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Chen512829 2014-12-28
2.2. Material Characterizations. A field emission scanning electron microscope (SEM, JEOL 6701F) was used to investigate the morphologies, particle sizes of the samples. Transmission electron microscopy and elemental compositions of the ... 2.2. Material Characterizations. A field emission scanning electron microscope (SEM, JEOL 6701F) was used to investigate the morphologies, particle sizes of the samples. Transmission electron microscopy and elemental compositions of the samples were determined by JEM-2100F (JEOL) coupled with an energy-dispersive X-ray spectroscopy (EDX, Phoenix) system. Wide-angle and low-angle X-ray powder diffraction (XRD) of the as-obtained samples were recorded on a Rigaku D/max-2500 with Cu Kα radiation (λ = 1.540 56 Å) operated at 40 kV and 200 mA. Raman measurements were performed using a DXR from Thermo Scientific with a laser wavelength of 532 nm. To calculate the pore size distribution and pore volumes, the nitrogen absorption and desorption isotherms were measured at 77.3 K with an Autosorb-1 specific surface area analyzer from Quantachrome. The content of N in N-doped porous carbon was determined by NHC elemental analysis using Flash EA 1112. Thermogravimetric (TG) analysis of S/C composite was performed on TG/DTA 6300 in an N2 flow to obtain the S content in the composite. A four-contact method was applied to measure the powder electronic conductivity of porous carbons. The powder sample was pressed to disk at 4 MPa with two stainless-steel plungers, whose resistance was measured by a Keithley 2400 digital multimeter in fourwire mode. The conductivity of the sample was calculated according to the resistance and the size of the disk. Information of the surface elements was obtained by X-ray photoelectron spectroscopy (XPS) performed on the Thermo Scientific ESCALab 250Xi using 200 W monochromatic Al Kα radiation. The 500 μm X-ray spot was used for XPS analysis. The base pressure in the analysis chamber was about 3 × 10−10 mbar. All reported data of XPS binding energy are calibrated based on the hydrocarbon C 1s line at 284.8 eV from adventitious carbon. Spectra were fitted with Lorentzian−Gaussian functions and smart background using Thermo Avantage software.
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东霞云霞
2.2。材料特征。场发射扫描
电子显微镜(SEM,JEOL6701F)被用来研究
的形貌,样品的颗粒尺寸。透射电子
样品的显微镜和元素的组合物均
通过JEM-2100F(日本电子)测定加上能量分散
X射线检测器(EDX,菲尼克斯)系统。广角和低角度
将作为得到的样品的X射线粉末衍射(XRD)是
记录在日本理学D / MAX-2500与Cu靶辐射(λ=1.54056
Å)运行在40千伏和200毫安。拉曼光谱测量结果
使用来自Thermo Scientific的一个DXR用激光进行
波长为532纳米。来计算孔径分布和
孔体积,氮吸附和脱附等温线
在77.3ķ测定用AUTOSORB-1的比表面积分析仪
从康塔。的N的N掺杂多孔碳含量为
通过使用Flash EA1112 NHC元素分析法测定。
进行热重(TG)分析,S / C复合材料
上TG / DTA6300在N2
流,以获得在S含量
复合材料。
一个四接触方法应用于测量粉末
多孔炭的电子导电性。的粉末样品是
用两个不锈钢柱塞,其压向磁盘在4MPa
阻力在四线吉时利2400数字万用表测量
模式。样品的导电率,根据算出
电阻和盘的尺寸。
通过X射线得到的表面元件的信息
光电子能谱(XPS)对热进行
科学ESCALAB250Xi使用200瓦单色铝Kα
辐射。在500微米的X射线斑点用于XPS分析。该基地
在分析腔室压力为约3×10 -10毫巴。所有
XPS结合能报告的数据是基于已校准
烃Ç1S线从外来碳284.8电子伏特。谱
分别配备了洛伦兹 - 高斯函数和智能背景
使用热爱维稳特软件。
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