JP2014511816A - 層結合構造を有する多孔性炭素生成物およびその製造方法およびその使用方法 - Google Patents
層結合構造を有する多孔性炭素生成物およびその製造方法およびその使用方法 Download PDFInfo
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- JP2014511816A JP2014511816A JP2014503066A JP2014503066A JP2014511816A JP 2014511816 A JP2014511816 A JP 2014511816A JP 2014503066 A JP2014503066 A JP 2014503066A JP 2014503066 A JP2014503066 A JP 2014503066A JP 2014511816 A JP2014511816 A JP 2014511816A
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- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000010000 carbonizing Methods 0.000 claims abstract description 9
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- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 4
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- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
最近ではリチウム2次バッテリの技術的な重要性が増大している。リチウム2次バッテリでは、カソード(正の電極)およびアノード(負の電極)は、リチウムイオンのインタカレーションおよびデインタカレーション(intercalationおよびdeintercalation)に適切であり、かつリチウムイオンの移動を可能にする電解質に接する材料から構成される。アノード材料としては複数の多孔性炭素構造部が使用され、これらの多孔性炭素構造部は、それらの構造的および電気的な特性を実質的に変化させることなく、リチウムイオンを可逆的に受け取りおよび放出することができる。リチウムイオン2次バッテリのカソードは、主に、例えばコバルトリチウム酸(LiCoO2)のようなリチウムおよび遷移金属の複合酸化物からなる。電解質の種類に応じてリチウム2次バッテリは、リチウムイオンバッテリ(LIB)およびリチウムポリマバッテリ(LPB)に分けられる。リチウムイオンバッテリでは、液体の電解質が使用され、リチウムポリマバッテリでは、ポリマ電解質が使用される。理論的なセル電圧は、約3.7Vであり、(約90%の)高効率時におけるエネルギ密度は、タイプに応じて120〜210Wh/kgの範囲にある。理論的な最大容量は、約300mAh/gに制限される。
上記の炭素構造用に公知の出発成分を製造することには費用がかかり、またここから形成される電極は相応に高価になる。
上記の方法についての課題は、本発明により、以下のステップを含む方法によって解決される。すなわち、
(a) 球形のナノ粒子および孔を含む無機材料製のテンプレートを準備するステップと、
(b) このテンプレートの孔に第1変種の炭素用の前駆体を注入するステップと、
(c) ナノ粒子に第1の細孔率を有する内側層を形成して炭化するステップと、
(d) 第2変種の炭素用の前駆物質を上記のテンプレートの残りの孔に注入するステップと、
(e) この前駆物質を炭化するステップであって、第1の細孔率よりも低い第2の細孔率を有する外側層を上記の内側層上に形成するステップと、
(f) 層結合構造を有する炭素生成物を形成してテンプレートを除去するステップを有しており、この層結合構造は、キャビティ側を向いた覆われていない面を有しかつ大きい方の第1の細孔率を有する炭素からなる内側層と、キャビティとは反対側を向いた覆われていない面を有しかつ小さい方の第2の細孔率を有する炭素からなる外側層とを有する。
ステップ(d)による注入のため、有利にはグラファイト化可能な炭素用の前駆物質を、殊にピッチを使用する。
以下では、実施例および図面に基づき、本発明を詳しく説明する。
このようにして形成した顆粒状粒子13は、多孔性炭素フレークを製造するためのテンプレートとして使用される。このことは、図3〜6に略示されている通りであり、またこのことをこれらの図に基づいて詳しく説明する。
例1とは異なり、外側層32の製造は、顆粒状粒子30と、細かく碾いたピッチ粉末とを1.6:1(ピッチ:顆粒状粒子)の重量比で混ぜ合わせることによって行われる。この比は、ピッチがほぼ完全に消費され、孔が充填されてあまり大きな、覆われていない細孔容積がもはや残っていないように選択される。
上記の方法についての課題は、本発明により、以下のステップを含む方法によって解決される。すなわち、
(a) 球形のナノ粒子および孔を含む無機材料製のテンプレートを準備するステップと、
(b) このテンプレートの孔に第1変種の炭素用の前駆体を注入するステップと、
(c) 第1変種の炭素用の前駆体を炭化して、第1の細孔率を有する内側層をナノ粒子に形成するステップと、
(d) 上記のステップ(b)による注入プロセスおよびステップ(c)による炭化の後に残っているテンプレートの孔容積体に第2変種の炭素用の前駆物質を注入するステップと、
(e) この前駆物質を炭化するステップであって、第1の細孔率よりも低い第2の細孔率を有する外側層を上記の内側層上に形成するステップと、
(f) 層結合構造を有する炭素生成物を形成してテンプレートを除去するステップを有しており、この層結合構造は、キャビティ側を向いた覆われていない面を有しかつ大きい方の第1の細孔率を有する炭素からなる内側層と、キャビティとは反対側を向いた覆われていない面を有しかつ小さい方の第2の細孔率を有する炭素からなる外側層とを有する。
Claims (16)
- 層結合構造を有する多孔性炭素生成物(35)を製造する方法において、
(a) 球形のナノ粒子および孔を含む無機材料からなるテンプレート(30)を準備するステップと、
(b) 前記テンプレート(30)の孔に第1変種の炭素用の前駆体を注入するステップと、
(c) 前記ナノ粒子に第1細孔率を有する内側層(31)を形成して炭化するステップと、
(d) 前記テンプレート(30)の残りの孔に第2変種の炭素用の前駆物質を注入するステップと、
(e) 前記前駆物質を炭化するステップであって、前記第1の細孔率よりも小さい第2の細孔率を有する外側層(32)を前記内側面(31)に形成するステップと、
(f) 層結合構造を有する炭素生成物(35)を形成して前記テンプレート(30)を除去するステップとを有しており、前記層結合構造は、キャビティ(36)側を向いた覆われていない面を有しかつ大きい方の第1の細孔率を有する炭素からなる内側層(31)と、前記キャビティ(36)とは反対側の覆われていない表面を有しかつ小さい方の第2の細孔率を有する炭素からなる外側層(32)とを有する、
ことを特徴とする方法。 - 請求項1に記載の方法において、
前記ステップ(b)にしたがって注入するため、グラファイト化できない炭素用の前駆体を使用し、殊に水溶性炭水化物、有利にはサッカロースを使用する、
ことを特徴とする方法。 - 請求項1または2に記載の方法において、
前記炭化の後、前記内側層はBET法による400ないし600m2/gの範囲の比表面積を有する、
ことを特徴とする方法。 - 請求項1から3までのいずれか1項に記載の方法において、
前記炭化の後、前記内側層(31)は、1ないし50nmの範囲の、有利に2ないし10nmの範囲の平均層厚を有する、
ことを特徴とする方法。 - 請求項1から4までのいずれか1項に記載の方法において、
前記ステップ(d)にしたがって注入するため、グラファイト化可能な炭素用の前駆物質を使用し、例えばピッチを使用する、
ことを特徴とする方法。 - 請求項1から5までのいずれか1項に記載の方法において、
前記炭化の後、前記外側層(32)は、50m2/g未満の範囲のBET法による比表面積を有する、
ことを特徴とする方法。 - 請求項1から6までのいずれか1項に記載の方法において、
前記炭化のあと、前記外側層(32)は、少なくとも2nmの平均層厚を有する、
ことを特徴とする方法。 - 請求項1から7までのいずれか1項に記載の方法において、
前記ステップ(d)にしたがって注入する際に、前記テンプレート(30)の前記孔の残りの細孔容積の少なくとも50%に、有利には少なくとも70%に前記前駆物質を充填する、
ことを特徴とする方法。 - 請求項1から8までのいずれか1項に記載の方法において、
前記テンプレート(30)の前記準備には、スートデポジットプロセスが含まれており、
該プロセスでは、供給材料を熱分解または加水分解によってテンプレート材料粒子に変換し、前記テンプレート材料からスート基体を形成して前記テンプレート材料粒子を堆積面上にデポジットし、
前記スート基体をテンプレート粒子に粉砕する、
ことを特徴とする方法。 - 請求項1から9までのいずれか1項に記載の方法において、
前記炭素生成物(35)は、多孔性微粒子炭素フレークの形態で形成される、
ことを特徴とする方法。 - 第2の炭素変種からなる外側層(32)に接する第1の炭素変種からなる内側層(31)を有する、層結合構造を備えた多孔性炭素生成物において、
前記内側層(31)は、第1の細孔率と、キャビティ(36)側を向いている覆われていない表面とを有しており、
前記外側層(32)は、前記第1の細孔率よりも小さい第2の細孔率と、前記キャビティ(36)とは反対側を向いている覆われていない表面とを有している、
ことを特徴とする多孔性炭素生成物。 - 請求項11に記載の炭素生成物において、
前記内側層(31)は、乱層炭素からなり、1ないし50nmの範囲の、有利には2ないし10nm範囲の平均層厚を有する、
ことを特徴とする炭素生成物。 - 請求項11または12に記載の炭素生成物において、
前記外側層(32)は、グラファイトに類似する炭素から構成されており、少なくとも2nmの平均層厚を有する、
ことを特徴とする炭素生成物。 - 請求項11から13までのいずれか1項に記載の炭素生成物において、
該炭素生成物は、階層的な多孔構造を有する、
ことを特徴とする炭素生成物。 - 請求項11から14までのいずれか1項に記載の炭素生成物において、
当該炭素生成物は、10μmないし500μmの範囲の、有利に20μmないし100μmの、殊に有利には50μm未満の平均層厚を有する炭素層からなる多孔性炭素フレークの形態である、
ことを特徴とする炭素生成物。 - 再充電可能リチウム硫黄バッテリ用の電極を製造するために請求項11から15までのいずれか1項に記載の炭素生成物を使用する、
ことを特徴とする使用方法。
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US9520594B2 (en) | 2016-12-13 |
US20140045072A1 (en) | 2014-02-13 |
CN103460451B (zh) | 2016-05-04 |
JP5916841B2 (ja) | 2016-05-11 |
TW201305085A (zh) | 2013-02-01 |
WO2012136513A1 (de) | 2012-10-11 |
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