Procedury charakteryzacji nanoproszków

Agnieszka Opalińska 1,2Anna Swiderska-Sroda 1Jan Mizeracki 1Adam M. Presz 1Tadeusz Chudoba 1Witold Łojkowski 1,3

1. Polish Academy of Sciences, Institute of High Pressure Physics (UNIPRESS), Sokolowska 29/37, Warszawa 01-142, Poland
2. Warsaw University of Technology, Faculty of Materials Science and Engineering (InMat), Wołoska 141, Warszawa 02-507, Poland
3. Instytut Wysokich Ciśnień PAN (IWC), Sokołowska 29/37, Warszawa 01-142, Poland

Abstract

Kluczowym etapem procesów technologicznych takich jak produkcja nanoproszków jest ich poprawna charakteryzacja. Przy tak małym rozmiarze ziaren/ krystalitów rzędu 100nm tradycyjne metody charakteryzacji mogą prowadzić do błędnych wyników i ich interpretacji.

A przecież właściwości nanoproszków zależą między innymi od wielkości krystalitów, ich rozkładu, struktury krystalicznej warstwy powierzchniowej oraz grubości tej warstwy, która może zawierać wodorotlenki lub inne nieprzereagowane reagenty.

Szczególna uwagę należy zwrócić na gęstość otrzymanych nanoproszków. Wykazano, że gęstość piknometryczna jest doskonałym narzędziem do odróżnienia „dobrej jakości proszku” (wartość gęstości zbliżona do teoretycznej) – od „słabych proszków” (wartość gęstości znacznie odbiegająca od teoretycznej) – zawierających znaczna ilość wodorotlenków i innych faz na powierzchni.  W 2007 roku wprowadzono nową metodę charakteryzacji nanoproszków w postaci pozycji nanoproszku na wykresie we współrzędnych B.E.T/gęstość (Rys.1). Metoda ta pozwala ocenić jaki jest udział faz powierzchniowych w objętości nanoproszków. Jest to w oczywisty sposób fundamentalna cecha nanoproszków.

Graph1_do_procedur.JPG

Rys. 1. Charakteryzacja nanoproszków na wykresie B.E.T/gęstość

To uzmysławia nam jak ważna jest poprawna interpretacja wyników i stosowanie właściwych metod charakteryzacji nanoproszków. Ze względu na brak ogólnie przyjętych  metod charakteryzacji, opracowaliśmy normy charakteryzacji nanoproszków.

Badania podzielono na dwie grupy: 

·         Badania obligatoryjne – dla badań tych opracowano szczegółowe procedury charakteryzacji

  • Procedura XRD/1: Procedura jakościowej analizy składu fazowego materiałów proszkowych z zastosowaniem dyfrakcji rentgenowskiej”. 
  •  „Procedura RO/1: Procedura pomiaru gęstość szkieletowej materiałów proszkowych z zastosowaniem piknometru helowego”.
  • Procedura BET/1: Procedura pomiaru powierzchni właściwej materiałów proszkowych z zastosowaniem izotermy Brunauera, Emmetta i Tellera (izoterma BET)”.

·         Badania dodatkowe – są to badania opcjonalne lub przeprowadzane okresowo

  • Skaningowa Mikroskopia Elektronowa,
  • Transmisyjna Mikroskopia Elektronowa.

Ze względu na różnorodność metod badawczych opracowywanie procedur charakteryzacji proszków nanometrycznych wymaga dalszych prac.

 

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Presentation: Poster at Nanotechnologia PL, by Anna Swiderska-Sroda
See On-line Journal of Nanotechnologia PL

Submitted: 2010-08-19 17:48
Revised:   2010-08-26 13:32