Thickness of carbon coatings on silicon materials determined by hard X-ray photoelectron spectroscopy at multiple photon energies

2019 ◽  
Vol 26 (6) ◽  
pp. 1936-1939 ◽  
Author(s):  
Noritake Isomura ◽  
Naoko Takahashi ◽  
Satoru Kosaka ◽  
Hiroyuki Kawaura

Hard X-ray photoelectron spectroscopy at multiple photon energies is used to investigate the surface structure of carbon coatings on silicon materials destined for use as negative electrodes in lithium-ion batteries. The photoelectron intensity from the carbon coatings decreases with an increase in the kinetic energy of the photoelectron. By fitting the photoelectron intensity versus energy to numerically derived curves, the thickness and coverage of the carbon coatings can be obtained. The results are in agreement with the values suggested by the cross-sectional secondary-electron microscopy images of the carbon coatings, although the thickness should be corrected by accounting for the rectangular parallelepiped structure of the silicon material.

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Yang Liu ◽  
Hongtao Yu ◽  
Xie Quan ◽  
Shuo Chen

MoS2/CdS photocatalyst was fabricated by a hydrothermal method for H2production under visible light. This method used low toxic thiourea as a sulfur source and was carried out at 200°C. Thus, it was better than the traditional methods, which are based on an annealing process at relatively high temperature (above 400°C) using toxic H2S as reducing agent. Scanning electron microscopy and transmission electron microscopy images showed that the morphologies of MoS2/CdS samples were feather shaped and MoS2layer was on the surface of CdS. The X-ray photoelectron spectroscopy testified that the sample was composed of stoichiometric MoS2and CdS. The UV-vis diffuse reflectance spectra displayed that the loading of MoS2can enhance the optical absorption of MoS2/CdS. The photocatalytic activity of MoS2/CdS was evaluated by producing hydrogen. The hydrogen production rate on MoS2/CdS reached 192 μmol·h−1. This performance was stable during three repeated photocatalytic processes.


2008 ◽  
Vol 23 (11) ◽  
pp. 3048-3055 ◽  
Author(s):  
K. Polychronopoulou ◽  
J. Neidhardt ◽  
C. Rebholz ◽  
M.A. Baker ◽  
M. O’Sullivan ◽  
...  

Nanocomposite Cr–B–N coatings were deposited from CrB0.2 compound targets by reactive arc evaporation using an Ar/N2 discharge at 500 °C and −20 V substrate bias. Elastic recoil detection (ERDA), x-ray photoelectron spectroscopy (XPS), x-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), and selected-area electron diffraction (SAED) were used to study the effect of the N2 partial pressure on composition and microstructure of the coatings. Cross-sectional scanning electron microscopy (SEM) showed that the coating morphology changes from a glassy to a columnar structure with increasing N2 partial pressure, which coincides with the transition from an amorphous to a crystalline growth mode. The saturation of N content in the coating confirms the formation of a thermodynamically stable CrN–BN dual-phase structure at higher N2 fractions, exhibiting a maximum in hardness of approximately 29 GPa.


2005 ◽  
Vol 20 (9) ◽  
pp. 2462-2473 ◽  
Author(s):  
Zhaoming Zhang ◽  
Mark G. Blackford ◽  
Gregory R. Lumpkin ◽  
Katherine L. Smith ◽  
Eric R. Vance

We have characterized thermally annealed perovskite (CaTiO3) surfaces, both before and after aqueous dissolution testing, using scanning electron microscopy, cross-sectional transmission electron microscopy, x-ray photoelectron spectroscopy, and atomic force microscopy. It was shown that mechanical damage caused by polishing was essentially removed at the CaTiO3 surface by subsequent annealing; such annealed samples were used to study the intrinsic dissolution behavior of perovskite in deionized water at RT, 90 °C, and 150 °C. Our results indicate that, although mechanical damage caused higher Ca release initially, it did not affect the long-term Ca dissolution rate. However, the removal of surface damage by annealing did lead to the subsequent spatial ordering of the alteration product, which was identified as anatase (TiO2) by both x-ray and electron diffraction, on CaTiO3 surfaces after dissolution testing at150 °C. The effect of Ca2+ in the leachant on the dissolution reaction of perovskite at 150 °C was also investigated, and the results suggest that under repository conditions, the release of Ca from perovskite is likely to be significantly slower if Ca2+ is present in ground water.


Coatings ◽  
2019 ◽  
Vol 9 (4) ◽  
pp. 253 ◽  
Author(s):  
Wei-Chun Chen ◽  
Chao-Te Lee ◽  
James Su ◽  
Hung-Pin Chen

Zirconium diboride (ZrB2) thin films were deposited on a Si(100) substrate using pulsed direct current (dc) magnetron sputtering and then annealed in high vacuum. In addition, we discussed the effects of the vacuum annealing temperature in the range of 750 to 870 °C with flowing N2 on the physical properties of ZrB2 films. The structural properties of ZrB2 films were investigated with X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM), and X-ray photoelectron spectroscopy (XPS). The XRD patterns indicated that the ZrB2 films annealed at various temperatures exhibited a highly preferred orientation along the [0001] direction and that the residual stress could be relaxed by increasing the annealing temperature at 870 °C in a vacuum. The surface morphology was smooth, and the surface roughness slightly decreased with increasing annealing temperature. Cross-sectional TEM images of the ZrB2/Si(100) film annealed at 870 °C reveals the films were highly oriented in the direction of the c-axis of the Si substrate and the film structure was nearly stoichiometric in composition. The XPS results show the film surfaces slightly contain oxygen, which corresponds to the binding energy of Zr–O. Therefore, the obtained ZrB2 film seems to be quite suitable as a buffer layer for III-nitride growth.


2020 ◽  
Vol 20 (5) ◽  
pp. 2911-2916
Author(s):  
Zhen Zhang ◽  
Xiao Chen ◽  
Guangxue Zhang ◽  
Chuanqi Feng

The MoO3/V2O5/C, MoO3/C and V2O5/C are synthesized by electrospinning combined with heat treatment. These samples are characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy and thermogravimetric analysis (TG) techniques. The results show that sample MoO3/V2O5/C is a composite composed from MoO3, V2O5 and carbon. It takes on morphology of the nanofibers with the diameter of 200~500 nm. The TG analysis result showed that the carbon content in the composite is about 40.63%. Electrochemical properties for these samples are studied. When current density is 0.2 A g−1, the MoO3/V2O5/C could retain the specific capacity of 737.6 mAh g−1 after 200 cycles and its coulomb efficiency is 92.99%, which proves that MoO3/V2O5/C has better electrochemical performance than that of MoO3/C and V2O5/C. The EIS and linear Warburg coefficient analysis results show that the MoO3/V2O5/C has larger Li+ diffusion coefficient and superior conductivity than those of MoO3/C or V2O5/C. So MoO3/V2O5/C is a promising anode material for lithium ion battery application.


2019 ◽  
Vol 6 (2) ◽  
pp. 181116 ◽  
Author(s):  
Qian Kang ◽  
Yimin Zhang ◽  
Shenxu Bao ◽  
Guobin Zhang

VO 2 (B) has shown excellent cathode performance in lithium batteries and become a hot research topic in recent years. A stripped vanadium solution extracted from vanadium-bearing shale containing a high concentration of vanadium and certain amounts of impurities was used as a vanadium source to synthesize VO 2 (B) by hydrothermal process. The VO 2 conversion rate can reach as high as 99.47% in a reaction time of 8 h, and this is the highest result reported. The crystalline structure and morphology of the synthesized products were characterized by X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), Scanning electron microscopy (SEM) and Transmission electron microscopy (TEM). Furthermore, the electrochemical properties of VO 2 (B) in lithium-ion batteries were investigated. The results indicated that the VO 2 (B) has the initial specific discharge capacity of 192.0 mAh g −1 . Stripped vanadium solution is a raw material for producing V 2 O 5 and NH 4 VO 3 , which are indispensable vanadium sources in VO 2 synthesis. Therefore, synthesis of VO 2 via hydrothermal reduction by oxalic acid using stripped vanadium solution extracted from vanadium-bearing shale as a direct vanadium source is an eco-friendly, innovative and efficient method, and will have a great impact on VO 2 synthesis.


Author(s):  
K. Ganesh Kumar ◽  
P. Balaji Bhargav ◽  
C. Balaji ◽  
Ahmed Nafis ◽  
K. Aravinth ◽  
...  

Abstract Owing to high lithium ion conductivity and good stability with lithium metal, Li7La3Zr2O12 (LLZO—a solid electrolyte) has emerged as a viable candidate for solid-state battery applications. In the current study, Al-substituted LLZO (Al-LLZO) powder is synthesized using a typical solid-state reaction. The pellets are made with the synthesized powder and are subjected to annealing for different durations and its effect on the structural properties of the Al-LLZO is investigated in detail. Reitveld refinement of the powder X-ray diffraction pattern reveals that the sintered Al-LLZO belong to the cubic system with the Ia-3d space group at room temperature. Morphology and microstructural properties of sintered powder are analyzed using field emission scanning electron microscopy (FESEM) and high-resolution transmission electron microscopy (HRTEM)/selected area electron diffraction (SAED), respectively. The FESEM image of LLZO pellets shows well-structured cubic grains spread evenly over on the surface after sintering. The chemical compositions of the sample are identified using energy dispersive X-ray analysis (EDAX). The surface chemistry of the prepared samples is examined by X-ray photoelectron spectroscopy (XPS), which states that the observed photoelectron signals from O 1s at about 531 eV and Li1s at 54.52 eV correspond to the Li-O bond in Al-LLZO. Raman spectra have been analyzed and the observed Raman peaks appearing at 299 cm−1, 393 cm−1, 492 cm−1, and 514 cm−1 were assigned to Eg, F2g, A1g, and F2g, respectively. Phase transformation from C-LLZO to the pyrochore LZO phase is noticed when the sample is sintered for 12 h at 1100 °C. The impedance analysis is carried out to measure the conductivity of the Al-LLZO pellet and is found to be 0.3 × 10−5 S cm−1, which is suitable for solid electrolyte applications in lithium ion batteries.


2008 ◽  
Vol 8 (6) ◽  
pp. 3203-3207 ◽  
Author(s):  
Changjie Mao ◽  
Xingcai Wu ◽  
Jun-Jie Zhu

A large number of β-AgVO3 nanowires with diameter of 30–60 nm, and length of 1.5–3 μm have been successfully synthesized by a simple and facile low-temperature sonochemical route. The morphologies and structures of the nanowires were characterized by X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), scanning transmission electron microscopy (SEM), and thermal gravimetric analysis (TGA). Cyclic voltammetry and charge–discharge experiments were applied to characterize the electrochemical properties of the nanowires as cathode materials for lithium-ion batteries. In the initial discharge and charge process, the as-prepared β-AgVO3 nanowires showed the initial charge and discharge capacities of 69 and 102 (mAh)/g, respectively. It is anticipated that the β-AgVO3 nanostructures are promising cathode candidates in the application of primary lithium-ion batteries.


2002 ◽  
Vol 17 (10) ◽  
pp. 2578-2589 ◽  
Author(s):  
M. L. Carter ◽  
E. R. Vance ◽  
D. R. G. Mitchell ◽  
J. V. Hanna ◽  
Z. Zhang ◽  
...  

The dissolution in de-ionized water (DIW) at 90 and 150 °C of Cs and Ba from mechanically polished Cs-doped Ba hollandite samples is essentially congruent. The normalized Ba and Cs release rates were <0.001 g/m2/day after 56 days in DIW at 90 °C, and the Ba normalized release rate of a Cs-free sample was 0.01 g/m2/day after 56 days in DIW at 150 °C. Varying the pH between approximately 2.5 and 12.9 affected only the Ba dissolution rates of hollandite by half an order of magnitude. The dissolution rates of all species decrease with increasing leaching time due to the formation of partly impervious surface coatings of Al- and Ti-rich species. These surface coatings were investigated by scanning electron microscopy, and in some cases by cross-sectional transmission electron microscopy and x-ray photoelectron spectroscopy.


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