JP2017128472A - 硫黄含有酸化グラフェン又は硫黄含有グラフェン及びその製造方法 - Google Patents
硫黄含有酸化グラフェン又は硫黄含有グラフェン及びその製造方法 Download PDFInfo
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Abstract
Description
本発明の硫黄含有酸化グラフェンは、酸化グラフェンを含む。酸化グラフェンは、天然又は人工グラファイトを酸化し、単層又は多層に剥離させ、単層酸化グラフェン又は多層酸化グラフェンの形態で調製できる。
本発明の硫黄含有グラフェンは、還元処理により完全に還元されており、グラフェンに硫黄原子がドープされている。硫黄含有グラフェンにおいても、硫黄原子は、前記グラフェンを構成する炭素原子と化学結合又は共有結合(C−S−C結合、C−SOX−C結合)しているため、前記グラフェンの表面に均一に硫黄原子をドープでき、導電性を向上できるとともに、硫黄原子の脱離も抑制できる。
本発明の硫黄含有酸化グラフェンのうち、還元処理されていない硫黄含有酸化グラフェンにおいて、硫黄原子の原子割合は、酸化グラフェンを構成する炭素原子に対して1〜15%であってもよく、例えば1.5〜10%、好ましくは2〜5%、さらに好ましくは3〜5%程度である。硫黄原子の割合が少なすぎると、導電性が低下する虞があり、多すぎると、製造が困難となる虞がある。
本発明の硫黄含有酸化グラフェンは、酸化グラフェン及び硫黄含有化合物を含むスラリーを液中プラズマ(ソリューションプラズマ)処理して酸化グラフェンに硫黄原子をドープするドープ工程を経て得られる。
実施例及び比較例で得られた硫黄含有酸化グラフェンの硫黄原子の含有量及び結合状態、酸素原子の含有量については、以下の測定装置を用いて、以下の測定条件で測定した。
測定条件:Al Monochrolated 7mm filament Kα線、絞り800μmφ、X線出力 350W。
評価用サンプルをロレスターGP((株)三菱アナリテック製)を用いて測定した。プローブとしては薄膜測定用のPSPを用いた。
(液中プラズマ処理)
イオン交換水20gを、1重量%酸化グラフェンスラリー((株)NISHINA materials製「RapGO−10」)80gと混合攪拌し、液中パルスプラズマ装置((株)栗田製作所製「MPPHV04」)を用いて、表1に示す条件で液中プラズマ処理を行った。反応後の温度は61℃であった。
得られたプラズマ処理溶液を、遠心分離機(日立工機(株)製「CR22N」)を用いて10,000Gで5分間遠心処理を行った後、上澄みを除去した。沈殿物にイオン交換水を添加して、再度、遠心処理した。この操作を3回繰り返し、精製スラリーを得た。
精製スラリーを約2重量%になるように稀釈し、ガラス基板にキャストし、ホットプレートを用いて45℃で1時間乾燥させた。乾燥後、真空乾燥機を用いて40℃で12時間乾燥させた後、さらに窒素雰囲気下で室温から200℃まで1時間かけて昇温し、還元サンプルを得た。
イオン交換水の代わりに、同量のDMSO((株)和光純薬製)を用いて液中プラズマ処理(反応後の温度71℃)する以外は比較例1と同様にして還元サンプルを得た。
反応時間を30分から90分に変更して液中プラズマ処理(反応後の温度84℃)する以外は実施例1と同様にして還元サンプルを得た。
Claims (11)
- 酸化グラフェンに硫黄原子がドープした硫黄含有酸化グラフェンであって、前記硫黄原子が、前記酸化グラフェンを構成する炭素原子と化学結合している硫黄含有酸化グラフェン。
- 硫黄原子の原子割合が、酸化グラフェンを構成する炭素原子に対して1〜30%である請求項1記載の硫黄含有酸化グラフェン。
- 表面抵抗が107Ω/□以下である請求項1又は2記載の硫黄含有酸化グラフェン。
- 表面抵抗が50Ω/□以下の導電性グラフェンである請求項1〜3のいずれかに記載の硫黄含有酸化グラフェン。
- 酸化グラフェン及び硫黄含有化合物を含むスラリーを液中プラズマ処理して酸化グラフェンに硫黄原子をドープするドープ工程を含む請求項1〜4のいずれかに記載の硫黄含有酸化グラフェンの製造方法。
- 硫黄含有化合物が低分子硫黄含有化合物である請求項5記載の製造方法。
- スラリーが水を含む請求項5又は6記載の製造方法。
- 硫黄原子がドープした酸化グラフェンを還元する還元工程をさらに含む請求項5〜7のいずれかに記載の製造方法。
- 還元工程において、不活性ガス雰囲気下、硫黄原子がドープした酸化グラフェンを加熱して還元する請求項8記載の製造方法。
- グラフェンに硫黄原子がドープした硫黄含有グラフェンであって、前記硫黄原子が、前記グラフェンを構成する炭素原子と化学結合している硫黄含有グラフェン。
- 酸化グラフェン及び硫黄含有化合物を含むスラリーを液中プラズマ処理して酸化グラフェンに硫黄原子をドープするドープ工程及び硫黄原子がドープした酸化グラフェンを還元する還元工程を含む請求項10記載の硫黄含有グラフェンの製造方法。
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JP2011126742A (ja) * | 2009-12-17 | 2011-06-30 | Sekisui Chem Co Ltd | 薄片化黒鉛分散液の製造方法、薄片化黒鉛の製造方法、及び、複合材料の製造方法 |
JP2013501696A (ja) * | 2009-08-07 | 2013-01-17 | ガーディアン・インダストリーズ・コーポレーション | グラフェンの広い領域の堆積およびドーピング、ならびにそれを含む生成物 |
JP2013139377A (ja) * | 2011-12-28 | 2013-07-18 | Qinghua Univ | 硫黄−グラフェン複合材料の製造方法 |
WO2015076565A1 (ko) * | 2013-11-19 | 2015-05-28 | 한화케미칼 주식회사 | 관능화 그래핀의 제조 방법, 제조 장치, 및 관능화 그래핀 |
WO2016005665A1 (en) * | 2014-07-09 | 2016-01-14 | Aalto University Foundation | Method for forming a graphene based material and a product |
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JP2013501696A (ja) * | 2009-08-07 | 2013-01-17 | ガーディアン・インダストリーズ・コーポレーション | グラフェンの広い領域の堆積およびドーピング、ならびにそれを含む生成物 |
JP2011126742A (ja) * | 2009-12-17 | 2011-06-30 | Sekisui Chem Co Ltd | 薄片化黒鉛分散液の製造方法、薄片化黒鉛の製造方法、及び、複合材料の製造方法 |
JP2013139377A (ja) * | 2011-12-28 | 2013-07-18 | Qinghua Univ | 硫黄−グラフェン複合材料の製造方法 |
WO2015076565A1 (ko) * | 2013-11-19 | 2015-05-28 | 한화케미칼 주식회사 | 관능화 그래핀의 제조 방법, 제조 장치, 및 관능화 그래핀 |
WO2016005665A1 (en) * | 2014-07-09 | 2016-01-14 | Aalto University Foundation | Method for forming a graphene based material and a product |
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