1
Akademia Górniczo-Hutnicza im. Stanisława Staszica
Wydział Inżynierii Materiałowej i Ceramiki
Katedra Biomateriałów
Rozprawa doktorska
FUNKCJONALNE POWŁOKI
ORGANICZNO-NIEORGANICZNE,
OTRZYMYWANE METODĄ ZOL-ŻEL, DO
ZASTOSOWAŃ MEDYCZNYCH
mgr inż. Anna Donesz-Sikorska
Wydział Mechaniczny, Katedra Mechaniki i Inżynierii Materiałowej
Politechnika Wrocławska
Promotorzy:
Dr hab. inż. Jerzy Kaleta, prof. nadzw. PWr.
Wydział Mechaniczny, Katedra Mechaniki i Inżynierii Materiałowej
Politechnika Wrocławska
Prof. Dr hab. inż. Elżbieta Pamuła
Wydział Inżynierii Materiałowej i Ceramiki,
Katedra Biomateriałów, AGH w Krakowie
2015-2
Spis treści
Wstęp ... 4
I. CZĘŚĆ LITERATUROWA ... 6
1. Matryca krzemionkowa – właściwości, charakterystyka, biokompatybilność ... 6
2. Metoda zol-żel, otrzymywanie powłok i ich aktywacja ... 8
2.1. Hydroliza i polikondensacja ... 9
2.2. Dojrzewanie i stabilizacja ... 11
2.3. Metody nanoszenia powłok otrzymywanych metodą zol-żel ... 12
3. Powłoki organiczno-nieorganiczne ... 14
3.1. Powłoki krzemionkowe – niedomieszkowane oraz funkcjonalizowane substancją
aktywną ... 18
3.2. Powłoki hybrydowe ... 20
3.2.1. Powłoki krzemionkowo-tytanianowe ... 21
3.2.2. Powłoki krzemionkowo-cyrkoniowe ... 22
3.2.3. Powłoki krzemionkowo-glinowe ... 22
II. Teza, zakres i cel pracy ... 24
III. CZĘŚĆ EKSPERYMENTALNA ... 26
1.
Materiały ... 26
1.1.
Synteza ... 26
1.1.1.
Bazowe powłoki krzemionkowe ... 26
1.1.2. Powłoki hybrydowe ... 28
1.1.3. Funkcjonalne powłoki krzemionkowe ... 30
1.2. Procedura nanoszenia powłok ... 33
2. Metody ... 34
2.1. Ocena powierzchni oraz składu pierwiastkowego – analiza SEM-EDX ... 34
2.2. Spektroskopia Ramana ... 34
2.3. Zwilżalność i swobodna energia powierzchniowa (SEP) ... 35
2.4. Pomiar grubości ... 35
2.5. Profilomeria ... 36
2.6. Badania elektrochemiczne (badania odporności korozyjnej) ... 37
2.7. Badania biologiczne in vitro ... 38
2.7.1. Badania in vitro na linii osteoblastopodobnej MG-63 ... 38
2.7.2. Badania in vitro na macierzystych komórkach AdMSCs ... 40
2.8. Badania mikromechaniczne ... 43
2.8.1. Badania scratch-test ... 43
3
3. Wyniki i dyskusja ... 46
3.1. Bazowe powłoki krzemionkowe ... 46
3.1.1. Wyniki badań strukturalnych i fizykochemicznych ... 46
3.1.2. Wyniki badań elektrochemicznych ... 52
3.1.3. Wyniki badań biologicznych ... 55
3.1.4. Wyniki badań mikromechanicznych ... 63
3.1.5. Dyskusja wyników ... 68
3.2. Powłoki hybrydowe ... 76
3.2.1. Wyniki badań strukturalnych i fizykochemicznych ... 76
3.2.2. Wyniki badań elektrochemicznych ... 86
3.2.3. Wyniki badań biologicznych ... 94
3.2.4. Wyniki badań mikromechanicznych ... 102
3.2.5. Dyskusja wyników ... 107
3.3. Funkcjonalne powłoki krzemionkowe ... 114
3.3.1. Wyniki badań strukturalnych i fizykochemicznych ... 114
3.3.2. Wyniki badań elektrochemicznych ... 125
3.3.3. Wyniki badań biologicznych ... 128
3.3.4. Dyskusja wyników ... 135
PODSUMOWANIE I WNIOSKI ... 141
PROPONOWANE OBSZARY DALSZYCH BADAŃ NAUKOWYCH ... 145
Podziękowania ... 146
Literatura ... 147
SPIS RYSUNKÓW ... 156
147
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