脉冲激光沉积制备的HT-LiCoO2薄膜中Li离子表观扩散的研究

采用脉冲激光沉积(PLD)方法在镀Pt的Si衬底上制备了LiCoO2薄膜,运用XRD、Raman光谱、SEM和循环伏安等方法对其结构与电化学性能进行表征,在此基础上着重采用电位间歇滴定技术(PITT)对其Li离子表观扩散进行了分析.结果表明,600 ℃制备的LiCoO2薄膜为HT-LiCoO2相,呈柱状晶结构,平均晶粒尺寸在100 nm以下,结晶度高,并且具有明显的[001]择优取向,但少量缺Li.伏安循环曲线表明,该LiCoO2薄膜具有良好的电化学可逆性,但只在3.9 V(vs Li/Li )附近出现一对氧化还原峰.PITT测试表明,PLD方法制备的HT-LiCoO2薄膜的Li离子扩散系数在10-8-10-9cm2/s,与其它方法(如射频磁控溅射)制备的HT-LiCoO2薄膜相比,扩散系数高1-2个数量级;并且PLD方法制备的HT-LiCoO2薄膜中Li离子扩散系数与相变有关,在两相共存区,由于相界钉扎的作用,Li离子扩散系数比其它区域小1-2个数量级.     

电场辅助化学溶液工艺技术制备硅酸锂(Li2SiO3)陶瓷薄膜

采用了一种新的电场辅助化学溶液工艺技术制备了硅酸锂(Li2SiO3)陶瓷薄膜.结果表明,这种方法可在较低的温度下获得成分单一的硅酸锂(Li2SiO3)陶瓷薄膜.利用X射线衍射技术(XRD)对薄膜的晶体结构进行了表征;利用扫描电子显微技术(SEM)观察了薄膜的表面形貌;并对硅酸锂(Li2SiO3)陶瓷薄膜的制备过程进行了详细的分析和讨论.     

掺F锂离子电池正极材料Li1.03Co0.10Mn1.90FzO4-z的制备及电化学性能

以Li2CO3、Mn2O3、Co2O3及LiF为原料,采用高温固相法合成了掺F的Li1.03Co0.10Mn1.90FzO4?z锂电池正极材料。通过离子发射光谱(ICP)和电位分析法确定了材料的化学组成,用X-射线衍射(XRD)、扫描电子显微镜(SEM)和电化学测试仪分析了 F 掺杂量对材料结构、形貌和电池性能的影响。结果表明,掺 F 的Li1.03Co0.10Mn1.90FzO4?z正极材料为尖晶石结构,在F掺入量z≤0.10时,随着掺杂量的增加晶胞参数逐渐增加,当F掺杂量继续增加时,晶胞参数的增幅有所减小。适量的F?与金属离子Li+、Co+的复合掺杂提高了材料的放电比容量,同时增强了材料结构的稳定性。电化学性能测试表明,Li1.03Co0.10Mn1.90F0.15O3.85的首次放电比容量达到111.0 mA·h/g,0.2C倍率下30次循环后容量保持率为97.0%。     

微波法一步合成锂离子电池正极材料Li_3V_2(PO_4)_3的研究(英文)

以NH4H2PO4、Li2CO3和V2O5为原料,采用微波法快速合成了锂离子电池正极材料Li3V2(PO4)3。考察了微波功率、加热时间及产品中的理论碳含量对材料物理及电化学性能的影响。添加的乙炔黑具有还原剂、微波吸收体及导电剂的多重作用。XRD测试表明采用该法可以获得单相的Li3V2(PO4)3。电化学测试表明含2%C的Li3V2(PO4)3具有较好的充放电性能,充放电电流密度为7mA·g-1时,首次放电比容量为115.7mAh·g-1,20次循环后容量保持率为87.5%。与传统方法相比,微波法具有工艺简单,效率高,经济性好的优点。     

磁控溅射Al-Mg-B薄膜成分优化

采用多靶磁控共溅射技术,利用高纯度Al,Mg和B单质靶材为溅射源,室温下在单晶Si(100)表面上成功制备了低摩擦系数的非晶态Al-Mg-B硬质薄膜.通过改变Al/Mg混合靶体积配比及靶材溅射功率来调控薄膜成分,最终制备的Al-Mg-B薄膜成分接近AlMgB_(14)相的元素成分比,其Vickers硬度约为32 GPa.XRD及HR-TEM分析表明.制备的薄膜均为非晶态XPS测试表明薄膜内部存在B-B及Al-B单键;FTIR进一步测试表明,在波数1100 cm~(-1)处出现较为明显的振动吸收峰,证明制备的薄膜中含有B_(12)二十面体结构,这也是薄膜具有超硬性的主要原因.薄膜摩擦磨损测试表明薄膜摩擦系数在0.07左右.     

脉冲激光沉积技术制备Li2O-V2O5-SiO2薄膜

采用355nm脉冲激光沉积(PLD)技术,以Li6.16V0.61Si0.39O5.36为靶材制备Li2O-V2O5-SiO2薄膜,考察了反应气氛压强、激光能量密度、基片温度等对薄膜结构和性质的影响.结果表明,随着基片温度升高及激光能量密度增大Li2O-V2O5-SiO2薄膜更致密,且室温离子电导率随之增大.在O2压强6.7Pa、激光能量密度12J/cm2和基片温度300℃条件下制备了室温离子电导率为4×10-7S/cm、离子迁移数接近1.O(tion＞99.99%)、厚度均匀、无针孔和裂缝的非晶态Li2O-V2O5-SiO3薄膜.     

纯相磷酸铁锂PLD靶材合成和表征

本研究着眼于确定制备纯相Li Fe PO4脉冲激光沉积靶材的合成条件。通过TG-DTA实验分析合成过程,XRD检测确定晶相,SEM观察表面形貌。结果表明,采用液相法在800℃、通有氩气(93%)和氢气(7%)的混合气体中焙烧制得纯相的Li Fe PO4粉末,经压合焙烧获得了纯相、高结晶度、大晶粒的Li Fe PO4靶材。利用脉冲激光技术沉积Li Fe PO4薄膜,薄膜结构致密,晶粒粒径达纳米级别。     

Zr对Li1.3 Ti1.7Al0.3(PO4)3传导材料中Na/Li离子交换反应的影响

Li13Ti17Al0.3(PO4)3是具有Nasicon骨架的锂离子传导材料,其中的Li 很容易被溶液中的Na 置换.研究了在Li1.3Ti1.7Al0.3(PO4)3结构中掺入Zr来替代Ti,以提高Na/Li离子交换速度.结果表明:增加Zr元素比例可显著提高Li1.3Ti1.7-xZrxAl0.3(PO4)3材料中Na/Li离子交换反应速度.Li1.3Ti1.7-xZrxAl0.3(PO4)3材料中的Na/Li离子交换反应动力学过程可近似由JMAK方程描述.     

Gd掺杂PZT铁电薄膜的微观结构和铁电性研究

采用溶胶-凝胶技术制备稀土Gd掺杂的PZT(PGZT)前驱体溶胶.以(111)Pt/Ti/SiO2/Si(100)为衬底,采用旋涂法和快速热处理技术制备PGZT薄膜.X射线衍射(XRD)分析结果表明,450℃预烧,650℃快速热处理得到(100)择优取向的薄膜.用扫描电镜(SEM)对稀土Gd不同掺入量薄膜的表面形貌进行分析,薄膜的表面平整,无裂纹;用原子力显微镜(AFM)对薄膜表面的粗糙度进行分析.PGZT薄膜铁电性能测试结果表明,1%(摩尔分数,下同)Gd-PZT薄膜的剩余极化强度(2Pr)为46.373μC/cm2,经1010次极化循环后,剩余极化值减小45%;当Gd掺入量大于1%时,薄膜的剩余极化强度减小.对稀土Gd3+掺杂改性机理进行初步分析,可能是由于稀土掺入量小于1%时,稀土起施主掺杂剂作用,而施主掺杂可以明显改善PZT的疲劳特性;当稀土掺入量大于1%时,稀土起受主掺杂剂作用.     

CSTR系统制备高性能Ni0.6Co0.2Mn0.2(OH)2及电化学性能研究

采用共沉淀法在CSTR(连续搅拌反应器系统)工艺体系中批量合成出镍钴锰三元氢氧化物前驱体Ni0.6Co0.2Mn0.2(OH)2 (622),掺入适量的Li2CO3高温焙烧后得到锂离子二次电池正极材料Li[Ni0.6Co0.2Mn0.2]O2。使用扫描电子显微镜(SEM)观察样品形貌,X射线衍射仪(XRD)及透射电子显微镜(TEM)分析合成样品的具体结构,充放电循环测试系统测试其电化学性能。SEM测试表明产物为二次粒子团聚而成类球形颗粒;XRD及TEM结果表明合成的样品具有典型的层状α-NaFeO2结构。在电压范围为2.8 V-4.3 V,0.2 C倍率条件下,首次充放电容量分别为206 mAh g-1 和176 mAh g-1,100次循环后容量保持率达到85%。     

Realization of stable p-type ZnO thin films using Li-N dual acceptors

Lithium and nitrogen dual acceptors-doped p-type ZnO thin films have been prepared using spray pyrolysis technique. The influence of dual acceptor (Li, N) doping on the structural, electrical, and optical properties of (Li, N):ZnO films are investigated in detail. The (Li, N):ZnO films exhibit good crystallinity with a preferred c-axis orientation. From AFM studies, it is found that the surface roughness of the thin films increases with the increase of doping percentage. The Hall Effect measurements showed p-type conductivity. The Hall measurements have been performed periodically up to seven months and it is observed that the films show p-type conductivity throughout the period of observation. The samples with Li:N ratio of 8:8 mol% showed the lowest resistivity of 35.78 Ω cm, while sample with Li:N ratio of 6:6 mol% showed highest carrier concentration. The PL spectra of (Li, N):ZnO films show a strong UV emission at room temperature. Furthermore, PL spectra show low intensity in deep level transition, indicating a low density of native defects. This indicates that the formation of intrinsic defects is effectively suppressed by dual acceptor (Li, N) doping in ZnO thin films. The chemical bonding states of N and Li in the films were examined by XPS analysis.     

Dy~(3+)掺杂BiFeO_3薄膜的晶格转变和磁性能研究(英文)

以硝酸铋、硝酸铁以及硝酸镝等无机硝酸盐为原料通过化学液相法在Pt(111)/Ti/SiO_2/Si上制备了Dy~(3+)掺杂的BiFeO_3薄膜,研究了Dy~(3+)掺杂量的变化对Bi_(1-x)Dy_xFeO_3薄膜的晶体结构和磁性的影响.Dy~(3+)掺杂量不高于10%的Bi_(1-x)Dy_xFeO_3薄膜可以得到与纯BiFeO_3相同的晶体结构.随着Dy3+掺杂量的进一步增大,Bi_(1-x)Dy_xFeO_3薄膜的晶体结构发生变化,晶格从菱心结构转变为单斜或四方结构.磁性测试显示:随着Dy~(3+)掺杂量的增加Bi_(1-x)Dy_xFeO_3薄膜的磁性增强,同时从无饱和磁化强度和零磁滞的S型磁化曲线的形状判断,薄膜由于铁磁反铁磁转变时两磁性相竞争表现出自旋玻璃态的特征.     

Mn掺杂对0.7BiFeO3-0.3PbTiO3薄膜铁电性能的影响

利用溶胶-凝胶法在La Ni O3/Si O2/Si衬底上制备了掺Mn量为0%、1%、5%、10%(质量分数)的0.7Bi Fe O3-0.3Pb Ti O3(BFMPT7030/x,x=0,0.01,0.05,0.1)薄膜。XRD测试表明,薄膜均完全结晶,呈现高度(100)择优取向。通过对薄膜晶体结构分析,发现BFMPT7030/0.05薄膜具有最小的晶粒尺寸(258 nm)及最小的晶胞体积(61.25×10-3 nm3)。SEM测试结果显示样品晶粒生长充分,晶粒尺寸在150~300 nm之间。铁电性能测试结果表明,当Mn含量为5%时,铁电性能较好,电滞回线形状最好,最为饱和。漏电流测试结果表明随着掺Mn量增加,BFMPT7030薄膜的漏电流随电场增大而增加的趋势减弱。     

Tb掺杂对CoNbZr纳米薄膜软磁性和微波磁性的影响

采用磁控溅射工艺制备CoNbZrTb纳米薄膜,研究了掺杂稀土元素Tb对薄膜软磁性能、微波磁导率及其频谱特性的影响.结果表明:少量Tb 掺杂(＜2%,摩尔分数)对该类薄膜的微结构和软磁性能影响较小,薄膜仍可保持非晶态结构和良好的软磁性能,但Tb掺杂可以显著增强薄膜磁谱的弛豫性,从而影响其微波磁导率和磁损耗;随Tb 掺杂量的增加,薄膜的磁各向异性场和共振频率得以有效提高;薄膜样品在2 GHz处复磁导率的虚部均大于200.掺杂少量Tb的CoNbZrTb非晶态纳米薄膜在109 Hz微波段具有较高磁损耗,有望在超薄层吸波材料中获得应用.     

Structural,Optical, and Electrical Properties of Zn-Doped CdO Thin Films Fabricated by a Simplified Spray Pyrolysis Technique

Thin films of zinc-doped cadmium oxide with different Zn-doping levels(0, 2, 4, 6, and 8 at%) were deposited on glass substrates by employing an inexpensive, simplified spray technique using perfume atomizer at relatively low substrate temperature(375 °C) compared with the conventional spray method. The effect of Zn doping on the structural,morphological, optical, and electrical properties of the films was investigated. XRD patterns revealed that all the films are polycrystalline in nature having cubic crystal structure with a preferential orientation along the(1 1 1) plane irrespective of Zn-doping level. Zn-doping level causes a slight shift in the(1 1 1) diffraction peak toward higher angle. The crystallite size of the films was found to be in the range of 28–37 nm. The band gap value increases with Zn doping and reaches a maximum of 2.65 eV for the film coated with 6 at% Zn doping and for further higher doping concentration it decreases.Electrical studies indicate that Zn doping causes a reduction in the resistivity of the films and a minimum resistivity of15.69 X cm is observed for the film coated with 6 at% Zn.     

Mn 掺杂 SiC 基稀磁半导体薄膜的结构和磁性研究

目的从原子水平探究Mn掺杂SiC薄膜的磁性起源。方法采用射频磁控溅射技术制备不同掺杂浓度的Mn掺杂SiC薄膜,并采用X射线衍射技术、X光电子能谱、同步辐射X射线近边吸收精细结构技术、物理性质测试系统对薄膜的结构、组分和磁性能进行研究。结果晶体结构和成分分析表明,1200℃退火后的薄膜形成了3C-SiC晶体结构,且随着Mn掺杂浓度的增加,3C-SiC晶体的特征峰向低角度移动。在Mn掺杂浓度(以原子数分数计)为3%,5%,7%的薄膜中,掺杂的Mn原子以Mn2+的形式存在;而在9%Mn掺杂的SiC薄膜中,则有第二相化合物Mn4Si7形成。局域结构分析表明,薄膜中均不存在Mn金属团簇和氧化物,在3%,5%和7%Mn掺杂的薄膜中,掺杂的Mn原子主要以代替C位的形式进入3C-SiC晶格中,而在9%Mn掺杂的薄膜中,掺杂的Mn原子以C替位形式和Mn4Si7共存。磁性测试表明,制备的Mn掺杂SiC薄膜具有室温铁磁性,且饱和磁化强度随着Mn掺杂浓度的提高而增加。结论薄膜的室温铁磁性是本征的,磁性来源与掺杂的Mn原子以Mn2+取代SiC晶格中C位后导致的缺陷有关,符合缺陷导致的束缚磁极子机制。     

Characteristics of atomic layer deposited transparent aluminum-doped zinc oxide thin films at low temperature

Various aluminum-doped zinc oxide(AZO) films were prepared on Si substrate by atomic layer deposition(ALD) at 100℃. The effect of the composition of AZO films on their electrical, optical characteristics,structural property and surface topography was investigated. The appearance of electrical resistivity shows their semiconducting properties. In most of the visible light band, all the AZO films present transparency of more than 80%. Al doping suppresses the AZO film crystallization.When the Al doping concentration increases up to 3.95 at%, the AZO film has some small multicrystal grains with random orientation. Al doping improves the roughness of i-ZnO film. The root mean square(RMS) roughness of samples prepared by ALD is much smaller than that prepared by radio-frequency magnetron sputtering reported.     

Effect of gallium doping on the magnetocaloric effect of LaFe11.2Co0.7Si1.1

The lattice parameter and magnetocaloric properties of three samples of LaFe11.2Co0.7Si1.1-xGax with x = 0,0.03 and 0.05 have been investigated by X-ray powder diffraction and magnetization measurements.The lattice parameter increases slightly and the Curie temperature increases somewhat with increasing gallium content.However,a small amount of Ga doping into the sample decreases the magnetic entropy change of the sample.All the samples remain in the first-order magnetic phase transition.The most striking effect of the Ga doping is that the cooling capacity in the samples increases significantly.The maximum magnetic entropy change,-△SM,max,and the cooling capacity of the sample LaFe11.2Co0.7Si1.07Ga0.03 are 11.9 J·kg-1.K-1 and 254.8 J.kg-1,respectively.     

磁场约束下碳钢表面Ni-W合金电镀层的制备与性能

研究了施加稳恒磁场(0～1 T)对碳钢表面电镀Ni-W合金的影响。测定了不同方向、不同强度稳恒磁场下的电流效率、合金组成及镀层硬度,并用X射线衍射对镀层的微观结构进行了分析。对实验结果进行了分析讨论,找出了稳恒磁场对上述性能的影响规律。结果表明:与不施加磁场相比,施加磁场后镀层的含钨量上升:当磁场方向垂直于电场方向(B⊥J),B=1.0 T时,含钨量上升了约11%;当磁场方向平行于电场方向(B∥J),B=1.0 T时,含钨量上升了约13%;镀层的非晶化程度增强;镀层的硬度提高、孔隙率下降;但Ni-W合金电沉积的电流效率降低。     

Effect of annealing atmosphere on magnetic properties of pure ZnO and Na: ZnO films

Pure ZnO and Zn0.96Na0.04O films were grown on quartz substrates by sol-gel technology.The XRD analysis revealed that all thin films had hexagonal wurtzite structure and obvious c-axis preferred orientation.Ferromagnetism was precisely measured by an alternating gradient magnetometer (AGM).To explore the nature original ferromagnetism,the effect of annealing atmosphere on magnetic properties of the films was studied.Compared with pure ZnO,magnetic hysteresis loops showed that doping Na atoms enhanced saturation magnetism.The magnetism of the films annealed in the air atmosphere was significantly better than that in the O2 atmosphere.The photoluminescence (PL) spectrum analysis suggested that the ferromagnetism was due to the defects in the films.