退火对ZnO薄膜光学特性的影响

用射频磁控溅射法在蓝宝石衬底上制备出ZnO薄膜,通过X射线衍射(XRD)、扫描电镜(SEM)和光致发光(PL)谱等研究了退火温度对ZnO薄膜结构和光学性质的影响。测量结果显示,所制备的ZnO薄膜为六角纤锌矿结构,具有沿c轴的择优取向;随着退火温度的升高,(002)XRD峰强度和平均晶粒尺寸增大,(002)XRD峰半高宽(FWHM)减小,光致发光紫外峰强度增强。结果证明,用射频磁控溅射法通过适当控制退火温度可得到高质量ZnO薄膜。     

非晶态Se向纳米晶体Se的转变

采用水淬法制备出块状非晶态硒,通过非晶晶化法获得了六方晶型结构的、晶粒尺寸为6—45nm的块状纳米晶硒,X射线衍射及热分析研究表明非晶态硒向纳米晶硒的转变是由一步晶化完成的,激活能为54—60kJ/mol.并证实了非晶硒的短程序与六方晶型硒相同以及非晶硒的无规线团结构.根据不同方向的晶粒尺寸与晶化温度的关系,发现沿c轴的生长速率大于沿a轴的生长速率.采用无规线团形的分子链在晶界处折叠或延伸到相邻晶粒中的晶化机制解释了晶化过程中激活能低和生长速率沿c轴方向较大的实验结果. 关键词：     

退火温度对低温生长MgxZn1-xO薄膜光学性质的影响

用射频磁控溅射法在80℃衬底温度下制备出MgxZn1-xO(x=0.16)薄膜,用X射线衍射(XRD)、光致发光(PL)和透射谱研究了退火温度对MgxZn1-xO薄膜结构和光学性质的影响.测量结果显示,MgxZn1-xO薄膜为单相六角纤锌矿结构,并且具有沿c轴的择优取向;随着退火温度的升高,(002)XRD峰强度、平均晶粒尺寸和紫外PL峰强度增大,(002)XRD峰半高宽(FWHM)减小.结果证明,用射频磁控溅射法通过适当控制退火温度可得到高质量MgxZn1-xO薄膜.     

PAN基碳纤维在表面处理中的拉曼光谱研究

采用激光拉曼光谱研究了PAN基碳纤维在表面处理中的微结构变化,分析了表面处理前后碳纤维的一级拉曼光谱特性。结果表明：拉曼光谱中主要的D峰和G峰的拉曼频移、半高宽以及各个不同拉曼频移位置对应肩峰的积分面积比是表征碳纤维物相结构变化的重要参数。经过不同的表面处理,PAN基碳纤维的一级拉曼光谱参数发生了一定程度变化,D峰和G峰的拉曼峰位向高波数偏移,表征石墨微晶尺寸的R值有所提高,这说明在表面处理后碳纤维的石墨微结构受到刻蚀,微晶尺寸有所减小,石墨微晶的边界活性增大;此外,表征碳纤维结构有序程度和缺陷多少的D峰和G峰的半高宽均有减小,表征无定型碳结构或某种有机官能团的A峰和D″峰的相对积分面积减小,这说明与乱层石墨结构相比,碳纤维中存在的无定型碳结构更容易被刻蚀,经过表面处理之后无定型碳的物相比例减小,这与碳纤维XRD图谱中表观结晶度提高的规律相一致。因此,利用激光拉曼光谱可研究碳纤维物相结构的变化规律。     

溅射气氛对RF反应磁控溅射制备ZnO薄膜微结构及光致发光特性的影响

用射频反应磁控溅射法在不同溅射压强和氩氧比下制备了ZnO薄膜,通过X射线衍射(XRD)、扫描电镜(SEM)和光致发光(PL)谱等研究了溅射压强和氩氧比对ZnO薄膜结构和光学性质的影响。测量结果显示,所制备的ZnO薄膜为六角纤锌矿结构,具有沿c轴的择优取向;溅射压强P=0.6Pa,氩氧比Ar/O2=20/5.5sccm时,(002)晶面衍射峰强度和平均晶粒尺寸较大,(O02)XRD峰半峰全宽(FWHM)最小,光致发光紫外峰强度最强。     

无氟PA-MOD法制备SmBa2Cu3O7-x薄膜的热处理研究

采用无氟(PA-MOD)在(00l)取向的LaAlO3单晶基底上制备SmBa2Cu3O7-x(SmBCO)超导薄膜,研究了不同成相热处理温度对薄膜性能的影响.X射线衍射(XRD)分析结果表明,经过高温处理的SmBCO薄膜其晶粒具有良好的c轴生长取向.扫描电镜(SEM)分析表明,790℃成相的SmBCO薄膜的表面更加平整致密.物理性能测试系统(PPMS)测试结果表明SmBCO样品的超导临界温度Tc为89.74K.研究了高温热处理过程中不同熔融温度制备SmBCO薄膜的影响.     

衬底温度对ZnO薄膜晶体结构和电学性质的影响研究

由GDARE法在较低温度下,以玻璃为衬底沉积ZnO薄膜,用SEM、AFM、XRD及交流阻抗谱测量等方法研究了衬底温度对薄膜表面形貌、晶体结构以及晶体导电性质的影响.研究结果表明,室温下沉积的薄膜为颗粒致密的非晶相结构,晶界电阻较小.在衬底温度大于50℃时,由GDARE法可沉积出具有一定c轴取向的ZnO薄膜.随衬底温度的升高,薄膜沿c轴择优生长趋势明显增强,内应力减小,晶界效应增强,晶界电阻增大.衬底温度大于100℃后,沿c轴的取向度增强趋势减缓.在衬底温度180～200℃时,可获得高度c轴取向的ZnO超细微粒薄膜,其结晶性能良好,表面光滑,平均粒径30～40nm,晶粒尺寸均匀,晶形规则,沿c轴的内应力很小,取向度达0.965.此时薄膜的晶界效应增强,晶界电阻明显大于室温下沉积的薄膜,而晶粒电阻所占比例很小,总阻抗以晶界电阻为主.同时还讨论了衬底温度对薄膜晶体结构及晶界特性的影响机理.     

联合体驱使生长法制备ZnO纳米棒及其表征

在常压环境下采用联合体驱使生长(Aggregation-driven growth)法在镀有ZnO纳米薄膜的医用盖玻片衬底和锌箔上制备了不同直径、高取向、密集生长的ZnO纳米棒阵列结构,发现平均直径与生长时间呈线性关系。X射线衍射(XRD)谱图中出现了较强的(002)峰,表明制备的纳米棒阵列具有高度c轴择优生长取向;高分辨透射电子显微镜(HRTEM)和选区电子花样衍射图谱(SAED)结果表明我们得到的单根纳米棒为沿(002)生长的单晶结构。分析确定盖玻片上的纳米棒阵列是以ZnO纳米薄膜缓冲层上的ZnO种子颗粒为成核点生长形成的。     

退火温度对低温生长MgxZn1－xO薄膜光学性质的影响

用射频磁控溅射法在80℃衬底温度下制备出Mg_xZn_1-xO(x=0.16)薄膜，用X射线衍射(XRD)、光致发光(PL)和透射谱研究了退火温度对Mg_xZn_1-xO薄膜结构和光学性质的影响.测量结果显示，Mg_xZn_1-xO薄膜为单相六角纤锌矿结构，并且具有沿c轴的择优取向；随着退火温度的升高，(002)XRD峰强度、平均晶粒尺寸和紫外PL峰强度增大，(002)XRD峰半高宽(F 关键词： xZn_1-xO薄膜')" href="#">Mg_xZn_1-xO薄膜 射频磁控溅射 退火     

RF磁控溅射条件对ZnO薄膜结构的影响

采用RF磁控溅射法在Si（001）衬底上制备ZnO薄膜。研究发现了工作中溅射频率、氧气和氩气流量比对样品结构的影响。样品的XRD图谱显示了强的（002）ZnO衍射峰，表明ZnO薄膜为c轴高取向生长。比较不同条件下制备的ZnO薄膜，研究发现当氧气和氩气的流量比相同时，随着溅射功率的增加，样品的（002）衍射峰增强，半高全宽变小。而当溅射功率相同时，随着氧气和氩气的流量比增加，样品的（002）衍射峰也增强，半高全宽同样变小。此外，本文还分析了溅射工艺和薄膜晶体质量之间关系，发现在相同的功率条件下，溅射率低时晶粒尺寸更大且薄膜的结晶性更好。     

Surface functionalization of carbon nanofibers by sol-gel coating of zinc oxide

In this paper the functional carbon nanofibers were prepared by the carbonization of ZnO coated PAN nanofibers to expand the potential applications of carbon nanofibers. Polyacrylonitrile (PAN) nanofibers were obtained by electrospinning. The electrospun PAN nanofibers were then used as substrates for depositing the functional layer of zinc oxide (ZnO) on the PAN nanofiber surfaces by sol-gel technique. The effects of coating, pre-oxidation and carbonization on the surface morphology and structures of the nanofibers were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) and Scanning electron microscopy (SEM), respectively. The results of SEM showed a significant increase of the size of ZnO nanograins on the surface of nanofibers after the treatments of coating, pre-oxidation and carbonization. The observations by SEM also revealed that ZnO nanoclusters were firmly and clearly distributed on the surface of the carbon nanofibers. FTIR examination also confirmed the deposition of ZnO on the surface of carbon nanofibers. The XRD analysis indicated that the crystal structure of ZnO nanograins on the surface of carbon nanofibers.     

Effects of carbon fibers on the transcrystalline interphase in poly(phenylene sulfide) of different molecular weights

Composite films of different molecular weight poly(phenylene sulfide) (PPS) and three types of carbon fibers (Pitch, PAN, and Rayon-based fibers) have been studied by optical microscopy and wide-angle X-ray diffraction. Transcrystallization of growing spherulites on carbon fibers is found under all thermal conditions of growth on Rayon and Pitch-based carbon fibers for all types of matrices. For composite films with PAN carbon fibers transcrystallization of growing spherulites is not uniform and sometimes is not found at all. Existence of b axial orientation of twisted lamellae for transcrystalline zone of PPS is demonstrated by X-ray diffraction technique and compared with orientation of the stretched sample. The new induction time quantitative approach is applied to the transcrystalline growth of PPS spherulites on the surface of carbon fibers. The interfacial free energy difference for fiber/crystallite and heterogeneities/ crystallite systems in the melt that is defined from growth and nucleation studies are calculated and compared. The relative tendency for a polymer to crystallize at the fiber surface rather than in the bulk is demonstrated.     

X射线粉末衍射的新起点——Rietveld全谱拟合

Ｒｉｅｔｖｅｌｄ全谱拟合法及高分辨Ｘ射线粉末衍射实验方法的出现与发展，使Ｘ射线粉末衍射进入了一个新阶段，不但提高了分析结果的质量，并且使从头晶体结构测定成为可能。本文扼要介绍了Ｒｉｅｔｖｅｌｄ全谱拟合法的理论；高分辨高准确的粉末衍射装置，从头晶体结构测定方法及多晶材料结构表征的全谱拟合法（包括作物相定性分析、物相定量分析、晶粒大小及点阵畸变的测定等）     

Densification mechanism of polyacrylonitrile-based carbon fiber during heat treatment

Polyacrylonitrile (PAN)-based carbon fibers were heat treated at various temperatures for varying durations to simulate the graphitization process in the manufacture of C/C composites. Densification of the resulting fibers was confirmed by density measurement. The composition and structure of the fibers were investigated by means of elemental analysis, X-ray diffraction and Raman spectroscopy. For specified isothermal heat treatment time, the structural parameters depended strongly on heat treatment temperature. The nitrogen content decreased with increased heat treatment temperature and extended time at constant temperature. Nitrogen loss was complete at temperatures above 1900 °C. The graphite crystallite size increased rapidly with increasing heat treatment temperature, and slowly with extended isothermal heat treatment time. At 2100 °C a more ordered graphitic structure appeared. Denitrogenation induced “puffing”, which made the fibers expand. Decrease in density in the heat treatment temperature range 1500-1900 °C originated from the abrupt evolution of nitrogen, and above 1900 °C the graphitization transition induced steadily increasing density. Densification of the carbon fibers was determined both by the rate of denitrogenation and the rearrangement of carbon atoms.     

Effect of Jet Swell and Jet Stretch on the Structure of Wet-Spun Polyacrylonitrile Fiber

The jet swell effect in the wet spinning of polyacrylonitrile (PAN) fiber was studied by optical microscopy and the jet swell ratio was obtained through directly measuring the diameter of the freely extruded fibers. For reflecting the actual drawing situation of the fibers in the coagulation process, the jet stretches were then corrected from the apparent values to the true values, and their effect on the cross-sectional morphology, internal structure, and orientation of the wet-spun PAN fibers was studied by optical microscopy, scanning electron microscopy, and X-ray diffraction, respectively. The results showed that jet stretch plays an important role in eliminating the adverse effects caused by the jet swell effect and affects the fiber structure; PAN fibers of uniform denier, dense and homogenous structure, and high orientation can only be obtained at a suitable jet stretch.     

The interpretation of X-ray diffraction from the pyrocarbon in carbon/carbon composites with comparison of TEM observations

Three different carbon/carbon (C/C) composites based on needle-punched felt made of layered T700 carbon fiber cloth were fabricated by chemical vapor infiltration and were studied using transmission electron microscopy (TEM) and X-ray diffraction (XRD). The TEM observations show that one of the composites contains only low-textured pyrocarbon. The other two contain both low-textured and high-textured pyrocarbon, one with predominantly low-textured and the other with mainly high-textured pyrocarbon. High-resolution TEM images show that the high-textured pyrocarbon in the two composites has the same microstructure as local areas with the graphite structure. XRD measurements show that the interlayer spacing and crystallite size of pyrocarbon are not only affected by the poorly graphitized carbon fiber phase, but also by the amounts of the different types of pyrocarbon and the orientation of crystallites. Comparison of the TEM observations and the XRD measurements reveals that structural parameters, such as the interlayer spacing and crystallite size, of pyrocarbon in C/C composites as determined by XRD are not accurate. Therefore, XRD profiles of C/C composites should be interpreted with caution. TEM observations for detailed microstructure analysis of C/C composites are thus important.     

Microstrain in hydroxyapatite carbon nanotube composites

Synchrotron radiation diffraction data were collected from hydroxyapatite–carbon nanotube bioceramic composites to determine the crystallite size and to measure changes in non‐uniform strain. Estimates of crystallite size and strain were determined by line‐profile fitting of discrete peaks and these were compared with a Rietveld whole‐pattern analysis. Overall the two analysis methods produced very similar numbers. In the commercial hydroxyapatite material, one reflection in particular, (0 2 3), has higher crystallite size and lower strain values in comparison with laboratory‐synthesized material. This could indicate preferential crystal growth in the [0 2 3] direction in the commercial material. From the measured strains in the pure material and the composite, there was a degree of bonding between the matrix and strengthening fibres. However, increasing the amount of carbon nanotubes in the composite has increased the strain in the material, which is undesirable for biomedical implant applications.     

EPR spectroscopic and X-Ray diffraction studies of carbon fibers with different mechanical properties

The carbon fibers obtained by carbonization of polyacrylonitrile fibers were studied by electron paramagnetic resonance and X-ray diffraction analysis in the range of small and wide scattering angles. Their elastic and strength characteristics were also studied. The concentration of the paramagnetic centers was correlated with the mechanical properties of carbon fibers. The wide-angle X-ray diffraction study did not reveal essential structural differences in the carbon fiber samples with different mechanical properties. At the same time, the small-angle X-ray scattering study showed that the fiber nanostructures with different mechanical properties differ substantially.     

Antistatic behavior of PAN-based low-temperature carbonaceous fibers

A kind of antistatic coatings which were applied to nonconductive surfaces were prepared with polytetrafluoroethylene (PTFE) paint as matrix, polyacrylonitrile (PAN)-based low-temperature carbonaceous fibers as conductive filler. The influences of carbonaceous fiber content, carbonization temperature, size and testing voltage on the surface resistivity of the coating were investigated. The surface resistivity could be well controlled in the static dissipative range (10⁶–10⁹ Ω) by changing the content, size and carbonization temperature of carbonaceous fibers. The present study could be useful for the application of chopped carbonaceous fibers in antistatic materials.