Porowaty węgiel grafityzowany otrzymywany techniką zol-żel

• Autorzy: Kiciński, W.

Warianty tytułu

EN

Porous graphitic carbon produced with sol-gel processing

• Języki publikacji: PL

Abstrakty

PL

Wykorzystując technikę zol-żel podjęto próbę syntezy materiału węglowego o dobrze rozwiniętej strukturze porowatej, dużej wartości powierzchni właściwej i możliwie wysokim stopniu grafityzacji. Materiały takie mają unikatową kombinację właściwości fizykochemicznych i powierzchniowych - - wysoką przewodność elektryczną i termiczną, odporność na korozję chemiczną, stabilność termiczną, trwałość mechaniczną, małą gęstość, a przy tym mogą być otrzymywane z tanich i szeroko dostępnych surowców. Mogą więc znaleźć zastosowanie jako materiał elektrodowy w elektrochemicznych zasobnikach energii. Pierwotną strukturę porowatą materiału formowano na etapie syntezy zol-żel i zachodzącej w wyniku polikondensacji rezorcyny i furfuralu separacji faz. Porowatość rozwijano, dodatkowo stosując w roli matrycy koloidalną krzemionkę. Syntezę prowadzono w wodno-metanolowym roztworze chlorku niklu(II) pełniącego rolę prekursora katalizatora grafityzacji. Otrzymany w procesie zol-żel kserożel organiczny poddawano karbonizacji w temperaturze 1050°C, w wyniku czego następowała karbotermiczna redukcja NiCl2, grafityzacja matrycy węglowej i reorganizacja pierwotnej struktury porowatej kserożelu. Otrzymany w procesie pirolizy kompozyt kserożel węglowy/nikiel/krzemionka poddawano wymywaniu w kwasie fluorowodorowym. W wyniku takiego oczyszczania otrzymywano czysty materiał węglowy - zwany dalej kserożelem węglowym. Obecną w matrycy kserożelu węglowego fazę amorficzną usuwano następnie poprzez selektywne utlenianie w powietrzu w temperaturze 460°C. Powodowało to drastyczny spadek całkowitej objętości porów, redukcję wartości SBET oraz utratę wytrzymałości mechanicznej materiału. Otrzymane materiały węglowe analizowano za pomocą technik: SEM, XRD, niskotemperaturowej fizysorpcji azotu i TG-DTA. Przeprowadzono analizę porównawczą morfologii i struktury materiału węglowego przed i po procesie selektywnego utleniania fazy amorficznej węgla.

EN

The sol-gel process is applied to obtain nanoporous carbon material with both high surface area and high graphitization degree. Carbon materials characterized by 3D meso-, macroporous structure, well graphitized framework and large surface areas exhibit extraordinary performance as electrocatalyst supports and electrode materials (e.g. for fuel cells, double-layer capacitors and lithium ion batteries). The presence of well-interconnected meso- and macropores allows reduced diffusional limitations often occurring in classical carbon-supported catalysts, while the graphitization of the carbon matrix improves its electrical conductivity (Fig. 1). Graphitic nanoporous carbon was obtained via pyrolysis of organic xerogel doped with nickel(II) chloride (Fig. 2). Doping was realized through chloride solubilization in a water-methanol solution of resorcinol and furfural. During carbonization of the doped organic xerogel in 1050°C, metallic nanoparticles that catalyze the formation of graphitic structures were generated. The possibility of enhancing the porosity of the xerogel via templating with colloidal silica was investigated. The removal of the metal and silica templates leads to monoliths of carbon xerogel characterized by multimodal porosity with substantially enhanced mesoporosity resulting in a SBET of 268 m2/g (Tab. 1). Next, a selective-combustion process was used on the bulk carbon material produced by this solid-state synthesis process, yielding purified graphitic nanostructures. Removal of the amorphous carbon by a selectivecombustion process significantly reduced the material's mesoporosity and SBET, also causing loss of its mechanical strength. The carbon xerogel samples before and after selective-combustion were investigated by means of SEM (Fig. 3), XRD (Fig. 4), N2 physisorption (Fig. 5 and 6), and TG-DTA (Fig. 7). The results obtained for both materials were then compared.

Słowa kluczowe

PL

metoda zol-żel; kserożel węglowy; grafityzacja; karbonizacja; mezoporowatość

EN

sol-gel synthesis; carbon xerogel; graphitization; carbonization; mesoporosity

• Czasopismo: Inżynieria Materiałowa
• Rocznik: 2011
• Tom: Vol. 32, nr 2
• Strony: 115-121
• Opis fizyczny: Bibliogr. 69 poz., rys., tab.

Twórcy

autor

Kiciński, W.

• Instytut Chemii, Wydział Nowych Technologii i Chemii, Wojskowa Akademia Techniczna, Warszwa,

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