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METHOD FOR PRODUCING GRAPHENE, AND GRAPHENE PRODUCTION EQUIPMENT meetings

Foreign code F200010272
File No. 評18-0002KG
Posted date Nov 24, 2020
Country WIPO
International application number 2019JP045320
International publication number WO 2020105646
Date of international filing Nov 19, 2019
Date of international publication May 28, 2020
Priority data
  • P2018-218478 (Nov 21, 2018) JP
Title METHOD FOR PRODUCING GRAPHENE, AND GRAPHENE PRODUCTION EQUIPMENT meetings
Abstract Provided are: a method for producing graphene, the method including a stripping step for applying a voltage between a pair of electrodes 30, 32 in a state in which the pair of electrodes are disposed in an electrolyte solution 20 that includes water and at least one electrolyte selected from the group consisting of inorganic acids, inorganic salts, organic acids, and bases, and in which graphite 10 is disposed between the pair of electrodes without being in contact with the electrodes, whereby graphene is stripped from the graphite, and a recovery step for recovering the graphene generated by stripping from the graphite; and graphene production equipment for implementing the method.
Outline of related art and contending technology BACKGROUND ART
Is composed of carbon atoms in the graphene sheet-like crystallized carbon, electrically conductive, thermal stability, toughness, and has excellent characteristics such as flexibility, the semiconductor device, solar cell, the transparent conductive film or the like in various fields are expected to be used.
As a practical production technique of graphene, graphite or graphene by delamination as the starting material is a top-down technique has attracted attention. In general, such as potassium permanganate and sulfuric acid and a strong oxidizing agent is concentrated sulfuric acid (strong acid) is used, graphite and chemically, graphene is manufactured, a large amount of reagent required for the particular attention to handling pure water for consumption, is demanded the development of new peeling method.
In recent years, graphite as an electrode in the electrolytic solution is energized, causing delamination of the graphite, graphene may be the electrochemical peeling method has attracted attention (for example, see Patent Document 1-7). For example, graphite as an anode using a low-concentration sulfuric acid at a relatively low voltage (for example 10V) is subjected to electrolysis, 1 peeled off within a short period of time that the graphite, graphene can be obtained.
On the other hand, N- (Bu4NBF4) methyl-2-pyrrolidone and tetrabutylammonium tetrafluoroborate (NMP) solution including an organic electrolyte, anode, cathode, and graphite powder was immersed in a high voltage is applied to 1100V after, 330000/s 1 in the high shear treatment of the method of obtaining graphene has been known (see Non-Patent Document 1).
Scope of claims (In Japanese)[請求項1]
 無機酸、無機塩、有機酸、及び塩基からなる群より選ばれる少なくとも1種の電解質と水とを含む電解液中に、一対の電極を配置し、かつ、前記一対の電極間に、前記一対の電極とは接触せずにグラファイトを配置した状態で、前記一対の電極間に電圧を印加することにより、前記グラファイトからグラフェンを剥離させる剥離工程と、
 前記グラファイトから剥離して生成したグラフェンを回収する回収工程と、
を含むグラフェンの製造方法。

[請求項2]
 前記電解液が、前記電解質として硫酸を含む請求項1に記載のグラフェンの製造方法。

[請求項3]
 前記電解液における前記硫酸の濃度が、1mM以上0.5M以下である請求項2に記載のグラフェンの製造方法。

[請求項4]
 前記グラファイトが、粒子状又は粉末状である請求項1~請求項3のいずれか1項に記載のグラフェンの製造方法。

[請求項5]
 前記グラファイトを、前記電解液が透過可能なフィルターに収容した状態で、前記一対の電極間に電圧を印加する請求項1~請求項4のいずれか1項に記載のグラフェンの製造方法。

[請求項6]
 前記一対の電極間に印加する電圧が、5V~80Vの範囲である請求項1~請求項5のいずれか1項に記載のグラフェンの製造方法。

[請求項7]
 無機酸、無機塩、有機酸、及び塩基からなる群より選ばれる少なくとも1種の電解質と水とを含む電解液が収容された容器と、
 前記容器内に配置された一対の電極と、
 前記一対の電極間に電圧を印加する電源と、
 前記容器内に配置された前記一対の電極間に、前記一対の電極とは接触せずにグラファイトを配置させるグラファイト配置手段と、
を備えるグラフェン製造装置。

[請求項8]
 前記グラファイト配置手段が、前記グラファイトを保持する保持部材を含む請求項7に記載のグラフェン製造装置。

[請求項9]
 前記保持部材が、前記グラファイトを収容し、かつ、前記電解液が透過可能な絶縁性のフィルターを含む請求項8に記載のグラフェン製造装置。

[請求項10]
 前記電解液を攪拌することにより、前記電解液中の前記グラファイトを分散させる撹拌装置を含む請求項7に記載のグラフェン製造装置。

[請求項11]
 前記グラファイトを前記一対の電極間で移動させる移動装置を含む請求項7~請求項10のいずれか1項に記載のグラフェン製造装置。

[請求項12]
 前記容器内の前記電解液を循環させる循環装置を含む請求項7~請求項11のいずれか1項に記載のグラフェン製造装置。
  • Applicant
  • ※All designated countries except for US in the data before July 2012
  • KOGAKUIN UNIVERSITY
  • OKAYAMA UNIVERSITY
  • Inventor
  • HASHIMOTO, Hideki
  • ASOH, Hidetaka
  • NISHINA, Yuta
IPC(International Patent Classification)
Specified countries National States: AE AG AL AM AO AT AU AZ BA BB BG BH BN BR BW BY BZ CA CH CL CN CO CR CU CZ DE DJ DK DM DO DZ EC EE EG ES FI GB GD GE GH GM GT HN HR HU ID IL IN IR IS JO JP KE KG KH KN KP KR KW KZ LA LC LK LR LS LU LY MA MD ME MG MK MN MW MX MY MZ NA NG NI NO NZ OM PA PE PG PH PL PT QA RO RS RU RW SA SC SD SE SG SK SL SM ST SV SY TH TJ TM TN TR TT TZ UA UG US UZ VC VN ZA ZM ZW
ARIPO: BW GH GM KE LR LS MW MZ NA RW SD SL SZ TZ UG ZM ZW
EAPO: AM AZ BY KG KZ RU TJ TM
EPO: AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR
OAPI: BF BJ CF CG CI CM GA GN GQ GW KM ML MR NE SN ST TD TG
Reference ( R and D project ) http://www.ns.kogakuin.ac.jp/~wwb1027/
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