样品厚度对薄膜法X射线荧光光谱测量的影响研究

分别以富集有Cr,Pb和Cd三种元素的尼龙薄膜样品及玻璃纤维滤膜为研究对象,采用滤膜叠加的方式,通过XRF光谱仪测量不同样品厚度下薄膜样品的XRF光谱,根据测得的尼龙薄膜样品中Cr,Pb,Cd元素及玻璃纤维滤膜中Ca,As和Sr元素特征XRF性质的变化,研究样品厚度对薄膜法XRF光谱测量的影响。结果表明：薄膜样品厚度对不同能量区间上元素特征谱线荧光性质的影响并不相同。元素特征谱线能量越大,元素特征X射线荧光穿透滤膜到达探测器的过程中损失越少;但由薄膜样品厚度增加引起的基体效应却越强,相应特征谱线位置处的背景荧光强度就越大,因此样品厚度增加所引起的基体效应对薄膜法XRF光谱测量的灵敏度影响就越大。对于特征谱线能量较低(能量小于7 keV)的元素,以增加薄膜样品厚度的方式来增加待测组分的质量厚度浓度,并不能有效地提高薄膜法XRF光谱测量的灵敏度;对于特征谱线能量较高的元素(能量＞7 keV),可以通过适当增加样品厚度以增加被测组分的质量厚度浓度的方式来提高XRF光谱测量的灵敏度,薄膜样品厚度在0.96～2.24 mm内,更有利于XRF光谱的测量与分析。该研究为大气及水体重金属薄膜法XRF光谱分析中薄样制备及富集技术提供了重要的理论依据。     

Enhanced superprism effect based on positive/negative lateral shift of reflective beam in a Fabry-Perot filter

It is found that when a light beam is incident obliquely on a thin film Fabry-Perot filter (FPF) from different incident media (air or substrate), the reflective beam will be shifted in both the forward and the backward directions. Based on this inverted spatial dispersion effect, two thin film FPFs with different directional lateral shifts are assembled to get a thin film superprism with a wider dispersion band. The thin film samples are fabricated as well as tested, and the results are in approximate agreement with numerical simulation.     

Raman scattering of polycrystalline GaSb thin films grownby co-evapouration process

<正>This paper reports that GaSb thin films have been co-deposited on soda-lime glass substrates.The GaSb thin film structural properties are characterized by Raman spectroscopy.The Sb-A_1g/GaSb-TO ratio decreases rapidly with the increase of substrate temperature,which suggests a small amount of crystalline Sb in the GaSb thin film and suggests that Sb atoms in the thin film decrease.In Raman spectra,the transverse optical（TO） mode intensity is stronger than that of the longitudinal optical（LO） mode,which indicates that all the samples are disordered.The LO/TO intensity ratio increases with increasing substrate temperature which suggests the improved polycrystalline quality of the GaSb thin film.A downshift of the TO and LO frequencies of the polycrystalline GaSb thin film to single crystalline bulk GaSb Raman spectra is also observed.The uniaxial stress in GaSb thin film is calculated and the value is around 1.0 GPa.The uniaxial stress decreases with increasing substrate temperature.These results suggest that a higher substrate temperature is beneficial in relaxing the stress in GaSb thin film.     

Characteraction of Ag-doped ZnO thin film synthesized by sol–gel method and its using in thin film solar cells

Pure 2% and 4% Ag-doped ZnO thin films have been synthesized on glass substrates by sol–gel method. The structure, morphology and optical properties of the samples have been studied by X-ray diffractometer (XRD), scanning probe microscope, UV–vis spectrophotometer, respectively. The XRD result shows that the pure ZnO has a wurtzite hexagonal structure, no phase segregation is observed. The surface morphology of pure ZnO thin film shows that the grains are growing preferentially along the c-axis orientation perpendicular to the substrates. The transmittance spectra reveal that all samples have high transmittance above 90% in visible region. With Ag doping content increase, a red shift is observed. The performance of Ag-doped ZnO films using in thin film solar cells are simulated. The results show that 4% Ag-doped ZnO thin film can greatly improve the absorption of the cells. Compare to pure ZnO, solar cell's energy conversion efficiency improvement of 2.47% is obtained with 4% Ag doped ZnO thin film.     

Combinatorial thin film sputtering investigation of cerium concentration in Lu2SiO5 scintillators

Lutetium oxyorthosilicate (LSO) thin films with a cerium thickness gradient were sputter deposited to investigate the optimum cerium concentration for emission intensity. Thin film cerium concentration ranged from 0.06 to 0.88 at%. To compare the thin film samples to single crystal LSO, a set of single crystal LSO samples were investigated with cerium concentrations of 0.0015, 0.0095 and 0.078 at%. The thin film samples showed peak photoluminescence emission intensity at a cerium concentration of 0.35 at%; however, the single crystal samples exhibited peak photoluminescence emission intensity at a lower cerium concentration of 0.0095 at%. The photoluminescence excitation and emission spectra as a function of concentration demonstrate the concentration quenching behavior and the mechanisms are speculated to be due to radiative (self-absorption) and non-radiative energy transfer, which may be phonon assisted.     

Er3+注入CdTe薄膜的结构和光电性能研究

采用离子注入技术对近距离升华制备的CdTe薄膜进行Er³⁺掺杂研究.讨论了不同掺Er³⁺浓度对CdTe薄膜的结构和光电性能的影响.利用X射线衍射仪、扫描电子显微镜、紫外-可见分光光度计、霍耳效应测试系统和复阻抗分析仪对样品进行测试.结果表明，适当的掺杂量可以改善CdTe薄膜的结晶性能，降低晶界势垒高度，提高其导电性能.在一定掺杂范围内掺Er³⁺对CdTe薄膜的光能隙影响不大. 关键词： CdTe薄膜 离子注入 晶界势垒 光能隙     

退火处理对ZnO薄膜晶体结构和导电性能的影响

利用直流反应磁控溅射法在硅衬底上沉积C轴择优取向的ZnO晶体薄膜,将该样品进行退火处理,并测量了样品的导电性能,结果显示退火处理可以引起薄膜的重结晶,从而改善薄膜的结晶状况,改变薄膜中的化学配比.退火后样品的薄膜电阻相对较小,增加了薄膜中施主的浓度,增强了薄膜的导电性.     

双层光学薄膜参数的多入射角椭偏分析方法

本文讨论了多入射角椭偏测量中光学参数的误差因子以及最佳测量条件的选取.指出,当薄膜较厚时,多入射角椭偏测量可以精确确定膜系的光学常数和几何厚度,并用二例实测结果加以证实.本文的方法也适用于分析多层光学薄膜.     

Optical gas sensing selectivity property of ruthenium (II)-metalloporphyrins Langmuir–Blodgett films

This paper reports the study of the selectivity property of a metalloporphyrins derivative Langmuir–Blodgett thin film, n-octaethyl porphine ruthenium (II) carbonyl (RuOEPCO), to several organic gas samples, namely the saturated vapor of acetone, 2-propanol, ethanol and cyclohexane. The sensing sensitivity was based on the change in the optical property of the film upon exposure to the gas samples that was measured at a particular wavelength, λ = 514 nm, of the light source. It was observed that the thin film exhibited excellent selectivity property to the gas samples by presenting clear differences amongst its responses. The selectivity property of the thin film was found to depend on the structure of the gaseous molecules of which the highest sensitivity was shown for the gaseous molecules with planar structure, such as cyclohexane. The mechanism for the thin films-gas interaction that promotes the selectivity characteristic is proposed.     

金属铒和氟化铒掺杂的硫化锌薄膜的交流电致发光(ACEL)特性

本文报导了不同浓度的金属铒和氟化铒掺杂的硫化锌薄膜交流电致发光(ACEL)的特性,并进行了比较。实验结果表明:ZnS:ErF3薄膜ACEL的最佳浓度(5×10-3g/g)低于ZnS:Er3+薄膜ACEL的最佳浓度(1×10-2g/g)。在ZnS薄膜中掺入稀土离子,随着浓度的增加,稀土离子之间发生交叉弛豫,这一过程与稀土离子周围环境有关,这正是ZnS:ErF3和ZnS:Er3+薄膜ACEL具有不同的最佳浓度的主要原因。     

Study of preparation of Au-LiF-Au and Al-LiF-Au systems by vacuum evaporation

The structure of thin LiF film has been investigated with regard to its continuity in Au-LiF-Au, Al-LiF-Au systems. The samples have been evaporated on unheated glass substrates at 5×10^?5 torr without breaking vacuum. The number of short-circuited samples was evaluated in dependence on the angle of evaporation and thickness of the LiF film. It appears that the angle of evaporation of the value about ofω=20° already increases the number of short circuits in the case of Au-LiF-Au, meanwhile in the case of Al-LiF-Au it has no influence. Explanation is given by means of shadow effects which take place in thin LiF film in the system Au-LiF-Au. Replicas of LiF on Au and LiF on Al show in the first case that the layer consists of larger crystals and is less homogeneous. Difference between systems mentioned above can be seen also from the dependence of the number of short-circuited samples on the thickness of thin LiF film at the angle of evaporationω=0°. It is possible to draw boundary thicknesses of thin LiF film for obtaining non-short-circuited samples. In the case of Al-LiF-Au it is about 250 Å and in the case of Au-LiF-Au about 500 Å.     

水体中铬、镉和铅的X射线荧光光谱同时快速分析方法研究

以氢氧化钠和硫化钠为沉淀剂采用共沉淀法同时富集水体中的Cr,Cd和Pb,通过对Cr(OH)₃,Cd(OH)₂和PbS沉淀均匀悬浮液抽滤以制成Cr,Cd和Pb均匀分布的薄膜样品并进行能量色散XRF光谱测量,以实现水体中Cr,Cd和Pb的同时快速分析与检测。研究了富集过程中的反应时间和反应物摩尔比对薄膜样品XRF光谱强度的影响,确定了富集过程的最佳反应条件为沉淀反应时间为5 min,OH-与Cr3+的最佳摩尔比为5.0,OH-与Cd2+的最佳摩尔比为5.0,S2-与Pb2+的最佳摩尔比为2;对富集后不同浓度的薄膜样品进行了均匀性检验,富集区域6个不同位置荧光强度的相对标准偏差均小于4.8%,说明富集后的薄膜样品具有较好的均匀性;将不同浓度薄膜样品的理论浓度值与ICP-MS方法测得的浓度值进行对比分析,验证了该富集方法对水样中Cr,Cd和Pb的富集率均能达到90%以上;根据薄膜样品的荧光强度与ICP-MS测得的浓度值,建立了基于该富集方法的水体中Cr,Cd和Pb的X射线荧光光谱定量分析方法,Cr,Cd和Pb校准曲线的线性相关系数分别为0.997 3,0.995 0和0.999 8,当实际采集水样体积为50 mL时,Cr,Cd和Pb的检出限分别为7.4,29.6和8.5 μg·L-1,均低于《污水综合排放标准 GB 8978-1996》中Cr,Cd和Pb的最高允许排放浓度,因此该方法能够实现工业生产及生活排放污水中Cr,Cd和Pb的同时快速分析与检测。该研究为基于X射线荧光光谱法的水体多种重金属同时快速在线监测提供依据。     

基于FFT的薄膜厚度干涉测量新方法

在研究二维FFT法进行干涉测试基本原理的基础上,提出一种基于二维FFT的薄膜厚度测量新方法。利用搭建的泰曼-格林型干涉系统,用CCD接收、采集卡采集,可获得被测膜层的干涉条纹图像。编制算法处理软件,可实现对干涉条纹图中薄膜边缘识别、区域延拓、滤波、波面统一等的处理,从而获得带有薄膜信息的面形分布,实现对薄膜样片厚度的自动化测量。研究结果表明：所测薄膜厚度的峰谷值为0．2562,均方根值为0．068λ,说明采用基于FFT的薄膜厚度干涉测量新方法测量薄膜厚度具有较高的精度。     

Sn掺杂ZnO薄膜的室温气敏性能及其气敏机理

采用化学气相沉积方法在预制好电极的玻璃基底上制备出Sn掺杂ZnO薄膜和纯ZnO薄膜. 两种样品典型的形貌为四足状ZnO晶须, 其直径约为150-400 nm, 呈疏松状结构. 气敏测试结果显示Sn掺杂ZnO薄膜具有优良的室温气敏性, 并对乙醇具有良好的气敏选择性, 而纯ZnO薄膜在室温条件下对乙醇和丙酮均没有气敏响应. X射线衍射结果表明两种样品均为六方纤锌矿结构. Sn掺杂ZnO样品中没有出现Sn及其氧化物的衍射峰, 其衍射结果与纯ZnO样品对比, 衍射峰向小角度偏移. 光致发光结果表明, Sn掺杂ZnO薄膜与纯ZnO薄膜均出现紫外发光峰和缺陷发光峰, 但是Sn的掺杂使得ZnO的缺陷发光峰明显增强. 将Sn掺杂ZnO样品在空气中退火后, 其室温气敏性消失, 说明Sn掺杂ZnO样品的室温气敏性可能与其缺陷含量高有关. 采用自由电子散射模型解释了Sn掺杂ZnO薄膜的室温气敏机理.     

Multi-layer structures including zigzag sculptured thin films for corrosion protection of AISI 304 stainless steel

To increase corrosion resistance of the sample,its electrical impedance must be increased.Due to the fact that electrical impedance depends on elements such as electrical resistance,capacitance,and inductance,by increasing the electrical resistance,reducing the capacitance and inductance,electrical impedance and corrosion resistance can be increased.Based on the fact that these elements depend on the type of material and the geometry of the material,multilayer structures with different geometries are proposed.For this purpose,conventional multilayer thin films,multilayer thin film including zigzag structure(zigzag 1)and multilayer thin film including double zigzag structure(zigzag 2)of manganese nitride are considered to protect AISI 304 stainless steel against corrosion in salt solution.These multilayer coatings including zigzag structures are prepared by alternately using the conventional deposition of thin film and glancing angle deposition method.After deposition,the samples are placed in a furnace under nitrogen flux for nitriding.The cross sections of the structures are observed by field emission scanning electron microscopy(FESEM).Atomic force microscope(AFM)is used to make surface analyses of the samples.The results show that the multilayer thin films including zigzag structures have smaller grains than conventional multilayer thin films,and the zigzag 2 structure has the smaller grain than the other two samples,which is attributed to the effect of shadowing and porosity on the oblique angle deposition method.Crystallography structures of the samples are studied by using x-ray diffraction(XRD)pattern and the results show that nitride phase formation in zigzag 2 structure is better than that in zigzag 1 structure and conventional multilayer thin film.To investigate the corrosion resistances of the structures,electrochemical impedance spectroscopy(EIS)and potentiodynamic polarization tests are performed.The results reveal that the multilayer thin films with zigzag structures have better corrosion protection than the conventional multilayer thin films,and the zigzag structure 2 has the smallest corrosion current and the highest corrosion resistance.The electrical impedances of the samples are investigated by simulating equivalent circuits.The high corrosion resistance of zigzag 2 structure as compared with conventional multilayer structure and zigzag 1 structure,is attributed to the high electrical impedance of the structure due to its small capacitance and high electrical resistance.Finally,the surfaces of corroded samples are observed by scanning electron microscope(SEM).     

Probing the anisotropy constants of SmCo5 and PrCo5 by Hall resistance measurements in pulsed high magnetic fields up to 47 T

In order to assess the anisotropy constants of highly anisotropic thin film samples with anisotropy fields well above 10 T, Hall resistance measurements were conducted in pulsed magnetic fields. These measurements also deliver the anomalous Hall data, which are proportional to the perpendicular magnetisation. This specific approach combines the high field values obtainable by pulsed fields with a measurement technique sensitive enough to be applied to thin film samples. Two epitaxial Rare Earth-Cobalt thin films with large in-plane uniaxial magnetocrystalline anisotropy at room temperature were studied. The resulting anisotropy fields and constants are discussed with respect to measurements on single crystals and similar films investigated in quasi-static magnetic fields well below the anisotropy field. The present technique proved to be very valuable to highly anisotropic samples, as the approach to saturation is fully monitored and the data thus provides a more extended view on the hard axis magnetisation process.     

Structure and reflective properties of Al-Cu-Fe quasicrystalline thin film prepared by laser induced arc method

Al-Cu-Fe thin films were prepared by laser induced arc (laser-arc) method from a single source-Al63Cu25Fe12 alloy, which was proved to consist of quasicrystalline phase together with approximant phase. The composition of the deposited films meets the requirement for formation of icosahedral symmetry phase. Quasicrystalline phase was obtained after annealing the amorphous as-deposit film samples. The optical properties of the samples were investigated. Thin film samples of Al, Cu and Fe deposited under the same condition were employed for comparison. The results showed specific reflective properties of Al-Cu-Fe quasicrystal thin film in some wavelength range. The optical conductivity of the films exhibited a negative peak, centered about 440 nm in range of 190to 800 nm. The Al-Cu-Fe quasicrystal thin films could absorb almost all the ray in the wavelength range from 420nm to 450 nm. The ratio of absorption was greater than 99%.     

Mechanical properties of Al/a-C nanocomposite thin films synthesized using a plasma focus device

The Al/a-C nanocomposite thin films are synthesized on Si substrates using a dense plasma focus device with alu- minum fitted anode and operating with CH4/Ar admixture. X-ray diffractometer results confirm the formation of metallic crystalline Al phases using different numbers of focus shots. Raman analyses show the formation of D and G peaks for all thin film samples, confirming the presence of a-C in the nanocomposite thin films. The formation of Al/a-C nanocomposite thin films is further confirmed using X-ray photoelectron spectroscopy analysis. The scanning electron microscope results show that the deposited thin films consist of nanoparticles and their agglomerates. The sizes of th agglomerates increase with increasing numbers of focus deposition shots. The nanoindentation results show the variations in hardness and elastic modulus values of nanocomposite thin film with increasing the number of focus shots. Maximum values of hardness and elastic modulus of the composite thin film prepared using 20 focus shots are found to be about 10.7 GPa and 189.2 GPa, respectively.     

Investigation of ferromagnetic resonance and damping properties of CoFeB

In this study, the influences of thin film thickness and post-annealing process on the magnetic properties of CoFeB thin films were investigated. The angular dependency and linewidth of the ferromagnetic resonance signal were used to explore the magnetic behavior of sputtered single-layer and trilayer thin film stacks of CoFeB. A micromagnetic simulation model was employed based on the metropolis algorithm comprising the demagnetizing field and in-plane induced uniaxial anisotropy terms with all relevant contributions. Our results reveal that the direction of magnetization changes from in-plane to out-of-plane as a result of the annealing process and induces a perpendicular magnetic anisotropy in the 1-nm thick CoFeB thin film. The ferromagnetic resonance (FMR) linewidth can be defined well by the intrinsic Gilbert damping effect and the magnetic inhomogeneity contribution in both as-grown and annealed samples. The difference between the linewidths of the single and trilayer film is mainly caused by the spin pumping effect on damping which is associated with the interface layers.     

铋层状氧化物单晶薄膜多铁性研究进展

室温单相多铁材料非常稀缺,磁性元素掺杂的铋层状钙钛矿结构Aurivillius相氧化物是一类重要的单相室温多铁材料,但由于缺少单晶类样品,这一类多铁材料研究主要是围绕多晶类块体或者多晶薄膜展开,它们的磁、电等性能研究大都采用宏观探测方式,因此这类多铁材料的多铁性机理研究进行得非常困难.近年来在高质量单晶薄膜的基础上,研究了多种磁性元素掺杂和不同周期结构的铋层状氧化物多铁单晶薄膜.这些单晶薄膜在室温下大都具有层状面面内方向的铁电极化,以及比较小的室温磁化强度,低温区存在第二个磁性相变.通过X射线共振非弹性散射实验发现元素掺杂会改变金属和氧原子之间的氧八面体晶体场的劈裂,能够增强铁磁性.另一方面,通过极化中子反射实验发现薄膜主体的磁化强度远小于通常探测的宏观磁化强度,说明单晶薄膜中磁的来源及其磁电耦合机理和多晶块体很可能是不同的.铋层状单晶薄膜的多铁性对未来继续改善这类材料的多铁性能有很好的指导作用.