锂离子电池Sn-Al薄膜电极的制备及电化学性能研究

采用磁控溅射沉积技术制备了纳米级Sn-Al合金薄膜电极材料,并用X射线衍射和扫描电子显微镜进行表征,用高精度电池测试系统进行充放电和循环伏安测试.结果表明直流DC与射频RF两种不同的溅射方法制备的Sn-Al薄膜电极具有很大的性能差异,前者DC法制备的材料颗粒细小,表现出稳定的循环性能,其首次放电容量为1060 mAh/g,首次效率为71.7％,电极经过50次循环后比容量保持在700 mAh/g以上.后者RF法制备的材料颗粒较大,放电比容量开始上升,第五次循环后接着逐渐衰减,表现出较差的循环性能. 关键词： 锂离子电池 磁控溅射 Sn-Al合金 电化学性能     

锂离子电池SnSb/MCMB核壳结构负极材料嵌锂性能研究

以酸处理的中间相碳微球(MCMB)为载体, 用化学还原法在碳球表面沉积SnSb合金, 合成SnSb 包覆碳球的核壳结构负极材料. 采用XRD, SEM技术对材料的结构和形貌进行了表征, 用恒电流充放电(CC)、循环伏安(CV)和交流阻抗(EIS)测试了材料的电化学性能. 实验结果表明: SnSb/MCMB样品呈现纳米晶与非晶态的混合组织; 单一SnSb合金的容量衰减较快, 而对于SnSb/MCMB复合材料, 细小的合金颗粒均匀钉扎在MCMB表面, 不仅改善了颗粒的团聚现象, 而且增强了材料的导电能力, 使材料的循环稳定性得到改善, 复合材料具有936.161 mAh/g的首次放电比容量, 首次库仑效率80.3%, 50次循环后容量维持在498.221 mAh/g. 关键词： SnSb合金 锂离子电池 中间相碳微球(MCMB) 电化学性能     

氧化石墨制备温度对石墨烯结构及其锂离子电池性能的影响

采用改进的Hummers 法, 以石墨粉为原料制备氧化石墨, 然后使用微波还原法制备石墨烯, 最后以石墨烯作为负极材料组装锂离子电池. 系统的研究了高温氧化阶段中温度对氧化石墨的氧化程度、石墨烯的还原程度和比表面积以及锂离子电池性能的影响. 利用场发射扫描电镜(FESEM)、 X射线光电子能谱(XPS)、X射线衍射仪(XRD)、BET测量仪对氧化石墨和石墨烯的微观结构及比表面积等进行测试和表征. XRD, XPS及电化学测试的结果显示当高温阶段氧化温度为90 °C时, 氧化石墨的氧化程度最高, 相应的石墨烯也具有最高的还原程度和最大的比表面积423.2 m²/g, 同时石墨烯锂离子电池也具有更好的性能: 首次放电比容量为1555.5 mAh/g, 充电容量为1024.6 mAh/g, 其循环放电比容量达到600 mAh/g.     

锂离子电池LiMn1-xFexPO4(0<x<1)正极材料的制备及性能研究

本文采用固相法制备了纯相LiMn_1-xFe_xPO₄/C (x=0.2,0.4,0.6)正极材料,并用X射线衍射(XRD)和扫描电镜(SEM)进行表征,用高精度电池测试系统进行充放电和循环伏安测试.结果表明不同Mn和Fe原子比的电极材料具有很大的性能差异,其中当x=0.4时,材料具有优异的循环稳定性和较高的可逆容量.首次充电容量和放电容量分别达到141.5 mAh/g和125.7 mAh 关键词： 锂离子电池 固相法 1-xFe_xPO₄')" href="#">LiMn_1-xFe_xPO₄ 正极材料     

钠掺杂磷酸铁锂晶格变化和电化学性能

利用固相法合成了钠掺杂的LiFePO₄,结构表征显示钠离子成功地掺入到了晶格中．SEM显示其粒径在1～3 μm．XRD显示钠掺杂样品晶胞变大．电池测试表明样品0.1 C放电150 mAh/g,5和7.5 C下分别放电109和107 mAh/g．1和5 C循环时,与初始放电容量相比,样品容量保持率分别为84%(1000次循环后)和86%(350次循环后),表现了优异的结构稳定性和循环性能．研究表明钠离子掺杂可以有效地提高磷酸铁锂的电化学活性,尤其是循环性能．     

碳热还原法制备V2O3-C双层包覆磷酸铁锂及其电化学性能

通过V₂O₅的碳热还原反应制备了具有优异倍率性能和循环稳定性的V₂O₃-C双层包覆的磷酸铁锂正极材料. 粉末X射线衍射、元素分析、高分辨投射电镜和拉曼光谱研究表明V2O3相与碳层共包覆于磷酸铁锂颗粒表面. 在V₂O₅的碳热还原反应后,碳含量明显降低,但石墨化程度未发生明显改变. 电化学测试结果表明少量V₂O₃显著改善了磷酸铁锂正极材料的倍率性能和高温循环性能,包含1%氧化钒的复合正极材料在0.2 C放电容量为167 mAh/g,5 C时放电容量为129 mAh/g,并且循环稳定性优异;在55 oC和1 C时放电容量为151 mAh/g,循环100次后无明显容量衰减.     

铝掺杂锰酸锂正极材料制备及第一性原理研究

采用固相法制备出高纯度纳米LiAl0.25Mn1.75O4并用此制备成了半电池,对其进行充放电循环测试和阻抗测试,并与原始LiMn2O4的测试结果相比较。另采用基于密度泛函理论的第一原理方法,研究了掺铝锰酸锂LiAl0.25Mn1.75O4的能带结构、态密度和原子布居,实验与计算分析结果表明LiAl0.25Mn1.75O4在室温下0.01C放电时首次放电容量为124.8mAh/h,室温0.2C下50个循环周期后放电比容量保持率可达到83.6%;LiAl0.25Mn1.75O4的能带带隙为0.21eV,分态密度中Al-s轨道与O-s轨道在-20eV左右的明显杂化,均表明LiAl0.25Mn1.75O4材料具有高导电率、高结构稳定性、高比容量保持率的性能,这为推动锂离子电池锰酸锂正极材料的发展提供理论依据。     

Co$lt;sub$gt;2$lt;/sub$gt;SnO$lt;sub$gt;4$lt;/sub$gt;/Graphene复合材料的制备与电化学性能研究

实验首先采用改进的Hummers法制备氧化石墨,然后以氧化石墨烯为前驱体,通过水热法将锡酸钴纳米颗粒均匀镶嵌在石墨烯薄膜基片上,最终获得Co₂SnO₄/Graphene镶嵌复合材料. 采用X射线衍射（XRD）、扫描电子显微镜（SEM）对材料的结构和形貌进行表征,通过恒电流充放电（CC）、循环伏安法（CV）与交流阻抗法（EIS）测试了材料的电化学性能. 实验结果表明,石墨烯良好的分散性及较高的电子导电率,可以提高锡酸钴材料的电化学性能,材料首次可逆容量达到1415.2 mA·h/g,50次循环后仍能保持469.7 mA·h/g的放电比容量. 关键词： 2SnO₄')" href="#">Co₂SnO₄ 石墨烯 电化学性能 锂离子电池     

三维自支撑甲苯灰微球锂硫电池正极材料的制备与性能研究

新能源交通工具的飞速发展激发了人们对高能量密度电池技术的探索,锂硫电池因为具有较高的理论能量密度被视为锂离子电池的替代品。但由于硫具有导电性差和多硫化物的穿梭效应等问题,锂硫电池的商业化应用仍面临巨大的挑战。基于此,为改善锂硫电池的性能,设计了一种高导电性三维支撑的正极结构:多级交联的三维导电网络能够有效提高正极材料导电性;纳米碳球堆叠形成的孔道结构提供了丰富的反应活性点位和体积缓冲空间。测试结果表明,这种新型正极结构在0.15 C的电流倍率下放电比容量高达1 124 mAh g-1;在2 C的大电流倍率充放电200次循环后,放电比容量仍能保持在591 mAh g~(-1),表现出良好的循环稳定性和电化学稳定性。     

热聚合法制备纳米级Li3V2(PO4)3/C作为锂离子电池正极材料的性能研究

通过热聚合法成功制备出纳米级Li₃V₂（PO₄）₃/C正极材料,中间产物和最终材料的Li₃V₂（PO₄）₃/C颗粒均小于200 nm,无定形碳的含量为4.6%,处于Li₃V₂（PO₄）₃颗粒表面和颗粒与颗粒之间.该材料在3.0sim4.3 V和0.1 C电流下放电比容量为124 mAh/g,100次循环之后无衰减,表现出较好的循环性能.其倍率性能优异,在3.0sim4.3 V和20 C的条件下放电比容量达到80 mAh/g,在3.0sim4.8 V和10 C的条件下放电比容量达到100 mAh/g.     

Investigation of oxidation process and properties of indium and tin-based thin-film heterostructures

Solid-phase processes in thin films (～200 nm) based on tin and indium oxides (ITO structures) prepared by magnetron sputtering from a composite target (93 at % In and 7 at % Sn) and by layer-by-layer deposition of In/Sn/Si and Sn/In/Si structures from two magnetrons in a single vacuum cycle have been investigated in the work under their oxidation in an oxygen flow. Two ways of optically transparent semiconductor film formation have been compared using near-edge fundamental absorption spectroscopy, x-ray diffraction analysis, and electron microscopy and dynamics of the change in their optical and structure properties has been studied. In the case of oxidation of the layer-by-layer deposited structures, the heterogeneous phase composition of the film is confirmed both by the XRD data and by the optical results. Only wide-band-gap phases with an energy of direct transitions of 3.5–3.6 eV have been found in the films prepared by magnetron sputtering from a composite target after their oxidation. These wide-band-gap phases are associated with In₂O₃ oxide and a tin-doped indium oxide compound.     

Mg-Sn-Si合金中Mg2(Si,Sn)复合相的结构与性能研究

研究了铸态Mg-Sn-Si合金中Mg₂(Si,Sn)复合相的结构、 特性以及该相对Mg-Sn-Si合金变质作用的影响. 结果表明: Sn原子能取代Mg₂Si中的部分Si生成Mg₂(Si,Sn)复合相, 该三元相与Mg₂Si, Mg₂Sn相的结构相同, 属于面心立方结构, Mg₂(Si,Sn)相的元素含量并不固定, 在Si富集区形成的Mg₂(Si,Sn)相中, Si元素含量高, 在Si贫乏区形成的Mg₂(Si,Sn)相中, Si元素含量低. Si含量较多的Mg₂(Si,Sn)相性能与Mg₂Si相接近, Sn含量较多的Mg₂(Si,Sn)相性能与Mg₂Sn相接近, 实验中发现Mg₂(Si,Sn)复合相的纳米硬度、 弹性模量与维氏硬度等物理性能介于Mg₂Si与Mg₂Sn之间, Mg₂(Si,Sn)相对汉字状Mg₂Si相的变质处理起到桥梁作用. 关键词： Mg-Sn-Si合金 2Si')" href="#">Mg₂Si 2Sn')" href="#">Mg₂Sn 2(Si,Sn)复合相')" href="#">Mg₂(Si,Sn)复合相     

Effects of rapid thermal annealing on crystallinity and Sn surface segregation of Ge_(1-x)Sn_x films on Si(100) and Si(111)

Germanium-tin films with rather high Sn content(28.04% and 29.61%) are deposited directly on Si(100) and Si(111)substrates by magnetron sputtering. The mechanism of the effect of rapid thermal annealing on the Sn surface segregation of Ge_(1-x)Sn_x films is investigated by x-ray photoelectron spectroscopy(XPS) and atomic force microscopy(AFM). The x-ray diffraction(XRD) is also performed to determine the crystallinities of the Ge_(1-x)Sn_x films. The experimental results indicate that root mean square(RMS) values of the annealed samples are comparatively small and have no noticeable changes for the as-grown sample when annealing temperature is below 400℃. The diameter of the Sn three-dimensional(3 D) island becomes larger than that of an as-grown sample when the annealing temperature is 700℃. In addition, the Sn surface composition decreases when annealing temperature ranges from 400℃ to 700℃. However, Sn bulk compositions in samples A and B are kept almost unchanged when the annealing temperature is below 600℃. The present investigation demonstrates that the crystallinity of Ge_(1-x)Sn_x/Si(111) has no obvious advantage over that of Ge_(1-x)Sn_x/Si(100) and the selection of Si(111) substrate is an effective method to improve the surface morphologies of Ge_(1-x)Sn_x films. We also find that more severe Sn surface segregation occurs in the Ge_(1-x)Sn_x/Si(111) sample during annealing than in the Ge_(1-x)Sn_x/Si(100) sample.     

Sn doping effects on the electro-optical properties of sol gel derived transparent ZnO films

Undoped and tin (Sn) doped ZnO films have been deposited by sol gel spin coating method. The Sn/Zn nominal volume ratio was 1, 3 and 5% in the solution. The effect of Sn incorporation on structural and electro-optical properties of ZnO films was investigated. All the films have polycrystalline structure, with a preferential growth along the ZnO (002) plane. The crystallite size was calculated using a well-known Scherrer's formula and found to be in the range of 26-16 nm. X-ray diffraction patterns of the films showed that Sn incorporation leads to substantial changes in the structural characteristics of ZnO films. The SEM measurements showed that the surface morphology of the films was affected from the Sn incorporation. The highest average optical transmittance value in the visible region was belonging to the undoped ZnO film. The optical band gap and Urbach energy values of these films were determined. The absorption edge shifted to the lower energy depending on the Sn dopant. The shift of absorption edge is associated with shrinkage effect. The electrical conductivity of the ZnO film enhanced with the Sn dopant. From the temperature dependence of conductivity measurements, the activation energy of ZnO film increased with Sn incorporation.     

Electrochemical properties of Ti-Ni-Sn materials predicted by <Superscript>119</Superscript>Sn Mössbauer spectroscopy

The electrochemical activity of TiNiSn, TiNi ₂Sn and Ti ₆Sn ₅ compounds considered as negative electrode materials for Li-ion batteries has been predicted from the isomer shift- Hume-Rothery electronic density correlation diagram. The ternary compounds were obtained from solid-state reactions and Ti ₆Sn ₅ by ball milling. The ¹¹⁹Sn Mössbauer parameters were experimentally determined and used to evaluate the Hume-Rothery electronic density [e _av]. The values of [e _av] are in the region of Li-rich Li-Sn alloys for Ti ₆Sn ₅ and outside this region for the ternary compounds, suggesting that the former compound is electrochemically active but not the two latter ones. Electrochemical tests were performed for these different materials confirming this prediction. The close values of [e _av] for Ti ₆Sn ₅ and Li-rich Li-Sn alloys indicate that the observed good capacity retention could be related to small changes in the global structures during cycling.     

不同衬底上Pb(Zr0.52Ti0.48)O3择优取向铁电薄膜的制备和研究

通过MOD法在Si(100)和Pt(111)/Ti/SiO₂/Si基片上制备出LaNiO₃ ( LNO)薄膜.再通过修 正的Sol-gel法，在Pt(111)/Ti/SiO₂/Si,LNO/Si(100)和LNO/Pt/Ti/SiO_{2< /sub>/Si三种衬底上 制备出具有择优取向的Pb(Zr0.52Ti0.48)O3铁电薄膜. 经XRD分析表明，L NO薄膜具有(100)择优取向的类钙钛矿结构；PZT薄膜均具有钙钛矿结构，且在Pt(111)/Ti/S iO2/Si衬底上的薄膜以(110)择优取向，在LNO/Pt/Ti/SiO2/Si和LN O/Si(100)衬底上的 薄膜以(100)择优取向.经场发射SEM分析和介电、铁电性能测试表明，在LNO/Si和LNO/Pt/Ti /SiO2/Si衬底上的PZT薄膜的平均粒径、介电常数以及剩余极化强度均比以Pt/T i/SiO2/Si为衬底的薄膜大. 关键词： 3}薄膜')" href="#">LaNiO₃薄膜 PZT铁电薄膜 择优取向 剩余极化强度     

直流磁控溅射沉积含He钛膜的研究

研究了用He/Ar混合溅射气体的直流磁控溅射制备钛膜中，He的掺入现象.分析结果表明，大量的He原子（He/Ti原子比高达56%）被均匀地引入到Ti膜中，其He含量可由混合溅射气体的He分量精确控制.通过调节溅射参数，可实现样品中He的低损伤引入.研究还发现，溅射沉积的含氦Ti膜具有较高的He成泡剂量和高的固He能力，这可能是溅射沉积形成了纳米晶Ti膜所致.纳米晶Ti膜较粗晶材料具有很高浓度的He捕陷中心，使He泡密度增大而泡尺寸减小.随He引入量的增加，Ti膜的晶粒尺寸减小，He引起的晶体点阵参数和X射线衍射峰宽度增大，晶体的无序程度增加.Helium trapping in the Ti films deposited by DC magnetron sputtering with a He/Ar mixture was studied. He atoms with a surprisingly high concentration (He/Ti atomic ratio is as high as 56%)incorporate evenly in deposited film. The trapped amount of He can be controlled by the helium partial amount. The introduction of the helium with no extra damage(or very low damage) can be realized by choosing suitable deposition conditions. It was also found that because of the formation of nanophase Ti film a relative high He flux for bubble formation is needed and the amount of the retain He in sputtering Ti films is much higher than that in the coarse grain Ti films. The nanophase Ti film can accommodate larger concentration of trapped sites to He, which results in a high density and small size of the He bubbles. With the increasing He irradiation flux, the grain size of Ti film decreases and the lattice spacing and width of the X ray diffraction peak increase due to the He introduction, and the film tends to amorphous phase.     

PIIID复合强化处理轴承钢表面TiN膜层的XPS表征

用等离子体浸没离子注入与沉积(PIIID)复合强化新技术在AISI52100轴承钢基体表面成功合成了硬而耐磨的氮化钛薄膜。膜层表面的化学组成和相结构分别用X射线衍射(XRD)和X射线光电子能谱(XPS)表征;膜层表面的原子力显微镜(AFM)形貌显示出TiN膜结晶完整,结构致密均匀。XRD测试结果表明,TiN在(200)晶面衍射峰最强,具有择优取向。Ti(2p)的XPS谱峰泰勒拟合分析揭示出,Ti(2p_1/2)峰和Ti_2p3/2峰均有双峰出现,表明氮化物中的Ti至少存在不同的化学状态;N(1s)的XPS谱峰在396.51, 397.22和399.01 eV附近出现了三个分峰,分别对应于TiNO_y,TiN和N—N键中的氮原子。结合O(1s)的XPS结果,证实膜层中除生成有稳定的TiN相外,还有少量钛的氧化物和未参与反应的单质氮。整个膜层是由TiN,TiO₂,Ti—O—N化合物和少量单质氮组成的复合体系。     

Co,Sn共掺ZnO薄膜结构与光致发光的研究

采用溶胶-凝胶旋涂法在玻璃衬底上制备了Co,Sn掺杂ZnO系列薄膜.通过金相显微镜和X射线衍射(XRD)研究了Co与Sn掺杂对薄膜的表面形貌和微结构的影响.XRD结果表明,所有ZnO薄膜样品都存在(002)择优取向,特别Sn单掺ZnO薄膜的c轴择优取向最为显著,而且晶粒尺寸最大.XPS测试表明样品中Co和Sn的价态分别为2+和4+,证实Co²⁺,Sn⁴⁺进入了ZnO的晶格.室温光致发光谱(PL)显示在所有的样品中都有较强的蓝光双峰发射和较弱的绿光发 关键词： ZnO薄膜 溶胶-凝胶 掺杂 光致发光     

Specific character of the 119Sn thin films growth on amorphous Si by the CBPLD method

The research of the ¹¹⁹Sn thin films growth on amorphous Si that is important for the multilayer periodical spin-tunnel nanostructures creation have been investigated in this paper. The ¹¹⁹Sn mono-isotopic thin films on the silicon substrates (100) had been received by crossed-beam pulsed laser deposition method (CBPLD). Similarly the [Fe/Si/Sn/Si] multilayer periodical structures have been deposited. The received samples were investigated by atomic-force microscopy, electronic microscopy and X-ray reflectometry methods. It has been established that at ¹¹⁹Sn film thickness up to 3 nm it is possible to received atomic-smooth surfaces with 0.5 nm roughness.