单氮杂冠醚的合成及性质研究（Ⅱ）：两亲分子的合成及在水…

以酰氯或酸酐与Ｎ－（３＇－氨苯基）氮杂冠醚反应合成了一系列含长脂链基团的单氮杂冠醚两亲分子，电镜观测结果表明：系列两亲分子在稀溶液中均能自组织稳定的以双分子膜为基本结构的囊光，其大小为３０－１５０ｎｍ，泡壁厚度为５－２５ｎｍ，并用ＵＶ－Ｖｉｓ和微量得差示扫描量热研究了双分子膜中分子的聚集态和相变过程。     

钛－硅沸石的结构表征及其催化性能

ＸＲＤ，ＩＲ，２９ＳｉＭＡＳＮＭＲ，ＵＶ－ＶＩＳ及ＸＰＳ能谱表征证实钛原子进入了钛－硅五元环沸石的骨架晶格位（不含铝）．ＴＧ－ＤＴＡ结果表明，钛原子进入沸石骨架导致沸石骨架的热稳定性提高，超过１４７３Ｋ．氯丙烯与Ｈ２Ｏ２（３０％）的环氧化反应结果表明钛－硅沸石具有优异的氧化性能，这也从另一个侧面证实了钛原子位于沸石骨架晶格位．     

莨菪类生物碱毛细管电泳分析

采用毛细管区带电泳方法对阿托品（ＤＬ－莨菪碱）、东莨菪碱、山莨菪碱和樟柳碱进 行了系统分离，以 ５０ ｍｍｏｌ／Ｌ磷酸盐缓冲液（ｐＨ ８．０）－四氢呋喃（９：１，Ｖ／Ｖ）作背景电介质， 操作电压为１１ ｋＶ，柱温２４℃，电迁移进样５ ｋＶ×５ｓ，柱上２００ｎｍ检测，４种莨菪类生物碱 可在４０ ｃｍ×５０μｍ的石英毛细管柱上５．５ｍｉｎ之内实现基线分离。     

PP－g－PMMA在PP／PVDF共混体系中的应用

利用聚丙烯等离子体接枝甲基丙烯酸甲酯共聚物（ＰＰ－ｇ－ＰＭＭＡ）作增容剂，研究了其在聚丙烯／聚偏氟乙烯（ＰＶＤＦ）共混体系中的作用。增容是通过ＰＭＭＡ与ＰＶＤＦ的偶极－偶极相互作用实现的。接枝共聚物使共混体系的抗张强度和模量均有提高，由不同等离子体处理时间所得的ＰＰ－ｇ－ＰＭＭＡ，接枝率在７．７％～３００％具有最好的增容效果；而由不同后聚合时间所得的共聚物，接枝率在３０％～８０％具有最好的增容效果。     

二巯基丙醇衍生气相色谱-微波诱导等离子体-原子发射光谱测定砷的研究

用气相色谱－微波等离子体－原子发射光谱检测器（ＧＣ－ＭＩＰ－ＡＥＳ）测定水中微量无机砷．在酸性条件下，Ａｓ（Ⅲ）与２，３－二巯基丙醇（ＢＡＬ）反应生成挥发性的环状二硫胂衍生物，被甲苯萃取．在１８１．３７９ｎｍ和１８９．０４１ｎｍ处ＧＣ－ＭＩＰ－ＡＥＳ分别检测衍生物中硫砷的发射信号．检出限为１５ｐｇ（以砷计），加标回收率９６．３５－１０６．０３％，变异系数＜４．５％．     

测定大豆和葛根中异黄酮的高效液相色谱法

建立了测定大豆和葛根７种异黄酮成分的高效液相色谱法,采用日本岛ｈｉｍ－ＰａｃｋＣＬＣＯＤＳ柱「１５０ｍｍ＊６．０ｍｍＩＤ;５μｍ）,Ｖ甲醇：Ｖ醋酸：Ｖ水＝３０：３．５：６６．５体系为流动相,０－８．５ｍｉｎ时流动相流速为１．０ｍＬ／ｍｉｎ,８．５－４７ｍｉｎ时流速为１．５ｍＬ／ｍｉｎ,柱温５０℃,检测波长２５４ｎｍ,外标法定量。     

C_（60）化学修饰的PNVC材料的UV－VIS谱研究

本实验采用金属有机化学方法成功地将富勒烯分子引入到ＰＮＶＣ侧链形成ＣＢＰ（ＣｈａｒｍＢｒａｃｅｌｅｔＰｏｌｙｍｅｒ）型共聚功能材料，研究了其ＵＶ－ＶＩｓ谱行为。结果表明，Ｃ_（６０）或Ｃ_（６０）／Ｃ_（７０）混合物化学修饰的产物其紫外可见谱明显向长波方向移动，谱峰范围由２８０ｎｍ扩展至８７０ｎｍ。Ｃ_（６０）含量增加，红移程度增大，在可见区域的吸收程度亦增加。产物主要存在５个特征峰，分别位于２１５ｎｍ、２６５ｎｍ、２９８ｎｍ、３３５ｎｍ、３４５ｎｍ处，其中２１５ｎｍ峰为Ｃ_（６０）仅存的特征峰。最后讨论了不同合成条件与产物硝化处理对其ＵＶ－ＶＩＳ谱行为的影响。     

去卤缩聚法合成蓝色电致发光聚合物聚（2,5—二庚基）对苯乙炔

利用双卤甲基苯衍生物在强碱诱导下的缩合反应，合成了共轭态可溶的聚对苯乙炔，并利用ＩＲ，ＵＶ－Ｖｉｓ，＾１Ｈ－ＮＭＲ，ＴＧＡ等对聚合物结构与性能进行了有征，其Ｎｎ＝０．４８×１０＾４。电致发光器件的发光峰值波长为４８６ｎｍ，起亮电压为２２Ｖ。     

抗心律失常新药氯苄律定及其相关物质的毛细管电泳分离与方法耐用性评价

采用毛细管区带电泳方法对抗心律失常新药氯苄律定及其合成前体盐酸黄连素和四氢黄连素进行了系统分离,以８０ ｍｍｏｌ／Ｌ磷酸盐缓冲液（ｐＨ ２．５）－乙醇（５：１,Ｖ／ Ｖ）为背景电介质,操作电压 １０ ｋＶ,毛细管柱温 ２５℃,电迁移进样 ４ ｋＶ ｘ ６ ｓ,柱上 ２３０ ｎｍ检测,盐酸黄连素、四氢黄连素、氯苄律定及内标物盐酸奎宁可在 ２０ ｃｍ ｘ ２５ μｍ涂层毛细管上 ６．０ ｍｉｎ之内实现基线分离。对优选的分离条件进行方法耐用性评价,其中乙醇含量和毛细管柱温显著影响电泳分离结果。     

核碎片激励下He－Ne－H_2激光体系的理论计算

本文较系统地收集了Ｈｅ－Ｎｅ－Ｈ＿２激光体系存在的各种碰撞反应，跃迁等速率常数共１２６个，应用原子分子反应的微观过程原理对反应产物作了判定，并对核反应与低温等离子体化学反应进行计算模拟，跟踪了核碎片激励条件下Ｎｅ的５８５．２ｎｍ谱线粒子数反转随时间的变化。得出实现Ｎｅ的５８５．２ｎｍ粒子数反转最优的Ｈｅ：Ｎｅ：Ｈ＿２是１０：１：０．０７５；最宜的总压是１．２～４．１ａｔｍ；同时还分析讨论了Ｎｅ的６３２．８ｎｍ，１．１５２ｕｍ两条谱线粒子数反转的问题。     

Surface hardness changes induced by O-, Ca- or P-ion implantation into titanium

Titanium or titanium alloys are very attractive biomedical materials. Biocompatible elements of oxygen, calcium and phosphorus were implanted into titanium and changes of surface hardness were measured using an ultra micro indenter (UMIS-2000). A multiple load-partial unload procedure that can reveal a hardness versus depth profile was adopted. Depth profiles of concentration of implanted ions were obtained by SIMS measurement. For O and P implantation, it is observed that the hardness increases with the increases in the dose. O implantation produced the largest increase in hardness, up to 2.2 times higher than the unimplanted titanium. On the other hand, Ca implantation produced only a small increase in the hardness that was independent of the ion dose. The surface oxide layer of a Ca implanted titanium sample was much thicker than the unimplanted samples or those implanted with O and P ions. The depth of maximum hardness increases with increasing energy of implanted ions. The depths of the maximum hardness occur at indentation depths of one-third to one-eighth of the mean ranges of implanted ions.     

Er3+、In3+等金属离子对多孔硅光致发光性质的影响

用阳极腐蚀的方法制备了多孔硅样品,用电化学方法在多孔硅中注入Er3+、In3+等金属离子,并对注入离子后多孔硅的光致荧光光谱进行了研究,结果表明：注入Er3+及In3+后的多孔硅在588nm处的发光峰强度大大增加,同时发光峰稍有展宽。随着离子注入时间的增长,强度继续增加,但当离子溶液浓度一定时,这种增强对时间具有饱和性。     

Ion induced controlled modifications in structural and optical properties of indium oxide thin films – studies with 25‐keV Co− and N+ beam implantations

Two sets of indium oxide thin films (~150 nm) grown on quartz substrates using thermal evaporation technique were processed separately with 25‐keV Co^? and N⁺ ions with several fluences ranging from 1.0 × 10¹⁵ to 1.0 × 10¹⁶ ions/cm². The pristine and the ion implanted films were characterized by Rutherford backscattering spectroscopy (RBS), X‐ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and UV–Vis spectrometry. The RBS spectra reveal signature of only cobalt and nitrogen in accordance to their fluences confirming absence of any contamination arising due to ion implantation. An increase in the average crystallite size (from 13.7 to 15.3 nm) of Co^? ions implanted films was confirmed by XRD. On the other hand, the films implanted with N⁺ ions showed a decrease in the average crystallite size from 20.1 to 13.7 nm. The XRD results were further verified by SEM micrographs. As seen in AFM images, the RMS surface roughness of the samples processed by both ion beams was found to decrease a bit (29.4 to 22.2 nm in Co^? implanted samples and 24.2 to 23.3 nm in N⁺ implanted samples) with increasing fluence. The Tauc's plot deduced from UV–visible spectroscopy showed that the band gap decreases from 3.54 to 3.27 eV in Co^? implanted films and increases from 3.38 to 3.58 eV for films implanted with N⁺ ions. The experimental results suggest that the modifications in structural and optical properties of indium oxide films can be controlled by optimizing the implantation conditions. Copyright © 2017 John Wiley & Sons, Ltd.     

Depth profiles of Al impurities implanted in Si wafers determined by means of the high-resolution grazing emission X-ray fluorescence technique

The synchrotron radiation based high-resolution grazing emission X-ray fluorescence (GEXRF) technique was used to extract the distribution of Al ions implanted with a dose of 10¹⁶ atoms/cm² in Si wafers with energies ranging between 1 and 100 keV. The depth distributions of the implanted ions were deduced from the measured angular profiles of the Al-Kα X-ray fluorescence line with nanometer-scale precision. The experimental results were compared to theoretical predictions of the depth distributions resulting from ion implantation. A good agreement between experiment and theory was found which proved that the presented high-resolution grazing emission X-ray fluorescence technique is well suited to perform depth profiling measurements of impurities located within the extinction depth, provided the overall shape of the distribution can be assumed a priori.     

Nanostructuring at the surface of low‐energy lead‐implanted silicon by electron beam annealing

Low‐energy lead ion implantation and high‐temperature electron beam annealing were used to study the potential of producing Pb nanostructures on Si. Pb⁺ ions were implanted at high dose into p‐type (100) Si to the depth of 8.0 nm. The implanted samples were annealed under high vacuum conditions with an electron beam at 200–700 °C for 15 s. Rutherford Backscattering Spectrometry (RBS) shows rapid out‐diffusion of Pb atoms above 400 °C. However, some Pb atoms are still present in the near‐surface region after annealing the implanted samples at 700 °C. Lead nanostructures were found on samples annealed above 300 °C. Annealing the samples at 450 °C causes the formation of nanostructures as tall as 4.1 ± 0.1 nm. Many of these are arranged in ‘web‐like’ strings that extend over micrometer distances. Occasionally, much larger nano‐features (as wide as 500 nm in diameter, average height of 1.5 nm) appear in the centre of the strings. Annealing samples well above the melting point of lead results in randomly distributed small nanometer‐sized Si nano‐dots. Copyright © 2008 John Wiley & Sons, Ltd.     

Density–depth profiles of an As‐implanted Si wafer studied by repeated planar sputter etching and total reflection x‐ray fluorescence analysis

The implantation of a high dose of high‐energy ions into an Si wafer causes amorphization of the original monocrystalline structure within a near‐surface layer. The in‐depth distribution of both Si atoms of the wafer and As ions implanted at a dose of 1 × 10¹⁷ ions cm^?2 and an energy of 100 keV is studied. A novel method combining a repeated planar and broad sputter etching with differential weighing, surface analysis by total reflection x‐ray fluorescence and Tolansky interferometry is used for this investigation. Different depth profiles are recorded on the nanometre scale for the concentration defined as the mole ratio of As and Si, for the mass density of the implanted layer and for the number density of As and Si. The results generally correspond with measurements of Rutherford backscattering spectrometry and only deviate when the assumptions made for the mass density do not fit well. An appropriate approach to this quantity involves the number density of implanted ions but, furthermore, considers a variation of the number density of Si atoms during implantation, especially for a high dose and high‐energy implantation. The variation can be taken into account by a factor γ, where γ > 1 indicates compression and γ < 1 indicates extension of the original crystalline structure. For the above mentioned implantation, γ is measured separately for each sublayer to obtain accurate depth profiles. Copyright © 2003 John Wiley & Sons, Ltd.     

Erbium Luminescence in Suboxide Films Derived from Triethoxysilane

Silicon nanoclusters formed in triethoxysilane during annealing at temperatures above 900°C are used for increasing the excitation cross section of Er atoms. A stronger sensitization of the Er luminescence is observed, for a given Er concentration, when the Er³⁺ ions are introduced in the matrix by ion implantation than when adding a salt to the precursor solution, because of a better dispersion of the implanted atoms. The logarithmic increase of the emission yield with the Er concentration up to 1 at% which is found in the case of implanted samples is ascribed to the quenching processes by interaction between neighbour Er³⁺ ions.     

Focused ion beam implantation of Ga in Si and Ge: fluence‐dependent retention and surface morphology

Focused ion beam implantation of 30‐keV Ga⁺ ions in single‐crystalline Si and Ge was investigated by SIMS, using Cs⁺ primary ions for sputtering. Nine different implantation fluences ranging from 1 × 10¹³ to 1 × 10¹⁷ Ga⁺‐ions/cm² were used, with implanted areas of 40 × 40 µm². The Ga concentration distributions of these implants were determined by SIMS depth profiling. Such 30‐keV Ga implantations were also simulated by a dynamic Monte‐Carlo code that takes into account the gradual change of the near‐surface composition due to the Ga incorporation. In both approaches, an essentially linear increase of the Ga peak concentrations with fluence is found up to ～1 × 10¹⁶cm^?2; for higher fluences, the Ga content approaches a saturation level which is reached at about (1–2) × 10¹⁷cm^?2. The measured and simulated peak concentrations of the Ga distributions are in good agreement. The most probable ranges obtained from the experiments correspond closely with the respective values from the simulations. The surface morphology caused by Ga⁺ implantation was investigated by atomic force microscopy (AFM). The AFM data indicate that for low fluences (<3 × 10¹⁵cm^?2) the surface within the implanted areas is growing outward (i.e. is swelling). For increasingly higher fluences, sputter‐induced erosion of the surface becomes dominant and distinct craters are formed for fluences above ～1 × 10¹⁶cm^?2. At the boundary of the implanted region a wall‐like structure is found to form upon Ga implantation; its height is growing with increasing fluence, reaching a value of ～15 nm at 1 × 10¹⁷ Ga⁺‐ions/cm². Copyright © 2008 John Wiley & Sons, Ltd.     

等离子体基低能离子注入的光谱诊断

采用发射光谱（ＯＥＳ）技术系统地研究了电子回旋共振（ＥＣＲ）微波等离子体基低能离子注入的等离子体特性。结果表明：纯氮气形成的等离子体中的活性粒子主要是Ｎ２和Ｎ＋２，等离子体中电子与气体分子碰撞使Ｎ２产生激发和电离，而使Ｎ２离解的作用很小；氮氩混合气形成的等离子体中，随着氩气分压的增加，Ｎ２和Ｎ＋２的浓度降低，同时氩气对氮分子离解的贡献很小；直接施加于试样的脉冲负偏压对等离子体特性没有明显影响，但存在着一定的溅射作用。     

吡柔比星在钴离子注入修饰微电极上电化学行为及其应用

吡柔比星在0.1mol/LHAc-NaAc(pH=5.05)缓冲溶液中,用Co离子注入修饰碳纤维微电极进行研究,得到一良好的还原峰,峰电位Ep=-0.520V(vs.SCE).峰电流与吡柔比星浓度在1.0×10^-7～6.0×10^-6mol/L范围内成线性关系,检出限为5.0×10^-8mol/L.用于病人尿样测定,回收率在91.6%～106.7%之间.吡柔比星的还原为可逆吸附过程,伴随着两个电子、两个氢离子参加电极反应.用扫描电子显微镜(SEM)和俄歇电子能谱(AES)两种表面分析技术对Co离子注入修饰微电极的表面状况、表面元素组成及深度分布进行测定.实验表明,Co离子确实被注入到碳纤维表面上.扫速对催化效率的影响实验证明体系存在催化作用.