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Publié par | friedrich-schiller-universitat_jena |
Publié le | 01 janvier 2005 |
Nombre de lectures | 9 |
Langue | English |
Poids de l'ouvrage | 8 Mo |
Extrait
Crystallisation of Semiconductive Oxides from
Borate Glasses
Dissertation
zur E rlangung des aka demischen G rades doc tor re rum naturalium
(Dr. rer. na t.)
vorgelegt dem Rat der Chemisch- Geowissenschaftlichen Fakultät der
Friedrich-Schiller-Universität Je na
von D ipl.-Chem. Ing. Ralitsa Pet eva Ro senow
geboren am 22.03. 1977 in Sofia, BulgarienGutachter:
1. Pr of. Dr . Dr . C . R üssel, O tto-Schott-Institut, F riedrich-Schilleriversität Jen a
2. Pr of. Dr . D . S tachel, Otto-Scho tt-Institut, F riedrich-Schilleriversität Jena
Tag d er öf fentlichen Ve rteidigung: 27.04.2005„I a m sin ging a song o f admiration o n the m erits
not of rubies, not of gol d but of glass....“
M. V. Lo monosov
For my husband Torsten
and my parentsII
Contents
1 Zusammenfassung....................................................................................................................... 1
1.1 Zusammenfassung fü r I n O und I n O :SnO (ITO)............................................................ 32 3 2 3 2
1.2 Z usammenfassung fü r SnO and S nO :Sb O ( ATO).......................................................... 52 2 2 3
2 Introduction................................................................................................................................. 7
2.1 Aim of th e wo rk................................................................................................................... 8
3 Ba ckground Th eory and L iterature Revi ew................................................................................ 9
3.1 I ndium oxi de ( In O )........................................................................................................... 92 3
3.1.1 I n O thi n f ilms 112 3
3.1.2 I n O nano-c rystals..................................................................................................... 122 3
3.2 I ndium tin oxide ( I TO) 13
3.2.1 I TO- thin films ............................................................................................................13
3.2.2 I n O : SnO (ITO)-nano- powders............................................................................... 162 3 2
3.3 Tin oxide (SnO )................................................................................................................ 172
3.3.1 SnO thin films ........................................................................................................... 182
3.3.2 SnO nano-c rystals..................................................................................................... 182
3.4 Antimon y dop ed SnO ( SnO : Sb O or A TO).................................................................. 192 2 2 3
3.4.1 ATO thi n f ilms 19
3.4.2 ATO n ano-c rystals......................................................................................................22
3.5 I n- and Sn-co ntaining glasses............................................................................................ 22
3.6 Crystallisation of melts 25
3.6.1 N ano-c rystallisation f rom gl asses............................................................................... 26
3.6.2 Pendulum eff ect th eory...............................................................................................27
4 Exper imental part...................................................................................................................... 28III
4.1 Methods fo r ana lysis.......................................................................................................... 28
4.1.1 X- ray diffraction (XRD) ............................................................................................. 28
4.1.2 Scanning Ele ctron M icroscopy ( SEM) . ..................................................................... 29
4.1.3 T ransmission E lectron M icroscopy ( TEM)................................................................ 29
4.1.4 Energy D ispersive X -ra y an alysis (EDX ) .................................................................. 30
4.1.5 Differential Th ermal An alyse (DTA)......................................................................... 34
4.1.6 UV-VIS-NIR-spectrometry......................................................................................... 34
4.1.7 F ourier-Tr ansform-I nfrared S pectrometry ( FTIR)...................................................... 34
4.2 Procedure f or preparation of In O -, In O :SnO -, S nO - 2 3 2 3 2 2
and SnO :Sb O - nano-pow ders f rom glasses.................................................................... 322 2 3
5 Results ...................................................................................................................................... 34
5.1 S ynthesis and op tical properties of In O -nano-pow der.................................................... 342 3
5.1.1 C hoice of th e g lass s ystem......................................................................................... 34
5.2 Melting and th ermal treatment of g lasses.......................................................................... 37
5.3 Dissolution of th e gl ass matrix and of non I n- containing pha ses..................................... 45
5.4 Sep aration of I n O nano-p articles...................................................................................... 472 3
5.5 Optical p roperties o f th e In O nano-p articles.................................................................... 542 3
5.5.1 H eat treatment in a ir................................................................................................... 54
5.5.2 I nfluence of the heat t reatment atmosphere................................................................ 55
5.6 S ynthesis, c haracterisation a nd opt ical properties of I n O :SnO nano-powd er................. 562 3 2
5.7 S ynthesis of S nO nano-powd er........................................................................................ 642
5.7.1 C hoice of th e g lass s ystem.......................................................................................... 64
5.7.2 Me lting pro cedure....................................................................................................... 66
5.7.2.1 SnO raw ma terial............................................................................................... 662
5.7.2.2 Co mplete d issolution of SnO in th e melt .......................................................... 672
5.7.3 Gl ass s amples th ermal treatment................................................................................ 70IV
5.7.4 Dissolution of th e m atrix........................................................................................... 76
5.7.5 Separation of th e SnO nano-c rystals......................................................................... 772
5.7.6 C haracterisation of SnO nano-c rystals...................................................................... 782
5.8 S ynthesis a nd op tical pr operties of S nO : Sb O nano-powd er.......................................... 842 2 3
6 Disc ussion.................................................................................................................................. 88
6.1 Disc ussion for In O and I n O :SnO -containing glasses, glass-ceramics2 3 2 3 2
and nano-powd ers.............................................................................................................. 88
6.2 Discussion fo r SnO and SnO :Sb O -containing glasses, glass-ceramics2 2 2 3
a nd n ano-powders90
7 Su mmary.................................................................................................................................... 93
7.1 Sum mary fo r In O and I n O :SnO (ITO)......................................................................... 932 3 2 3 2
7.2 Sum mary fo r SnO and SnO :Sb O ( ATO)...................................................................... 952 2 2 3
8 Bibl iography.............................................................................................................................. 97
9 List o f F igures.......................................................................................................................... 103 1 Zusammenfassung 1
1 Zusammenfassung
Halbleitende Nanokristalle aus Indiumoxid (INO), SnO dotiertem Indiumoxid (ITO),2
Zinnoxid (TO) oder Sb O dotiertem Zinnoxid (ATO) werden hauptsächlich als2 3
Beschichtungsmaterial für elektrisch leitende und transparente Schichten (z.B. als
Elektrodenmaterial in Flüssig-Kristall-Monitore (Liquid Crystal Displays) und in OLED-
Geräten (Organic Light Emitting Diodes) benutzt. Die ITO- und ATO- Nanopartikel auf
der anderen Seite zeigen gleichzeitig eine Undurchlässigkeit in NIR- und hohe
Transparenz in sichtbaren optischen Bereich. Deswegen finden sie u.a. Anwendung in IR
reflektierende und VIS-transparente Schichten auf Gläsern (z.B. Wärmeschutzgläser).
Die optischen und die elektrischen Eigenschaften dieser Nanoteilchen werden
hauptsächlich von den Defekten in der Kristallstruktur (Sauerstoffmangel) bestimmt. Es
gibt drei Möglichkeiten, um diesen Sauerstoffmangel zu beeinflussen: Bildung der
Kristalle bei hohen Temperaturen (z.B. bei CVD (Chemical Vapour Deposition