Glass formation in and structural investigation of Li2S+GeS2+GeO2 composition using Raman and IR spectroscopy

Kim, Young‐Sik; Saienga, Jason; Martin, Steve W.

doi:10.1016/j.jnoncrysol.2005.09.028

Cited by 46 publications

(42 citation statements)

References 24 publications

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“…While Kim et al 28 and Itoh et al 29 reported on the Li 2 S þ GeS 2 bulk glass system, detailed characterizations of thin films in this system have not been reported to date.…”

Section: Introductionmentioning

confidence: 99%

Structural Properties of Lithium Thio-Germanate Thin Film Electrolytes Grown by Radio Frequency Sputtering

Seo

Martin

2011

Inorg. Chem.

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In this study, lithium thio-germanate thin film electrolytes have been successfully prepared by radio frequency (RF) magnetron sputtering deposition in Ar gas atmospheres. The targets for RF sputtering were prepared by milling and pressing appropriate amounts of the melt-quenched starting materials in the nLi2S + GeS2 (n = 1, 2, and 3) binary system. Approximately 1 μm thin films were grown on Ni coated Si (Ni/Si) substrates and pressed CsI pellets using 50 W power and 25 mtorr (3.3 Pa) Ar gas pressures to prepare samples for Raman and Infrared (IR) spectroscopy, respectively. To improve the adhesion between the silicon substrate and the thin film electrolyte, a sputtered Ni layer (120 nm) was used. The surface morphologies and thickness of the thin films were determined by field emission scanning electron microscopy (FE-SEM). The structural properties of the starting materials, target materials, and the grown thin films were examined by X-ray diffraction (XRD), Raman, and IR spectroscopy. Disciplines Materials Science and Engineering | Physical Chemistry CommentsReprinted with permission from Inorganic Chemistry 50 (2011) ABSTRACT: In this study, lithium thio-germanate thin film electrolytes have been successfully prepared by radio frequency (RF) magnetron sputtering deposition in Ar gas atmospheres. The targets for RF sputtering were prepared by milling and pressing appropriate amounts of the meltquenched starting materials in the nLi 2 S þ GeS 2 (n = 1, 2, and 3) binary system. Approximately 1 μm thin films were grown on Ni coated Si (Ni/Si) substrates and pressed CsI pellets using 50 W power and 25 mtorr (∼3.3 Pa) Ar gas pressures to prepare samples for Raman and Infrared (IR) spectroscopy, respectively. To improve the adhesion between the silicon substrate and the thin film electrolyte, a sputtered Ni layer (∼120 nm) was used. The surface morphologies and thickness of the thin films were determined by field emission scanning electron microscopy (FE-SEM). The structural properties of the starting materials, target materials, and the grown thin films were examined by X-ray diffraction (XRD), Raman, and IR spectroscopy.

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“…While Kim et al 28 and Itoh et al 29 reported on the Li 2 S þ GeS 2 bulk glass system, detailed characterizations of thin films in this system have not been reported to date.…”

Section: Introductionmentioning

confidence: 99%

Structural Properties of Lithium Thio-Germanate Thin Film Electrolytes Grown by Radio Frequency Sputtering

Seo

Martin

2011

Inorg. Chem.

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“…This shows the existence of both of four-and six-coordination. The absorption at 500-600 cm -1 is attributed to the antisymmetrical bending vibration of a Pb-O-Pb chain [13] and also related to bending, and the symmetric stretching vibration of Ge-O-Ge in the GeO 4 tetrahedral unit [12]. The weak peak observed at 470 cm -1 is related to the symmetrical bending vibration of Pb-O in a PbO 4 tetragonal pyramid [14].…”

Section: Ftirmentioning

confidence: 93%

“…A wide and intense band at 650-850 cm -1 is deconvulated into two peaks at 710 and 770 cm -1 . These peaks are related to the stretching vibration mode of Ge-O-Ge bonds in GeO 6 octahedral units [11] and antisymmetric stretching vibrations of Ge-O-Ge bonds in GeO 4 tetrahedral units [12], respectively. This shows the existence of both of four-and six-coordination.…”

Section: Ftirmentioning

confidence: 98%

Characterization and Synthesis of Silver Nanostructures in Rare Earth Activated GeO2-PbO Glass Matrix Using Matrix Adjustment Thermal Reduction Method

Bahari

Zamiri

Sidek

et al. 2013

Entropy

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This paper reports matrix adjustment thermal reduction method to synthesize silver nanostructures in Er 3+ /Yb 3+ activated GeO 2 -PbO glass matrix. The GeO 2 -PbO glass, the medium of nanoparticle formation, doped with Er 2 O 3 , Yb 2 O 3 and AgNO 3 was prepared by a melt quenching method. Annealing of the glass for different times was utilized, not only due to thermally reduce Ag + ions to Ag nanostructures, but also to influence the glassy network. This is because, the glass structural transformation temperature is near to 435 °C and heating at more than this temperature can cause some structural changes in the glass matrix. According to TEM images, samples that tolerate 450 °C annealing temperature for one hour show the formation of basil-like silver nanostructures with a mean length of 54 nm and mean diameter of 13 nm embedded in the glass matrix, whereas with annealing at 450 °C for 5 to 20 h, silver nanoparticles of about 3-4 nm mean diameter size are formed. Annealing for 30 h causes silver nanoparticles to aggregate to form larger particles due to an Oswald ripening process. Observation of the characteristic Ag-NP SPR band at 400-500 nm in the UV-visible absorption spectra confirms the existence of silver OPEN ACCESSEntropy 2013, 15 1529 nanoparticles. The SPR band widens to longer wavelengths in one hour annealed samples, which relates to the existence of nanostructures with different size or fractal shapes. In addition, an increment in the peak of the SPR band by increasing the duration of annealing indicates the formation of more nanoparticles. Furthermore, the existence of a peak at 470 cm -1 in the FTIR spectra of annealed samples and its absence in the samples not exposed to an annealing process suggests that the glass matrix is polymerized by Pb-O chains during the 450 °C annealing process. This is the main source of different nanostructures because of the dissimilar stabilizing media. The tighter media cap the particles to form small and dense nanoparticles but a loose environment leads to the creation of basil-like particles in the glass matrix.

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“…These intensities are attributable to PS 4 and GeS 4 units in the SE structure, respectively. 26,27 The decrease in the intensity of the Raman bands indicates a distortion of the polyhedral units or decomposition of the materials incorporating the specific units, 28,29 indicating that the mechanical milling either reduced the symmetry of these local structures or decomposed the SE. On the other hand, the diffraction peaks in the XRD pattern result from long-range ordering of the crystal structure, which is composed of the ordered arrangements of polyhedral units.…”

Section: ¹1mentioning

confidence: 99%

Composite Sulfur Electrode for All-solid-state Lithium–sulfur Battery with Li2S–GeS2–P2S5-based Thio-LISICON Solid Electrolyte

et al. 2018

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Composite sulfur electrodes are prepared by prolonged mechanical milling (;300 min) for use in all-solid-state lithium-sulfur batteries, and their structure and electrochemical properties are investigated. These batteries exhibit a high initial discharge capacity (>1500 mAh g −1). Sulfur, acetylene black, and the solid electrolyte Li 3.25 -Ge 0.25 P 0.75 S 4 are mixed by planetary ball milling to form composites that contain amorphous phases of the starting materials, as well as a byproduct with a novel structural unit arising from the reaction between sulfur and the solid electrolyte. Batteries with a composite electrode/Li 3.25 Ge 0.25 P 0.75 S 4 /Li-In anode configuration exhibit a high initial discharge capacity (>1100 mAh g −1). However, the capacity fades during cycling (~500 mAh g −1 at the 30th cycle), possibly because of the increased resistance of the composite. Structural and compositional changes of the byproduct and the solid electrolyte itself during the battery reaction could contribute to the increase in resistance that cause the deterioration of cyclability.

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Glass formation in and structural investigation of Li2S+GeS2+GeO2 composition using Raman and IR spectroscopy

Cited by 46 publications

References 24 publications

Structural Properties of Lithium Thio-Germanate Thin Film Electrolytes Grown by Radio Frequency Sputtering

Structural Properties of Lithium Thio-Germanate Thin Film Electrolytes Grown by Radio Frequency Sputtering

Characterization and Synthesis of Silver Nanostructures in Rare Earth Activated GeO2-PbO Glass Matrix Using Matrix Adjustment Thermal Reduction Method

Composite Sulfur Electrode for All-solid-state Lithium–sulfur Battery with Li<sub>2</sub>S–GeS<sub>2</sub>–P<sub>2</sub>S<sub>5</sub>-based Thio-LISICON Solid Electrolyte

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