溶胶-凝胶法制备ZnO薄膜及其微结构特性研究

采用溶胶-凝胶法(Sol-Gel)制备氧化锌(ZnO)薄膜,研究镀膜层数和退火温度对ZnO薄膜晶体结构、光谱性质及表面形貌的影响.X射线衍射谱测试表明,退火温度为600℃、镀膜层数为10层时制备样品的晶粒尺寸最大,结晶度最好.紫外-可见透过谱发现,样品退火后其透过率曲线变得陡直,光学带隙随退火温度升高而逐渐减小.光致发光谱测试显示,ZnO薄膜的发光谱包含388 nm和394 nm附近的两个主要发光峰,分别对应于本征发射和缺陷发射,其强度随退火温度升高呈现相反的变化.原子力显微照片则显示了随退火温度的升高制备样品表面晶粒的分布趋于均匀而致密.     

钨酸铅纳米晶的制备及其发光性能研究

用沉淀法制备了钨酸铅纳米晶.对制备的钨酸铅纳米晶做了X射线和透射电镜分析,结果显示在100℃烘干后,样品已经结晶良好,晶粒度在10～20nm之间.将其在不同温度下退火后,用荧光谱仪测量了其发光光谱,结果显示其有蓝色、绿色和红色三组主要的发光峰.     

退火对电弧离子镀制备的ZnO薄膜的影响

采用阴极电弧离子镀在Si、Al2O3以及玻璃衬底上制备出具有择优取向的ZnO薄膜,并对其进行退火处理.利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、光致发光光谱(PL)、紫外-可见光光谱仪对ZnO薄膜的结构、表面形貌和光学性能进行分析.XRD结果表明,所制备的ZnO薄膜具有很好的ZnO(002)择优取向,退火使ZnO(002)衍射峰向高角度方向偏移.SEM结果表明,随着退火温度升高,表面晶粒由隆起的山脉或塔状变为平面状,晶粒002面呈六边状.PL谱结果表明,随着退火温度的升高,紫外发光峰强度逐渐增强,可见光发光峰强度逐渐相对减弱.紫外可见光透过谱结果表明,退火使可见光透过率增高,光学带隙发生红移.     

退火对Si(111)衬底上ZnO薄膜的结构和发光特性的影响

采用磁控溅射法在硅(111)衬底上制备了C轴高度取向的ZnO薄膜,并研究了退火温度和氧气气氛对ZnO薄膜晶体质量、晶粒度大小和光致发光谱的影响.X射线衍射表明,所有薄膜均为高度C轴择优取向,当退火温度低于900℃时,随着退火温度的升高,薄膜的取向性和结晶度都明显提高.室温下对ZnO薄膜进行了光谱分析,退火后的样品均可观测到明显的紫光发射.在一定的退火温度范围内,还可以观测到明显的紫外双峰.空气中退火的样品,当退火温度达到或高于600℃还可观测到绿光发射.实验结果表明,发光峰强度随退火温度和氧气气氛不同而不同,通过改变退火时的温度和氧气气氛可以改变ZnO薄膜的微结构和发光性质.     

基于PECVD制备多晶硅薄膜研究

基于PECVD以高纯SiH4为气源研究制备多晶硅薄膜,在衬底温度550℃、射频(13.56MHz)电源功率为20W直接沉积获得多晶硅薄膜.采用X射线衍射仪(XRD) 和场发射扫描电子显微镜(SEM) 对多个样品薄膜的结晶情况及形貌进行分析,薄膜结晶粒取向均为<111>、<220>、<311>晶向.对550℃沉积态薄膜在900℃、1100℃时进行高温退火处理,硅衍射峰明显加强.结果表明,退火温度越高,退火时间越长,得到多晶硅薄膜表面晶粒趋于平坦,择优取向为<111>晶向,晶粒也相对增大.     

共沉淀法制备BiFeO_3粉体

以Bi(NO_3)_3·5H_2O和Fe(NO_3)_3·9H_2O为原料,冰醋酸做溶剂,柠檬酸为络合剂,采用共沉淀法制备前驱物,对前驱物沉淀进行退火处理,制备出BiFeO_3纳米粉体.研究了煅烧温度和冰醋酸的加入量对BiFeO_3纳米粉体的晶粒尺寸及形貌的影响.采用X射线衍射仪(XRD)、场发射扫描电子显微镜(FE-SEM)对所制备的BiFeO_3纳米粉体进行表征,用EDS确定了样品的表面成分组成.结果表明:退火温度为450 ℃时出现BiFeO_3衍射峰,但存在杂相;退火温度为600 ℃时制备出了BiFeO_3纯相粉体,粉体为立方体结构.冰醋酸加入量由1 mL增大到1.8 mL时,粉体的晶粒尺寸由14.21 nm减小到11.65 nm.通过EDS能谱分析得出BiFeO_3粉体由Bi,Fe和O 三种元素组成.     

退火温度对Zn0.93Fe0.07O薄膜微结构和铁磁性能的影响

用射频磁控溅射方法在硅片上制备了Zn0.93Fe0.07O薄膜,并在空气中用不同温度进行热处理,利用X射线衍射仪和扫描电子显微镜对其微结构、表面和断面形貌进行测试.结果表明,薄膜沿c轴方向择优生长,呈六角纤锌矿结构,空气中450℃退火的样品XRD谱中出现最强的(002)衍射峰,晶粒尺寸变大,薄膜结晶和取向明显变好.用振动样品强磁计对样品铁磁特性进行测试,发现当退火温度的升高时,饱和磁化强度有所增加,并经分析认为这可能是薄膜中晶粒间的晶界缺陷引起的.     

蒸发电流对CdSe薄膜的结晶性能影响研究

采用真空热蒸发技术,选取系列蒸发电流在光学玻璃基底上制备出CdSe薄膜.利用X射线衍射仪、扫描电子显微镜和原子力显微镜对样品的结构和表面形貌进行了表征.结果显示:蒸发电流为75 A时,CdSe薄膜沿(002)方向择优生长,衍射峰较强,半峰宽较小,晶粒(约48 nm)分布较均匀,表面粗糙度低(5.58 nm),无裂纹.蒸发电流不改变薄膜的结晶取向,但电流过低时,薄膜的表面颗粒轮廓模糊且有间隙,结晶性差;电流高于75 A时,随电流升高,薄膜结晶性逐步降低,颗粒变小,半峰宽变大,部分样品表面晶粒生长不完整,表面出现裂纹.     

在钛酸锶衬底上外延生长ZnO薄膜及其性能研究

用脉冲激光淀积法(PLD)在(111)面SrTiO3衬底上外延生长ZnO单晶薄膜.样品分别在衬底温度为350℃、500℃、600℃下外延生长.X射线衍射(XRD)的结果表明,所得的ZnO单晶薄膜结晶性能好,只出现(002)和(004)两个衍射峰,(002)峰的半高宽度(FWHM)为0.23°.在荧光光谱中我们只观察到来源于带边激子跃迁的强UV发射,并且随着生长温度的升高,紫外峰的强度逐渐增强.样品的SEM图像表明所得ZnO薄膜表面平整,晶粒均匀.衬底温度为600℃时,所得到的ZnO薄膜结构完整,晶粒尺寸最大,均匀;而且紫外发射最强.     

射频磁控溅射生长ZnO薄膜及性能研究

采用射频磁控溅射技术在玻璃衬底生长ZnO及ZnO∶ Al薄膜,通过改变氩氧比、衬底温度和溅射功率获得样品.用X射线衍射仪、紫外-可见分光光度计、扫描电子显微镜进行表征.结果发现:室温下40W的溅射功率1h的溅射时间,改变氩氧比获得样品.XRD图谱中无明显衍射峰出现;紫外可见光分光光度计测试结果显示400nm波长以下,透光率在90;以上.说明薄膜生长呈无定形.衬底温度高于200℃样品,XRD有明显(002)衍射峰出现,在400～ 800 nm波长范围,透光率在88;以上,衬底温度300℃时,XRD衍射峰半高宽最小,晶粒尺寸大.TEM显示:衬底300℃晶粒尺寸最大,晶体发育好.在200℃掺铝ZnO薄膜,(002)峰不明显,有(101)峰出现.     

Epitaxial growth in the (111)Ag/Cu and (111)Au/Cu systems

The initial stages of epitaxial growth in the (111)Ag/Cu and (111)Au/Cu systems were investigated using UHV-RHEED and TEM on the same specimens. Flat, monocrystalline (111)Cu substrates, 1100 Å thick, were formed in situ in the RHEED system on (111)NaCl/mica bilayers. The latter consisted of air-cleaved mica on which 150 Å of NaCl was vacuum-evaporated to form a (111)NaCl monocrystalline film. The NaCl layer allowed easy removal in water of the subsequently deposited bilayer metal film. RHEED showed that these Cu films grew with extremely flat surfaces at 400°C and 10 Å/sec deposition rates. They were then annealed at 500°C for 15 min to reduce their dislocation content and finally used as substrates for subsequent deposition of thin Ag or Au superlayers. The average Ag and Au superlayer thicknesses were varied from fractions of an Angstrom to approximately 20 Å. It was shown that despite the elongated streaks in the RHEED patterns, film growth occurred by an island mechanism, the islands having flat top surfaces. In the initial growth processes, the islands merely thickened. After a few average monolayers were deposited, the islands began to widen, often by means of much thinner islands, finally coalescing into a continuous film. The Au overgrowths became continuous in the 6–11 Å thickness range. In the case of Ag, there still were some open areas in the overgrowth at 20 Å. In both cases the continuous regions of the Ag and Au overgrowths consisted of sharply delineated thick and thin areas that gave rise to steps on the otherwise flat surface.     

Controllable one‐step synthesis of CuO,Cu2O and Cu

In the present report, CuO, Cu₂O and Cu have been successfully synthesized through a facile, one‐step hydrothermal method at a relative low temperature by controlling only the concentration of citric acid. Compared with other synthetic methods, the present method is mild, high‐efficient and nontoxic. The crystal structure and morphology of the as prepared samples were characterized by X‐ray diffraction and scanning electron microscopy, respectively. The mechanism for the crystal phase and morphological changes with different citric acid concentrations were discussed. The possible reaction process of the synthesis was also studied on the basis of the experimental results. We hope that this facile, one‐step hydrothermal method could be used in controlling synthesis of other metals and metal oxides under appropriate experimental conditions.     

Cu替位与空位及Cu、S共掺SnO2的光磁性质研究

运用第一性原理,基于密度泛函理论,计算了Cu分别以替位和空位两种方式掺杂SnO2的电子结构和光电特性,并对两种掺杂方式做了一定的比较研究;磁性方面,主要研究了Cu、S共掺SnO2后的磁学性能.计算表明,两种方式掺杂,都使SnO2具有半金属特性,Cu原子将与周围的O原子发生强烈的交换作用,Cu原子对态密度的贡献主要在费米能级附近.相比之下,空位掺杂后的晶胞体积略大于替位掺杂后的SnO2,对光的能量损耗也比替位掺杂的低.对于Cu、S共掺的体系,计算表明:每个Cu原子的掺入将产生0.46μB的磁矩,而一个S原子将引入0.36μB的磁矩,Cu原子周围的O原子也对磁矩有一定的贡献.经过分析,发现体系的磁性来源主要是Cu-3d和S-3p,以及Cu-3 d与O-2 p间的强烈耦合作用.     

Cu:KNSBN晶体生长及其光折变效应的研究

在KNSBN晶体中掺进CuO,采用硅钼棒作加热体,以Czochralski技术生长Cu:KNSBN晶体.以二波耦合光路,测试晶体的衍射效率和记录时间,计算折射率变化值Δn.Cu:KNSBN晶体的衍射效率,记录速度和折射率变化值皆高于Fe:LiNbO3晶体.尤其记录速度比Fe:LiNbO3晶体高一个数量级以上.测试Cu:KNSBN晶体位相共轭反射率R和自泵浦位相共轭反射率RC.Cu:KNSBN晶体的自泵浦位相共轭反射率RC值达到64;,是纯KNSBN晶体的二倍.以Cu:KNSBN晶体自泵浦位相共轭镜进行消畸变实验.实验结果表明:输出光波确系输入探测光波的位相共轭光波.     

Thermodynamics of the Cu/Cu-redox equilibrium in soda-silicate and soda-lime-silicate melts

The thermodynamics of the redox equilibrium of Cu⁺/Cu²⁺ were determined by square-wave voltammetry in glass melts with the base mol% compositions x Na₂O · (100 − x) SiO₂ (x = 15, 20, 26 and 33) and (26 − x) Na₂O · x CaO · 74 SiO₂ (x = 0, 5, 10 and 15) doped with 1 mol% CuO in the temperature range from 850 to 1150 °C. All recorded voltammograms showed two maxima attributed to the reductions of Cu²⁺ to Cu⁺ and Cu⁺ to metallic copper. Both peaks are shifted to smaller potentials with decreasing temperature. With increasing melt basicity, the [Cu⁺]/[Cu²⁺]-ratio first increases, and remains constant for optical basicities >0.56. The effect of composition on the redox equilibrium is explained by the incorporation of both Cu⁺ and Cu²⁺ in octahedral coordination into the melt structure.     

Electronic properties of Cu/SiO2/Cu structures at different temperatures

In this experimental work, some electronic properties of vacuum evaporated Cu/SiO₂/Cu structures such as circuiting I_c and emission I_e currents versus the applied voltage, electron attenuation lengths in both copper and SiO₂ layers and the role of the latter layers have been investigated. Experimental results show that these devices undergo an electroforming process leading to resistivity decrease of several orders of magnitude along with a negative resistance region in their current–voltage characteristics. By decreasing the temperature, both I_c and I_e are decreased and at low temperatures the negative resistance region disappears completely. Electron attenuation lengths are measured between 6 and 14 V for copper and SiO₂ layers and their significance are discussed on the base of electron-impurity and electron-defect scatterings. The conduction mechanism is also discussed on the base of a filamentary model.     

Cu3N薄膜的制备及其霍尔效应研究

采用反应射频磁控溅射的方法在纯氮气气氛下、氮气流量为12sccm、衬底温度为100℃的条件下,在玻璃基底上成功制备了氮化铜(Cu3N)薄膜.XRD显示薄膜择优[100]晶向生长.用扫描电子显微镜(SEM)和原子力显微镜(AFM)观察了样品的表面形貌,发现样品表面平整、结构紧密.用四探针法检测了薄膜的霍尔特性,发现随温度的降低薄膜的霍尔系数、霍尔电阻率均增加.霍尔迁移率在高温范围也呈降低的趋势,但是变化的范围比较小,在低温范围又有所增加.随温度的降低薄膜的载流子浓度降低.我们还通过变温的霍尔系数估算了氮化铜薄膜的禁带宽度约为1.35eV.     

Growth and luminescence of CsBr:Cu crystals

Special features of the incorporation of a copper impurity into CsBr crystals are studied for different types of impurities (metallic copper, CuO, and CuBr₂) and crystal-growth techniques (the Bridgman method or the method of isothermal evaporation from solution). The optical characteristics of these crystals (absorption, photoluminescence, and photostimulated-luminescence spectra) are investigated. The copper impurity is shown to enter CsBr:Cu_met crystals in the monovalent state Cu⁺ and CsBr:CuO and CsBr:CuBr₂ crystals in the divalent state Cu²⁺. It is found that the CsBr crystals doped with Cu⁺ and Cu²⁺ ions exhibit intense photostimulated luminescence and can be used as storage phosphors for visualization of X-ray images.     

Structural distribution and rigidity of the glass network determined by EPR of Cu

The linewidth-broadening of the EPR spectra of Cu²⁺ in silicate, borate and phosphate glasses was analyzed in terms of the distribution of g_| and A_| (δ_| and δA_|) and related to the distribution of the rigidity of the network structure. X- and K-band spectra were measured for the glasses doped with ⁶³Cu²⁺ (93% abundance). The linewidth of the HFS shoulders with parallel orientation to H increased linearly with increasing m or microwave frequency. δg_| and δA_| showed a marked dependence on glass composition. For example, in Na₂O---B₂O₃ glasses, on going from x (mol% of Na₂O) being small through intermediate to large, δg_| varied from small through large to negligibly small. In contrast to these glasses δg_| was extremely large for 75PbO · 25B₂O₃ glass. The large δg_| for the Na₂O---B₂O₃ glassesof intermediate x was attributed to the coexistence of various borate groups competitively coordinating to Cu²⁺. Negligibly small δg_| for 70Na₂O · 30B₂O₃ glass and extremely large δg_| for 75PbO ·25B₂O₃ glass, both with a narrower structural distribution, reflect regidity of the glass network. The Pb---O bonding is strong enough to distort the coordination of Cu²⁺-complex. The situation is the reverse in Na₂O---B₂O₃ glasses.     

Structure and electrochemical properties of carbon aerogels polymerized in the presence of Cu

Copper-loaded organic aerogels were prepared by sol–gel polymerization of resorcinol and formaldehyde in a solution of Cu(NO₃)₂. Carbon aerogels derived from the heat-treatment of the organic precursor kept their particulate structure, according to TEM observations. The particle size in Cu-loaded carbon aerogel samples becomes larger with a higher concentration of Cu incorporated into their texture, due to the presence of Cu²⁺ rather than the pH conditions in the sol–gel process. The nitrogen adsorption measurement of Cu-loaded samples showed their characteristic pore structure, i.e., a combination of microporosity and mesoporosity both developed in their texture. Especially, their advanced microporosity, which was still found after carbonization at 1273 K, was very unique, considering that micropores in organic aerogels often decreased in size during heat-treatment around this temperature range. This microporosity could be related to their stacking structure of aromatic layers revealed by STAC–XRD analysis, indicating a looser packing of aromatic layers in their structure. Application of Cu-loaded samples to electric double-layer capacitor is also discussed from the viewpoint of the amount of Cu as well as the pore structure of the samples.