玻璃衬底上中温制备多晶硅薄膜的量子态现象

用PECVD法直接沉积的非晶硅(a-Si:H)薄膜用传统炉在中温退火,然后用拉曼光谱、XRD和SEM分析,发现晶粒大小随退火温度和退火时间呈现量子态现象.分析发现在传统炉中850℃下退火三个小时晶粒大小出现极大值,平均晶粒尺寸为30nm左右.     

基于直流磁控溅射室温制备ZnO薄膜研究

采用直流磁控溅射法在P型<100>晶向单晶硅衬底上室温制备ZnO薄膜,对室温制备的ZnO薄膜分别在500℃、600℃、700℃进行高温退火,通过采用X射线衍射(XRD)、拉曼光谱和场发射扫描电子显微镜(SEM)、HP4145B型半导体参数测试仪分析不同退火温度对室温生长ZnO薄膜微结构、表面形貌和,Ⅰ-Ⅴ特性影响.实验结果表明,室温生长的ZnO薄膜为非晶态,随退火温度增加,ZnO薄膜出现(002)、(100)、(101)晶面衍射峰且逐渐增强,晶粒大小相对增加,在700℃退火后,呈高度c轴择优取向,晶粒间界明显,拉曼光谱E2模增强.     

PbTiO3-CoFe2O4复合薄膜的溶液法制备及其微观结构研究

以乙二醇甲醚为溶剂,采用溶液法成功制备了致密的、铁电相和铁磁相共存的0-3型磁电复合薄膜.采用X射线衍射(XRD)、原子力显微镜(AFM)、X射线能潜分析(EDAX)、压电响应力显微镜(PFM)分析了退火时间对两相结构、晶粒大小、薄膜形貌、电畴及磁畴的影响.结果表明,退火20 min 对于 PbTiO3相晶粒的生长已经足够,随着退火时间的延长,CoFe2O4相的品粒逐渐长大,薄膜的均方根粗糙度有所提高;同时因为磁件相品粒的长大复合薄膜电畴的取向发生了极大地变化.复合薄膜中同时存在的电畴和磁畴证明了其同时具有的铁电性和磁性.     

常规退火与光退火固相晶化的对比

为研究传统炉子退火与光退火固相晶化的不同特点,用石英玻璃作衬底,在室温、350℃和450℃下用PECVD法直接沉积非晶硅(a-Si:H)薄膜,把沉积的样品分别在850℃下用传统炉子退火3h、用光快速热处理(RTP)5min,然后用Raman、XRD和SEM分析对比,发现传统炉子退火后的晶粒分布不均匀,光退火后的晶粒分布均匀.XRD分析发现两种方法晶粒尺寸均为30nm左右.     

用快速光热退火制备多晶硅薄膜的研究

用等离子体增强型化学气相沉积先得到非晶硅(a-Si:H)薄膜,再用卤钨灯照射的方法对其进行快速光热退火(RPTA),得到了多晶硅薄膜.然后,进行XRD衍射谱、暗电导率和拉曼光谱等的测量.结果发现,a-Si:H薄膜在RPTA退火中,退火温度在750℃以上,晶化时间需要2min,退火温度在650℃以下,晶化时间则需要2.5h;晶化后,晶粒的优先取向是(111)晶向;退火温度850℃时,得到的晶粒最大,暗电导率也最大;退火温度越高,晶化程度越好;退火时间越长,晶粒尺寸越大;光子激励在RPTA退火中起着重要作用.     

退火对电子辐照氮化镓光电性能的影响

本文对10 MeV电子辐照的GaN进行了不同温度的热退火处理.用光致发光谱和霍尔测量了样品的光电性能随退火温度的变化.实验结果表明:黄光带强度、电子浓度和电子迁移率随退火温度呈非线性变化.在200～600℃退火范围内,黄光带、电子浓度和电子迁移率的变化是由于辐照Ga空位与O施主杂质的结合和断裂引起的.800℃退火后黄光带、电子浓度和电子迁移率的变化与电子辐照引入的N空位有关.     

碲锌镉单晶体的正电子寿命研究

用正电子湮没技术(PAT)研究了原料富Cd改进布里奇曼法生长的碲锌镉单晶样品退火前后的缺陷.刚生长的样品缺陷寿命值较高,其内部存在的点缺陷主要是占优势的Cd空位,用富Cd同成份源Cd1-xZnxTe气氛对样品在不同温度下等时退火后,发现样品的正电子寿命参数对退火温度表现出很强的依赖关系,通过对样品退火过程中空位的迁移、聚集及消失情况分析,得出较适宜的退火温度约为700℃.     

脉冲退火法制备多晶硅薄膜的研究

用射频等离子体化学气相沉积(RF-PECVD)法在普通玻璃衬底上低温制备了μc-Si:H薄膜.采用快速光热退火炉(RTP),分别用低温(＜650℃)和中温(＜750℃)脉冲法(PRTP)对薄膜进行了退火处理.用拉曼光谱和扫描电子显微镜(SEM)研究了不同条件下退火薄膜散射谱的特征和表面形貌.结果显示,脉冲退火法晶化的薄膜,晶化率达到了53;,部分颗粒团簇的尺寸已达到200nm左右.用声子限域理论和表面尺寸效应对薄膜频谱的"红移"和"蓝移"现象进行了分析.     

多晶硅薄膜结晶团晶化机理的研究

本文用PECVD法在石英玻璃上沉积非晶硅薄膜,然后用快速光退火和传统电阻炉退火方法晶化生长多晶硅薄膜,用拉曼光谱仪、XRD和场发射扫描电镜观察分析薄膜,发现在制备的多晶硅薄膜表面存在结晶团现象,并对这一现象的晶化机理进行了分析.     

纳米Al粉体性能及热稳定性研究

本文采用等离子体电弧法制备了纳米Al粉末,用XRD、TEM、TG、DTA、热处理等测试技术研究了纳米Al粉末的组成结构、晶粒大小、晶粒形貌和热稳定性情况.结果表明,该粉体平均粒径是39nm,晶粒形貌为球状,热稳定性好.     

Synthesis,Characterization, Crystal Structure,and Thermal Analysis of 4-[(3-acetylphenyl)amino]-2-methylidene-4-oxobutanoic Acid

4-[(3-Acetylphenyl)amino]-2-methylidene-4-oxobutanoic acid (1) is synthesized by a ring opening reaction of itaconic anhydride with 3-aminoacetophenone and characterized by FT-IR, ¹H NMR, UV-Vis, TGA, DTA, and single crystal X-ray diffraction. The crystal of 1 belongs to triclinic unit cell in the P-1 space group with the unit cell dimensions a = 4.9485(3), b = 5.3614(6), c = 22.457(2) Å, α = 88.295(8), β = 89.379(7), γ = 84.495(7), and Z = 2 The crystal structure is solved by direct methods using single-crystal X-ray diffraction data collected at room temperature and refined by full-matrix least-squares procedures to a final R-value of 0.0467 for 1623 observed reflections. Intermolecular N&;sbnd;H?…O and O&;sbnd;H?…O hydrogen bonds links the molecules into chains along [010] direction. In addition the thermal stability of the 1 is determined by using DTA, TGA analysis, and wavelength absorption at λ_max = 297 nm is determined by UV-Vis spectrophotometer.     

纤蛇纹石的水热生长机制研究

以氧化镁和二氧化硅为原料,采用水热法在不同反应时间下合成了一系列纤蛇纹石纳米管.利用X-射线衍射(XRD)、红外光谱(IR)、扫描电镜(SEM)、高分辨透射电镜(TEM)等手段研究了纤蛇纹石晶体生长和晶体结构随反应时间的变化过程.X-射线衍射和红外光谱分析表明:随着反应时间的增加所得到的纤蛇纹石样品结晶逐渐完善、卷曲程度逐渐增大;电镜分析表明:获得的纳米管的外径和内径分别为15～40 nm和6～9 nm,长度为50～300 nm,出现了双层管式结构.根据实验结果,结合负离子多面体配位生长理论对纤蛇纹石的生长机理研究表明,纤蛇纹石是由片状逐渐卷曲成管状的.     

Self‐template hydrothermal synthesis ZnS microspheres

Zinc sulfide (ZnS) microspheres were synthesized by a self‐template hydrothermal route using thiourea as sulphur source. The formation of these hollow spheres was mainly attributed to the oriented aggregation of ZnS nanocystals around the gas‐liquid interface between gas (H₂S, NH₃, or CO₂) and water followed by an Ostwald ripening process. The gas bubbles of H₂S, NH₃, or CO₂ produced during the reaction might play a soft‐template to form ZnS hollow microspheres. The products were characterized by X‐ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), electron diffraction (ED), and photoluminescence (PL). The crystal structure of prepared ZnS microspheres is hexagonal phase polycrystalline. The average microspheres diameter is 1.5 ‐ 6 µm. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and characterization of a micro scale zinc oxide–PVA composite by ultrasound irradiation and the effect of composite on the crystal growth of zinc oxide

Micro scale zinc oxide-polyvinyl alcohol (ZnO–PVA) composite has been synthesized by ultrasound irradiation. The properties of the as-prepared ZnO–PVA composite material are characterized by X-ray diffraction (XRD), thermo gravimetric analysis (TGA), transmission electron microscopy (TEM), and diffuse reflection spectroscopy (DRS). A band gap of 3.25 eV is estimated from DRS measurements. The controlled crystal growth of zinc oxide has been studied by using the as-prepared micro scale ZnO–PVA composite as seeds for the crystal growth of ZnO.     

溶剂热法合成纳米结构四氧化三铁空心微球磁性研究

通过溶剂热反应合成了Fe3O4空心微球.采用X射线衍射仪(XRD)、透射电子显微镜(TEM)和扫描电子显微镜(SEM)对样品的结构和形貌进行了表征.结果表明,所制备的单分散Fe3O4空心微球为立方多晶结构,其直径约400 nm,是由约40 nm纳米颗粒组装而成.用振动样品磁强计(VSM)测量了Fe3O4空心微球的室温和变温磁性.室温磁滞回线表明不同反应时间所得产物均表现为良好的亚铁磁性,其饱和磁化强度Ms随反应时间的增加先升后降.由反应时间为12 h所得的Fe3O4空心微球在1000 Oe下的M-T曲线测得其居里温度为778 K,并测得其在外磁场H=5000 Oe场冷却至液氮温度再升至不同温度(100 K,200 K,300 K)时的磁滞回线,发现不同温度时测得的Fe3O4空心微球磁滞回线都是左右对称的,没有明显的交换偏置效应,且随测量温度增加,其饱和磁化强度Ms和矫顽力Hc均降低.     

Crystal and molecular structure of nitrato-1,4,10-trioxa-7,13-diazacyclopentadecanecopper(II) nitrate,C10H22N2O3·Cu(NO3)2

The copper(II) dinitrate complex of the title heteromacrocycle has been investigated by X-ray diffraction. The structure was solved by direct methods and refined by a full-matrix least-squares, givingR=0.0318 with 1778 unique reflections. The Cu(II) cation is coordinated inside the N(7), N(13)-folded macrocycle. The coordination sphere of Cu(II) is a distorted square pyramid with N(7), O(10), N(13) of the macrocycle and O(1a) of the nitrate anion atoms occupying the corners of the base of the pyramid and the O(1) macrocycle atom in the apical position. The other nitrate group was found in a remote position with respect to the Cu(II) cation.     

以2-甲基-丙烯酸,4-(吡啶-4-偶氮)-苯酯为配体的四个配位化合物的合成、晶体结构和紫外吸收

4个单核配位化合物,[Zn(Maape)2(H2O)2(NO3)2] (1, 单核), [Cu(Maape)2(H2O)2(NO3)2] (2, 单核), [Zn(Maape)2Cl2] (3, 单核), [Zn(Maape)(H2O)4SO4] (4, 单核),都是用过渡金属盐和配体2-甲基-丙烯酸,4-(吡啶-4-偶氮)-苯酯合成的.四个化合物由单晶X-射线衍射和结构分析表明都是单核化合物.另外,还通过红外和元素分析对其进行表征.配位化合物的结构不仅受配位金属离子的影响还受不同配位阴离子的影响.化合物1和2的结构都是由一个金属离子中心、2个配位硝酸根离子和2个配体分子组成的单核配合物.化合物3的单核结构中包含一个Zn(II)、2个氯离子和2个配体分子.而化合物4的不对称单元[Zn(Maape)(H2O)4SO4]中Zn(II)中心位于二重对称轴上.在本文中,配体和4个化合物都在323 nm处有最高紫外吸收峰.     

The role of the main silica precursor and the additive in the preparation of low-density xerogels

The incorporation of an additive during sol-gel synthesis reduces shinkage during ambient drying. The following additives have been studied: 3-(2-aminoethylamino)propyltrimethoxysilane (EDAS), 3-aminopropyltriethoxysilane (AES) and 3-(2-aminoethylamino)propyltriethoxysilane (EDAES) and the main silica precursors were tetraethylorthosilicate (TEOS) and tetrapropylorthosilicate (TPOS). When the additive contains methoxy groups (EDAS), it acts as a nucleation agent of the silica particles and exactly the same properties (pore volume, specific surface area, particle and aggregate size) are obtained whether the main reagent is TEOS or TPOS. The nucleation mechanism is based on the difference in reactivity between additive and main reagent. In case of nucleation by the additive, the nucleation agent fixes the properties whatever the main silica precursor is. When both the additive and the main reagent contain ethoxy groups (series AES-TEOS and EDAES-TEOS), there is no nucleation mechanism by the additive, and the silica particle size remains nearly constant. With less reactive main reagent (series AES-TPOS and EDAES-TPOS), pore volumes up to 17 cm³/g have been obtained with pore sizes up to nearly 10 μm and very big particles (∼100 nm). The absence of nucleation by the additive for the couples AES-TPOS and EDAES-TPOS could be due to the fact that the difference in reactivity between ethoxy groups and propoxy groups is not sufficient to initiate the nucleation mechanism by the additive. In the absence of nucleation by the additive, the main reagent plays a role: highly porous materials with very large pores are prepared with TPOS.     

铒掺杂g-C3N4催化剂的合成及其红光催化降解活性的研究

石墨相氮化碳(g-C₃N₄)的研究已成为光催化领域热点。本文以三聚氰氨为前驱体,采用甲醇回流法制备Er掺杂的g-C₃N₄催化剂。利用扫描电镜(SEM)、X射线光电子能谱(XPS)、X射线衍射仪(XRD)、紫外-可见-近红外分光光度计(UV-Vis-NIR DRS)、傅里叶红外光谱仪(IR)、荧光光谱(PL)、物理吸附(N₂-physisorption)及共聚焦显微镜(CLSM)等手段对Er/g-C₃N₄催化剂进行系统表征。结果表明,稀土金属Er高分散于g-C₃N₄上,促使氮化碳表面氮空穴的产生。Er掺杂优化了氮化碳的能带结构,增强了其对可见光的吸收,提升电子-空穴对的分离效率,此外还发现Er/g-C₃N₄具有较强的上转换能力。在660 nm红光LED照射下,对罗丹明B的水溶液进行光催化降解,发现Er/g-C₃N₄的降解速率是g-C₃N₄的2.0倍,且发现超氧自由基为该体系中的主要活性物种。     

溶剂热法制备双螺旋ZnS纳米结构研究

采用溶剂热法以醋酸锌和硫化钠反应成功制备了具有双螺旋结构的一维ZnS纳米棒,利用X射线衍射(XRD)、高分辨透射电子显微镜(HRTEM)、选区电子衍射(SAED)、X射线能量色散分析谱仪(XEDS)、紫外吸收光谱(UV-vis)和光致发光谱(PL)等测试手段对样品的化学成分、形貌、晶体结构和光学性质等进行了表征分析.实验结果表明样品为一维六方纳米晶结构,沿着[001]方向生长,并具有双螺旋结构,长度分布在100～200 nm范围,直径约为5 ～15 nm,螺距约为20 nm.双螺旋ZnS纳米结构的吸收峰与块体材料相比发生了蓝移.