The Use of Electron Probe MicroAnalysis to Determine the Thickness of Thin Films in Materials Science

Christien, Frédéric; Ferchaud, E.; Nowakowski, Paweł; Allart, Marion

doi:10.5772/28877

Cited by 6 publications

(5 citation statements)

References 11 publications

(15 reference statements)

Supporting

Mentioning

Contrasting

Order By: Relevance

“…The software Stratagem was used for EDX measurements because first the volume irradiated by the electron beam and second the X-ray collected are related to a larger depth than the thickness of the top layer. [31] The atomic percentages were determined by considering a theoretical model for the probed zone [32]. For this, three layers were considered: first, Raman spectroscopy measurements were performed using a microconfocal Raman microscope (Renishaw inVia).…”

Section: Characterization Of the Nc Thin Filmsmentioning

confidence: 99%

TiO₂–SiO₂ nanocomposite thin films deposited by direct liquid injection of colloidal solution in an O₂/HMDSO low-pressure plasma

Mitronika¹,

Profili²,

Goullet³

et al. 2020

J. Phys. D: Appl. Phys.

View full text Add to dashboard Cite

TiO2 nanoparticles (NPs), 3 nm in size, were injected inside a very-low-pressure O2 plasma reactor using a liquid injector and following an iterative injection sequence.Simultaneously, hexamethyldisiloxane (HMDSO) vapor precursor was added to create a SiO2 matrix and a TiO2-SiO2 nanocomposite (NC) thin film. Both the liquid injection and vapor precursor parameters were established to address the main challenges observed when creating NCs. In contrast to most aerosol-assisted plasma deposition processes, Scanning/Transmission Electron Microscopy (S/TEM) indicated isolated (i.e. non-agglomerated) NPs distributed in a rather uniform way in the matrix. The fraction of the TiO2 NPs inside the SiO2 matrix was estimated by SEM, Spectroscopic Ellipsometry (SE), and X-ray Photoelectron Spectroscopy.All techniques provided coherent values, with percentages between 12 and 19%. Despite the presence of TiO2 NPs, SE measurements confirmed that the plasma-deposited SiO2 matrix was dense with an optical quality similar to the one of thermal silica. Finally, the percentage of TiO2 NPs inside the SiO2 matrix and the effective refractive index of the NCs can be tuned through judicious control of the injection sequence.

show abstract

Section: Characterization Of the Nc Thin Filmsmentioning

confidence: 99%

TiO₂–SiO₂ nanocomposite thin films deposited by direct liquid injection of colloidal solution in an O₂/HMDSO low-pressure plasma

Mitronika¹,

Profili²,

Goullet³

et al. 2020

J. Phys. D: Appl. Phys.

View full text Add to dashboard Cite

show abstract

“…An accelerating voltage of 20 keV and a beam current of 20 nA were used with a defocused 3 μm beam. The produced X-ray intensities were subject to a PAP (phi-rho-z) matrix correction algorithm as described by Pouchou and Pichoir (1987) and reported by Christien et al, 63 and converted to concentrations by comparison to metal oxide standards. The concentration data for the major elements were collected on pressed power samples.…”

Section: ■ Experimental Sectionmentioning

confidence: 99%

Catalytic Transfer Hydrogenolysis of Switchgrass Lignin with Ethanol Using Spinel-Type Mixed-Metal Oxide Catalysts Affords Control of the Oxidation State of Isolated Aromatic Products

Godwin,

Babusci,

Wonderling

et al. 2024

ACS Sustainable Chem. Eng.

View full text Add to dashboard Cite

Chemical reductions of lignin are useful to remove oxygen and create product slates that can function as renewable platform molecules for new fuels and chemicals. Catalytic transfer hydrogenolysis (CTH) is an underexplored method to reduce lignin that obviates the use of dangerous and nonrenewable hydrogen gas. While noble metals are used extensively as catalysts for transfer hydrogenation, sustainability remains a major challenge to their deployment. In this work, we synthesized mixed-metal oxides of earth-abundant Co and Ni and characterized the catalysts using powder X-ray diffraction (XRD). Catalyst reactivity for the CTH of acetophenone was also assessed. Among the catalysts tested, spinel NiCo 2 O 4 demonstrated the highest conversion of acetophenone (75%) and the highest selectivity for ethylbenzene (90%); thus, we applied it to valorize switchgrass lignin, extracted under mild operating conditions by cosolvent enhanced lignocellulosic fractionation (CELF). The catalytically depolymerized lignin showed an increase in the number of selectively deoxygenated monomeric compounds. As demonstrated using 2D-NMR spectroscopy, the lignin displayed highly reduced aliphatic carbons, resulting from the catalyst-mediated reduction reaction at the Cα sites. These results are critical to the further development of the lignin-first biorefinery as they demonstrate the use of sustainable catalyst materials and mild transformation conditions to generate and refine a suite of new bioproducts.

show abstract

“…An accelerating voltage of 20 keV and a beam current of 20 nA were used with a defocused 3 µm beam. The produced X-ray intensities were subject to a PAP (phi-rho-z) matrix correction algorithm as described by Pouchou and Pichoir (1987) and reported by Christien et al, 63 and converted to concentrations by comparison to metal oxide standards. The concentration data for the major elements were collected on pressed power samples.…”

Section: Catalyst Characterizationmentioning

confidence: 99%

Catalytic transfer hydrogenolysis of switchgrass lignin with ethanol using spinel-type mixed-metal oxide catalysts affords control of the oxidation state of isolated aromatic products

Godwin,

Babusci,

Wonderling

et al. 2023

Preprint

View full text Add to dashboard Cite

Chemical reductions of lignin are useful to remove oxygen and create product slates that can function as renewable platform molecules for new fuels and chemicals. Catalytic transfer hydrogenolysis (CTH) is an underexplored method to conduct reductions of lignin that obviates the use of dangerous and non-renewable hydrogen gas. While noble metals are used extensively as catalysts for transfer hydrogenation, one major challenge for their deployment is related to their sustainability. In this work, we synthesized mixed-metal oxides of earth-abundant Co and Ni. We characterized these catalysts using powder x-ray diffraction (XRD) and tested their reactivity for CTH of acetophenone. Among the catalysts we tested, we noted that the spinel NiCo2O4 demonstrated the highest conversion of acetophenone (75%) and highest selectivity for ethylbenzene (90%), so we applied it to valorization of switchgrass lignin extracted under mild operating conditions by cosolvent enhanced lignocellulosic fractionation (CELF). The catalytically depolymerized lignin showed an increase in selectively deoxygenated monomeric compounds. Using 2D-NMR spectroscopy, we demonstrated the lignin displayed highly reduced aliphatic carbons resulting from the reduction reaction at the Cα sites mediated by our catalyst material. These results are critical to the further development of the lignin-first biorefinery as they demonstrate the use of sustainable catalyst materials and mild transformation conditions to generate and refine a suite of new bioproducts.

show abstract

The Use of Electron Probe MicroAnalysis to Determine the Thickness of Thin Films in Materials Science

Cited by 6 publications

References 11 publications

TiO₂–SiO₂ nanocomposite thin films deposited by direct liquid injection of colloidal solution in an O₂/HMDSO low-pressure plasma

TiO₂–SiO₂ nanocomposite thin films deposited by direct liquid injection of colloidal solution in an O₂/HMDSO low-pressure plasma

Catalytic Transfer Hydrogenolysis of Switchgrass Lignin with Ethanol Using Spinel-Type Mixed-Metal Oxide Catalysts Affords Control of the Oxidation State of Isolated Aromatic Products

Catalytic transfer hydrogenolysis of switchgrass lignin with ethanol using spinel-type mixed-metal oxide catalysts affords control of the oxidation state of isolated aromatic products

Contact Info

Product

Resources

About

The Use of Electron Probe MicroAnalysis to Determine the Thickness of Thin Films in Materials Science

Cited by 6 publications

References 11 publications

TiO2–SiO2 nanocomposite thin films deposited by direct liquid injection of colloidal solution in an O2/HMDSO low-pressure plasma

TiO2–SiO2 nanocomposite thin films deposited by direct liquid injection of colloidal solution in an O2/HMDSO low-pressure plasma

Catalytic Transfer Hydrogenolysis of Switchgrass Lignin with Ethanol Using Spinel-Type Mixed-Metal Oxide Catalysts Affords Control of the Oxidation State of Isolated Aromatic Products

Catalytic transfer hydrogenolysis of switchgrass lignin with ethanol using spinel-type mixed-metal oxide catalysts affords control of the oxidation state of isolated aromatic products

Contact Info

Product

Resources

About

TiO₂–SiO₂ nanocomposite thin films deposited by direct liquid injection of colloidal solution in an O₂/HMDSO low-pressure plasma

TiO₂–SiO₂ nanocomposite thin films deposited by direct liquid injection of colloidal solution in an O₂/HMDSO low-pressure plasma