化学反应在发射光谱分析上的应用——Ⅲ、花岗岩中痕量Nb、Ta、W、Hf的同时测定

本方法系利用热化学试剂CdCl_2+AgCl在室电极内与岩石中的难挥发元素Nb、Ta、W、Hf发生化学反应,形成易挥发氯化物的办法,使这些元素的直接测定下限降低到ppm级(Nb、W—5ppm;Ta、Hf—8ppm)。测定的相对标准偏差,当浓度为50ppm时,不超过9%。鉴于Nb、Ta、Hf的矿物较其氧化物更难于被氯化的事实,标准样品应采用有正确分析结果的天然样品。     

电感耦合等离子体-质谱法测定纯铪或氧化铪中的25种杂质元素

建立了用电感耦合等离子体-质谱法(ICP-MS)测定纯铪或氧化铪中的Mg、Al、Si、P、Ca、Ti、V、Cr、Mn、Fe、Ni、Co、Cu、Zn、As、Zr、Nb、Mo、Cd、Sn、Sb、Ta、W、Pb和Bi等25种杂质元素含量的方法。铪金属室温条件下混酸溶解后可直接进样分析,氧化铪采用微波消解,辅助溶解后用ICP-MS测定。利用建立的方法,对铪及氧化铪中的杂质元素进行测定,加标回收率为86%—120%。各金属杂质含量均为10ng/mL的混合标准溶液平行7次进样的相对标准偏差均小于5%。方法操作简便、快速,检出限低,能够满足纯度为99.99%的铪金属或氧化铪中杂质分析的需要。     

端视ICP-AES测定铀化合物中的40种微量杂质元素

本文叙述一种用TEHP(磷酸三辛酯)—Kel-F(聚三氟氯乙烯粉)反相分配色层使铀与微量杂质元素分离,用端视ICP—AES测定多种铀化合物中共计40种微量杂质元素的分析方法。该方法,在取样200mg和选定的端视ICP条件下,能一次同时测定40个元素。在重加回收中,除Ta和Mo的回收率稍差外,其余元素的回收率是84—118%,大多数元素的测定精密度(RSD)<±10%,考核结果令人满意,实际样品分析与其它方法分析结果基本相符。并作了Fe、Na、Ca的干扰实验。     

质子引起Ta,Au和BiL—亚壳层电离

0.4—2.75Mev能量的质子轰击薄的Ta,Au和Bi的单元素靶。Si(Li)探测器测量L—壳x射线能谱。利用亚壳层荧光产额和Coster-Kronig跃迁率的理论值,得到2S_(1/2)2P_~(1/2)和2P_(3/2)亚壳层电离截面。测量的L—亚壳层电离截面和它们的比与ECPSSR理论预言值进行了比较。     

在强碳化物形成元素衬底上生长金刚石薄膜的物理机制探索

作者在研究金刚石表面金属化机理中发现,该物理过程是用化学气相沉积(CVD)方法在强碳化物形成元素上生长金刚石薄膜的逆物理过程。推断在强碳化物形成元素上,诸如WSi,Ta等,生长金刚石薄膜,其界面有相应的碳化物,诸如WC,SiC,TaC等出现,继而生长的金刚石薄膜实质是在相应的碳化物背底上择优取向成核生长的。从而揭示在强碳化物形成元素上生长金刚石薄膜的物理机制是:W(Si,Ta)等→WC(SiC,TaC)等→金刚石薄膜。 关键词：     

FCVAD合成Ta-C(N)薄膜及其Raman和XPS分析

掺N非晶金刚石Ta—C(N)薄膜是合成β—C3N4研究中出现的一种新型固体薄膜材料,近年来由于其优异的电化学性能受到越来越多的关注。我们用磁过滤阴极真空弧等离子体沉积(FCVAD)方法在不同N2分压下,在Si衬底上合成了Ta—C(N)薄膜。Raman和XPS分析表明Ta—C：N薄膜中的N主要以C—N的方式与C结合。N2分压越大,N／C原子比越高,最高可达31．1％。但同时sp^3键含量越低,并且合成Ta-C：N薄膜的速度越慢。     

粉煤灰地聚合物固封Cr3+的FTIR和XPS研究

采用傅里叶变换红外光谱(FTIR)和X射线光电子能谱分析(XPS)研究了粉煤灰地聚合物固封Cr3 的机理。含Cr的污泥由人工合成,主要成分是Cr(OH)3。浸出试验采用ICP-AES方法,测试了固封Cr3 前后,粉煤灰地聚合物中Al和Si的浸出量;研究结果表明,掺入含Cr的污泥后,粉煤灰地聚合物中Si和Al元素的浸出量较不掺污泥时减少了,且浸出Si元素减少的幅度比浸出Al元素降低的幅度要大。FTIR结果显示,Cr3 的掺入削弱了粉煤灰地聚合物主峰的强度,增加了Si—O—Si和Al—O—Si的振动波数;XPS测试结果表明,O(1s),Si(2p)和Cr(2p)的结合能都有不同程度的改变,而Al(2p)的结合能几乎没有发生变化;结果揭示Cr3 参与了粉煤灰地聚合物中硅酸结构的聚合,粉煤灰地聚合物固封Cr3 ,不仅仅只是物理性的包裹作用,而且主要是化学反应的结果。     

古交飞灰不同粒径颗粒的XRD及FTIR研究

我国每年产生大量的粉煤灰,不同粒径的粉煤灰在处置利用方面存在较大差异。为探究不同粒径粉煤灰物质组成及结构的差异,选取古交飞灰为研究对象,将其筛分成8个粒度级别,运用X射线衍射(XRD)及傅里叶变换红外光谱(FTIR)表征。结果表明:XRD图谱显示古交飞灰主要物质组成为非晶相玻璃体(61.93%～74.76%),莫来石(20.45%～29.59%)与少量石英(1.23%～5.64%)。随着粒径的增加,莫来石含量降低,石英含量先增加后降低,而玻璃体呈现整体上升的趋势。FTIR图谱显示Si—O(Si, Al)反对称伸缩振动峰为主要化学键(58.86%～67.39%),其次为Si—O—(Si)弯曲振动(15.28%～21.40%), Si—O—Si对称伸缩振动(6.18%～9.67%), Si—O—(Al)对称伸缩振动(0.79%～4.02%)。随着粒径的增加, Si—O(Si, Al)反对称伸缩振动相对增加, Si—O—(Si)弯曲振动降低,而Si—O—Si对称伸缩振动与Si—O—(Al)对称伸缩振动波有明显变化规律。FTIR中Si—O(Si, Al)反对称伸缩振动峰主要为飞灰中的玻璃体的吸收峰,其相对含量随着粒度的增加而增加与XRD定量所得玻璃体含量变化趋势整体一致。464 cm~(-1)附近石英的Si—O—(Si)弯曲振动, 1 090 cm~(-1)附近石英的Si—O—Si反对称伸缩振动相对含量的变化趋势与XRD定量所得石英百分含量的结果基本一致。不同粒飞灰中莫来石556 cm~(-1)处强吸收峰的相对含量(y)与XRD计算所得莫来石含量(x%)呈线性关系:y=0.396x-1.997,R~2=0.868。     

Ni-based Ni-Fe-B-Si-Ta bulk metallic glasses

The glass-forming ability and properties of Ni-based Ni-Fe-B-Si-Ta bulk metallic glasses are explored in this work. The alloy compositions are determined by using a combination of the cluster line approach, the multi-alloying strategy and the substitutions of similar elements. Bulk metallic glasses with diameters of 3 mm take shape at compositions formulated under the clus- ter-plus-glue-atom model [M9B]B~[(Ni1-xFex)7.71(Si0.66Ta0.34)1.29B]B0.94=(Ni1-xFex)70.5B17.7Si7.8Ta4, x=0.35–0.45, where the bracketed part is the cluster and the unbracketed part is the glue atoms. These alloys exhibit good magnetic properties. The maximum Is is found in the (Ni0.55Fe0.45)70.5B17.7Si7.8Ta4 alloy which reaches 0.51 T, with its Hc as low as 8.5 A/m. Interestingly, these alloys display dual glass transitions at (Ni0.65Fe0.35)70.5B17.7Si7.8Ta4, (Ni0.60Fe0.4)70.5B17.7Si7.8Ta4 and (Ni0.55Fe0.45)70.5B17.7- Si7.8Ta4 as unveiled by Temperature-Modulated Differential Scanning Calorimetry.     

硫脲为络合剂原子吸收测定钯银硅铁非晶合金中的银

以硫脲为络合剂,在低酸性介质中原子吸收测银已被用于矿石样品分析中、文献曾对矿石中一定量的Fe~(3+)、Cu~(2+)、Mn~(2+)、Au~(3+)、Ni~(2+)、Al~(3+)、Ca~(2+)、Cr~(6+)、K~+,Na~+等元素进行试验,结果证明上述元素共存基本不干扰银的测定。大量钯对银的影响未见报导。作者分析Pd-Ag-Si-Fe样品中的Ag时,(Pd80—90%、Ag2.0—12.5%,Si—4%,Fe0.6—13.5%)     

Theoretical analysis and simulation of conjugate heights for dual-conjugate AO system in lidar

A multi-conjugate adaptive optics （MCAO） can offer a possibility of widening field of view （FOV） characterized by the isoplanatic angle, and the choose of conjugate height becomes a basic problem for MCAO, which influences the size of iosplanatic angle. Considering the application of lidar, the isoplanatic angle＇s expressions of two deformable mirrors （DMs） MCAO for uplink and downlink are deduced. The effects of conjugate heights for dual-conjugate AO are thoughtfully discussed, and the isoplanatic angles are further analyzed. The results show that the isopanatic angle varies with the conjugate height and reaches the maximum as the conjugate height is at the optimal altitude. Moreover, the optimal conjugate height changes with the propagation distance.     

Quick single-photon detector with many avalanche photo diodes working on the time division

Due to the limit of response speed of the present single-photon detector, the code rate is still too low to come into practical use for the present quantum key distribution (QKD) system.A new idea is put up to design a quick single-photon detector.This quick single-photon detector is composed of a multi-port optic-fiber splitter and many avalanche photo diodes (APDs).Au of the ports with APDs work on the time division and cooperate with a logic discriminating and deciding unit driven by the clock signal.The operation frequency lies on the number N of ports, and can reach N times of the conventional single-photon detector.The single-photon prompt detection can come true for high repetition-rate pulses.The applying of this detector will largely raise the code rate of the QKD, and boost the commercial use.     

Characterization of PolyA and PolyC mismatches by Raman spectroscopy

A.C mismatches are studied by Raman spectral characterization of PolyA, PolyC, and their equimolar complex in solution of 0.14 mol/L Na ,pH7.0.Experimental results show that A·C mismatches occur to be A/B (mainly A) conformers, and unlike Watson-Crick base pairing, this kind of mismatches is stabilized by only one hydrogen bond involving cytosine N4H2 and adenine N7.The formation of A·C complex makes the base stacking interactions much stronger, and conformation of the backbone more ordered, which leads to obvious Raman hypochromic effect with some shifts in corresponding bands.     

Improvement of four-wave mixing-based wavelength conversion efficiency in dispersion shifted fiber by 40-GHz clock pumping

40-GHz clock modulated signal as a pump to improve the efficiency of four-wave mixing (FWM)-based wavelength conversion in a 26.5-km dispersion shifted fiber (DSF) is investigated. The experimental results demonstrate that the conjugated FWM component has higher intensity with the clock pumping than that with the continuous-wave (CW) light pumping. The improvement of FWM-based wavelength conversion efficiency is negligible when the pump power is less than Brillouin threshold. But when the pump power is greater than Brillouin threshold, the improvement becomes significant and increases with the increment of pump power. The improvement can increase up to 9 dB if pump power reaches 17 dBm.     

Multi-pulse operation of a Kerr-lens mode-locked femtosecond laser

Our experimental results show that the presence of a proper amount of negative group velocity dispersion is essential to multi-pulse operation of a Kerr-lens mode-locked femtosecond laser. We demonstrate that the pulse separations and the number of pulses contained within a cavity round trip are strongly dependent on the initial perturbations. The results allow us to get a better understanding on the influences of the convoluted self-phase modulation and intra-cavity dispersions on the stable multi-pulse oscillation in a Kerr-lens mode-locked femtosecond laser.     

Propagation of Helmholtz-Gauss beams in weak turbulent atmosphere

Based on the Rytov approximation of light propagation in weak turbulent atmosphere,the closed-form expressions of field and average irradiance of each one of the four fundamental families of Helmholtz-Gauss (HzG)beams:cosine-Gauss beams,stationary Mathieu-Gauss beams,stationary parabolic-Gauss beams,and Bessel-Gauss beams,which are propagating in weak turbulent atmosphere,are obtained.The results show that the field and average irradiance can be written as the product of four factors:complex amplitude depending on the z-coordinate only,a Ganssian beam.a factor of complex phase perturbation induced by atmospheric turbulence,and a complex scaled version of the transverse shape of the non-diffracting beam.The effect of weak atmospheric turbulence on irradiance distribution of the HzG beam can be ignored.     

An effective method for reducing speckle noise in digital holography

An effective method for reducing the speckle noise in digital holography is proposed in this paper.Different from the methods based on classical filtering technique,it utilizes the multiple holograms which are generated by rotating the illuminating light continuously.The intensity images reconstructed by a series of holograms generated by rotating the illuminating light possess different speckle patterns.Hence by properly averaging the reconstructed intensity fields,the speckle noises can be reduced greatly.Experimental results show that the proposed method is simple and effective to reduce speckle noise in digital holography.     

Influence of purity of HfO2 on reflectance of ultraviolet multilayer

The impurities in two kinds of HfO2 materials and in their corresponding single layer thin films were determined through glow discharge mass spectrum technology and secondary ion mass spectrometry(SIMS) equipment respectively.It was found that ZrO2 was the main impurity in the two kinds of HfO2 either in the original HfO2 materials or in the electron beam deposited films.In addition,the difference of Zr content in the two kinds of HfO2 single laver films was much laxger than that of the other impurities such as Ti and Fe.which showed that it was just ZrO2 that made the difference between the optical performance of the film products including the two kinds of HfO2.With these two kinds of HfO2 and the same kind of SiO2.we deposited HfO2/SiO2 multilayer reflective coatings at the wavelength of 266 nm.Experimental results showed that the reflectances of these two mirrors were about 99.85% and 99.15% respectively,which agreed well with the designed results what were based on the optical constants obtained from the corresponding single layer thin films.     

Speech enhancement by array crosstalk resistant ANC and spectrum subtraction

Microphone array-based speech enhancement has great importance for speech communications and speech recognition. To reduce the aperture of the microphone array and to increase the effect of the speech enhancement will greatly broaden the application areas of the microphone array. An array crosstalk resistant adaptive noise cancellation method is therefore presented. And then an improved spectral subtraction algorithm is further cascaded to obtain better enhancement results. Theoretic analysis and experiments indicate that the proposed scheme needs only a very small microphone array while it simultaneously achieves a higher SNR improvement. Besides, the proposed scheme can be used in many noisy environments and is easy for real-time implementation.