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Transcript of 8. Poröse Materialien Proteine mikroporösmesoporös 2 nm makroporös ZeolitesMCMsBio-foams 50 nm...
![Page 1: 8. Poröse Materialien Proteine mikroporösmesoporös 2 nm makroporös ZeolitesMCMsBio-foams 50 nm Moleküle.](https://reader035.fdocument.pub/reader035/viewer/2022062818/55204d6349795902118b8870/html5/thumbnails/1.jpg)
8. Poröse Materialien
Proteine
mikroporös mesoporös
2 nm
makroporös
Zeolites MCMs Bio-foams
50 nm
Moleküle
![Page 2: 8. Poröse Materialien Proteine mikroporösmesoporös 2 nm makroporös ZeolitesMCMsBio-foams 50 nm Moleküle.](https://reader035.fdocument.pub/reader035/viewer/2022062818/55204d6349795902118b8870/html5/thumbnails/2.jpg)
% C12TA Cl
Chiuz, 2005, 39, 36-44
0 20 40 60 80 100
Tem
pera
tur
kubi
sch
Mizellen hexa
gona
l
kubi
sch
lam
ella
r
c.m.c = 0,45 %
c.m.c = critical micellar concentration
N+
Selbstorganisation von Tensiden
![Page 3: 8. Poröse Materialien Proteine mikroporösmesoporös 2 nm makroporös ZeolitesMCMsBio-foams 50 nm Moleküle.](https://reader035.fdocument.pub/reader035/viewer/2022062818/55204d6349795902118b8870/html5/thumbnails/3.jpg)
Mizellen sind über einen größeren Bereich regelmäßig angeordnet
Stäbchenmizellen:
HexagonalPeriodisch in zwei Dimensionen
aa
![Page 4: 8. Poröse Materialien Proteine mikroporösmesoporös 2 nm makroporös ZeolitesMCMsBio-foams 50 nm Moleküle.](https://reader035.fdocument.pub/reader035/viewer/2022062818/55204d6349795902118b8870/html5/thumbnails/4.jpg)
N+
Hexadecyltrimethylammoniumbromid
2 nm
Synthese von MCM41
Angew. Chem. 2006, 118, S. 5335; Angew. Chem. 2003, 115, 3730
![Page 5: 8. Poröse Materialien Proteine mikroporösmesoporös 2 nm makroporös ZeolitesMCMsBio-foams 50 nm Moleküle.](https://reader035.fdocument.pub/reader035/viewer/2022062818/55204d6349795902118b8870/html5/thumbnails/5.jpg)
Si
OEt
EtO O
OEt
Si
OEt
OEt
O Si
OEt
OEt
O Si
OEt
OEt
O Si
OEt
OEt
OEt
Si
OEt
EtO OEt
OEt
Si
OEt
EtO OH
OEt
Si
OEt
EtO OH
OEt
Si
OEt
HO OEt
OEt
Si
OEt
EtO O
OEt
Si
OEt
OEt
OEt
H2O
Hydrolyse
Kondensation - H2O
Oligokieselsäure
Kondensation der Silikatvorstufen
![Page 6: 8. Poröse Materialien Proteine mikroporösmesoporös 2 nm makroporös ZeolitesMCMsBio-foams 50 nm Moleküle.](https://reader035.fdocument.pub/reader035/viewer/2022062818/55204d6349795902118b8870/html5/thumbnails/6.jpg)
Si
OEt
EtO O
OEt
Si
OEt
OEt
O Si
OEt
OEt
O Si
OEt
OEt
O Si
OEt
OEt
OEt
Si
OEt
EtO O
O
Si
OEt
O
O Si
OEt
O
O Si
OEt
O
O Si
OEt
OEt
O
Si
O
EtO O Si
O
O Si
O
O Si
O
O Si
O
OEt
O O O O O
Si
O
EtO O
OEt
Si
O
OEt
O Si
O
OEt
O Si
O
OEt
O Si
O
OEt
OEt
![Page 7: 8. Poröse Materialien Proteine mikroporösmesoporös 2 nm makroporös ZeolitesMCMsBio-foams 50 nm Moleküle.](https://reader035.fdocument.pub/reader035/viewer/2022062818/55204d6349795902118b8870/html5/thumbnails/7.jpg)
True Liquid Crystal Templating (LCT)
Bei hohen Tensidkonzentrationen
LC
LC-Bildung Auffüllen
![Page 8: 8. Poröse Materialien Proteine mikroporösmesoporös 2 nm makroporös ZeolitesMCMsBio-foams 50 nm Moleküle.](https://reader035.fdocument.pub/reader035/viewer/2022062818/55204d6349795902118b8870/html5/thumbnails/8.jpg)
Kooperativer Mechanismus
Silikat-anionen
LC-Bildung
Si
OEt
HO OEt
OH
Si
OEt
O OEt
O
NH3
![Page 9: 8. Poröse Materialien Proteine mikroporösmesoporös 2 nm makroporös ZeolitesMCMsBio-foams 50 nm Moleküle.](https://reader035.fdocument.pub/reader035/viewer/2022062818/55204d6349795902118b8870/html5/thumbnails/9.jpg)
aa
sin = /2d =1,5405 / (2•39) = 0,0198
1/d2 = 4(h2 + hk + k2)/(3a2) + l2/c2
a = 45 Åd100 = 31/2a/2
d100 = 39 Å
2 = 2.26°
d100
Pulverdiffraktogramme
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J. S. Beck et al., J. Am. Chem. Soc. 1992, 114, 10837.
dp = 2 nm dp = 4 nm
dp = 6,5 nm dp = 10 nm
SiO2
Transmissionselektronenmikroskopie
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Andere Mesostrukturen
MCM-41
MCM-48
MCM-50
0 20 40 60 80 100
Tem
pera
tur
kubi
sch
Mizellen
hexa
gona
l
kubi
sch
lam
ella
r
![Page 12: 8. Poröse Materialien Proteine mikroporösmesoporös 2 nm makroporös ZeolitesMCMsBio-foams 50 nm Moleküle.](https://reader035.fdocument.pub/reader035/viewer/2022062818/55204d6349795902118b8870/html5/thumbnails/12.jpg)
Andere Materialien
TiO2
CdS
Pt
C
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TiO2
Antonelli, Angew. Chem. 1995, 107, 2203.
Calc.
350°C
TiO2TiO2•H2O
Ti
OEtO
EtO
EtO
Ti
OEt
EtO OEt
OEt
H2O
Hydrolyse
O
Ti
OEtO
EtO
HO O
acac
- EtOH
OP
O
O OTensid
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CdS
OO
OOH
Flüssigkristall
Cd(NO3)2 H2S
CdS
Tohver, Chem. Mater. 1997, 9, 1495.
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Metalle
Flüssigkristall
H2PtCl6 N2H4
Pt-Metall
C16EO8
OO
OOH
Attard, Angew. Chem. 1997, 109, 1372.
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Kohlenstoff: CMK-3
Sacharose (Rohrzucker)
+
H2SO4
PyrolysePyrolyse HF or NaOHHF or NaOH
Nanocasting
Mesoporöses SiOMesoporöses SiO22 (SBA-15)(SBA-15)
SiOSiO22/Kohlenstoff/Kohlenstoff
KompositKomposit
Mesoporöser Mesoporöser Kohlenstoff (CMK-3)Kohlenstoff (CMK-3)
Carbon Mesostructured by Kaist
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Profil
Porengröße: 3-5 nm
Spez. OF: 700-1500 m2g-1
Geordnet
Zusammensetzung
Oberflächenfunktionalität
Anwendungen
Katalyse
Membranen
Adsorbentien
Quantenstrukturen
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Epoxidierung
O
Ti-Zeolith OH2C CH2
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Epoxidierung
Statt H2O2 auch TBHP:
O
OH
Ti
OSi
OSi
OHSiO TiSiO
SiOO
SiOO
H
O H H2C CH2H2O2
TiSiO
SiOO
SiO
O H
H
O H
H2C CH2
H
TiSiO
SiO
SiO OH
O
+
+ H2O
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Epoxidierung
Ti-MCM-41
O
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H2
Pd/Al-MCM-41
Saure Crackfunktion
Palladium Metall: Hydrierfunktion
Hydrocracken
AlO
Si
H
AlO
Si
H
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Metallierte Silicaphasen
Pd H2
350°CPd Metall
Gasphasenabscheidung
Pd
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Feinchemie: Heck Reaktion
R
R
X
+
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Mechanismus der Heck Reaktion
PdL2
Pd
L
L
Ar X
ArX
Pd
L
Ar X
R
L
R
PdL
X
LAr
R
L
Pd
L
L
H X
B
BHX
Ar
R
Oxidative Addition
Migratorische Insertion
ß-Hydrideliminierung
Regenerierung
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Veankerung von Basischen Zentren an MCM-41
triazabicyclodecene
OCN
COOEt
O
CN
EtOOC
+MCM-TBD
Si OO
O
O O
NH N
N
Si O
OH
N N
N
O
O
O
pKB = 25
•High activity•Good reusability•low thermal stability
Y. V. S. Rao, D.E. De Vos, P.A. Jacobs, Angew. Chem. Int. Ed. Engl. 1997, 36, 2661- 2663.
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Komplexe
OH
OH
OH
Si
Si
O
OSi ClO
O
O
Si
- 3 MeOH
Si ClO
O
OMeMe
Me
3-Chlorpropyl-trimethoxysilan
N
R
R
N
N O
R
R
Mn
O
Cl
•Katalytisch aktive Komplexe (Epoxidierung)
•Leichte Abtrennbarkeit
(Salicylidenaminopropyl)amin
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Epoxidierung mit Mangan (III)
Mn(III)
O=Mn(V)
Oxidationsmittel:HOCl
O
OH
IO
Iodosylbenzol
O
Kochi, J. Am. Chem. Soc. 1986, 108, 2309.
MnN
O O
N
O+
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Polymerisation
SiO
SiSi
SiO
SiSi Zr
ClCl
AlO
Cl
Cl
Zr CH3+
MAO
Polyethylen, Polypropylenz.T. verbesserte Polymereigenschaften
Zr CH3+
Zr+Zr
+Zr+
![Page 29: 8. Poröse Materialien Proteine mikroporösmesoporös 2 nm makroporös ZeolitesMCMsBio-foams 50 nm Moleküle.](https://reader035.fdocument.pub/reader035/viewer/2022062818/55204d6349795902118b8870/html5/thumbnails/29.jpg)
O
Regenerierung120-150°C
O
Adsorption
Mitsubishi Heavy Industries
M41 Materialien als Adsorbentien
![Page 30: 8. Poröse Materialien Proteine mikroporösmesoporös 2 nm makroporös ZeolitesMCMsBio-foams 50 nm Moleküle.](https://reader035.fdocument.pub/reader035/viewer/2022062818/55204d6349795902118b8870/html5/thumbnails/30.jpg)
OH
OH
OH
Si
Si
O
OSi ClO
O
O
Si
SH
Hg2+ Pb2+
Feste Anbindung von Hg2+ oder Pb2+
Poröser Filter
M41 Materialien als Adsorbentien
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Wu und Bein., Chem. Mater. 1994, 6, 1109.
Elektrisch Leitendes Polyanilin in MCM-41
Mesoporöse Wirtsgitter
NH
NH
N
NH
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Metallische Nanodrähte
HFPt(NH3)4(NO3)2
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Halbleiter
CdS, ZnS, GaN
Ener
gie
Größe der Partikel
Porengröße Hirai, J. Phys. Chem. B, 1999, 103, 4228.
3,8 nm
3,6 nm2,0 nm
Porengröße
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Oxidpartikel
ZrO2 Nanopartikel
ZrOCl2
Lösung
Erhitzen
SBA-15
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Problem 1: Defekte
Problem 2: Orientierung
Poröse Membranen
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Poröse Membranen
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Aluminiumoxid
Aluminium
Al2O3
+
-Wässr. Schwefelsäure
z.B. 15 % H2SO4: Al2O3 geringfügig löslich
2 Al 2 Al3+ + 6e-
6 H+ + 6e- 3 H2
2 Al3+ + 3 OH- Al2O3 + 3 H+
2 Al + 3 H2O Al2O3 + 3 H2
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Struktur
20 – 100 nm
Al
ca. 75 nm
Sander et al., Chem. Mater. 2003, 15, 335.
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Geordnete Strukturen
Al
Periodischer Stempel (SiC oder Si3N4, Lithographisch)
Al
Defekterzeugung Anodisierung
Al
H. Masuda, K. Fukuda, Science 1995, 268, 1466.
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Membranen
Al
Oxidation in Lösung 5% H3PO4
HgCl2
Monodisperse Emulsionstropfen(SiO2 Nanopartikel)
Na2SiO3
Yanagishita, Langmuir 2004, 20, 554.
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Anderer Anwendungen: Färbung von Aluminium
Al
Farbstoff
z. B. PbCrO4
Oder organische Farbstoffe
AlErhitzen in Wasser
Versiegeln
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Al
Au-elektrode
I
Feuchtigkeitssensor: Stromstärke ändert sich mit H2O-Gehalt.
Sensoren
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Katalytische Anwendungen
Al
1-2 m
Metall z. B. Pt
H
CH H
H
OC
O
+ O2
z.B. katalytische Verbrennung
O2 O
AgOder Epoxidierung
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Nanodrähte
Al
H3PO4
AlAl
+-
Ag+ Ag+
Al
Cross section Choi et al., Chem. Mater. 2003, 15, 776.
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Mikroreaktionstechnik: Ermöglicht die sichere Reaktionsführung in explosiven Reaktionsgemischen
O2
O
Ehrfeld Mikrotechnik
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Integrierter Mikro-Reaktor in Si Technologie (H2-Dampfreformer)
Silizium Reaktor mit integrierter Palladium-Membran zur Wasserstofferzeugung
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etched silicon-plates
Housing from high temp.steel (1.4841)
15 mm
12 mm
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17,6µm
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• <100> p-type silicon wafers (5-1000 cm), 300µm thick, 10cm diameter• H2SO4 / H2O2 cleaning• anodic etchig using electrolyte containing aqueous HF / DMF –solution (Dimethylformamide) • galvanostatic condition (constant current)
Lehmann et al. Journal of the Electroch. Society146 (8) 2968-2975 (1999)
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Silicon substrate
Silicon substrateSi-nitride (SiO2)
photo resist
1
2
Silicon substrate
Silicon substrate
3
4
lithographyand oxide etching
KOH - etching
KOH etches silicon very selectively to the crystal orientation, (111) planes are etched very slowly.
Formation of inverted pyramids
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<100> Silicon substratePd, (PdCu0.4) /Pt
Pd, (PdCu0.4) /Pt
Pd/Pt back metal sputtering
Deep anodic etching
5
6
HF:H2O:Iso-Prop. {5:25:9}(j=15mA/cm2, galvanostatic conditions)
Wafer etch through in 3h35‘
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