衬底温度对脉冲激光沉积多晶锗薄膜的影响

以p型单晶硅为衬底基板,在不同衬底温度下,采用脉冲激光沉积法结合退火处理,制备了多晶锗薄膜。利用包括拉曼光谱仪和椭圆偏振仪等各种测试方法,对薄膜的形貌和微观结构进行了分析表征。结果表明,不同衬底温度下制备的锗薄膜的形貌结构有明显不同。当硅衬底的温度为300℃时,锗薄膜已经完全晶化,是结晶质量良好的多晶锗薄膜,拉曼峰谱位于297cm~(-1)处,晶体取向为(111),(220),(311)。而衬底温度低于100℃时,获得的是非晶锗薄膜,只有经过450℃以上的退火处理后,才转化为多晶锗薄膜,拉曼光谱位于298.2cm~(-1)处,半高宽9.5cm~(-1),是具有(111)择优取向的多晶锗膜。     

接枝聚乙烯/改性SiO_2共混物的结构及性能

通过预辐照接枝和悬浮接枝技术制备流滴树脂复配物和纳米SiO_2与流滴剂司班(SP)接枝物SiO_2-g-SP的共混物。采用红外光谱、差示扫描量热分析、扫描电子显微镜、旋转流变仪、加速流滴测试仪、材料试验机及液滴形状分析仪对共混物的结构、性能进行了表征。结果表明,SiO_2-g-SP相比改性纳米SiO_2在2920 cm~(-1)、2850 cm~(-1)、1728 cm~(-1)、1456 cm~(-1)和722 cm~(-1)出现了新的特征吸收峰。其中1728 cm~(-1)是酯类羰基的特征峰,2920 cm~(-1)和2850 cm~(-1)处的峰为碳氢键不对称和对称伸缩振动特征峰,这说明SP已接枝到了改性纳米SiO_2表面。通过改性纳米SiO_2接枝SP的方法引入SiO_2,使得共混物熔融温度降低,结晶温度升高;流滴剂与聚乙烯相容性变好,容易加工;共混物流滴性能得到改善,流滴期最多延长6 d,力学性能得到改善,拉伸强度最多提高了2. 5 MPa。     

预辐照聚丙烯悬浮接枝聚苯乙烯的制备及结构性能

通过预辐照和悬浮接枝技术制备聚丙烯接枝聚苯乙烯(PP-g-PS)。利用红外光谱、核磁共振、X射线衍射、差示扫描量热分析、旋转流变仪及高压击穿实验对PP-g-PS的结构和性能进行了表征。结果表明,PP-g-PS的FT-IR在1493cm~(-1),1601 cm~(-1)和3027 cm~(-1)处出现了新的吸收峰,其中1601 cm~(-1)和3027 cm~(-1)分别为PS苯环上C=C和C-H的特征吸收峰;1H-NMR在1.2,1.4和2.0位置处出现新的化学位移峰,在δ7.1和7.2处出现2组峰,这是PS苯环上氢的化学位移,证明PS已接枝到PP的大分子链上。与PP相比,PP-g-PS的熔融温度和结晶度降低,结晶温度升高;随接枝率增大,PP-g-PS的结晶温度升高;PP-g-PS的耐电压击穿性能好,其击穿场强可达PP的1.4倍。     

石灰基材料对生土改性效果及机制研究

针对当前石灰、矿渣、粉煤灰等作为生土改性剂的研究主要是在力学性能及耐久性等宏观性能方面,尝试从上述改性材料对生土改性前后的矿物组成、官能团特征峰、微观结构等微观角度来阐述生土改性的内在作用机制。试验结果表明,(1)单掺石灰时,生土改性效果随石灰掺量增加而提高,最佳掺量为10%,其28 d抗压强度和软化系数分别达到3.69 MPa和0.80,原因是其板状的Ca(OH)_2水化产物填充生土颗粒间的空隙,达到饱和后的Ca(OH)_2仅其骨架作用;(2)当10%石灰分别复掺5%矿渣和5%粉煤灰时,28 d抗压强度分别增长了8.1%和2.4%,软化系数分别达到了0.92和0.90,原因是粉煤灰和矿渣发生二次水化反应,其中Mg—O、Al—O等键断裂,Al~(3+)、Mg~(2+)等阳离子与Ca(OH)_2发生置换反应,致使1 436.47 cm~(-1)处的峰位偏移至1 400 cm~(-1)附近,同时出现了1 030 cm~(-1)附近的C-S-H凝胶特征峰以及3 120 cm~(-1)处左右的火山灰反应特征峰;(3)掺矿渣改性效果优于单掺石灰,而复掺粉煤灰的改性效果不佳。     

二甲基硅油 C-Si 伸缩振动模式红外光谱研究

在303~393 K温度范围内,采用变温傅里叶变换衰减全反射红外光谱技术(ATR-FTIR)研究了二甲基硅油的一维红外光谱、二阶导数红外光谱、四阶导数红外光谱和去卷积红外光谱。实验发现,在1800~600 cm~(-1)范围内,二甲基硅油主要存在CH_3伸缩振动模式(νCH_3)、CH_3变形振动模式(δCH_3)、CH_3摇摆振动模式(ρCH_3)、Si-O伸缩振动模式(νSi-O)和Si-C伸缩振动式(νSi-C)等5种红外吸收模式,其中782 cm~(-1)和789 cm~(-1)处的红外吸收峰归属于二甲基硅油νSi-C。以二甲基硅油νSi-C为研究对象,进一步开展相关二维红外光谱的研究。结果发现,随着测定温度的升高,二甲基硅油νSi-C红外吸收强度的变化快慢顺序为:789 cm~(-1)782 cm~(-1)。本项研究拓展了ATR-FTIR技术在二甲基硅油热变性方面的研究范围。     

大型体育球馆用铝网壳结构表面三价铬转化膜性能研究

为探究大型体育馆网壳结构用AA 3003铝合金表面转化膜性能,利用高倍电子显微镜、能谱分析、经典电化学测试方法和高分辨拉曼光谱研究了三价铬转化膜微观组织结构、化学组分、成膜过程及电化学性能。结果表明：AA 3003铝合金表面三价铬转化膜表面致密,其主要成分Cr/Zr原子比约为0.34,化学组分是ZrO₂(拉曼光谱特征谱峰为470 cm^-1)和Cr₂O₃(拉曼光谱特征谱峰为537 cm^-1)。成膜过程的开路电位最小值和最终值分别为-1.32和-1.15 V（vs SCE）。三价铬转化膜显著降低了合金在0.1 mol/L NaCl溶液的腐蚀电流密度,并在阴极抑制方面显著。     

外电场极化对纳米氧化锌结构性能的影响

提高气体选择性是半导体金属氧化物气敏材料研究的关键问题。本文采用微波法制备了纳米ZnO,进一步对其进行了外电场极化处理,研究极化效应对纳米氧化锌性能的影响规律及机制。采用X射线衍射仪(XRD)、扫描电镜(SEM)及拉曼光谱仪(Raman)对产物的结构、微观形貌、拉曼活性等进行了表征,测定了其在乙醇、丙酮气氛中的气敏特性。结果表明,外电场极化导致ZnO在438cm~(-1)处的拉曼特征峰强度明显降低。随着极化时间延长,纳米ZnO气敏元件在丙酮气体中的灵敏度逐渐升高,在乙醇气体中的灵敏度逐渐降低,外电场极化提高了纳米ZnO对乙醇和丙酮气体的选择性。     

DC-HCPCVD法低温低压下纳米金刚石膜的制备及生长特性研究

在CH4/H2气氛下,利用直流热阴极PCVD(Plasma chemical vapor deposition)设备,在低温低压下制备纳米金刚石膜。对制备的样品通过扫描电子显微镜、拉曼光谱仪、X射线衍射仪对其进行表征。结果表明:低温低压下制备的纳米膜,由于晶粒之间的团簇,导致表面粗糙度较大,拉曼测试中存在1132 cm-1处的反式聚乙炔的γ1谱峰及1190 cm-1处低聚乙烯的γ1峰,同时1550 cm-1处的G峰相对强度较高,非金刚石相成分较多,但膜的导电性能较好。     

地开石-醋酸铯插层复合物的制备及机理

采用机械研磨法制备地开石-醋酸铯插层复合物,利用TG-DTA,FTIR,XRD和FESEM表征并分析该插层复合物的形成过程。XRD结果显示地开石的层间距d(002)由0.72nm增至1.42nm,表明醋酸铯已成功进入地开石层间;FTIR谱显示新增3603cm~(-1)峰表明醋酸根离子与地开石内表面羟基形成氢键,新增3548cm~(-1)峰表明有部分水进入地开石层间;TG-DTA结果分析表明,插层复合物在110℃以下可以稳定存在,脱羟基温度降低180℃;FESEM研究表明:地开石骨架清晰,插层后形貌未发生大的变化。结合理论计算,推断水与醋酸铯分子一起进入地开石层间,与地开石内表面羟基相结合,并建立醋酸铯插层地开石的机理模型。     

退火对Mg离子注入p-GaN薄膜性能的影响

在用 MOCVD 方法生长的 p-GaN 薄膜中注入 Mg 离子,然后在 N_2气氛下在850～1150℃之间快速退火,研究了 Mg~+离子注入后样品退火前后的结构、光学和电学性质．结果表明,离子注入使 GaN 晶体沿着 a 轴和 c 轴方向同时膨胀．在离子注入后的 p-GaN 薄膜的拉曼散射谱中出现波数为300 cm~(-1)和360 cm~(-1)两个新峰,其强度随着退火温度而变化．这两个新峰分别对应于布里渊区边界的最高声学声子支的振动模式和局域振动模式．消除这两个损伤引起的峰的临界温度是不同的．注入剂量1×10~(14)cm~(-2)是一个临界值,对于注入剂量高于这个临界值的样品,高温退火不能使其晶体质量全部恢复．     

Intensities of calcium dipicolinate and Bacillus subtilis spore Raman spectra excited with 244 nm light

Ultraviolet (UV) resonance Raman spectra of Bacillus subtilis endospores have been excited at 244 nm. Spectra can be interpreted in terms of contributions from calcium dipicolinate and nucleic acid components. Differences between spectra of spores and vegetative cells are very large and are due to the dominance of the dipicolinate features in the spore spectra. Because the DNA and RNA composition of B. subtilis spores is known and because the cross-sections of Raman bands belonging to DNA and RNA bases are known, it is possible to calculate resonance Raman spectral cross-sections for the spore Raman peaks associated with the nucleic acids. The cross-sections of peaks associated with calcium dipicolinate have been measured from aqueous solutions. Cross-section values of the dominant 1017 cm(-1) calcium dipicolinate peak measured from the Bacillus spores have been shown to be consistent with a calcium dipicolinate composition of ten percent or less by weight in the spores. It is suggested that spectral cross-sections of endospores excited at 244 nm can be estimated to be the sum of the cross-sections of the calcium dipicolinate, DNA, and RNA components of the spore. It appears that the peaks due to DNA and RNA can be used as an internal standard in the calculation of spore Raman peak cross-sections, and potentially the amount of calcium dipicolinate in spores. It is estimated on the basis of known nucleic acid base cross-sections that the most intense Raman band of the Bacillus subtilis spore spectra has a cross-section of no more than 4 x 10(-18) cm(2)/mol-sr.     

Raman spectroscopic imaging markers for fatigue-related microdamage in bovine bone

Raman spectroscopic markers have been determined for fatigue-related microdamage in bovine bone. Microdamage was induced using a cyclic fatigue loading regime. After loading, the specimens were stained en-bloc with basic fuchsin to facilitate damage visualization and differentiate fatigue-induced damage from cracks generated during subsequent histological sectioning. Bone tissue specimens were examined by light microscopy and hyperspectral near-infrared Raman imaging microscopy. Three regions were defined-tissue with no visible damage, tissue with microcracks, and tissue with diffuse damage. Raman transects, lines of 150-200 Raman spectra, were used for initial tissue surveys. Exploratory factor analysis of the transect Raman spectra has identified spectroscopically distinct chemical microstructures of the bone specimens that correlate with damage. In selected regions of damage, full hyperspectral Raman images were obtained with 1.4-microm spatial resolution. In regions of undamaged tissue, the phosphate nu1 band is found at 957 cm(-1), as expected for the carbonated hydroxyapatic bone mineral. However, in regions of visible microdamage, an additional phosphate nu1 band is observed at 963 cm(-1) and interpreted as a more stoichiometric, less carbonated mineral species. Raman imaging confirms the qualitative relationship between the Raman spectral signature of bone mineral and the type of microdamage in bovine bone. Two tentative explanations for the presence of less carbonated phosphate in damaged regions are proposed.     

Interaction Studies of Anticancer Drug Lomustine with Calf Thymus DNA using Surface Enhanced Raman Spectroscopy

Drug–DNA interaction study plays a significant role in understanding the drug action at molecular level and hence rationale drug designing. Lomustine (1-[2-chloroethyl]-3-cyclohexyl-1-nitroso-urea) is an alkylating antineoplastic nitrosourea derivative, used to treat various types of cancer. In the present investigation, conformational and structural effects of lomustine on DNA structure are analyzed using surface enhanced Raman spectroscopy. Different drug/DNA molar ratios are studied to determine the binding sites and binding mode of lomustine with DNA. Results suggest binding of lomustine with nitrogenous bases guanine and cytosine alongwith weak interaction to the sugar–phosphate backbone of DNA. The present study may support rational drug designing efforts to develop nitrosourea based novel therapeutics.     

Surface-enhanced Raman spectra of calf thymus DNA adsorbed on concentrated silver colloid

Raman and surface-enhanced Raman scattering (SERS) spectra of calf thymus DNA were investigated. We have carried out improvements to the silver colloid preparation method of Lee and Meisel in two respects. In one method, the silver sol was boiled with rapid stirring for over two hours. In the second method, the silver sol was concentrated by centrifugation before adding it to the DNA solution. The resulting hydrosol could be stored for 15 months because of its high stabilization. Structural information with respect to the phosphate backbone, deoxyribose, and four bases of DNA could be obtained before and after the DNA solutions were added to the concentrated Ag colloid substrate. The intensities of almost all characteristic bands assigned to various groups of the components of DNA were enhanced to a remarkable degree. The enhancement effect of the DNA solution at neutral pH 7.0 was obviously much better than that at acidic pH 3.4 or at alkaline pH 8.5. Intensity increases of the SERS bands of the DNA solution with time were observed. The SERS signals obtained 16 hours after the interaction of the Ag colloid with the DNA solution were much better than the SERS signals obtained just after the mixed liquid was prepared. This method can be widely used to store the Ag colloid for long times and to obtain the SERS spectra of DNA molecules, and it can further be used to study the adsorption behavior of solute biomacromolecules in different solvents.     

溶胶-凝胶法制备YAG荧光粉及其性能研究

以金属硝酸盐为原料,柠檬酸为络合剂,采用溶胶一凝胶法制备出了Y_3Al_5O_(12):Ce~(3+)黄色荧光粉.用X射线粉晶衍射(XRD)对其进行了物相鉴定,表明900℃时已经得到纯的钇铝石榴石相(YAG).用红外吸收光谱对所得粉体进行分析表明,当煅烧温度升高到900℃时,在低频区出现了位于724cm~(-1)、792cm~(-1)的峰,这是YAG晶相金属与氧原子间的特征振动峰,说明YAG相已经形成.用扫描电镜(SEM)对其形貌分析,结果表明得到的产物粒径大致在3～10μm之间,平均粒径为6μm.用荧光光谱仪对其荧光光谱进行了研究,结果显示,在煅烧温度为1200℃时,其发光光谱强度最大.     

An improved algorithm to remove cosmic spikes in Raman spectra for online monitoring

Raman spectral analysis integrated with multivariate calibration is a fast and effective solution to monitor chemical product properties. However, Raman instruments utilizing charge-coupled device (CCD) detectors suffer from occasional spikes caused by cosmic rays. Cosmic spikes can disturb or even destroy the meaningful chemical information expressed by normal Raman spectra. In online monitoring, some cosmic spikes have intensity and bandwidth similar to normal Raman peaks of chemical components when a low resolution and cost-effective Raman instrument is used. Moreover, the online Raman spectra always contain variations of strong Raman peaks and fluorescence. Current spike-removal methods seem to have difficulty detecting and recovering cosmic spikes in these online Raman spectra. Therefore, an improved algorithm is proposed. In this algorithm, a new scheme composed of intensity identification and local moving window correlation analysis is introduced for cosmic spike detection; intensity identification based on derivative spectra and local linear fitting approximation are used for the recovery of cosmic spikes. The algorithm is proved to be simple and effective and has been applied in an online Raman instrument installed at a continuous catalytic reforming unit in a refinery.     

Growth of oriented aluminium nitride films on silicon by chemical vapour deposition

Aluminium nitride films were grown on silicon substrates using the chemical vapour deposition (CVD) method. The properties of the films were studied by scanning electron microscopy (SEM), atomic force microscope (AFM) measurements, X-ray diffraction and Raman scattering. The resulting films were strongly textured and had a preferential orientation with the c-axis normal to the surface, the Raman spectra showed two peaks at 607 and 653 cm^–1 and two large bands at 750 and 900 cm^–1 of smaller intensity. Both the macro- and micro-Raman spectra showed the same peaks.     

Raman active E2 modes in aluminum nitride films

The vibrational spectrum of AlN thin films has been studied in recent years by theoretical and experimental methods, but there is still a lack of full knowledge of the Raman shift of the active E₂ modes of this material. Early work by Carlone et al. [1] has indicated that the E₂ modes of AlN deposited on Si occur at frequencies of 303cm^-1 and 426cm^-1. In the present study, Raman spectra of AlN deposited by magnetron sputtering on polished Si, quartz and BK7 substrates and also the Raman spectrum of pure Si, were compared to show that these peaks can actually be assigned as Raman peaks of Si, instead of AlN Raman peaks. We show that the Raman lines at 240cm^-1 and 650cm^-1 are the true AlN E₂ Raman peaks in agreement with calculated and experimental works reported in the literature that indicate the occurrence of the low and high E₂ Raman modes of AlN in the ranges (228-252)cm^-1 and (631-665)cm^-1, respectively.     

Raman spectroscopy of amorphous, nanostructured, diamond-like carbon, and nanodiamond

Raman spectroscopy is a standard characterization technique for any carbon system. Here we review the Raman spectra of amorphous, nanostructured, diamond-like carbon and nanodiamond. We show how to use resonant Raman spectroscopy to determine structure and composition of carbon films with and without nitrogen. The measured spectra change with varying excitation energy. By visible and ultraviolet excitation measurements, the G peak dispersion can be derived and correlated with key parameters, such as density, sp(3) content, elastic constants and chemical composition. We then discuss the assignment of the peaks at 1150 and 1480 cm(-1) often observed in nanodiamond. We review the resonant Raman, isotope substitution and annealing experiments, which lead to the assignment of these peaks to trans-polyacetylene.     

Experimental vibrational study of imidazolium-based ionic liquids: Raman and infrared spectra of 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide and 1-ethyl-3-methylimidazolium ethylsulfate

The vibrational structure of two room-temperature ionic liquids with the cation 1-ethyl-3-methylimidazolium [EMIM] and the respective anions bis(trifluoromethylsulfonyl)imide [TFSI] and ethylsulfate [EtOSO(3)] is investigated. In particular, attenuated total reflection (ATR) infrared (IR) as well as Raman spectra in the spectral range from 500 to 3500 cm(-1) have been recorded and analyzed. Moreover, the depolarization ratios of the Raman lines are determined. The individual peaks are assigned to the corresponding vibrational modes of the molecules. While the CH stretching region around 3000 cm(-1) is dominating in Raman spectra, it is remarkably weak in IR spectra. Finally, the results for 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide are compared to previous studies of single ions available in the literature. This comparison shows good agreement.