血小板的软X射线谱学显微成像研究

探索性地应用软X射线谱学显微技术研究血小板的结构及钙元素成像的变化,采用谱学显微术对制取的SD大鼠血小板形态扫描透射成像并对血小板作钙元素双能对比衬度成像。血小板成像可看到血小板大小不等,有的伸出伪足;钙元素分布成像血小板在静息状态时胞内钙元素主要分布于质膜侧凹陷的钙池,诱导聚集后则扩散分布于胞质。软X射线谱学显微成像能反应血小板钙元素分布,为钙的探测提供一种新方法。

同步辐射红外谱学显微光束线站的空间分辨率测试

同步辐射红外光源具有宽光谱范围、高准直性、高亮度等特点。相比于传统的红外热光源,同步辐射红外光源的尺寸非常小,空间分辨率可达到衍射极限。为了得到准确的空间分辨率信息,对上海光源BL01B1红外谱学显微光束线站的空间分辨率进行了测试。使用刀片法和鉴别率板对上海光源BL01B1红外谱学显微光束线站水平和垂直方向的空间分辨率进行了详细测量,两种测试方法的结果都表明在所测的中红外波段,同步辐射红外谱学显微技术的空间分辨率达到衍射极限,与理论值十分符合。

软X射线谱学显微光束线单色器结构设计及精度测试

针对上海光源谱学显微光束线站的性能要求,对其核心部件单色器进行结构设计。阐述了单色器的扫描运动原理,论述了波长扫描机构的设计方案,具体分析平面镜和光栅的转角重复精度影响因素;描述光栅切换机构,着重分析其水平偏差、垂直偏差、滚角、摆角和投角的精度问题;采用六杆并联机构的方案完成镜箱调节机构的设计,分析其支杆的调节范围和分辨力情况。给出了单色器的结构,并且对其精度进行了测试。测试结果表明,平面镜和光栅的转角重复精度分别为0.166″和0.149″;光栅切换机构的滚角、摆角和投角的重复精度分别为0.08″、0.12″和0.05″。这说明了单色器的结构设计方案和机械精度满足技术要求。

基于点扫描的同步辐射红外三维谱学显微研究

同步辐射红外(SRIR)光具有光谱范围宽、发散角小、亮度高以及信噪比高等优点,结合传统红外谱学技术,采用SRIR谱学显微技术对样品进行红外谱学显微,可以获得样品微米级别的空间光谱信息。利用MiTeGen聚亚酰胺小环作为样品,以上海光源BL01B1线站的SRIR光为光源,通过点扫描采样方式进行同步辐射红外三维谱学显微实验研究。通过获得聚亚酰胺小环在不同角度下的SRIR二维显微光谱信息,选取波数范围为1495~1485 cm-1的显微光谱信息处理,用代数迭代算法对聚亚酰胺小环的化学组分酰胺Ⅱ进行SRIR三维显微重构,获得了完整的三维重构图。实验表明本文方法能够以较高的信噪比重构出样品化学组分的三维红外显微结构。

人体胆汁及胆囊癌组织的同步辐射显微红外光谱研究

同步辐射红外光源的亮度是普通光源的100~1 000倍,在测试微小样品时具有更高的空间分辨率和信噪比。本文利用同步辐射显微红外比较了患有良性和恶性肿瘤病人的胆汁样品,在测试过程中将新鲜胆汁滴在基片上,能无损测试样品。通过比较发现患良性肿瘤病人的胆汁样品中具有更高含量的脂类,而患恶性肿瘤病人的胆汁样品则含有较高含量的磷酸脂,且两者含有的胆红素和蛋白质在组成和结构上有较大的差异。同时,利用同步辐射显微红外对患胆囊癌病人的癌症组织和癌旁组织进行微区成像,并且利用层次聚类分析可知,癌症组织比癌旁组织具有更高的脂质含量。

首届国际材料科学同步辐射会议概述

首届国际材料科学同步辐射会议于1996年7月29日至8月2日在美国芝加哥举行。主办单位是伊利诺伊理工学院。来自美、英、法、德、日、意、加等10余个西方主要工业国家的100余名代表参加了会议。笔者是唯一的中国代表。会议交流了口头报告30篇,张贴报告40余篇,内容包括结构和电子态这两个当今材料科学研究中最受人重视的领域。笔者向大会提交的论文"硫钝化GaAs表面的同步辐射光电子能谱研究"介绍了我们课题组研究硫化物处理对GaAs表面电子态所产生作用的最新结果。这一工作是在我国自己的专用同步辐射设施——合肥国家同步辐射实验室完成的。日本NTT公司研究小组的代表和英国谢菲尔德大学研究小组的代表,与笔者就用同步辐射光电子能谱研究Ⅲ-Ⅴ族化合物半导体的表面与界面的一些具体学术和技术问题,进行了讨论。

Multi-domain High-Resolution Platform for Integrated Spectroscopy and Microscopy Characterizations

In recent decades,materials science has experienced rapid development and posed increasingly high requirements for the characterizations of structures,properties,and performances.Herein,we report on our recent establishment of a multi-domain(energy,space,time)highresolution platform for integrated spectroscopy and microscopy characterizations,offering an unprecedented way to analyze materials in terms of spectral(energy)and spatial mapping as well as temporal evolution.We present several proof-of-principle results collected on this platform,including in-situ Raman imaging(high-resolution Raman,polarization Raman,low-wavenumber Raman),time-resolved photoluminescence imaging,and photoelectrical performance imaging.It can be envisioned that our newly established platform would be very powerful and effective in the multi-domain high-resolution characterizations of various materials of photoelectrochemical importance in the near future.

Distribution and occurrence of trace elements in the No.14 coal from the Huolinhe mine

Optical microscopy, and scanning electron microscopy in conjunction with energy dispersed X-ray spectrometry （SEM-EDX）, have been used to study the minerals and the concentrations of 12 trace elements in the No.14 coal from the Huolinhe mine, Inner Mongolia China. The distribution, affinity and removability of the trace elements were studied by float-sink experiments and petrological methods. A high mineral content, dominated by clay minerals, was found in the No.14 coal from the Huolinhe mine. The concentrations of As, Sb and Hg are relatively high compared to the average values for Chinese coals. As, Cr, Hg, Li, Mn, Pb are mainly associated with the minerals while Cd, Co, Ni, Sb, and Se are evenly distributed between the minerals and the organic matter. Be and Ba are mainly distributed in the minerals with a minor proportion in the organic matter. Most elements have a low organic affinity, although Sb, Se, Co, Cd, Ni are closely integrated with the organic matter. High theoretical removabilities are indicated for most trace elements. So it may be possible to lower the concentrations of trace elements during coal preparation.

Corrosion behaviors and mechanism of electroless Ni-Cu-P/n-TiN composite coating

In the present investigation, electroless Ni-Cu-P/n-TiN composite coating was prepared using alkaline citrate-based bath. X-ray diffraction （XRD）, scanning electron microscopy（SEM）, energy-dispersive spectroscopy（EDS）, electrochemical measurements, weight loss tests and Raman spectrometer were used to character the properties of the coating. As the Cu content increased from 7.3 wt% to 24.8 wt%, the corrosion current density of the Ni-Cu-P/n-TiN coating decreased from 10.80 to 4.34 ~tA. And the inclusion of Cu in NiP alloy resulted in refinement and less porosity in microstructure. The addition of TiN resulted in a slight decline in anti-corrosion property of the coating. As the mass loss test showed, Ni-24.8%Cu-P exhibited perfect corrosion resistance. Studies by Raman spectroscopy on coatings proved that Cu（II）3（PO4）（OH）3, Cu（OH）2 and CuO were examined while no compound of nickel was found, and Cu exhibited preferred corrosion in saline solution, providing cathodic protection to Ni alloy.

Swelling and breaking characteristics of limestone under high temperatures

The elemental composition,heat expansibility and breaking characteristics of limestone have been investigated with the use of an energy spectrum analyzer,a SEM,an optical microscope and an experimental heat swelling power system.The results show that 1) the heat expansibility of limestone has anisotropic properties,and 2) the heat expansion rate in the direction perpendicular to stratification is eight times greater than the rate parallel to stratification.The changes in heat expansibility as a function of heating temperature is essentially coincident with that of swelling and breaking of mineral particles and the appearance of cracks,indicating that the reason for causing the heat expansion of rock are the structural changes of limestone caused by thermal stress,crystal transformation and mineral decomposition.The apparent destruction of limestone under high temperatures is largely characterized by rock stratification breaks.When the limestone is heated beyond a certain limit,the rock destroys into crazed cracks.

Corrosion detection of tinplate cans containing coffee using EIS/EN sensor

The corrosion behavior of tinplate cans containing coffee was investigated using novel electrochemical impedance spectroscopy(EIS) and electrochemical noise(EN) sensors.The contents of iron and tin dissolved in cans were detected by inductively coupled plasma mass spectrometer(ICP-MS),and the morphology of corroded surface was observed by optical microscopy and scanning probe microscopy(SPM).The results reveal that the coating resistance,charge transfer resistance and noise resistance decrease with the prolongation of storage time.The iron and tin contents in cans increase with the storage time,while the bump height of coating surface increases from 30 nm to 80 nm during the corrosion of twelve months.The existence of deformation would enhance the corrosion process of tinplate cans.Finally,the corrosion mechanism of tinplate cans in coffee was proposed.

Corrosion Process Detection of Tinplate in Deaerated Functional Beverage by EIS

The corrosion process of tinplate in deaerated functional beverage was investigated by using electrochemical impedance spectroscopy (EIS) combined with scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) techniques. The results reveal that the uncoated tinplate shows a poor corrosion resistance and the corrosion type is detinning. During the initial stage of immersion, EIS spectrum consisted of two capacitance arcs with obvious time-constant dispersion effect, which was attributed to the two-dimensional and three-dimensional inhomogeneous distribution of the electrode surface. With the increase of immersion time, the capacitance arc of high frequency shrunk and degenerated, due to the corrosion of tin coating. The pore resistance of tin coating and the charger transfer resistance of substrate, which are determined from the electrochemical equivalent circuit, can be used as the indicators of tinplate corrosion process. The decrease of the pore resistance of tin coating indicates that the corrosion degree of tin layer becomes more severe, whereas the decrease of the charger transfer resistance of substrate implies that the corrosion degree of steel substrate also becomes more severe as the immersion time prolongs.

Fouling evaluation on membrane distillation used for reducing solvent in polyphenol rich propolis extract

Membrane distillation(MD) has not been widely studied in the concentrate of phenolic rich solution in comparison to osmotic distillation. In this work, the potential of MD to reduce solvent in the polyphenol rich propolis extract was further investigated. Polyvinylidene fluoride(PVDF) membranes were engineered with the smaller pore size for the less hydrophobic surface in order to avoid wetting, allowing only the solvent vapor to be transferred from the warm feed into the cold permeate. All the membranes exhibited more than 95% rejection of phenolic and flavonoid compounds. Although the hydrophilic membranes exhibited less fouling, they displayed a lower flux than the hydrophobic membrane due to the hindrance in the wetted pores. The hydrophobic membrane was seriously fouled by the phenolic acid as shown in the Fourier transform infrared spectroscopy spectrum. Pore plugging occurred on these hydrophobic membranes as confirmed in the scanning electron microscope images.

Corrosion Behavior of Anodic Oxidized TiO_2 Film in Seawater

TiO2 films were formed on metallic titanium substrates by the anodic oxidation method in H2SO4 solution under the 80V D.C..Phase component and microstructure were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM).Water contact angles on titanium oxide film surface were measured under both dark and sunlight illumination conditions.Corrosion tests were carried out in seawater under different illumination conditions by electrochemistry impedance spectrum (EIS) and polarization curves.The result showed that the TiO2 film prepared by the anodic oxidation method was anatase with a uniform structure and without obvious pores or cracks on its surface.The average water contact angle of the film was 116.4? in dark, in contrast to an angle of 42.7? under the UV illumination for 2 hours, which demonstrates good hydrophobic property.The anti-corrosion behavior of the TiO2 film was declining with the extended immersion time.Under dark conditions, however, the hydrophobic TiO2 film retarded the water infiltrating into the substrate.The impedance changed slowly and the corrosion current density was 2 orders of magnitude lower than that with the film illuminated by sunlight.All of those mentioned above indicate that the TiO2 film possesses much better performance under dark condition, and it can be applied as an engineering material under dark seawater environment.

Corrosion behavior of 907 steel under thin electrolyte layers of artificial seawater

The corrosion behavior of 907 steel under thin electrolyte layer(TEL) has been investigated by means of cathodic polarization curve measurement, electrochemical impedance spectroscopy(EIS) and scanning electron microscopy(SEM). The results show that the cathodic diffusion current density presents the variation trend of initial increase and subsequent decrease with the decrease of TEL thickness, and the maximum deposits at 58 μm. The cotangent-hyperbolic impedance(O) is rationally first introduced to study the diffusion process of the reactants through the corrosion products layer with many permeable holes. The initial corrosion rate of 907 steel under different TEL thickness increases with the decrease of TEL thickness except that of 104 μm,whereas the corrosion rate after long time corrosion can be ranked as 104 μm﹥402 μm﹥198 μm﹥301 μm﹥bulk solution.

Generation reason and corrosion characteristicof cavity of tinplate alloy layer

The surface morphology of alloy layer of tinplate was studied by means of scanning electron microscopy. By using the layer on layer debonding technology of glow discharge spectrum, the contents of C and O at the boundary of alloy layer and black plate were analyzed. And the corrosion characteristic of cavity of tinplate alloy layer was studied on-line and in-situ by means of electrochemical atomic force microscope. The corrosion depth of cavity of alloy layer in-situ after different corrosion time was measured. The results show that the cavity of alloy layer is a critical factor causing rapid decline of corrosion resistance of tinplate, and the formation of cavity of alloy layer is due to incorrect pretreatment of black plate before electrotinning. The cavity of alloy layer is the internal factor causing pitting corrosion of tinplate when the tinplate is applied to food packaging material. And the dynamic equation of pitting corrosion generated in the cavity of alloy layer conforms to logarithm law.

Stability of [BMIM]HSO_4 for using as additive during zinc electrowinning from acidic sulfate solution

The stability of ionic liquid additive 1-butyl-3-methylimidazolium hydrogen sulfate （[BMIM]HSO4） during zinc electrowinning from acidic sulfate solution was investigated by cyclic voltammetry, electrochemical impedance spectroscopy and scanning electron microscopy. Compared with the traditional industrial additives, gelatine and gum arabic, [BMIM]HSO4 has more excellent chemical and thermal stabilities. The inhibition effects of gelatine and gum arabic on the zinc electrocrystallization are observed to markedly weaken due to their part degradation after 12 h longtime successive electrolysis and high temperature （90 ℃） treatments. In contrast, the activity of [BMIM]HSO4 is practically unaffected after 24 h longtime successive electrolysis and high temperature treatments. These results are corroborated with the corresponding morphological analysis of the cathodic deposits.

Pre-dispersed carbon black as conductive agent for LiFePO_4 cathodes

High dispersed carbon black was applied for LiFePO4 cathodes as conductive agent.Nano-conductive carbon agent was pre-dispersed with poly acrylic acid(PAA) as dispersant in organic N-methyl-pyrrolidone(NMP) solvent system.The dispersion property of nano-conductive carbon agent was evaluated using particle size distribution measurements,scanning electron microscopy(SEM) and transmission electron microscope(TEM).LiFePO4 cathode with as-received nano-conductive carbon agent(SP) and LiFePO4 cathode with pre-dispersed nano-conductive carbon agent(SP-PAA) were examined by scanning electron microscopy(SEM),cyclic voltammetry(CV),electrochemical impendence spectroscopy(EIS) and charge/discharge cycling performance.Results show that the dispersion property of carbon black is improved by using PAA as the dispersant.The LiFePO4 cathodes with SP-PAA exhibit improved rate behaviors(4C,135.1 mAh/g) and cycle performance(95%,200 cycles) compared to LiFePO4 cathodes with SP(4C,103.9 mAh/g and 83%,200 cycles).Because pre-dispersed carbon black(SP-PAA) is dispersed homogeneously in the dried composite electrode to form a more uniform conductive network between the active material particles,electrochemical performances of the LiFePO4 cathodes are improved.

Adsorption isotherm and inhibition effect of a synthesized di-(m-Formylphenol)-1,2-cyclohexandiimine on corrosion of steel X52 in HCl solution

The potential of di-(m-Formylphenol)-1,2-cyclohexandiimine as an environmentally friendly corrosion inhibitor for steel was investigated in 1 mol/L HCl using potentiodynamic polarization, electrochemical impedance spectroscopy and chronoamperometry measurements. All electrochemical measurements suggest that this compound is an excellent corrosion inhibitor for mild steel and the inhibition efficiency increases with the increase in inhibitor concentration. The effect of temperature on the corrosion behavior of mild steel with the addition of the Schiff base was studied in the temperature range from 25 °C to 65 °C. It is found that the adsorption of this inhibitor follows the Langmuir adsorption isotherms. The value of activation energy and the thermodynamic parameters such as ΔHads, ΔSads, Kads and ΔGads were calculated by the corrosion currents at different temperatures using the adsorption isotherm. The morphology of mild steel surface in the absence and presence of inhibitor was examined by scanning electron microscopy(SEM) images.

Rapid biosorption and reduction removal of Cr(Ⅵ) from aqueous solution by dried seaweeds

Four types of common seaweeds(Laminaria japonica,Undaria pinnatifida,Porphyra haitanensis,and Gracilaria lemaneiformis) were examined to remove Cr(Ⅵ) ions from aqueous solution.The experimental parameters that affected the biosorption process including pH,biomass dosage,contact time and temperature were investigated via batch experiments.The surface characteristics of seaweeds before and after Cr(Ⅵ) adsorption were studied with scanning electron microscopy and Fourier transform infrared spectroscopy.The results show that an initial solution with the pH of 1.0 is most favorable for Cr(Ⅵ) adsorption.Rapid adsorption is observed in the initial stage and adsorption equilibrium state is reached within 1 h.The adsorption efficiency by Porphyra haitanensis is the maximum among four types of seaweed powders,followed by Laminaria japonica and Undaria pinnatifida with biosorption efficiency up to 90%.The removal rate of Gracilaria lemaneiformis is less than 60%.The kinetic data obtained using the seaweeds are found to follow pseudo-second order kinetic model.Experimental sorption data adequately correlate with the Langmuir model.FTIR indicates that amino and carboxyl groups play an important role in the process of Cr(Ⅵ) adsorption and a large percentage of Cr(Ⅵ) ions are reduced by reductive groups on the surface of seaweeds.