JP2019535915A - 高炭素質材料の新規製造方法及び得られた高炭素質材料 - Google Patents
高炭素質材料の新規製造方法及び得られた高炭素質材料 Download PDFInfo
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- JP2019535915A JP2019535915A JP2019521485A JP2019521485A JP2019535915A JP 2019535915 A JP2019535915 A JP 2019535915A JP 2019521485 A JP2019521485 A JP 2019521485A JP 2019521485 A JP2019521485 A JP 2019521485A JP 2019535915 A JP2019535915 A JP 2019535915A
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- carbonaceous material
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Abstract
Description
−環状又は芳香族有機化合物堆積物で覆われた繊維又は繊維セットを得るための組合せ前駆体の熱安定化及び寸法安定化工程、及び
−高炭素質材料を得るための環状又は芳香族有機化合物堆積物で覆われた前記繊維又は繊維セットの炭化工程
をさらに含む。
構造化前駆体10は、繊維又は繊維セットを含む。該繊維又は繊維セットは、本発明に従う方法に関連してそれらの取扱いを容易にするために、前処理を受けていてもよい。それにもかかわらず、前駆体として使用される場合、この繊維又は繊維セットは、炭化工程を経ていない。したがって、構造化前駆体10に使用される該繊維又は繊維セットは、75%未満、有利には65%未満の炭素重量濃度を有することが好ましい。
−リグニン又はリグニン誘導体、セルロース、デンプン、グリコーゲン、アミロース、アミロペクチン、デキストラン、ヘミセルロース等の多糖類、又はフルクトース若しくはグルコース等の他のより単純な糖類及びそれらの誘導体から選択される生物起源の生成物;
−ピッチ、ナフタレン、フェナントレン、アントラセン、ピレン、又はナフタレンスルホネート等の置換多環芳香族炭化水素から選択される石油又は鉱業資源から得られる生成物;
−フェノール樹脂、フェノプラスト樹脂、又はポリエポキシド樹脂から選択される合成製品;並びに
−不活性雰囲気下での熱分解後に炭素残渣を生じる任意の他の物質又は有機配合物。
本発明による組合せ工程100は、構造化前駆体10を非構造化前駆体15と接触させることに対応する。この組合せは一般に−10℃〜80℃、好ましくは20℃〜60℃の範囲の温度で、いくつかの代替方法によって行うことができる。例えば均熱、噴霧又は含浸(例えば、パディングによる)を行うことが可能である。好ましくは、組合せ工程100は含浸である。
本発明による製造方法1は、環状又は芳香族有機化合物堆積物30で覆われた繊維又は繊維セットを得るために、組み合わされた前駆体20の熱安定化及び寸法安定化工程200をさらに含む。
本発明による製造方法1は、高炭素質材料2を得るために、環状又は芳香族有機化合物堆積物30で覆われた繊維又は繊維セットを炭化させる工程300をさらに含む。
本発明による製造方法は、炭化工程300の前に、以下の工程をさらに含むことができる。
−環状又は芳香族有機化合物堆積物で被覆された繊維又は繊維セットを、少なくとも1つの難燃性化合物を含む水溶液と接触させるサイジング工程210であって、難燃性化合物は、カリウム、ナトリウム、リン酸塩、酢酸塩、塩化物、尿素の中から選択することができる工程、及び
−乾燥後の乾燥工程220
本発明による製造方法は、周囲温度で又は加熱処理を伴う、任意に構造化工程に連結される、押出、圧縮、カレンダー加工、延伸又は成形等の任意の成形工程による高炭素質材料2の成形工程400をさらに含んでもよい。この成形により、本発明の方法によって得られる高炭素質材料の最終形状を正確に制御することが可能になる。成形はまた、生成される材料の多孔性を制御することを可能にする。
本発明による製造方法は、炭化工程300の後に黒鉛化工程500を含むことができる。この黒鉛化工程500は、1000℃〜2800℃の間、好ましくは1100℃以上の温度で実施することができる。黒鉛化工程500は、例えば2〜60分、好ましくは2〜20分続くことができる。この黒鉛化工程500は、温度の漸増を含むことができる。
本発明による製造方法は、炭化工程300の後に、高炭素質材料2を、少なくとも1つのシラン若しくはシラン誘導体及び/又は少なくとも1つのシロキサン若しくはシロキサン誘導体を含むことができる有機成分の溶液と接触させるサイジング工程600をさらに含むことができる。このサイジング工程600は、黒鉛化工程500の後に実施することもできる。プラズマ、マイクロ波、及び/又は電気化学的処理工程を、黒鉛化工程500とサイジング工程600との間で行うこともできる。
−陰極保護用陽極
−燃料電池用電極
−一次電池及び充電式電池用電極素子
−リチウム又はナトリウム電池の陽極又は陰極用集電体
−リチウム−硫黄電池用集電体
−リチウム−ポリマー電池用集電体
−鉛酸電池用、特に鉛−酸又は鉛−炭素超電池用電極素子
−充電式リチウム電池用電極素子
−スーパーコンデンサ用電極素子
−触媒担体、特に空気浄化用触媒担体、及び
−リチウム−空気電池用触媒担体
<出発物質の説明>
構造化前駆体を構成する水和セルロース繊維を、リグニン溶液、すなわち非構造化前駆体に7分間含浸させる。
リグニン含浸繊維を換気オーブン中で80℃で1時間乾燥させた。
窒素雰囲気下、縦型静止オーブンで炭化を行った。毎分5℃の温度勾配を1200℃の温度まで適用した。
水和セルロース繊維上のリグニンの堆積は9重量%であった。リグニン堆積の重量の定量は、工程1の前、次いで乾燥工程2の後に水和セルロース繊維を秤量することによって得ることができる。
炭素収率(CY)は炭化後に計算した。
CY=(1mあたりの炭素質材料/1mあたりの前駆体)×100
炭素収率の結果(炭化後)は次の通りである。
図2Aは、DAHP(A)と組合せた後に得られた、実施例における炭素質材料、すなわち炭素繊維の断面の走査型電子顕微鏡法によって得られた画像を示し、画像2Bは、本発明の方法によって得られた炭素質材料の走査型電子顕微鏡法によって得られた画像を示す。図2Bは、リグニンから生じる炭素堆積物が繊維表面に強固に結合しており、構造化部分、すなわち繊維と、非構造化部分、すなわちリグニンからの炭素堆積物との間の界面を顕微鏡で確認することが不可能であることを示す。反対に、図2Aは、DAHP堆積物が、構造化部分の周囲にこの非構造化炭素重量の生成を可能にしないことを示す。
リグニンの堆積を実施例1のように行ったが、0.2%のCNTを添加した水和セルロース繊維上に行った。同じプロトコールを炭化にも適用した。
炭素収率の結果(炭化後)は次の通りである。
Claims (36)
- 繊維又は繊維セットを含む構造化前駆体(10)と流体の形態の非構造化前駆体(15)との組合せ(100)を含むことを特徴とする高炭素質材料(2)の製造方法(1)であって、前記流体が、組合せ工程が行われる温度で45,000mPa.s−1未満の粘度を有し、前記非構造化前駆体(15)によって覆われた前記構造化前駆体(10)に対応する組合せ前駆体(20)を得るために、溶融状態で又は溶液中に65重量%以下の濃度で少なくとも1つの環状有機又は芳香族化合物を含み、前記方法がさらに以下の工程、すなわち
−環状又は芳香族有機化合物堆積物(30)で覆われた繊維又は繊維セットを得るための、前記組合せ前駆体(20)の熱安定化及び寸法安定化(200)工程、及び
−高炭素質材料(2)を得るための環状又は芳香族有機化合物堆積物(30)で覆われた前記繊維又は繊維セットの炭化(300)工程
を含む製造方法。 - 前記環状又は芳香族有機化合物が、リグニン、セルロース、デンプン、グリコーゲン、アミロース、アミロペクチン、デキストラン、ヘミセルロース、フルクトース又はグルコース及びそれらの誘導体から選択される生物起源生成物;ピッチ、ナフタレン、フェナントレン、アントラセン、ピレン又はナフタレンスルホネートから選択される石油又は鉱業資源から得られる生成物;並びにフェノール樹脂、フェノプラスト樹脂又はポリエポキシ樹脂から選択される合成生成物から選択されることを特徴とする、請求項1に記載の製造方法。
- 前記非構造化前駆体(15)が、5重量%〜50重量%の環状有機又は芳香族化合物を含むことを特徴とする、請求項1又は2に記載の製造方法。
- 前記流体が、水溶液、有機溶液、又は両者の混合物であることを特徴とする、請求項1〜3のいずれか一項に記載の製造方法。
- 前記流体が、溶融材料であることを特徴とする、請求項1〜3のいずれか一項に記載の製造方法。
- 前記環状有機又は芳香族化合物が、500g/molを超える分子量を有することを特徴とする、請求項1〜5のいずれか一項に記載の製造方法。
- 前記非構造化前駆体(15)が、金属充填剤、炭素に富む化合物、及び有機粒子から選択される少なくとも1つの追加の化合物をさらに含むことを特徴とする、請求項1〜5のいずれか一項に記載の製造方法。
- 前記金属充填剤が、以下の金属、すなわち、ホウ素、ケイ素、ゲルマニウム、ヒ素、リチウム、ナトリウム、カリウム、チタン、バナジウム、マンガン、鉄、コバルト、ニッケル、モリブデン、アルミニウム及び鉛から選択される金属を含むことを特徴とする、請求項7に記載の製造方法。
- 前記炭素に富む化合物が、以下の化合物、すなわち、活性炭、天然無煙炭、合成無煙炭、カーボンブラック、天然黒鉛又は合成黒鉛から選択されることを特徴とする、請求項7に記載の製造方法。
- 前記有機粒子が、以下の化合物、すなわち、ナノセルロース、タンニン、キトサン、又は溶解可能でも可溶性でもない他の生体高分子から選択されることを特徴とする、請求項7に記載の製造方法。
- 前記構造化前駆体(10)が、直径が、0.5〜300μm、好ましくは1μm〜50μmである、少なくとも1つの一定の繊維(11)を含むことを特徴とする、請求項1〜10のいずれか一項に記載の製造方法。
- 前記構造化前駆体(10)が、撚られたマルチフィラメント、撚られていないマルチフィラメント、不織繊維セット、又は織繊維セットを含むことを特徴とする、請求項1〜11のいずれか一項に記載の製造方法。
- 前記構造化前駆体(10)が、セルロース繊維、水和セルロース繊維、リグニン繊維、ピッチ繊維、又はPAN繊維を含むことを特徴とする、請求項1〜12のいずれか一項に記載の製造方法。
- 前記構造化前駆体(10)及び/又は前記非構造化前駆体(15)が、炭素質ナノフィラーを含み、該炭素質ナノフィラーが、0.0001重量%〜30重量%、好ましくは0.01重量%〜5重量%の濃度で存在することを特徴とする、請求項1〜13のいずれか一項に記載の製造方法。
- 前記組合せ工程(100)並びに前記熱的安定化及び寸法安定化工程(200)が、1回以上繰り返されることを特徴とする、請求項1〜14のいずれか一項に記載の製造方法。
- 室温で又は熱処理による、押出圧縮、カレンダー加工、延伸又は成形等の任意の成形処理による前記高炭素質材料(2)の成形工程(400)をさらに含むことを特徴とする、請求項1〜15のいずれか一項に記載の製造方法。
- 黒鉛化工程(500)をさらに含むことを特徴とする、請求項1〜16のいずれか一項に記載の製造方法。
- 中間製品としての有機堆積物(30)で覆われた繊維又は繊維セットであって、前記有機堆積物が、
−リグニン又はリグニン誘導体、セルロース、デンプン、グリコーゲン、アミロース、アミロペクチン、デキストラン、ヘミセルロースのような多糖類又はフルクトース若しくはグルコース及びそれらの誘導体、
−ピッチ、ナフタレン、フェナントレン、アントラセン、ピレン又はナフタレンスルホネートのような置換多環芳香族炭化水素、及び
−フェノール樹脂、フェノプラスト樹脂又はポリエポキシド樹脂
から選択される少なくとも1つの環状又は芳香族有機化合物を含むことを特徴とし、環状有機又は芳香族化合物の重量に対する繊維の重量の比が、1/5〜100/1であることを特徴とする繊維又は繊維セット。 - 炭化繊維又は炭化繊維セットを含む構造化部分と、炭化された環状有機又は芳香族化合物を含む非構造化部分とを含むように二重構造化され、全体的な多孔性が5%超、好ましくは10%超であることを特徴とする高炭素質材料(2)。
- 前記構造化部分が、40%未満、好ましくは30%未満の多孔性を有し、前記非構造化部分が、7%超、好ましくは10%超の多孔性を有することを特徴とする、請求項19に記載の高炭素質材料(2)。
- 前記非構造化部分の体積に対する前記構造化部分の体積の比が、1/5〜100/1であることを特徴とする、請求項19又は20のいずれか一項に記載の高炭素質材料(2)。
- 前記方法の請求項1〜8に記載の非構造化部分に導入された金属充填剤及び/又は金属塩等の添加剤を含むことを特徴とする、請求項19〜21のいずれか一項に記載の高炭素質材料(2)。
- 炭素繊維、撚られたマルチフィラメント、撚られていないマルチフィラメント、不織炭素繊維セット又は織炭素繊維セットの形態であることを特徴とする、請求項19〜22のいずれか一項に記載の高炭素質材料(2)。
- 請求項19〜23のいずれか一項に記載の高炭素質材料の使用であって、熱可塑性又は熱硬化性タイプの複合材料部品の製造のための使用。
- 請求項19〜23のいずれか一項に記載の高炭素質材料の使用であって、電気化学的プロセスにおいて電極として使用され得る部品の製造のための使用。
- 陰極防食のための陽極として使用され得る部品の製造のための、請求項19〜23のいずれか一項に記載の高炭素質材料の使用。
- 請求項19〜23のいずれか一項に記載の高炭素質材料の使用であって、燃料電池用の電極として使用され得る部品の製造のための使用。
- 請求項19〜23のいずれか一項に記載の高炭素質材料の使用であって、一次電池及び充電式電池用の電極要素として使用され得る部品の製造のための使用。
- 請求項19〜23のいずれか一項に記載の高炭素質材料の使用であって、リチウム電池又はナトリウム電池の陽極又は陰極のための集電体として使用され得る部品の製造のための使用。
- 請求項19〜23のいずれか一項に記載の高炭素質材料の使用であって、リチウム−硫黄電池用の集電体として使用され得る部品の製造のための使用。
- 請求項19〜23のいずれか一項に記載の高炭素質材料の使用であって、リチウム−ポリマー電池用の集電体として使用され得る部品の製造のための使用。
- 請求項19〜23のいずれか一項に記載の高炭素質材料の使用であって、鉛酸電池、特に鉛又は鉛炭素超電池用の電極要素として使用され得る部品の製造のための使用。
- 請求項19〜23のいずれか一項に記載の高炭素質材料の使用であって、充電式リチウム電池用の電極要素として使用され得る部品の製造のための使用。
- 請求項19〜23のいずれか一項に記載の高炭素質材料の使用であって、スーパーコンデンサの電極素子として使用され得る部品の製造のための使用。
- 請求項19〜23のいずれか一項に記載の高炭素質材料の使用であって、触媒担体、特に空気の精製のための触媒担体として使用され得る部品の製造のための使用。
- 請求項19〜23のいずれか一項に記載の高炭素質材料の使用であって、リチウム−空気電池の触媒担体として使用され得る部品の製造のための使用。
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FR1660536A FR3058167B1 (fr) | 2016-10-28 | 2016-10-28 | Nouveau procede de fabrication de materiaux hautement carbones et materiau hautement carbone obtenu |
FR1660536 | 2016-10-28 | ||
PCT/FR2017/052949 WO2018078287A1 (fr) | 2016-10-28 | 2017-10-26 | Nouveau procede de fabrication de materiaux hautement carbones et materiau hautement carbone obtenu |
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KR (1) | KR20190069540A (ja) |
CN (1) | CN110062825A (ja) |
CA (1) | CA3039721A1 (ja) |
FR (1) | FR3058167B1 (ja) |
IL (1) | IL266085A (ja) |
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FR3058166B1 (fr) * | 2016-10-28 | 2018-11-23 | Arkema France | Procede de fabrication de fibres de carbone a partir de precurseurs biosources et fibres de carbone obtenues |
CN109020508B (zh) * | 2018-07-12 | 2021-04-23 | 吉林长玉特陶新材料技术股份有限公司 | 一种三维石墨烯桥连氧化物陶瓷及其制备方法 |
KR102075114B1 (ko) * | 2019-06-21 | 2020-02-07 | 국방과학연구소 | 라이오셀계 탄소섬유 제조를 위한 탄소 나노 튜브 코팅 및 열처리 |
CN112010283A (zh) * | 2019-08-30 | 2020-12-01 | 南京理工大学 | 高性能生物质基碳质电极材料的制备方法 |
CN110649355B (zh) * | 2019-09-29 | 2021-06-25 | 四川天邑康和通信股份有限公司 | 一种射频电缆及其制备工艺 |
CN111547719A (zh) * | 2020-04-13 | 2020-08-18 | 上海应用技术大学 | 一种3d多孔碳材料及其制备方法与应用 |
CN112812796B (zh) * | 2021-01-13 | 2022-02-11 | 中国石油大学(华东) | 一种生物基针状焦及其制备方法 |
FR3138140B1 (fr) * | 2022-07-22 | 2024-07-19 | Safran Ceram | procédé de préparation d’un matériau composite à matrice carbone |
CN116371364A (zh) * | 2023-05-26 | 2023-07-04 | 昆明理工大学 | 一种碱改性生物炭及其制备方法与应用 |
CN116960308B (zh) * | 2023-08-22 | 2024-05-14 | 广东钠壹新能源科技有限公司 | 一种碳包覆改性聚阴离子型正极材料及其制备方法与应用 |
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- 2017-10-26 CN CN201780065889.3A patent/CN110062825A/zh active Pending
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IL266085A (en) | 2019-06-30 |
FR3058167A1 (fr) | 2018-05-04 |
US20190270678A1 (en) | 2019-09-05 |
US11214523B2 (en) | 2022-01-04 |
RU2019116177A3 (ja) | 2021-02-19 |
WO2018078287A1 (fr) | 2018-05-03 |
CA3039721A1 (fr) | 2018-05-03 |
KR20190069540A (ko) | 2019-06-19 |
RU2019116177A (ru) | 2020-11-30 |
EP3532660A1 (fr) | 2019-09-04 |
RU2765203C2 (ru) | 2022-01-26 |
FR3058167B1 (fr) | 2019-11-22 |
CN110062825A (zh) | 2019-07-26 |
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