x-ray photoelectron spectroscopy (xps)€¦ · a result of released energy due to atom from higher...

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X-ray Photoelectron Spectroscopy (XPS)

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Page 1: X-ray Photoelectron Spectroscopy (XPS)€¦ · A result of released energy due to atom from higher energy level filling gap of emitted electron from same Laura Trapiella-Alfonso,

X-ray Photoelectron Spectroscopy (XPS)

Page 2: X-ray Photoelectron Spectroscopy (XPS)€¦ · A result of released energy due to atom from higher energy level filling gap of emitted electron from same Laura Trapiella-Alfonso,

Contents

WHAT is XPS?

HOW does it work? An

in-depth look at each

component of the

instrument

WHERE can this

technique be applied?

Page 3: X-ray Photoelectron Spectroscopy (XPS)€¦ · A result of released energy due to atom from higher energy level filling gap of emitted electron from same Laura Trapiella-Alfonso,

WHAT is XPS?

https://slideplayer.com/slide/13488710/

• Quantitative surface analysis technique

• Provides spatial distribution information

via mapping or depth profiling

• Binding energy is measured giving

information on the origin of the

photoelectron

Page 4: X-ray Photoelectron Spectroscopy (XPS)€¦ · A result of released energy due to atom from higher energy level filling gap of emitted electron from same Laura Trapiella-Alfonso,

HOW does this instrument work?

Page 5: X-ray Photoelectron Spectroscopy (XPS)€¦ · A result of released energy due to atom from higher energy level filling gap of emitted electron from same Laura Trapiella-Alfonso,

Applications: Elemental

composition in wide scans

Page 6: X-ray Photoelectron Spectroscopy (XPS)€¦ · A result of released energy due to atom from higher energy level filling gap of emitted electron from same Laura Trapiella-Alfonso,

A result of released

energy due to atom

from higher energy

level filling gap of

emitted electron

from same

Laura Trapiella-Alfonso, Fanny D’Orlye, Philani Mashazi, Anne Varenne*, Tebello Nyokong. Physical and in-solution characterisation of graphitic carbon nitride, graphene and nitrogen-doped graphene quantum dots*, work in progress

Page 7: X-ray Photoelectron Spectroscopy (XPS)€¦ · A result of released energy due to atom from higher energy level filling gap of emitted electron from same Laura Trapiella-Alfonso,

S.R Nxele, T. Nyokong, Conjugation of Azide-functionalised CdSe/ZnS Quantum Dots with Tetrakis(5-hexyn-oxy) Fe(II)

phthalocyanine via Click Chemistry for Electrocatalysis, Electrochim. Acta 194 (2016) 26-39.

1200 1000 800 600 400 200 0

Inte

nsi

ty (

cps)

Binding Energy (eV)

Bare GCP

N(1s)

Zn(2p)

S(2p)

Se(3d)

GSH-capped QDs

N(1s)Cd(3d)

Cd(3d)

Azide-QDs

Fe(2p) N(1s)

C(1s)

O(1s)

clicked FePc-QDs

Analysis done on glassy carbon plates

Page 8: X-ray Photoelectron Spectroscopy (XPS)€¦ · A result of released energy due to atom from higher energy level filling gap of emitted electron from same Laura Trapiella-Alfonso,

Applications: Elemental

composition and bond-types in

high resolution scans

Page 9: X-ray Photoelectron Spectroscopy (XPS)€¦ · A result of released energy due to atom from higher energy level filling gap of emitted electron from same Laura Trapiella-Alfonso,

Physical characterisation: XPS N1s/C1s high

resolution scans & RNH/COOH values

GQDs

0

2

4

6

8

10

12

280282284286288290292

Inte

ns

ity (

x 1

03

cp

s)

Binding energy (eV)

C 1s

0

1

2

3

4

5

6

7

396398400402404

Inte

ns

ity (

x1

03

cp

s)

Binding Energy (eV)

N 1s

Element Binding energy (eV) Peak assignment

C1s 287.5 COOH

286.2 C-O

284.8 C=O

283.9 C=N

N1s 400.9 NH

402.1 NC=O

399.3 N=C

397.4 C-N-C

RNH/COOH = 0.20

9Laura Trapiella-Alfonso, Fanny D’Orlye, Philani Mashazi, Anne Varenne*, Tebello Nyokong. Physical and in-solution characterisation of graphitic carbon nitride, graphene and nitrogen-doped graphene quantum dots*, work in

progress

Page 10: X-ray Photoelectron Spectroscopy (XPS)€¦ · A result of released energy due to atom from higher energy level filling gap of emitted electron from same Laura Trapiella-Alfonso,

Physical characterisation: XPS N1s/C1s high

resolution scans & RNH/COOH values

GQDs

0,0

0,5

1,0

1,5

2,0

2,5

280282284286288290292

Inte

ns

ity (

x 1

04

cp

s)

Binding Energy (eV)

C 1s

0

0,4

0,8

1,2

1,6

2

396398400402404

Inte

ns

ity (

10

3c

ps

)

Binding Energy (eV)

N 1s

Element Binding energy (eV) Peak assignment

C1s

288.4 COOH

286.8 C-O

284.9 C=N

N1s

401.1 NH

399.4 N=C

398.1 C-N-C

RNH/COOH = 0.0410

Page 11: X-ray Photoelectron Spectroscopy (XPS)€¦ · A result of released energy due to atom from higher energy level filling gap of emitted electron from same Laura Trapiella-Alfonso,

Physical characterisation: XPS N1s/C1s high

resolution scans & RNH/COOH values

GQDs

Element Binding energy (eV) Peak assignment

C1s 288.6 COOH

287.2 C=O

285.8 C-O

284.7 C=N

283.4 C-C

N1s 402.4 N-C=O

401.1 N-H

399.2 N=C

398.4 C-N-C

RNH/COOH = 0.4511

Page 12: X-ray Photoelectron Spectroscopy (XPS)€¦ · A result of released energy due to atom from higher energy level filling gap of emitted electron from same Laura Trapiella-Alfonso,

12

390 392 394 396 398 400 402 404 406 408 410

Inte

nsit

y (

cp

s)

Binding Energy (eV)

Azide QDs

Clicked FePc-QDs

405.5

404.6

399.6

399.4

N=N+=N

-

N=N+=N

-

S.R Nxele, T. Nyokong, Conjugation of Azide-functionalised CdSe/ZnS Quantum Dots with Tetrakis(5-hexyn-oxy) Fe(II)

phthalocyanine via Click Chemistry for Electrocatalysis, Electrochim. Acta 194 (2016) 26-39.

Page 13: X-ray Photoelectron Spectroscopy (XPS)€¦ · A result of released energy due to atom from higher energy level filling gap of emitted electron from same Laura Trapiella-Alfonso,

13

David O. Oluwolea*, Sello L. Manotob, Patience Mthunzi-Kufab and Tebello Nyokong, Evaluation of the

Photophysicochemical Properties and Photodynamic Therapy of Zinc Phthalocyanine–Metallic Nanoparticles

Conjugates

Page 14: X-ray Photoelectron Spectroscopy (XPS)€¦ · A result of released energy due to atom from higher energy level filling gap of emitted electron from same Laura Trapiella-Alfonso,

Final remarks

XPS is one of the best techniques to characterize molecules and

determine their elemental composition

It also is good for determining bonds formed between molecules

It is also a useful technique as it gives quantitative data or

information

Page 15: X-ray Photoelectron Spectroscopy (XPS)€¦ · A result of released energy due to atom from higher energy level filling gap of emitted electron from same Laura Trapiella-Alfonso,