Tender X-ray Photoelectron Spectroscopy (TX-XPS, 1.75~6 keV)

柔X光光電子能譜(TX-XPS, 1.75~6 keV)

X-ray Photoelectron Spectroscopy (XPS) is a surface-sensitive quantitative detection and analysis technology. Monochromatic X-rays are used to enter the sample, causing photoelectron emission, and an energy spectrometer is used to analyze the energy of the emitted electrons to obtain surface element information related to the sample.

柔X光光電子能譜(TX-XPS, 1.75~6 keV)

 

The advantage of the synchrotron radiation light source is that the X-ray energy incident on the sample can be adjusted very conveniently. According to the diagram on the left of the electron kinetic energy and mean free path, the effective depth of the sample detected will also change with different X-ray energies.

 

XPS depth analysis in traditional laboratories must be combined with ion beam processing to remove surface materials in order to measure deeper signals. However, this also destroys the sample structure and may affect the characteristics of the sample.

 

Synchrotron radiation XPS can use continuous energy adjustment to detect sample signals at different depths without destroying the surface structure of the sample, thereby ensuring the integrity of the sample structure and the authenticity of the signal.

柔X光光電子能譜(TX-XPS, 1.75~6 keV)

Photoelectrocatalytic

 

XPS analyzes of the NTG photoanode were conducted to determine its chemical environment. The wide scan spectra ( Figure 2a ) identified C 1s, O 1s, Ti 2p, and N 1s. The XPS O 1s spectrum ( Figure 2b ) exhibited contributions at 530.35 eV (Ti-O bound) and 532.85 eV (C=O on the NTG film surface). The high-resolution XPS C 1s spectrum ( Figure 2c ) indicated the presence of residual carbon at 289.5 eV and COC bonds. Additionally, the high- resolution _ _ _  _ _  _ _  _ _  _ _ 2e ) revealed contributions at 399.7 eV and 407.4 eV, linked to substitutional and interstitial nitrogen in N-Ti-N and NO-Ti type structures. XPS spectra indicated the N-doping of TiO 2  with the presence of nitrogen in the TiO 2  lattice.

 

Reference:
MI Carreño-Lizcano, Andrés F. Gualdrón-Reyes, V. Rodríguez-González, JA Pedraza-Avella, ME Niño-Gómez. Photoelectrocatalytic phenol oxidation employing nitrogen-doped TiO2-rGO films as photoanodes. Catalysis Today 2020, 341, 96-103. 
https://www.sciencedirect.com/science/article/abs/pii/S0920586119300495

 

 

 

 

柔X光光電子能譜(TX-XPS, 1.75~6 keV)

Chemistry

 

XPS was utilized to gain a structural understanding of two types of dimensionally controllable 2D-WS 2  colloidal nanoflakes (NFLs) synthesized through a surfactant-assisted non-hydrolytic route. The XPS analysis of NFLs sample B ( blue ) revealed the presence of both 2H and 1T/1T' forms of WS 2 , with 1T'-WS 2  being the predominant form (56.8 ± 5.4%), as depicted in  Figure 3a . Evidence of partial oxidation was observed in signals corresponding to WO x  species. In  Figure 3b , the S 2p region displays three components, indicating the presence of S 2−  ions in WS 2  and two types of sulfur ions (S 2 2−  and S 2− ) associated with WO x S y  formation. The ratio between the doublet peaks of S 2p species at higher binding energy exceeded the theoretical value, possibly due to minor contributions from other sulfur species. The atomic ratio between S 2p and W 4f aligned with the stoichiometric ratio. Similar chemical composition and structure were noted in WS 2  NFLs sample A ( green ), suggesting that alkylamines influenced reactivity and lateral size but not atomic structure. The effectiveness of the XPS technique was evident in providing information on both chemical speciation and the existence of two crystal phases, 1T/1T' and 2H.

 

Reference:
Scarfiello R., Mazzotta E., Altamura D., Nobile C., Mastria R., Rella S., Giannini C., Cozzoli PD, Rizzo A., Malitesta C. An Insight into Chemistry and Structure of Colloidal 2D- WS 2  Nanoflakes: Combined XPS and XRD Study. Nanomaterials 2021, 11, 1969. https://doi.org/10.3390/nano11081969

柔X光光電子能譜(TX-XPS, 1.75~6 keV)

Corrosion Studies

 

The study focused on the corrosion reaction characteristics, employing XPS depth profiling to understand the elemental composition changes in corroded FeSiAl alloy (FSA).  Figure 4a  shows a survey spectrum of identified surface elements (Fe, Si, Al, O, C, Cl) . Elemental concentrations were calculated with Ar ion beam dissection of the FSA at various sputtering times (0-390s) as shown in  Fig. 4b . Fe, O, and C dominated the after-corroded surface, showing the prevalence of Fe-based matter . Deep-level XPS analysis explored Fe and C composition and oxidation states. Fe 2p3/2 spectra indicated a shift in Fe concentration with increased sputtering time ( Fig. 4c ). Fe transitions (Fe 0  → Fe 2+  → Fe 3+ ) were observed, with identified compounds such as FeCl 3 , Fe 2 O 3 , FeO, and Fe 3 O 4 . Deeper regions revealed varied compositions, showcasing the complexity of corrosion layers. High-resolution C1s spectra analysis displayed C–O, C= OC=C/C–C, and C–C bonds ( Fig. 4j ). The presence of oxygen-containing groups and molecular CO x  indicated the involvement of CO 2  in the corrosion process. Chemical composition changes during sputtering time demonstrated the transformation process from Fe 0  → Fe 2+  → Fe 3+ . The study provided detailed insights into the corrosion behavior and composition evolution of FSA, crucial for understanding corrosion mechanisms in materials.

 

Reference:

Guo, Yang; Ali, Rashad; Zhang, Xingzhong; Tian, ​​Wei; Zhang, Li; Lu, Haipeng; Jian, Xian; Xie, Jianliang; Deng, Longjiang (2020). Raman and XPS depth profiling technique to investigate the Corrosion behavior of FeSiAl alloy in salt spray environment. Journal of Alloys and Compounds, 834(), 155075–. doi:10.1016/j.jallcom.2020.155075

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