In Situ IR and Raman Spectroscopic Studies of Nanostructured Pt Film Array Prepared by Square Wave Potential Methods

纳米结构薄膜具有许多特殊的光、电、磁、热等优良性能，引起了多学科广泛的研究兴趣。表面增强和异常光学效应是纳米结构薄膜普遍具有的特殊光学性能，与薄膜的组成、结构和厚度有密切关系。纳米结构薄膜的制备、表征和特殊性能研究已经成为当前多学科交叉的前沿研究热点之一。 本论文主要采用三种方波电位法制备一系列不同纳米结构Pt薄膜阵列。控制的实验参数主要有方波上下限电位（El，Eu）、停留时间（tl，tu）、频率（f）以及介质溶液和处理时间（t）等。SEM、AFM和STM的研究表明，三种方法制备的Pt薄膜具有不同的纳米结构。低频对称方波电位法制备的薄膜上Pt纳米粒子随着t的增加从岛状逐渐转变成羽状结构；低频...Nanostructured films which are remarkably different from their bulk counterparts have attracted extensive multidisciplinary interests due to their intriguing optical, electrical, magnetic, thermal properties. Surface enhanced and abnormal optical effects are ubiquitous and particular optical properties of nanostructured films, and they depend largely on the constitution, structure and thickness of...学位：理学硕士院系专业：化学化工学院化学系_物理化学(含化学物理)学号：20012507

江西靖安老虎墩东汉墓发掘简报

靖安县博物馆2009年10月--2010年1月,江西靖安老虎墩遗址联合发掘队对位于靖安县高湖镇中港邓家的老虎墩遗址进行发掘期间,在发掘区内清理东汉时期墓葬2座,分别编号为09JglM0、09JglM50,以下简称M0、M50。现将墓葬清理情况简报如下。发掘区地层堆积:第1层为耕土层;第2层为明代堆积;第3层为汉晋时期堆积;第4层及以下为新石器时代晚期堆积。M0和M50均开口于3层下,打

A Comparison on Digital Terrain Models of Different Scales in Loess Hill and Gully Area

黄土丘陵沟壑区地形变化异常复杂 ,1∶5万地形图对原始 1∶1万地形图等高线形态综合、取舍程度很大 ,这些都在不同程度上影响了地形分析结果的准确性。以高精度的 1∶1万比例尺DEM为校准值 ,运用 1∶1万及 1∶5万比例尺DEM叠合比较分析的方法 ,研究 1∶5万DEM的地形信息容量及提取不同地形要素的精度。试验结果表明 ,在黄土丘陵区 ,与 1∶1万DEM相比 ,1∶5万DEM在所提取的地面坡度、地面曲率、沟壑量等地形定量指标方面均都存在着较大的误差

Nanostructured Films Prepared on Pt Microelectrode through Square Wave Oxidation reduction Cycles and Their Particular IR Properties

运用方波电位法处理Pt微电极,制备一系列具有较高表面粗糙度的纳米结构薄膜.扫描隧道显微镜(STM)观察到薄膜由Pt金属岛组成,并测得所研制的薄膜虽然其平均厚度从58nm增加到139nm,但Pt金属岛的平均尺度仅从102nm增加到114nm,而岛的平均高度也只在15～18nm之间变化.以CO为探针分子,结合原位FTIR反射光谱研究,发现所制备的纳米结构薄膜上吸附态CO的红外吸收都给出类Fano光谱,初步归结为Pt金属岛的尺度效应.A series of nanostructured films exhibiting high surface roughness were prepared by using square wave oxidation reduction cycles (SWORC) on Pt microelectrodes.Scanning tunneling microscope (STM) studies illustrated that all the films were made up of Pt islands.Measurement showed that along with the increase of average thickness of nanostructured films from 58 to 139 nm,the average dimension of Pt islands in the film increased solely from 102 to 114 nm,and the average height of Pt islands varied from 15 to 18 nm.Employing CO adsorption as molecule probe reaction,IR properties of the prepared nanostructured Pt films of different roughness were investigated by using in situ FTIR spectroscopy.The results revealed that CO linearly adsorbed (COL) on all nanostructured Pt films prepared in this paper yielded Fano like spectra,i.e.,the IR absorption of COL on nanostructured Pt film gave rise to a bipolar IR band (asymmetric line shape),which may be attributed primarily to the size effect of Pt islands.国家自然科学基金(90206039,20021002);; 国家重点基础研究发展规划(2002CB211804)资助项目~

Preparation of Nanostructured Films on Surface of Pd Microelectrode Array by Square Wave Potential and Their Anomalous IR Properties

制备了单根可寻址Pd微电极阵列,运用方波电位法对阵列上每根Pd微电极处理不同时间,诱导生成一系列不同纳米结构的Pd薄膜.以CO为探针分子,结合原位显微傅里叶变换红外反射光谱进行表面组合电化学研究,一次性地获得CO吸附在不同纳米结构Pd薄膜上的红外光谱.观察到随方波电位法处理时间的逐步增加,桥式吸附态CO的红外光谱峰从正常吸收光谱到类Fano光谱,再到异常红外光谱的转变过程.结合扫描电子显微镜观察纳米薄膜的形貌,发现不同红外光谱特征都对应着特定的纳米结构.An individually addressable array of Pd microelectrodes was combined with in situ microscope FTIR reflection spectroscopy in the current paper to carry out surface combinatorial studies. Pd film of different nanostructures on the array was prepared electrochemically by applying the method of square wave potential. The electrochemical behavior and surface structure of the Pd film were investigated respectively by using cyclic voltammetry and scanning electron microscopy. It revealed that, through the surface combinatorial studies, with the increase of treatment time of the square wave potential, the spectral IR characteristics of bridge bonded CO on the array was transformed successively from normal absorption band to Fano-like spectral line shape, and finally to abnormal IR features. The results demonstrate that the anomalous IR properties of Pd thin film depend strongly on the nanostructure of the film.国家自然科学基金(批准号:90206039,20021002);; 国家“九七三”计划项目(批准号:2002CB211804)资助

Solid/Liquid Interfacial In Situ IR Microscope and Step-Scan Time-Resolved FTIR Spectroscopy and Applications in Studies of Nanomaterials

结合红外显微镜和步进扫描FTIR光谱仪 ,发展了固 /液界面电化学原位显微镜红外反射光谱和步进扫描快速时间分辨FTIR反射光谱 ,并应用于纳米材料特殊性能和电化学反应动力学的研究。研制纳米结构Pt微电极 ,获得CO吸附的红外特征随纳米结构和纳米尺度变化的原位显微镜红外谱图。利用纳米结构Pt微电极的异常红外效应 ,显著提高电化学原位红外反射光谱的灵敏度 ,获得分辨率达 5 0 μs的步进扫描时间分辨光谱。不仅发展了固 /液界面显微镜原位红外反射光谱新方法 ,并且拓展了电化学原位红外反射光谱在纳米材料科学研究中的应用。Electrochemical in situ microscope IR reflection spectroscopy and step-scan time-resolved FTIR reflection spectroscopy were established by using an IR-plan advantage microscope and a Nexus 870 FTIR instrument, and a home-made signal synchronizer that harmonizes electrode polarization potential and step-scan spectral data collection sequence. These new techniques have been applied in studies of particular IR properties of 2-dimensional nanomaterials. By applying a treatment of fast potential cycling with different time (τ), a set of nanostructured Pt microelectrodes were prepared. CO adsorption was employed as a probe reaction together with in situ developed microscope FTIR spectroscopy. The results illustrated the variation of abnormal IR features with the nanostructure and the thickness (i.e., the size) of film formed on Pt microelectrode, i.e., following the increase of τ in fast potential cycling treatment, the direction of CO band was turned from absorption to antiabsorption direction, and the intensity and the width of CO band were increased. By taking the advantage of the abnormal infrared effects of nanostructured Pt microelectrode, the sensitivity of in situ IR reflection spectroscopy has been significantly improved, and spectra of time-resolution as fast as 50 μs have been recorded at solid/liquid interfaces. The current studies demonstrated not only the success of development of new techniques of in situ IR spectroscopy, but also the exploitation of the established techniques in studies of nanomaterials.国家自然科学基金 (2 0 0 2 1 0 0 2 ,90 2 0 60 39);; 教育部科学研究基金 (0 1 1 0 1 )资助项

木质素灰分含量控制及其影响研究

木质素是自然界中含量最丰富的天然芳香族高分子,含有丰富的碳元素,是制备碳纤维的理想原料。但是,工业木质素的杂质含量普遍较高,不能满足碳纤维制备要求。为此,本文采用盐酸沉析、离心分离和酸洗的方式对某种国产工业木质素进行纯化处理,考察了盐酸用量及纯化次数对木质素灰分含量的影响,并采用GPC、FT-IR和DSC研究了木质素的分子量、化学结构和反应活性随纯化处理次数的变化规律。结果表明:随着纯化次数的增加,木质素的灰分含量大幅降低,反应活性显著提高;随着盐酸用量的增加,在一次提纯时,木质素的灰分含量先大幅降低,当浓盐酸与木质素的质量比大于0.6:1时,木质素的灰分含量趋于稳定;经四次纯化处理后,木质素的灰分含量降低至0.77%