非水纳米分散系的冷冻蚀刻电镜表征及与激光散射法的对比研究

报道了利用改进的冷冻蚀刻制样技术对非水介质中原位合成的纳米分散系进行的电子显微镜表征结果。研究了冷冻蚀刻电镜技术观测原位合成纳米分散系的制样步骤、制样方法，并利用冷冻蚀刻电镜技术原位观测了3种纳米分散相的粒径、粒径分布和聚集状态。激光散射法与冷冻蚀刻电镜表征的对比表征结果表明：纳米分散系中纳米相的粒径和粒径分布用两种表征方法所得结果基本一致，但冷冻蚀刻电镜表征与激光散射法相比具有准确、直观、清晰、立体的特点，并且可同时采集多种信息。与激光散射法相比，是一种表征非水纳米分散系的理想方法。     

三元复合驱低浓度体系相行为及中间混合层结构分析

低浓度的表面活性剂ASP(碱/表面活性剂/聚合物)驱油体系溶液与模拟原油混合,研究该体系的相行为和界面张力的变化情况,并应用粒度分析仪和冷冻蚀刻透射电子显微镜技术,对中间混合层的粒径分布及其结构进行研究.发现中间混合层的体积随各组分的浓度变化而有一定的规律性,中间混合层与油相和水相之间的界面张力均能达到超低.特别是得到了冷冻蚀刻电子显微镜照片, 并提出中间混合层为胶束、微乳液、乳状液等表面活性剂聚集体的共存体系,其中微乳液结构占主要地位.这对丰富表面活性剂的理论研究及探讨三元复合驱的驱油机理必将起到重要作用.     

明胶和阳离子表面活性剂CTAB的相互作用

采用电导法、荧光法、pH等方法研究了明胶与十六烷基三甲基溴化铵 (CTAB)的相互作用.结果表明,在CTAB/明胶 /水体系中,明胶浓度的增大使得CTAB分子的cac₁,cac₂,cmc值均上升,胶束的聚集数下降.冷冻蚀刻透射电镜实验(FFTEM)的结果证实了明胶分子与CTAB分子之间形成了复合物,随着CTAB浓度的增加,结构从线状、卷曲、珍珠项链状、棒状至网状依次变化.     

原位冷冻电子断层扫描的发展及在生物研究方面的应用

对生物大分子复合物的研究和结构分析对于全面了解其功能和生物学意义至关重要. 冷冻电子显微镜在提供生物大分子结构及大分子分布等方面起到重要的作用. 近年来, 冷冻电子显微镜的硬件和软件的发展进一步提高了冷冻电子显微镜的有效性, 使其对各种生物结构、 蛋白质结构的解析更加准确快捷. 但是, 对于生物系统来说, 蛋白质和大分子复合物等均处于复杂的生理环境中, 因此原位检测生物分子的三维结构对于生物体系和结构生物学具有重要意义. 冷冻电子断层扫描作为一种功能强大的技术, 可以无需标记直接通过冷冻样品的固有衬度识别生物大分子的结构, 并且可在原位生理环境中对生物分子进行纳米级分辨率的三维成像. 本文综述了与冷冻电子断层扫描相关的样品制备和数据处理技术, 并总结了冷冻电子断层扫描技术在分离的大分子复合物和整个细胞或组织中的生物学应用.     

冷冻电镜技术——2017年诺贝尔化学奖介绍

介绍了2017年诺贝尔化学奖的3位获得者在冷冻电镜领域的主要贡献，同时介绍了冷冻电镜技术的用途、一般工作流程和其局限性，以及中国学者在冷冻电镜技术应用研究中的贡献。     

电镜-能谱仪在柳树叶重金属污染研究中的应用

采用自然干燥、化学处理、冷冻处理3种方法制备待测样本,运用扫描电镜和透射电镜结合X射线能谱仪研究柳树叶肉组织对重金属的累积状况,并定位到栅栏组织的细胞壁,为定性定量以及定位分析组织细胞固定、转移重金属污染探索合适的制样方法.结果表明:(1)重金属Pb、Cu、Cd、Zn在柳树叶肉组织被检测到,并已进入到细胞壁内,同时定量结果显示污染越严重,重金属累积量越多,证明了柳树叶对重金属污染的吸收能力;(2)通过综合比较,认为冷冻处理的样本比较适合进行植物组织微区的元素定性定量以及定位分析,因此推测冷冻制样加冷冻电镜的方法将会最为理想.     

PET/HBA/TA/HQ四元共聚酯形态及相结构的研究

研制了一套蚀刻方法并对聚对苯二甲酸乙二醇酯/对羟基苯甲酸/对苯二甲酸/对苯二酚(PET/HBA/TA/HQ)体系的共聚酯液晶试样断面进行蚀刻,并用扫描电镜观察,发现此类共聚酯中存在两相结构.当PET摩尔分数小于50％时,分散相呈球状且富含PET,连续相富含全芳族链段;当PET摩尔分数等于或大于50％时,分散相和连续相结构发生颠倒,连续相富含PET,分散相球状粒子富含全芳族链段且为纤维状结构.因此可以断言,用熔融缩聚方法制备的PET/HBA/TA/HQ四元共聚酯不是无规共聚物,而是嵌段共聚物.     

综述(187~191)利用冷冻聚焦离子束制备冷冻含水切片技术问题探讨

冷冻聚焦离子束制备冷冻含水切片为研究细胞内原位结构打开了窗口, 其切片质量直接影响了后续冷冻电子断层扫描成像数据的收集及处理.目前, 这一技术的应用还存在各种各样的问题, 总结了近期文献中的相关解决之道, 以期为制备冷冻含水切片的研究者提供参考.     

具有包藏结构的三元聚丙烯纳米复合材料结构与性能关系的研究

制备了一种新型聚丙烯 丁苯橡胶 纳米碳酸钙三元纳米复合材料 .研究结果显示 ,复合材料中的大多数纳米碳酸钙粒子被包藏在丁苯橡胶中 ,并与之共同形成分散于聚丙烯树脂中的分散相 ,这种聚丙烯纳米复合材料具有高刚性、高韧性、高耐热性和高的结晶速率 .系统研究了成核剂苯甲酸钠的加入和纳米碳酸钙的用量对该类纳米复合材料相态结构、结晶形态和结晶动力学的影响 ,以及具有包藏结构的分散相粒径和PP中β晶含量对材料性能的影响 .结果表明 ,苯甲酸钠的加入和纳米碳酸钙用量的提高均可使体系中分散相粒径减小 ,结晶速率加快 ,进而使材料的韧性、刚性和耐热性提高 .     

亚微米锥形光纤的制备及硅烷化修饰

采用氢氟酸(HF)蚀刻方法制备亚微米结构的锥形光纤,考察了不同HF浓度和蚀刻时间对亚微米光纤几何构型的影响,用SEM表征光纤的几何形状.实验表明,当HF:H2O=1:1、蚀刻时间约为5h时,得到了亚微米锥形光纤,且其表面光滑.亚微米锥形光纤在甲基三氯硅烷混合溶液中进行硅烷化反应后,与吖啶橙相互作用,用其尖端的荧光强度的变化来表征亚微米光纤尖端活性基团的键合程度.该方法可用于检测光纤尖端键合的活性基团,也可以检测耦合的靶分子,这为纳米光纤生物传感器的研制奠定了基础.     

Dispersion of nano-carbon filled polyimide composites using self-degradated low molecular poly(amic acid) as impurity-free dispersant

Polyimide (PI)-based composite films incorporated with carbon black (CB), carbon nanotube (CNT) and carbon nanofiber (CNF), respectively, were prepared using low-molecular-weight poly(amic acid) (PAA), a precursor of PI, as an impurity-free dispersant. High-energy ball mill was employed not only to downsize the nano-carbon agglomerates, but also to cut off the PAA chains for in-situ stabilizing the dispersion. Effect of the ball milling time, procedure, and filler species on the filler dispersion was investigated by means of electrical resistivity reproducibility, morphology observation, and mechanical testing. Comparing with direct dispersion of the nano-carbon in PAA, the composite films fabricated by a two-step approach, that is dispersion from the in-situ degradated low-molecular-weight PAA stabilized nano-carbon slurry, presented a uniform electrical conductivity with a lower percolation concentration and excellent reproducibility in the percolation region. A significant improvement in the Young’s modulus for the CNT loaded PI film was achieved, which was much more effective than those filled with CB or CNF.     

Radiation synthesis and magnetic properties of novel Co0.7Fe0.3/Chitosan compound nanoparticles for targeted drug carrier

Chitosan coated Co_0.7Fe_0.3 compound nanoparticles were successfully synthesized through a γ-radiation route in inverse microemulsion system. An observation of transmission electron microscope (TEM) showed that the diameter of these nanoparticles was about 50 nm with narrow size-distribution. Investigations of properties of nanoparticles were also conducted with fourier transform infrared spectrometer (FT-IR), X-ray diffraction (XRD) and energy dispersion spectrum (EDS). Analysis of vibrating sample magnetometer (VSM) indicated that the nanoparticles were superparamagnetic with a saturation magnetization of 24 emu/g. These compound nanoparticles were undertaken to allow for the magnetically targeted cancer.     

On-line method for measurement of the dispersion coefficient of radionuclide migration using a column method

An on-line method to obtain breakthrough curves from a conservative tracer generated in crushed rock columns has been introduced. The breakthrough curve can be used to evaluate some important hydrologic parameters for studying radionuclide migration in groundwater system. These parameters include the dispersion coefficient, average flow yelocity, effective porosity, and retardation factor of the columns tested. A conservative radiotracer,¹³¹I, was used to generate the breakthrough curves, and linear regression analysis was applied to obtain the optimum value of dispersion coefficient. The effects of the injected volume of radioactive tracer, average flow velocity, and effective diameter of packed material on the dispersion coefficient as well as the stability of the packed material, and their in-situ application are discussed.     

二氧化碳-环氧丙烷共聚物电纺纤维形貌研究

利用电纺丝技术制备了二氧化碳环氧丙烷共聚物超细纤维,研究了喷丝口电势、纺丝距离、浓度、溶剂等因素对纤维形貌、直径及均一性的影响.实验结果表明,利用电纺丝法可以制备直径在小于200nm到7μm二氧化碳环氧丙烷共聚物纤维;喷丝口电势和浓度对于共聚物电纺丝纤维是否形成串珠结构有重要影响;电势、距离和纺丝液浓度都对纤维直径及分散系数有较大影响,在一定范围内,随着喷丝口电势增加,纤维平均直径变大而分散系数变小;纺丝距离增大使得纤维平均直径变小,分散系数变大;浓度的增大使得纤维平均直径变大,分散系数变小;不同溶剂配制的溶液体系制备的电纺丝纤维形貌有很大差异,在二氯甲烷和丁酮的体系中,分别观察到了两组较为集中的直径分布.     

Solid-liquid phase transition of tin particles observed by UHV high resolution transmission electron microscopy: pseudo-crystalline phase

Solid-liquid transition of fine tin particles having diameter of 2–10 nm is studied in-situ by high-resolution transmission electron microscopy under a ultra-high vacuum condition. Melting temperature is confirmed to decrease with the decrease of particle diameter. The particles less than the critical size, 2r _c?5 nm, are found to have a specific phase between the solid and the liquid phase. The particle in this “pseudo-crystalline” phase contains crystalline embryos in it. Particles larger than the critical size have sharp liquid-solid transition, which completed within the time resolution of our microscope observation, 33 ms upon heating or cooling process. Large solid particles have Wulff's polyhedron, while particles around the critical diameter have rather spherical shape. Structural anomaly at the critical size occurs all over the outer most surface layer slightly below the melting temperature. Origin of the “pseudo-crystalline” phase and surface pre-melting phenomena are discussed.     

Synthesis and spectroscopic studies of stable aqueous dispersion of silver nanoparticles

A facile approach for the synthesis of stable aqueous dispersion of silver nanoparticles (AgNPs) using glucose as the reducing agent in water/micelles system, in which cetyltrimethylammonium bromide (CTAB) was used as capping agent (stabilizer) is described. The evolution of plasmon band of AgNPs was monitored under different conditions such as (a) concentration of sodium hydroxide, (b) concentration of glucose, (c) concentration of silver nitrate (d) concentration of CTAB, and (e) reaction time. AgNPs were characterized by UV-visible spectroscopy, transmission electron microscopy (TEM), fluorescence spectroscopy and FT-IR spectroscopy. The results revealed an easy and viable strategy for obtaining stable aqueous dispersion of AgNPs with well controlled shape and size below 30 nm in diameter.     

多孔聚苯胺-稻壳基白炭黑复合物的制备及循环伏安特性

以工业生产废弃的稻壳灰为原料,采用化学沉淀法制备了大孔径多孔稻壳基白炭黑,并在多孔白炭黑(RHSi)分散体系中,采用原位聚合法制备了聚苯胺(PAn)-稻壳基白炭黑复合物.采用热重分析、傅里叶红外光谱、透射电镜、低温氮吸附法和循环伏安法研究了复合物的结构及电化学性能.结果表明:聚苯胺-稻壳基白炭黑复合物具有多孔聚集体结构.当m_(PAn)/m_(RHSi)＝0.434时,复合物的比表面积为42.1 m~2/g,最可几孔径约为22 nm,适宜负载生物大分子,且在酸性及中性溶液中具有良好的电化学可逆性.     

Thermal stability of functionalized carbon nanotubes studied by in-situ transmission electron microscopy

The thermal stability of funtionalized carbon nanotubes (CNTs) has been studied experimentally by direct in-situ observations using a heating stage in a transmission electron microscope, from room temperature (RT) to about 1000 °C. It was found that the thermal stability of the functionalized CNTs was significantly reduced during the in-situ heating process. Their average diameter dramatically expanded from RT to about 500 °C, and then tended to be stable until about 1000 °C. The X-ray energy dispersive spectroscopy analysis suggested that the diameter expansion was associated with coalescence of the carbon structure instead of deposition with additional foreign elements during the heating process.     

铅纳米微粒用作油性润滑的摩擦学性能研究

The solution dispersion method has been successfully used to prepare Pb nanoparticles in a paraffin oilpolyglycol mixed solution by directly dispersing melted Pb granules. In this solution system,paraffin oil was used as reacting media and polyglycol served as an antioxidant to protect Pb nanoparticles from oxidizing. The size and structure of the prepared Pb nanoparticles were characterized by means of the transmission electron microscopy （TEM）and powder X-ray diffraction（XRD）. Their tribological behavior was evaluated with a four-ball tester. The TEM and XRD investigations reveal that the prepared Pb nanoparticles,with the average particle diameter of 70 nm,appear to be of close spherical shape and possess the same crystal structure as the bulk Pb. The tribological results show that the Pb nanoparticles as an oil additive exhibit good friction-reduction and antiwear properties at different additive concentration and applied load. Meanwhile,they can also strikingly improve the load-carrying capacity of the base oil. The rubbed surface was also investigated by the scanning electron microscope（SEM）and energy dispersive spectroscopy（EDS）. However,there was not presence of Pb element on the worn surfaces,which indicated that no chemical reaction occurred between the Pb nanoparticles and the rubbing surfaces. In addition,the tribological mechanism of the formation of the sliding-bearing system was also proposed.