JP2016175828A - 酸化グラフェンの取得方法 - Google Patents
酸化グラフェンの取得方法 Download PDFInfo
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- JP2016175828A JP2016175828A JP2016051329A JP2016051329A JP2016175828A JP 2016175828 A JP2016175828 A JP 2016175828A JP 2016051329 A JP2016051329 A JP 2016051329A JP 2016051329 A JP2016051329 A JP 2016051329A JP 2016175828 A JP2016175828 A JP 2016175828A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 117
- 238000000034 method Methods 0.000 title claims abstract description 60
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 55
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 61
- 239000010439 graphite Substances 0.000 claims abstract description 61
- 238000002156 mixing Methods 0.000 claims abstract description 21
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 13
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 10
- 150000003839 salts Chemical class 0.000 claims abstract description 7
- 238000000746 purification Methods 0.000 claims description 7
- 239000002356 single layer Substances 0.000 abstract description 40
- 238000004519 manufacturing process Methods 0.000 abstract description 17
- 238000007306 functionalization reaction Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract 1
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 24
- 239000000463 material Substances 0.000 description 21
- 238000007254 oxidation reaction Methods 0.000 description 14
- 238000011282 treatment Methods 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 12
- 239000004317 sodium nitrate Substances 0.000 description 12
- 235000010344 sodium nitrate Nutrition 0.000 description 12
- 230000003647 oxidation Effects 0.000 description 8
- 238000000527 sonication Methods 0.000 description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 6
- 229910017604 nitric acid Inorganic materials 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 5
- 239000007770 graphite material Substances 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 238000004630 atomic force microscopy Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000004299 exfoliation Methods 0.000 description 4
- 239000007800 oxidant agent Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 229910021382 natural graphite Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 229910016001 MoSe Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002717 carbon nanostructure Substances 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000002800 charge carrier Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- -1 oxygen peroxide Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- 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
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
- C01B32/178—Opening; Filling
-
- 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
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
- C01B32/192—Preparation by exfoliation starting from graphitic oxides
-
- 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
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/23—Oxidation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
Description
酸化グラフェンを取得する方法であって、
a)グラファイトに酸及び塩を添加して酸化グラファイトを取得するステップ、
b)前記酸化グラファイトを混合することによって該酸化グラファイトを剥離するステップ
を含み、
前記ステップa)及びb)は高せん断混合機内で同時に行われることを特徴とする、前記方法を提供する。
−高い官能基化レベルの酸化グラフェン
−高い単層含有量(>99.8%)
−短い生成時間
−高い全生成量
−環境保全性
−容易に拡張可能な生成方法。
最も好ましくは、前記ステップa)又はb)において他の成分を添加しない。具体的には、好ましい実施形態に従って、本発明において硝酸ナトリウムは使用しない。
c)精製が完了した後に前記高せん断混合機内で第2の混合ステップを行うステップ
を含む。
従って、前記反応が完了した後に前記物質を精製しかつ非常に高い割合(>99.8%)の単層の酸化グラフェン・フレークを取得するために第2の高せん断混合を行う。
a)グラファイトに酸及び塩を添加して酸化グラファイトを取得するステップ、
b)前記酸化グラファイトを混合することによって該酸化グラファイトを剥離するステップ
を含み、
前記ステップa)及びb)は高せん断混合機内で同時に行われる。
工業的展望から、生成方法は費用効率が高いことが要されるだけでなく再現性も極めて重要なファクターである。これに関連して、本発明者らは異なるバッチから生成された酸化グラフェン物質を分析することによって本発明の製造方法の再現性を評価した。元素分析は生成された酸化グラフェン・フレークの酸化レベルを決定するために使用した。観察できるように、酸化レベルは全ての製造バッチでほぼ同一である。
単層の酸化グラフェン・フレークを生成するための従来技術で最も確立された手順は精製した酸化グラファイト物質を超音波処理することである。前記超音波処理により酸化グラファイトは個々の単層の酸化グラフェン・フレークに剥離される。しかしながら、高濃度の分散物(2〜4g/L)を使用するので、高い単層の酸化グラフェン含有量を得るためには非常に長い剥離時間が必要とされる。前記超音波処理を本発明で行う処理と比較すると、提案した方法は格段に速いため、より費用効率が高くはるかに高い収率の単層フレークを生成すると明確に結論付けることができる。
図4A及び図4Bに、高せん断混合処理後の分散物の高い単層含有量を見ることができる。本発明の方法を用いて生成した酸化グラフェン・フレークの98%は単層であることは明らかである。実際、より暗い領域は互いに接触しているフレークに対応し二重層のフレークではない。
生成した単層の酸化グラフェン・フレークの厚みを証明するためにAFM(原子間力顕微鏡法)を使用する。図6及び図7に前記フレークの厚みは数ナノメーター、正確には酸化グラフェンの単層フレークに関して文献で報告された厚みであることが観察できる。
本発明の方法によって得られた酸化グラフェンを用い、型に高濃度の分散物を流し込み蒸発により水を除去することによって膜を調製することができる。乾燥後、この酸化グラフェン・ペーパーを前記型から容易に取り外しレーザー閃光技術を用いて熱伝導率を測定するために高温(300℃、600℃、1000℃)で小片を処理した。表3に見ることができるように、前記ペーパーを1000℃まで処理したとき、前記熱伝導率は15倍上昇した。
Claims (4)
- 酸化グラフェンを取得する方法であって、
a)グラファイトに酸及び塩を添加して酸化グラファイトを取得するステップ、
b)前記酸化グラファイトを混合することによって該酸化グラファイトを剥離するステップ
を含み、
前記ステップa)及びb)は高せん断混合機内で同時に行われることを特徴とする、前記方法。 - 前記酸は硫酸であり、前記塩は過マンガン酸カリウムである、請求項1に記載の方法。
- 前記ステップa)又はb)において他の成分を添加しない、請求項1又は2に記載の方法。
- 前記方法はさらに
c)精製が完了した後に前記高せん断混合機内で第2の混合ステップを行うステップ
を含む、請求項1乃至3のいずれか一項に記載の方法。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP15382123.6A EP3070053B1 (en) | 2015-03-17 | 2015-03-17 | Method for obtaining graphene oxide |
EP15382123.6 | 2015-03-17 |
Publications (2)
Publication Number | Publication Date |
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JP2016175828A true JP2016175828A (ja) | 2016-10-06 |
JP6893394B2 JP6893394B2 (ja) | 2021-06-23 |
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JP2016051329A Active JP6893394B2 (ja) | 2015-03-17 | 2016-03-15 | 酸化グラフェンの取得方法 |
Country Status (4)
Country | Link |
---|---|
US (1) | US9731973B2 (ja) |
EP (1) | EP3070053B1 (ja) |
JP (1) | JP6893394B2 (ja) |
ES (1) | ES2671498T3 (ja) |
Cited By (20)
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US9744617B2 (en) | 2014-01-31 | 2017-08-29 | Lockheed Martin Corporation | Methods for perforating multi-layer graphene through ion bombardment |
US9834809B2 (en) | 2014-02-28 | 2017-12-05 | Lockheed Martin Corporation | Syringe for obtaining nano-sized materials for selective assays and related methods of use |
US9833748B2 (en) | 2010-08-25 | 2017-12-05 | Lockheed Martin Corporation | Perforated graphene deionization or desalination |
US9844757B2 (en) | 2014-03-12 | 2017-12-19 | Lockheed Martin Corporation | Separation membranes formed from perforated graphene and methods for use thereof |
US9870895B2 (en) | 2014-01-31 | 2018-01-16 | Lockheed Martin Corporation | Methods for perforating two-dimensional materials using a broad ion field |
JP2018083722A (ja) * | 2016-11-21 | 2018-05-31 | 大阪瓦斯株式会社 | 薄片状カーボンの製造方法 |
US10005038B2 (en) | 2014-09-02 | 2018-06-26 | Lockheed Martin Corporation | Hemodialysis and hemofiltration membranes based upon a two-dimensional membrane material and methods employing same |
US10017852B2 (en) | 2016-04-14 | 2018-07-10 | Lockheed Martin Corporation | Method for treating graphene sheets for large-scale transfer using free-float method |
US10118130B2 (en) | 2016-04-14 | 2018-11-06 | Lockheed Martin Corporation | Two-dimensional membrane structures having flow passages |
US10203295B2 (en) | 2016-04-14 | 2019-02-12 | Lockheed Martin Corporation | Methods for in situ monitoring and control of defect formation or healing |
US10201784B2 (en) | 2013-03-12 | 2019-02-12 | Lockheed Martin Corporation | Method for forming perforated graphene with uniform aperture size |
US10213746B2 (en) | 2016-04-14 | 2019-02-26 | Lockheed Martin Corporation | Selective interfacial mitigation of graphene defects |
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US9833748B2 (en) | 2010-08-25 | 2017-12-05 | Lockheed Martin Corporation | Perforated graphene deionization or desalination |
US10653824B2 (en) | 2012-05-25 | 2020-05-19 | Lockheed Martin Corporation | Two-dimensional materials and uses thereof |
US10201784B2 (en) | 2013-03-12 | 2019-02-12 | Lockheed Martin Corporation | Method for forming perforated graphene with uniform aperture size |
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US9731973B2 (en) | 2017-08-15 |
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EP3070053A1 (en) | 2016-09-21 |
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US20160272499A1 (en) | 2016-09-22 |
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