J. AM. CHEM. SOC. 2008, 130, 7686-7694

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9JULY2011 SEOK, SANGJUN J. AM. CHEM. SOC. 2008, 130, 7686-7694

Transcript of J. AM. CHEM. SOC. 2008, 130, 7686-7694

Page 1: J. AM. CHEM. SOC. 2008, 130, 7686-7694

9JULY2011

SEOK, SANGJUN

J. AM. CHEM. SOC. 2008, 130, 7686-7694

Page 2: J. AM. CHEM. SOC. 2008, 130, 7686-7694

Abstract

+ + + + + + - - - - - - d- d+

protonated deprotonated

Page 3: J. AM. CHEM. SOC. 2008, 130, 7686-7694

Experimental Arrangement

a-Al2O3 (0001) sample

- Thickness 5-mm, root-mean-square roughness 0.2 nm

- Cleaned in a sonication (acetone, methanol, and pure water for 10, 10, and

60 min. mildly etched by 10-15 mM solution of HNO3 for 30 min.

As a sample for comparison (amorphous alumina)

- 10-nm thick was prepared by the atomic layer deposition (ALD) method on a

a-Al2O3 (0001) substrate using trimethyllaluminum (Al2(CH3)6.

- Cleaned in organic solvents as described above.

- The spectral intensity, comparison with monolayer of octadecanetrichlosilane,

indicates that the surface density of residual –CH3 contaminant is less than

1/nm2.

The pH solution

- Sodium hydroxide or hydrochloric acid (37 wt % water solution)

Page 4: J. AM. CHEM. SOC. 2008, 130, 7686-7694

Results – SSP SFVS of following interfaces :

a-Al2O3 (0001)/Air Interface A-Al2O3 (0001)/air after

cleaning

A-Al2O3 (0001)/H2O

A-Al2O3 (0001)/D2O

A-Al2O3 (0001)/air after

being retrieved from

D2O (60% relative hum.)

A-Al2O3 (0001)/air after

heating 600 C for 1 h

After being exposed to

ambient air for 48 h

SSP

These results suggest that the spectrum came from hydroxyls at the

alumina/air interface.

Page 5: J. AM. CHEM. SOC. 2008, 130, 7686-7694

Results – SFG with SSP, PPP, and SPS

a-Al2O3 (0001)/Air Interface

The much weaker 3700 cm-1 peaks in

SPS and PPP

The amplitude ratio : Aq,eff(SSP)Aq,eff(PPP)/Aq,eff(SPS)=1:0.42±0.03:0.06±0.03

The tilt angle of dangling OH bond is around 26±2

Page 6: J. AM. CHEM. SOC. 2008, 130, 7686-7694

Results – SSP SFVS

water/ a-Al2O3 (0001)Interface at different bulk pH values

+ + + + + + d-

- - - - - - d+

Positively

surface

Neutrally

surface

negatively

surface

icelike

negligible

Liquidlike

remain

Page 7: J. AM. CHEM. SOC. 2008, 130, 7686-7694

Results – SFG with SSP, PPP, and SPS

water/ a-Al2O3 (0001)Interface at different bulk pH values

Page 8: J. AM. CHEM. SOC. 2008, 130, 7686-7694

Results – SSP SFVS

water/ a-Al2O3 (0001)Interface at different bulk pH values

+ + + + + + d-

- - - - - - d+

positive neutral negative

Page 9: J. AM. CHEM. SOC. 2008, 130, 7686-7694

Results – point of zero charge (PZC) at neutral surface

water/ a-Al2O3 (0001)Interface at different bulk pH values

positive neutral negative

Langmuir, 9, 7 (1993)

Heterogeneity of proton binding sites at the oxide/solution

interface

Proton affinity

distribution from

isotherm

The degrees of

protonation of the

different categories of

sites (proton binding) Local adsorption

isotherm

Page 10: J. AM. CHEM. SOC. 2008, 130, 7686-7694

Results – point of zero charge (PZC) at neutral surface

water/ a-Al2O3 (0001)Interface at different bulk pH values

Langmuir, 9, 7 (1993)

Heterogeneity of proton binding sites at the oxide/solution

interface

Proton affinity

distribution from

isotherm

The degrees of

protonation of the

different categories of

sites (proton binding) Local adsorption

isotherm

pH= [(pK=6.7)+(pK=3)]/2

= 6.35

PZC

Page 11: J. AM. CHEM. SOC. 2008, 130, 7686-7694

Results – SSP SFVS

water/ a-Al2O3 (0001)Interface at different bulk pH values with Salt

solution

Screening of the

surface field by the

electrolyte

Salt ions are not

attracted to the

interface

Page 12: J. AM. CHEM. SOC. 2008, 130, 7686-7694

Results – SSP SFVS

water/ amorphous alumina Interface at different bulk pH values

PZC


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