Adsorption of Anhydrous Hydrogen Fluoride onto Silicon and Native Oxide by XPS

Saito, Yoji

doi:10.1116/1.1247921

Cited by 4 publications

(4 citation statements)

References 2 publications

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“…The fits were constrained by the fwhm and binding energies of the individual Si oxidation states as described in section II.1 . The binding energies of the silicon oxidation states of 4+, 3+, 2+, 1+, and 0 are shown by the dashed lines in Figure . − Figure a depicts the SiO 2 control sample with a broad peak at 104.3 eV. This peak position is consistent with literature values for SiO 2 and silicon atoms in the Si 4+ oxidation state…”

Section: Resultssupporting

confidence: 84%

“…The binding energy positions for the 3+, 2+, 1+, and 0 oxidation states were defined as −1, −2, −3, and −4 eV with respect to the 4+ peak. 25,26 The fwhm values of the 3+, 2+, 1+, and 0 oxidation states were set to 1.2 ± 0.1, 1.1 ± 0.1, 1.0 ± 0.1, and 1.0 ± 0.1 eV, respectively. 25−27 2.…”

Section: Methodsmentioning

confidence: 99%

“…The binding energy (104.3 eV) and fwhm (2.1 eV) of the 4+ oxidation state were imposed in the fittings of the TMA-only and TMA/HF exposed samples. The binding energy positions for the 3+, 2+, 1+, and 0 oxidation states were defined as −1, −2, −3, and −4 eV with respect to the 4+ peak. , The fwhm values of the 3+, 2+, 1+, and 0 oxidation states were set to 1.2 ± 0.1, 1.1 ± 0.1, 1.0 ± 0.1, and 1.0 ± 0.1 eV, respectively. − …”

Section: Experimental Sectionmentioning

confidence: 99%

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Thermal Atomic Layer Etching of SiO₂ by a “Conversion-Etch” Mechanism Using Sequential Reactions of Trimethylaluminum and Hydrogen Fluoride

DuMont

Marquardt

Cano

et al. 2017

ACS Appl. Mater. Interfaces

114

142

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The thermal atomic layer etching (ALE) of SiO was performed using sequential reactions of trimethylaluminum (TMA) and hydrogen fluoride (HF) at 300 °C. Ex situ X-ray reflectivity (XRR) measurements revealed that the etch rate during SiO ALE was dependent on reactant pressure. SiO etch rates of 0.027, 0.15, 0.20, and 0.31 Å/cycle were observed at static reactant pressures of 0.1, 0.5, 1.0, and 4.0 Torr, respectively. Ex situ spectroscopic ellipsometry (SE) measurements were in agreement with these etch rates versus reactant pressure. In situ Fourier transform infrared (FTIR) spectroscopy investigations also observed SiO etching that was dependent on the static reactant pressures. The FTIR studies showed that the TMA and HF reactions displayed self-limiting behavior at the various reactant pressures. In addition, the FTIR spectra revealed that an AlO/aluminosilicate intermediate was present after the TMA exposures. The AlO/aluminosilicate intermediate is consistent with a "conversion-etch" mechanism where SiO is converted by TMA to AlO, aluminosilicates, and reduced silicon species following a family of reactions represented by 3SiO + 4Al(CH) → 2AlO + 3Si(CH). Ex situ X-ray photoelectron spectroscopy (XPS) studies confirmed the reduction of silicon species after TMA exposures. Following the conversion reactions, HF can fluorinate the AlO and aluminosilicates to species such as AlF and SiOF. Subsequently, TMA can remove the AlF and SiOF species by ligand-exchange transmetalation reactions and then convert additional SiO to AlO. The pressure-dependent conversion reaction of SiO to AlO and aluminosilicates by TMA is critical for thermal SiO ALE. The "conversion-etch" mechanism may also provide pathways for additional materials to be etched using thermal ALE.

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Section: Resultssupporting

confidence: 84%

Section: Methodsmentioning

confidence: 99%

Section: Experimental Sectionmentioning

confidence: 99%

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Thermal Atomic Layer Etching of SiO₂ by a “Conversion-Etch” Mechanism Using Sequential Reactions of Trimethylaluminum and Hydrogen Fluoride

DuMont

Marquardt

Cano

et al. 2017

ACS Appl. Mater. Interfaces

114

142

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“…Here, HF addition may change the surface electrochemical conditions, which then changes the number density of the pyramid nuclei. It has been reported that HF can be adsorbed on a Si surface to form F–Si bonds. − The adsorption of F species on Si(111) was confirmed by X-ray photoelectron spectroscopy (XPS) measurements, as shown in Figure a. The photoelectron emission intensities from F 1s increased when the more concentrated HF is in the electrolyte solution, which indicated that the amount of F on the Si(111) surface increased.…”

Section: Results and Discussionmentioning

confidence: 72%

Effects of HF on the Lithiation Behavior of the Silicon Anode in LiPF₆ Organic Electrolyte Solution

2020

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As one of the major impurities in the organic electrolyte, HF can react with the alkali components in the solid electrolyte interphase (SEI), such as lithium alkoxide and lithium carbonate, to form more LiF-rich SEI. Here, the effects of HF on the lithiation behavior of the single crystal Si(111) anode were studied using scanning electron microscopy, soft X-ray emission spectroscopy, and windowless energy-dispersive X-ray spectroscopy. When the Li−Si alloy is formed in 1.0 M LiPF 6 in the propylene carbonate solvent, it has a layered structure that contained the first layer of crystalline Li 15 Si 4 (c-Li 15 Si 4 ) alloy pyramids, the second layer of amorphous Li 13 Si 4 (a-Li 13 Si 4 ) alloy, and a third layer of Li-diffused Li x Si alloy. When the more concentrated HF is in the electrolyte solution, less amount of the c-Li 15 Si 4 alloy is formed in the first layer. It suggests that the Si lithiation can form only amorphous Li x Si alloy relative to the components in the electrolytes. The study also explains why only amorphous Li x Si alloy formation was observed in some previous studies.

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UiO-66-NH2: a recyclable and efficient sorbent for dispersive solid-phase extraction of fluorinated aromatic carboxylic acids from aqueous matrices

Kumar

Sharma

2023

Anal Bioanal Chem

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Adsorption of Anhydrous Hydrogen Fluoride onto Silicon and Native Oxide by XPS

Cited by 4 publications

References 2 publications

Thermal Atomic Layer Etching of SiO₂ by a “Conversion-Etch” Mechanism Using Sequential Reactions of Trimethylaluminum and Hydrogen Fluoride

Thermal Atomic Layer Etching of SiO₂ by a “Conversion-Etch” Mechanism Using Sequential Reactions of Trimethylaluminum and Hydrogen Fluoride

Effects of HF on the Lithiation Behavior of the Silicon Anode in LiPF₆ Organic Electrolyte Solution

UiO-66-NH2: a recyclable and efficient sorbent for dispersive solid-phase extraction of fluorinated aromatic carboxylic acids from aqueous matrices

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Adsorption of Anhydrous Hydrogen Fluoride onto Silicon and Native Oxide by XPS

Cited by 4 publications

References 2 publications

Thermal Atomic Layer Etching of SiO2 by a “Conversion-Etch” Mechanism Using Sequential Reactions of Trimethylaluminum and Hydrogen Fluoride

Thermal Atomic Layer Etching of SiO2 by a “Conversion-Etch” Mechanism Using Sequential Reactions of Trimethylaluminum and Hydrogen Fluoride

Effects of HF on the Lithiation Behavior of the Silicon Anode in LiPF6 Organic Electrolyte Solution

UiO-66-NH2: a recyclable and efficient sorbent for dispersive solid-phase extraction of fluorinated aromatic carboxylic acids from aqueous matrices

Contact Info

Product

Resources

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Thermal Atomic Layer Etching of SiO₂ by a “Conversion-Etch” Mechanism Using Sequential Reactions of Trimethylaluminum and Hydrogen Fluoride

Thermal Atomic Layer Etching of SiO₂ by a “Conversion-Etch” Mechanism Using Sequential Reactions of Trimethylaluminum and Hydrogen Fluoride

Effects of HF on the Lithiation Behavior of the Silicon Anode in LiPF₆ Organic Electrolyte Solution