Lead

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Lead

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Orbitals and Energies #

Note – these are listed in BINDING ENERGY

 

Pb 4s ≈ 894 eV

Pb 4p ≈ 645 eV

Pb 4d ≈ 413 eV

Pb 44 ≈ 138 eV

Pb 5s ≈ 145 eV

Pb 5p ≈ 86 eV

Pb 5d ≈ 20 eV

 

Etched lead Survey With Peak Markers for Pb

Doublet Separations #

Pb 4f = 4.9 eV

Pb 4d = 22.1 eV

Pb 4p = ~ 118 eV

Pb 5d = 2.6 eV

Pb 5p = 22.4 eV

XPS of Pb 4f with doublet separation

Common Overlaps for Pb 4f #

Si 2s P 2p – Zn 3s – Tl 5s – Sn 4s – As 3p – Fr 5p – Gd 4d – Xe 4p – Tb 4d – Pb 5s – Sb 4s – Ra 5p

Pb 4f Region With Overlapping Peak Markers

Auger Energies #

Note – these are listed in KINETIC ENERGY

 

Pb NOO ≈ 260 eV

XPS of Pb NOO Region

Common Binding Energies – Pb 4f #

Species #

B.E. / eV #

Charge Ref #

Reference #

Pb Metal

136.6

Au 4f (83.8 eV)

PbF2

PbCl2

PbBr2

PbI2

PbO

PbS

PbSe

PbTe

PbAc2

2PbCO3.Pb(OH)2

PbCrO4

Pb(IO4)2

PbNCN

Pb(NO3)2

PbO2

Pb(OH)2

PbSiO3

PbSO4

PbTiO3

PbWO4

PbZrO3

138.3

138.7

138.6

138.15

137.5

137.3

137.4

137.05

137.05

138.2

138.1

138

137.3

138.3

137.2

137.75

138.45

139.8

137.8

138.5

138.3

C 1s (284.6 eV)

Theory and Background #

Lead compounds may be difficult to distinguish, particularly those of the oxides, due to similarities in binding energy. It is often advisable to record the Pb MNN auger to assist in speciation. (You can download the raw data for these Wagner plots in the supplementary section).

Wagner Plot for Selected Pb compounds
Wagner Plot for Selected Pb Compounds

Experimental Advice #

Pb(0) artefacts may be caused by X-ray photolysis, which induces the reduction of Pb(II) to Pb(0) under typical analytical conditions. Additionally, chemical changes due to film aging in air and the presence of PbI2 in the perovskite films can facilitate in situ reactions that generate these artefacts. To prevent Pb(0) artefacts, it is important to minimize X-ray exposure time to limit photolysis effects, perform XPS analysis on freshly prepared samples to reduce the impact of film aging, and conduct the analysis under a clean ultra-high vacuum (UHV) conditions to mitigate the influence of environmental factors.

See our article on X-ray damage for more information on preventing this.

Data Analysis Guidance #

Pb 4f peaks display symmetric, gaussian-like peaks, and do not display any particular irregularities.

Reference Datasets #

 

Coming soon

References #

  1. Pederson, L. R. “Two-dimensional chemical-state plot for lead using XPS.” Journal of Electron Spectroscopy and Related Phenomena 28.2 (1982): 203-209. Read it online here.