seconde couche de graphène qui est reliée à la première couche de graphène et qui est orientée dans une seconde direction croisant la première direction.
PCT/JP2016/065082 2015-05-22 2016-05-20 Graphène à faible réflexion, et graphène à faible réflexion destiné à être utilisé dans un élément optique WO2016190259A1 (fr)

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JP2015104186A JP6032446B1 (ja) 2015-05-22 2015-05-22 低反射グラフェン、光学部材用低反射グラフェン
JP2015-104186 2015-05-22

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
JP2020514835A (ja) * 2017-03-24 2020-05-21 ソウル大学校産学協力団Ｓｅｏｕｌ Ｎａｔｉｏｎａｌ Ｕｎｉｖｅｒｓｉｔｙ Ｒ＆Ｄｂ Ｆｏｕｎｄａｔｉｏｎ 機能性コンタクトレンズおよびその製造方法
WO2024024753A1 (fr) * 2022-07-26 2024-02-01 国立大学法人東海国立大学機構 Électrode pour un dispositif de stockage d'énergie, batterie secondaire et procédé de fabrication d'une électrode pour un dispositif de stockage d'énergie

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CN110615997B (zh) * 2019-08-26 2021-11-23 Tcl华星光电技术有限公司 复合材料及其制备方法、显示面板
JP7498922B2 (ja) * 2020-03-17 2024-06-13 三恵技研工業株式会社 光吸収材料及びその製造方法

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JP2011133239A (ja) * 2009-12-22 2011-07-07 Stanley Electric Co Ltd 光強度測定装置及びその製造方法
JP2013037781A (ja) * 2011-08-03 2013-02-21 Panasonic Corp 透明導電性部材の製造方法、及び中間部材
US8481153B1 (en) * 2010-05-20 2013-07-09 The United States Of America As Represented By The Secretary Of The Navy Apparatus and method for imparting wide angle low reflection on conductive surfaces

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US7850319B2 (en) * 2004-05-27 2010-12-14 Panasonic Corporation Light-absorbing member
JP2012058584A (ja) * 2010-09-10 2012-03-22 Tohoku Univ 反射防止光学構造付き基板および反射防止光学構造付き基板の製造方法
JP5739175B2 (ja) * 2011-01-24 2015-06-24 株式会社カネカ グラフェン／高分子積層体およびその利用

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Publication number Priority date Publication date Assignee Title
JP2011133239A (ja) * 2009-12-22 2011-07-07 Stanley Electric Co Ltd 光強度測定装置及びその製造方法
US8481153B1 (en) * 2010-05-20 2013-07-09 The United States Of America As Represented By The Secretary Of The Navy Apparatus and method for imparting wide angle low reflection on conductive surfaces
JP2013037781A (ja) * 2011-08-03 2013-02-21 Panasonic Corp 透明導電性部材の製造方法、及び中間部材

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2020514835A (ja) * 2017-03-24 2020-05-21 ソウル大学校産学協力団Ｓｅｏｕｌ Ｎａｔｉｏｎａｌ Ｕｎｉｖｅｒｓｉｔｙ Ｒ＆Ｄｂ Ｆｏｕｎｄａｔｉｏｎ 機能性コンタクトレンズおよびその製造方法
WO2024024753A1 (fr) * 2022-07-26 2024-02-01 国立大学法人東海国立大学機構 Électrode pour un dispositif de stockage d'énergie, batterie secondaire et procédé de fabrication d'une électrode pour un dispositif de stockage d'énergie

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