激光诱导击穿光谱技术对钕铁硼永磁材料中多元素的定量表征

“磁王”钕铁硼是现今性能最为优异的永磁体,因其优异的磁性能被广泛应用于工业互联网、新能源、 5G通讯等诸多高新科技领域。目前研究钕铁硼材料中元素成分的主要分析方法有电感耦合等离子体发射光谱(ICP-OES)和X射线荧光光谱(XRF),其中ICP-OES是湿法分析,样品前处理复杂,测试周期长,而XRF法可实现直接分析,但受制于其轻元素的检测能力很难满足对钕铁硼材料中主要轻元素B的分析需求。激光诱导击穿光谱(LIBS)技术具有分析效率高,样品前处理简单,多元素直接分析,适用于现场分析、在线分析等技术优点,使其在快速定量表征方面展现出其独有的优势。运用LIBS分析技术开展对钕铁硼材料中多元素定量表征的直接、快速分析的方法研究,首先针对钕铁硼材料中定量表征的九个元素Nd、 Co、 B、 Dy、 Tb、 Pr、 Cu、 Al、 Ga完成特征谱线的筛选,通过对系统激光器电压、激光剥蚀方式等因素在不同条件下对钕铁硼材料光谱信号稳定性的影响分析,优化并确立了分析条件,最终选用720V的激光器电压,15个预剥蚀脉冲15个剥蚀脉冲的激光剥蚀方式为钕铁硼样品的分析条件;其次,选取8个通过ICP-OES法定值...     

羧甲基交联壳聚糖树脂的合成、表征及其应用

羧甲基交联壳聚糖树脂(C-C-CTS)与普通壳聚糖树脂相比,既能在酸性介质中不溶又不失去其螯合性能.其合成采用简单的2步法,首先用还氧氯丙烷交联,然后羧甲基化.C-C-CTS的结构用红外光谱和X-ray光电子能谱进行表征.C-C-CTS树脂对重金属离子有很好的螯合吸附能力,每种树脂对Pb(Ⅱ),Cu(Ⅱ)和Zn(Ⅱ)的吸附能力分别为8.73,10.12和4.89 mg·g-1,并且在不同的pH条件下对Pb(Ⅱ)、Cu(Ⅱ)和Zn(Ⅱ)有很好的选择性吸附,最后还讨论了C-C-CTS树脂对Pb(Ⅱ)的吸附机理.     

布洛芬晶体转晶与表征

利用两种不同的有机溶剂乙醇和异丙醇以及三种添加剂葡萄糖、聚乙烯吡咯烷酮、十二烷基苯磺酸钠,通过非溶剂法转晶制得不同形态的布洛芬晶体,使用电子扫描显微镜(SEM),差热扫描量热仪(DSC),X射线粉晶衍射(XRPD)等方法对其进行了表征.利用表征结果研究了结晶体系极性和氢键对晶体生长的影响,发现溶剂和添加剂通过不同的作用方式影响晶体的生长规律.     

Bi2WO6纳米晶的制备、表征及光催化性能

以硝酸铋、钨酸钠等为原料,利用水热法在150℃下反应24h得到Bi2WO6纳米晶。X射线粉末衍射结果表明,所制备的Bi2WO6属于正交晶系,晶胞参数为a=5.457,b=16.435及c=5.438。XPS结果表明所制造的Bi2WO6纯度较高。研究了分别以水、N,N-二甲基甲酰胺、乙二醇为溶剂时所制备Bi2WO6样品在可见光激发下对罗丹明B的降解活性,结果表明,以乙二醇为溶剂时,Bi2WO6光催化活性最佳,主要是由于在乙二醇中制备的Bi2WO6分散性好,粒径小,对紫外-可见光具有较大波长范围的吸收所致。另外,研究了以水为溶剂时溶液pH及添加表面活性剂等对所制备Bi2WO6光催化活性的影响,结果表明,反应温度为140～150℃,pH在1.0附近及添加SDS后所制备Bi2WO6光催化活性较佳。荧光光谱分析发现,添加表面活性剂的样品发射荧光的强度较弱,表明载流子复合程度低,因而光催化效率高。     

Controllable synthesis,characterization,and growth mechanism of hollow Zn_x Cd_(1-x) S spheres generated by a one-step thermal evaporation method

Novel hollow ZnxCdl xS spheres that are uniform in size are synthesized through the one-step thermal evaporation of a mixture of Zn and CdS powder. From an X-ray diffraction （XRD） study, the hexagonal wurtzite phase of ZnxCdl_xS is verified, and the Zn mole fraction （x） is determined to be 0.09. According to the experimental results, we propose a mechanism for the growth of Zn0.09Cd0.91S hollow spheres. The results of the cathodoluminescence investigation indicate uniform Zn, Cd, and S distribution of alloyed Zn0.09Cd0.91S, instead of separate CdS, ZnS, or nanocrystals of a core- shell structure. To the best of our knowledge, the fabrication of ZnxCd1-xS hollow spheres of this kind by one-step thermal evaporation has never been reported. This work would present a new method of growing and applying hollow spheres on Si substrates, and the discovery of the Zn0.09Cd0.91S hollow spheres would make the investigation of ZnxCd1-xS micro/nanostructures more interesting and intriguing.     

Characterizing neural activities evoked by manual acupuncture through spiking irregularity measures

The neural system characterizes information in external stimulations by different spiking patterns. In order to examine how neural spiking patterns are related to acupuncture manipulations, experiments are designed in such a way that different types of manual acupuncture （MA） manipulations are taken at the ＇Zusanli＇ point of experimental rats, and the induced electrical signals in the spinal dorsal root ganglion are detected and recorded. The interspike interval （ISI） statistical histogram is fitted by the gamma distribution, which has two parameters： one is the time-dependent firing rate and the other is a shape parameter characterizing the spiking irregularities. The shape parameter is the measure of spiking irregularities and can be used to identify the type of MA manipulations. The coefficient of variation is mostly used to measure the spike time irregularity, but it overestimates the irregularity in the case of pronounced firing rate changes. However, experiments show that each acupuncture manipulation will lead to changes in the firing rate. So we combine four relatively rate- independent measures to study the irregularity of spike trains evoked by different types of MA manipulations. Results suggest that the MA manipulations possess unique spiking statistics and characteristics and can be distinguished according to the spiking irregularity measures. These studies have offered new insights into the coding processes and information transfer of acupuncture.     

由季戊四醇合成季戊四硫醇的新方法

以季戊四醇为原料,先合成四对甲苯磺酸季戊四醇酯,然后四对甲苯磺酸季戊四醇酯与硫氰酸钾在N,N-二甲基甲酰胺中加热反应,生成了2,3,7,8-四硫螺[4,4]壬烷,2,3,7,8-四硫螺[4,4]壬烷经四氢化铝锂还原、酸化,得到季戊四硫醇.产物结构经熔点、红外光谱、质子核磁共振谱、拉曼光谱鉴定.     

巨豆三烯酮的合成及表征

采用这种合成方法的优点是原料易得,反应条件温和,操作比较简单,主要步骤产率较高,是合成目标产物的一种新方法,国内外未见文献报道。根据拟定的合成路线,通过实验对各步反应进行了研究,部分中间体经过折光率、红外(IR)、核磁共振(HNMR)、质谱(MS)等分析确定了其结构。实验证明该合成方法简单可行,目标产物的产率达24.3%,具有一定的继续研究开发价值。     

片层硅酸盐用于热固性PU/PLS复合可能性探讨

高岭土(Kaolinite)和蒙脱土(Montromollite)等粘土,被广泛用作添加剂来改善聚合物的耐热性能。文章用各种先进技术对高岭土与蒙脱土的形态、组成和结构进行表征比较。电子透射电镜及电子探针(TEM/EDX)结果显示高岭土较蒙脱土有较大的粒径和较小的硅铝比,TEM还显示出这些粘土是由片层粒子堆积而成。热重分析(TGA)的结果表明蒙脱土由于失去吸附水从60 ℃升温至90 ℃失重明显(约7%),而高岭土在此温度下几乎不失水。高岭土脱除结构羟基官能团脱水失重的温度大约在510 ℃,低于蒙脱土的670 ℃。室温下光声傅里叶变换(PAS-FTIR)红外光谱显示蒙脱土在羟基吸收区有较强的吸附水的吸收,1 650 cm-1处孤立的弱吸收谱带可给予左证。变温红外和TGA的结果显示,片层硅酸盐表面的结构羟基从100～500 ℃非常稳定,它可以和异氰酸酯基团(NCO)封端的预聚物反应形成热固性PU/PLS复合聚合物。