Spectroscopic and AFM studies of the functionalisation of carbon

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Short presentation to the Faraday discussion No. 173 about our studies of functional groups at carbon surfaces. We have selectively derivatised oxygen groups and can unambiguously identify OH and C=O groups. We are also fairly confident about the presence of O-C-O!

Science

Surface science & catalysis group
Cardiff Catalysis Institute
3
Mild acid treatment of HOPG
(c) HCl/573K
(b) HCl
What are the oxygen states?
How do they affect Carbon-Metal interactions?
542 537 532 527
Binding energy /eV
O(1s)
(a) Clean
531.5
533.3
HOPG

Surface science & catalysis group
Cardiff Catalysis Institute
4
Molecule specific labeling:
Is OH(a) present?
OH(a) + CF3C(O)OC(O)CF3 (g) à CF3C(O)O-(a) + CF3CO2H(g)
688.8
F(1s)
(d) HCl/573 K
& TFAA
(c) HCl/TFAA
(a) Clean/TFAA
699 694 689 684 679
Binding energy /eV
532.6
534.0
531.6
O(1s)
(d) HCl/ 573 K
& TFAA
(c) HCl/TFAA
(a) Clean
542.0 537.0 532.0 527.0
Binding energy /eV
(b) HCl
OH(a)
532.6 eV
Not all OH is functionalised

Surface science & catalysis group
Cardiff Catalysis Institute
à CF3C(OH)O-(a) + H2O(g)
5
Is –CO2H present?
(c) HCl/573 K
& TFE
(b) HCl/TFE
-CO2H(a) + CF3CH2OH(g)
699 694 689 684 679
Binding energy /eV
F(1s)
(a) Clean/TFE
688.4
Not significantly!

Surface science & catalysis group
Cardiff Catalysis Institute
6
C=O ?
688.4
F(1s)
(d)
(c)
(a)
-CO(a) + CF3CH2NH-NH2 (g)
HCl /573 K /TFH
HCl /TFH
690 685 680
Binding energy /eV
Clean
à CF3CH2NH-N=(a) + H2O(g)
C=O(a)
531.5 eV
(c) HCl/573K
(b) HCl
542 537 532 527
Binding energy /eV
O(1s)
(a) Clean
531.5
533.3
OH(a)
532.6 eV
-C-O-C-(a)
533.3 eV

Surface science & catalysis group
Cardiff Catalysis Institute
7
Gold deposition
Au(4f)
84.9!
86.5! 84.0!
(c) HCl /573 K
& Au!
(b) HCl /Au!
(a) Clean!
93 Bindin8g8 energy /8e3V 78
HOPG
C=O
C-O-C
OH(a)
Cl(2p)
(c)
(b)
(a)
198.0
199.7
205 200 195
Binding energy /eV
Au0
Au3+

Surface science & catalysis group
Cardiff Catalysis Institute
8
The Stability of Functional Groups: DFT
• Calculated stable structure for
OH at graphite edges
• High OH density
• See Poster 38 for OH….Au

Surface science & catalysis group
Cardiff Catalysis Institute
9
Gold 2015
7th International Gold Conference
26th – 29th July 2015 in Cardiff, UK
www.cardiff.ac.uk/gold2015
Abstract submission 1st September – 14th October 2014

Surface science & catalysis group
Cardiff Catalysis Institute
10

The most difficult goal in the next few decades is the replacement of conventional petro-based fuels with more sustainable fuels that can be used in the existing infrastructure. By the use of Renewable energy or nuclear energy, CO2 and H2O can be recycled into liquid hydrocarbon fuels (the reverse of fuel combustion). Capture of CO2 from the atmosphere will form a close carbon-neutral fuel cycle loop. This article also reviews the aspects regarding thermodynamics involved, involved mechanisms and possible technological pathways for recycling CO2 into fuels using renewable energy. These pathways can be broken into three staged- CO2 capture from atmosphere, H2O and CO2 dissociation, and fuel synthesis.

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Spectroscopic and AFM studies of the functionalisation of carbon

1. Surface science & catalysis group Cardiff Catalysis Institute 1 XPS, AFM & DFT studies of the functionalization of graphite Dr Philip R. Davies Carlo Buonoa, Robert J. Daviesb, Thomas Jonesa, Jiří Kulhavýc, Ryan Lewisa, David J. Morgana, Neil Robinsona and David J. Willocka Cardiff Catalysis Institute School of Chemistry, Cardiff University Cardiff

2. Surface science & catalysis group Cardiff Catalysis Institute 2 Motivation • Carbon catalyst supports • Graphene based sensors • Intracellular nanodiamond sensors HOPG Strategy • Multilayer graphene • Ambient preparation conditions • Surface sensitive analysis • DFT analysis of surface chemistry Highly ordered pyrolytic graphite (HOPG)

3. Surface science & catalysis group Cardiff Catalysis Institute 3 Mild acid treatment of HOPG (c) HCl/573K (b) HCl What are the oxygen states? How do they affect Carbon-Metal interactions? 542 537 532 527 Binding energy /eV O(1s) (a) Clean 531.5 533.3 HOPG

4. Surface science & catalysis group Cardiff Catalysis Institute 4 Molecule specific labeling: Is OH(a) present? OH(a) + CF3C(O)OC(O)CF3 (g) à CF3C(O)O-(a) + CF3CO2H(g) 688.8 F(1s) (d) HCl/573 K & TFAA (c) HCl/TFAA (a) Clean/TFAA 699 694 689 684 679 Binding energy /eV 532.6 534.0 531.6 O(1s) (d) HCl/ 573 K & TFAA (c) HCl/TFAA (a) Clean 542.0 537.0 532.0 527.0 Binding energy /eV (b) HCl OH(a) 532.6 eV Not all OH is functionalised

5. Surface science & catalysis group Cardiff Catalysis Institute à CF3C(OH)O-(a) + H2O(g) 5 Is –CO2H present? (c) HCl/573 K & TFE (b) HCl/TFE -CO2H(a) + CF3CH2OH(g) 699 694 689 684 679 Binding energy /eV F(1s) (a) Clean/TFE 688.4 Not significantly!

6. Surface science & catalysis group Cardiff Catalysis Institute 6 C=O ? 688.4 F(1s) (d) (c) (a) -CO(a) + CF3CH2NH-NH2 (g) HCl /573 K /TFH HCl /TFH 690 685 680 Binding energy /eV Clean à CF3CH2NH-N=(a) + H2O(g) C=O(a) 531.5 eV (c) HCl/573K (b) HCl 542 537 532 527 Binding energy /eV O(1s) (a) Clean 531.5 533.3 OH(a) 532.6 eV -C-O-C-(a) 533.3 eV

7. Surface science & catalysis group Cardiff Catalysis Institute 7 Gold deposition Au(4f) 84.9! 86.5! 84.0! (c) HCl /573 K & Au! (b) HCl /Au! (a) Clean! 93 Bindin8g8 energy /8e3V 78 HOPG C=O C-O-C OH(a) Cl(2p) (c) (b) (a) 198.0 199.7 205 200 195 Binding energy /eV Au0 Au3+

8. Surface science & catalysis group Cardiff Catalysis Institute 8 The Stability of Functional Groups: DFT • Calculated stable structure for OH at graphite edges • High OH density • See Poster 38 for OH….Au

9. Surface science & catalysis group Cardiff Catalysis Institute 9 Gold 2015 7th International Gold Conference 26th – 29th July 2015 in Cardiff, UK www.cardiff.ac.uk/gold2015 Abstract submission 1st September – 14th October 2014

10. Surface science & catalysis group Cardiff Catalysis Institute 10

Spectroscopic and AFM studies of the functionalisation of carbon

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