Formation mechanisms of sub-micron pharmaceutical composite particles derived from far-and near-field Raman microscopy

Surface enhanced Raman spectroscopy(SERS) and confocal Raman microscopy are applied to investigate the structure and the molecular arrangement of sub-micron furosemide and polyvinylpyrrolidone(furosemide/PVP) particles produced by spray flash evaporation(SFE). Morphology, size and crystallinity of furosemide/PVP particles are analyzed by scanning electron microscopy(SEM) and X-ray powder diffraction(XRPD). Far-field Raman spectra and confocal far-field Raman maps of furosemide/PVP particles are interpreted based on the far-field Raman spectra of pure furosemide and PVP precursors.Confocal far-field Raman microscopy shows that furosemide/PVP particles feature an intermixture of furosemide and PVP molecules at the sub-micron scale. SERS and surface-enhanced confocal Raman microscopy(SECo RM) are performed on furosemide, PVP and furosemide/PVP composite particles sputtered with silver(40 nm). SERS and SECo RM maps reveal that furosemide/PVP particle surfaces mainly consist of PVP molecules. The combination of surface and bulk sensitive analyses reveal that furosemide/PVP sub-micron particles are formed by the agglomeration of primary furosemide nanocrystals embedded in a thin PVP matrix. Interestingly, both far-field Raman microscopy and SECo RM provide molecular information on a statistically-relevant amount of sub-micron particles in a single microscopic map;this combination is thus an effective and time-saving tool for investigating organic sub-micron composites.

Microstructure and Strength of Laser Welds of Sub-micron Particulate-reinforced Aluminum Matrix Composite Al_2O_(3p)/6061Al

The microstructure of laser welds of sub-micron particulate-reinforced aluminum matrix composite Al_2O_(3p)/6061Al and the weldability of the material were studied. Experimental results indicated that because of the huge specific surface area of the reinforcement, the interfacial reaction between the matrix and the reinforcement was re- strained intenslvely at elevated temperature and pulsed laser beam. The main factor affecting the weldability of the com- posite was the reinforcement segregation in the weld resulting from the push of the liquid/solid interface during the soli- dification of the molten pool. The laser pulse frequency directly affected the reinforcement segregation and the reinfor- cement distribution in the weld, so that the weldability of the composite could be improved by increasing the laser pulse frequency. On the basis of this, a satisfactory welded joint of sub-micron paniculate-reinforced aluminum matrix com- posite Al_2O_(3p)/6061Al was obtained by using appopriate welding parameters.

Effect of flow field distribution on the synthesis of sub-micron ZSM-5 molecular sieve in a quasi-solid system

Scale-up synthesis of sub-micron ZSM-5 molecular sieve in a quasi-solid system was investigated. Compared with traditional hydrothermal synthesis, the synthesis in a quasi-solid system has the advantages of high yield, short crystallization time, low energy consumption as well as low emissions. However, the high solid content in the quasi-solid system can cause the mass and heat transfer problems and make scalable production difficult. In order to solve the problem, we have developed a method for the optimization of the mass and heat transfer. By this method one can vary the flow field in the reactor by changing the stirrer speed. Scale-up synthesis of the sub-micron ZSM-5 molecular sieve in a quasi-solid system was carried out in a 5 L reactor with double propeller-type agitators. The process was investigated with product characterization using X-ray diffraction （XRD） and scanning electron microscopy （SEM） and the flow field information was collected using laser Doppler velocimetry （LDV）. The results showed that the flow field patterns can be tuned by using different stirrer speeds, the morphology and size of assynthesized of ZSM-5 can be effectively controlled.

A novel solution-based self-assembly approach to preparing ultralong titanyl phthalocyanine sub-micron wires

Ultralong titanyl phthalocyanine （TiOPc） sub-micron wires have been synthesized by a novel solution-based self- assembly method. By using different solvents, changing the mass concentration and the solvent vapor pressure, the length and the shape of the wires can be adjusted. The mixed-phase properties of the TiOPc sub-micron wires were investigated by the ultraviolet-visible （UV-vis） absorption spectrum and X-ray diffraction. Organic transistors based on these wires were studied, which show the typical p-channel characteristics.

Pattern imprinting in deep sub-micron static random access memories induced by total dose irradiation

Pattem imprinting in deep sub-micron static random access memories （SRAMs） during total dose irradiation is inves- tigated in detail. As the dose accumulates, the data pattern of memory cells loading during irradiation is gradually imprinted on their background data pattern. We build a relationship between the memory cell＇s static noise margin （SNM） and the background data, and study the influence of irradiation on the probability density function of ASNM, which is the difference between two data sides＇ SNMs, to discuss the reason for pattern imprinting. Finally, we demonstrate that, for micron and deep sub-micron devices, the mechanism of pattern imprinting is the bias-dependent threshold shift of the transistor, but for a deep sub-micron device the shift results from charge trapping in the shallow trench isolation （STI） oxide rather than from the gate oxide of the micron-device.

STUDY ON THE RELATION BETWEEN STRUCTURE AND HOT CARRIER EFFECT IMMUNITY FOR DEEP SUB-MICRON GROOVED GATE NMOSFET's

Grooved gate structure Metal-Oxide-Semiconductor (MOS) device is consideredas the most promising candidate used in deep and super-deep sub-micron region, for it cansuppress hot carrier effect and short channel effect deeply. Based on the hydrodynamic energytransport model, using two-dimensional device simulator Medici, the relation between structureparameters and hot carrier effect immunity for deep-sub-micron N-channel MOSFET's is studiedand compared with that of counterpart conventional planar device in this paper. The examinedstructure parameters include negative junction depth, concave corner and effective channel length.Simulation results show that grooved gate device can suppress hot carrier effect deeply even indeep sub-micron region. The studies also indicate that hot carrier effect is strongly influencedby the concave corner and channel length for grooved gate device. With the increase of concavecorner, the hot carrier effect in grooved gate MOSFET decreases sharply, and with the reducingof effective channel length, the hot carrier effect becomes large.

Sub-micron-structure machining on silicon by femtosecond laser

Sub-micron-structure machining on silicon substrate was studied by direct writing system of femtosecond laser with the central wavelength of 800 nm, pulse duration of 120 fs and repetition rate of 1 kHz. Three kinds of experiments were conducted: 1) the effect of photoresist on silicon; 2) machinability of different orientations of silicon; and 3) the size of micro-structure and the cross-section shape. Photoresist SU8 was coated onto silicon substrates in thicknesses of 100 μm. SU8 remained on the silicon substrate while the silicon under the machined SU8 was removed after laser machining. Orientations of (100), (110), and (111) silicon substrates were machined with the laser power of 60 μW and the scanning speed of 3 mm/min. Spike morphologies were observed on all three orientations of silicon substrates without obvious directional difference of these spikes on different silicon substrates. In addition, the ablation threshold energies were also similar. In the consideration of ablation energy, one numerical model of the machining parameters has been proposed to simulate the cross-section of the micro-structure. The predicted shape by simulation can fit the profile of the cross-section shape well.

Effect of sintering on microstructures and properties of sub-micron Ti(C,N)-based cermets

The influence of different sintering processes, including vacuum sintering, vacuum sintering followed by HIP and sintering-HIP, on the microstructure and properties of sub-micron Ti(C,N) cermets with various binder contents was studied. Image analysis based on back-scattered electrons image observations was used to determine the morphologic and structural characteristics. Transverse rupture strength(TRS), hardness, fracture toughness were measured and TRS data were treated by Weibull statistics further. It is shown that a very significant improvement in TRS can be obtained by HIP or sintering-HIP treatment for the alloys with lower and middle binder content at the controlled cooling rate, but the effect is not obvious for the alloys with higher binder content. HIP is also helpful for improving the hardness of sub-micron Ti(C,N) cermets, however, but can lower the fracture toughness. The variation of these properties was interpreted in terms of the difference in morphologic and structural characteristics.

Impact-disrupted gunshot residue：A sub-micron analysis using a novel collection protocol

The analysis of gunshot residue(GSR) has played an integral role within the legal system in relation to shooting cases. With a characteristic elemental composition of lead, antimony, barium, and a typically discriminative spheroidal morphology, the presence and distribution of GSR can aid in firearm investigations. In this experiment, three shots of low velocity rim-fire ammunition were fired over polished silicon collection substrates placed at six intervals over a 100 cm range. The samples were analysed using a Field Emission Gun Scanning Electron Microscope(FEG-SEM) in conjunction with an X-flash Energy Dispersive X-ray(EDX) detector, allowing for GSR particle analyses of composition and structure at the sub-micron level. The results of this experiment indicate that although classic spheroidal particles are present consistently throughout the entire range of samples their sizes vary significantly, and at certain distances from the firearm particles with an irregular morphology were discerned, forming "impactdisrupted" GSR particles, henceforth colloquially referred to as "splats". Upon further analysis, trends with regards to the formation of these splat particles were distinguished. An increase in splat frequency was observed starting at 10 cm from the firearm, with 147 mm^(-2) splat density, reaching a maximal flux at 40 cm(451 mm^(-2)), followed by a gradual decrease to the maximum range sampled. Moreover, the structural morphology of the splats changes throughout the sampling range. At the distances closest to the firearm, molten-looking particles were formed, demonstrating the metallic residues were in a liquid state when their flight path was disrupted. However, at increased distances-primarily where the discharge plume was at maximum dispersion and moving away from the firearm, the residues have had time to cool in-fight resulting in semi-congealed and solid particles that subsequently disrupted upon impact, forming more structured as well as disaggregated splats. The relative compositions of the characteristic elements that are present in GSR also change in the different splat morphologies sampled,which may contribute to the particles' physical structures. Two distinct populations of splats were also observed: circular and elongated, which suggest the residues hit the substrate at different angles. The difference in the splat impact angle can be ascribed to the position of the residues within the firearm discharge plume; particles get caught up in the vortex that is created by the discharge gases behind the projectile as it leaves the barrel, thereby affecting their directionality and flight time. This reasoning could also justify the existence of both spheroidal and splat particles at certain distances. The novel sampling and analytical techniques used in this experiment have provided previously unknown information in relation to GSR structure and formation which could have greater implications to its current analysis amongst laboratories and law enforcement agencies worldwide.

Effects of Mg content on aging behavior of sub-micron Al_2O_(3p)/Al-Cu-Mg composites

30%Al2O3p/Al-Cu-2.0Mg composite and Al2O3p/Al-Cu-2.5Mg composite with 0.3μm-Al2O3 particles were fabricated. Age-hardening behaviors of two composites and the related matrix alloys were studied by means of Brinell-hardness measurement, DSC and TEM. The results show that the hardness of the composite is improved obviously because of the addition of sub-micron Al2O3 particles. But the hardness increment of Al2O3p/Al composite after aging is lower than that of the related matrix alloy. Moreover, the formation of GP region is suppressed by the addition of sub-micron Al2O3 particles, which broadens the exothermic peak of S' phase. The increment of Mg content has a different influence on accelerating the aging processes of aluminum alloys and the composites, and the hardness also increases.

Photoelectrochemical performance of a sub-micron structured film with poly(3-methylthiophene) (P3MT)-modified CdTe/ZnO shell-core sub-micron tube arrays

A sub-micron structured film with a poly(3-methylthiophene) (P3MT)-modified CdTe/ZnO shell-core sub-micron tube array has been prepared by a series of electrodeposition processes, and a semiconductor-sensitized solar cell based on this structure was also fabricated. Vertically oriented ZnO sub-micron tubes were obtained on an indium tin oxide (ITO) substrate, and then CdTe nanocrystals and a thin P3MT layer were electrodeposited sequentially onto the walls of the ZnO sub-micron tubes. A suitable thickness of CdTe and P3MT could improve the photovoltaic properties of the solar cell, which was attributed to the enhancement in the light absorption and the decrease in the recombination of photogenerated carriers. In addition, a p–n heterojunction formed between the interface of CdTe and P3MT played an important part in the efficient separation and fast transport of photogenerated carriers in the sub-micron structure. A power conversion efficiency of 1.20% was obtained with this type of solar cell.

Surface plasmon interference pattern on the surface of a silver-clad planar waveguide as a sub-micron lithography tool

A new sub-micron photolithography tool has been realized by utilizing the interference of surface plasmon waves(SPWs) on the near surface of a silver(Ag)-clad ultraviolet(UV) planar waveguide.A laser beam with a wavelength of 325 nm was incident into the waveguide core,and suffered a series of total internal reflections on the interfaces between the waveguide core and the cladding layers.The incident light and the reflected light induced two beams of SPWs traveling in contrary directions,which interfered with each other and formed a standing wave as a sub-micron photolithography tool.A near-field scanning optical microscope(NSOM) was employed to measure the intensity distribution of the stationary wave field of the near surface of the Ag layer of the waveguide,anastomosed with theoretical values acquired by use of finite difference time domain(FDTD) simulations.And with this sub-micron photolithography tool a SMG with a period of 79.3 nm,in good agreement with the theoretical value of 80.1 nm,was inscribed on the surface of a self-processing hybrid SiO2/ZrO2 solgel film for the first time.

Strontium-substituted sub-micron bioactive glasses inhibit ostoclastogenesis through suppression of RANKL-induced signaling pathway

Strontium-substituted bioactive glass(Sr-BG)has shown superior performance in bone regeneration.Sr-BG-induced osteogenesis has been extensively studied;however,Sr-BG-mediated osteoclastogenesis and the underlying molecular mechanism remain unclear.It is recognized that the balance of osteogenesis and osteoclastogenesis is closely related to bone repair,and the receptor activators of nuclear factor kappaB ligand(RANKL)signaling pathway plays a key role of in the regulation of osteoclastogenesis.Herein,we studied the potential impact and underling mechanism of strontium-substituted sub-micron bioactive glass(Sr-SBG)on RANKL-induced osteoclast activation and differentiation in vitro.As expected,Sr-SBG inhibited RANKL-mediated osteoclastogenesis significantly with the experimental performance of decreased mature osteoclasts formation and downregulation of osteoclastogenesis-related gene expression.Furthermore,it was found that Sr-SBG might suppress osteoclastogenesis by the combined effect of strontium and silicon released through inhibition of RANKL-induced activation of p38 and NF-κB pathway.These results elaborated the effect of Sr-SBG-based materials on osteoclastogenesis through RANKLinduced downstream pathway and might represent a significant guidance for designing better bone repair materials.

Magnéli相亚氧化钛陶瓷的制备及其应用研究进展

Magnéli相亚氧化钛是一系列非化学计量比氧化钛的统称,主要包括Ti_(4)O_(7)、Ti_(5)O_(9)、Ti_(6)O_(11)和Ti_(8)O_(15)等相,其中以Ti_(4)O_(7)的导电性最好,其理论电导率可达1500 S·cm^(-1),约为石墨的二倍。此外,Magnéli相亚氧化钛在强酸、强碱环境中均表现出极强的耐蚀性能,并且能够在水溶液中保持3.0 V以上的稳定电位窗口。Magnéli相亚氧化钛优异的性能使其在化学电源如铅蓄电池、液流电池、锂硫电池、可再生燃料电池,电解水的催化剂载体,热电及光电材料,光催化制氢以及电催化氧化降解有机污染物等领域中展现出良好的应用前景。目前,科研人员已经开发出一系列制备亚氧化钛的方法。但是在高纯度、单相、纳米或亚微米尺度亚氧化钛粉体,大尺寸的一体式亚氧化钛电极和金属基亚氧化钛涂层电极的规模化生产和应用中依然存在许多问题,限制了亚氧化钛系列产品在上述领域中的广泛应用。基于Magnéli相亚氧化钛陶瓷的固有特性,重点介绍了亚氧化钛粉体、一体式电极和涂层电极的制备方法及应用现状,同时对亚氧化钛相关材料的应用前景进行了简要概述,为科研院所及相关企业提供了参考依据、研究思路和解决办法。

差动临界角法高精度动态检焦技术研究

基于临界角检焦技术具有光能量损耗小、组装相对简单、调试相对容易、系统分辨率高等特点,当引入差动信号处理技术,可放大提取的检焦信号,提升检测灵敏度和提高检焦曲线的光滑度,同时可实现更大的焦面检测范围,减少由于基底本身存在不平整影响到的检焦误差。本论文首先从差动临界角法检焦技术的基本原理出发,通过Fresnel公式和牛顿公式得到离焦量与离焦信号的关系。其次搭建差动临界角法检焦验证系统,利用四象限光电探测器采集单个临界角棱镜的离焦信号,并对两个垂直放置的四象限光电探测器接收到的离焦信号进行差动计算,以获得差动K值大小与离焦量z之间的关系。实验结果表明:采用波长532 nm的激光,数值孔径0.3的投影物镜时,检焦线性范围可达22μm;采用数值孔径0.45的投影物镜时,检焦线性范围可达14μm,差动临界角检焦法分辨率可达25 nm。

Low-Temperature and Surfactant-Free Synthesis of Mesoporous TiO_2 Sub-Micron Spheres for Efficient Dye-Sensitized Solar Cells

Dye-sensitized solar cells （DSSCs） are one of the most promising next-generation solar cells due to their advantages over other counterparts. The photoanode of DSSCs has a great effect on the photovoltaic per- formance. Traditional photoanode includes a bottom nanoparticle layer and an upper scattering layer for better light capture in longer wavelength. Mesoporous nanostructures with size comparable to the wavelength of visible light are considered to be excellent light scattering centers by providing extra places for dye loading. Developing a green synthetic method is of great importance. Herein we report a facile and surfactant-free synthesis of mesoporous futile TiO2 submicrometer-sized spheres at temperature as low as 70 ℃. DSSCs based on photoanodes with an upper scattering layer composed of as-obtained mesoporous spheres on nanoparticle dense layer demonstrate an 18.0% improvement of power conver- sion efficiency. This simple approach may offer an energy-efficient and environmentally friendly alternative for DSSCs fabrication.

激光扫描共聚焦显微分析技术表征页岩亚微米级孔隙中的含油性——以准噶尔盆地芦草沟组页岩为例

亚微米级孔隙及其含油性是页岩油勘探开发所需的重要信息。为应用激光扫描共聚焦显微镜有效观测亚微米级孔隙的含油性,修改了激光扫描共聚焦显微镜主分光器和检测器的前置滤光片配置,使之能较好地进行反射光和荧光联合扫描,消除矿物所发荧光的干扰,实现了亚微米级孔隙及其含油性的精确观测。该方法在准噶尔盆地吉木萨尔凹陷芦草沟组页岩油研究中进行了应用,发现了大量的亚微米级含油孔隙;页岩油多呈不规则形状、斑块状和星点状。这套页岩的有机质成熟度Ro为0.6%~1.1%,平均约为0.9%,但轻、重质组分的分布具有显著的非均一性,不完全受成熟度控制。在有些部位,轻质组分含量及其与重质组分的比值均较高,但在成熟度相近甚至稍高的邻近部位,却存在以重质组分为主的情况。页岩层系内部的油气运移也是一个重要的控制因素。页岩中的轻质和重质组分的观测与分布规律研究,对于页岩油勘探开发十分重要,激光扫描共聚焦显微新技术可成为重要的观测手段。

亚微米尺寸、高结晶度石墨烯增强间位芳纶纤维力学性能

芳纶纤维具有优异的综合性能,在各种工业应用中备受青睐。其中,间位芳纶纤维,也称聚间苯二甲酰间苯二胺(PMIA)纤维,兼具阻燃、耐高温、电隔离和高化学稳定性。其织物材料广泛应用于防火、防热等行业。然而,由于分子链中酰胺和苯环键之间缺乏偶联,内旋能低,导致PMIA纤维链段柔软、结晶度低,展现出较低的机械强度。因此,迫切需要改善这些纤维的机械特性,以扩大其应用范围。纳米复合材料的可以赋予基体材料许多独特特性。其中,石墨烯纳米复合材料占据突出地位。石墨烯面内的苯环结构使其可以有效增强芳香族和脂肪族类聚合物材料。此外,与大尺寸的石墨烯相比,小尺寸的石墨烯在聚合物基体中表现出更好的分散性,可在纤维类聚合物材料中展现出更明显的增强效应。因此,使用高品质、小尺寸的石墨烯是增强聚合物基体的有效手段。我们的研究展示了亚微米尺寸的石墨烯如何改善PMIA纤维的结构完整性和增加机械强度。结果显示,与未改性的PMIA纤维相比,拉伸强度显著提高46%。鉴于该方法的有效性,可以采用此种“小尺寸、高品质”的石墨烯来开发更强韧且更具商用价值的碳基纳米复合纤维。

鄂尔多斯盆地合水地区三叠系长7段页岩油储层特征及主控因素

鄂尔多斯盆地合水地区是长庆油田页岩油勘探开发的重点区块。根据铸体薄片、物性分析、扫描电镜、高压压汞及核磁共振等测试分析结果,对鄂尔多斯盆地合水地区三叠系长7段页岩油储层特征及其主控因素进行了研究。研究结果表明:(1)合水地区长7段页岩油储层主要为一套灰黑—黑色细—粉砂岩,以岩屑长石砂岩为主,填隙物的体积分数平均为16.71%。岩石物性较差,平均孔隙度为8.15%,平均渗透率为0.102 mD,为超低孔—特低孔、超低渗型储层。(2)研究区孔隙类型以长石溶孔和残余粒间孔为主,以亚微米孔(直径为0.1~1.0μm)含量最多,占总孔隙数量的75.56%,纳米孔隙(直径小于0.1μm)数量次之,占总孔隙数量的17.94%。孔喉类型较复杂,溶蚀成因的管束状喉道及压实成因的片状、弯片状喉道为储层主要的喉道类型。(3)沉积作用、成岩作用及构造作用共同控制了研究区长7段页岩油储层的质量和分布。沉积作用为储层提供了物质基础,储层主要形成于深水重力流沉积环境,可分为砂质碎屑流砂体和浊流砂体等2种类型。中等—强压实强度的压实作用和胶结作用降低了储层物性,溶蚀作用对于改善储层物性具有一定的积极作用,构造作用形成的裂缝提高了储层的渗流能力,并对后期的储层压裂改造具有重要意义。

亚微米级SiC颗粒增强铝基复合材料的拉伸性能与强化机制

用粉末冶金法制备了亚微米SiC颗粒增强纯铝基复合材料(Al MMC),对该材料的微观结构和拉伸性能进行了研究.结果表明,15％SiCp(150 nm)/Al MMC的拉伸强度和屈服强度分别为342.3和272.4 MPa,比纯铝分别提高了89.0％和117.9％,其延伸率为6.3％.拉伸断口观察表明,SiCp/Al MMC断裂机制为界面脱粘和SiC团聚体的脆断.该复合材料具有高强度的原因是基体的微观结构发生了变化,用位错密度强化和弥散强化机制对Al MMC的强化作用进行了评估,预测结果与实验值符合得很好.