SA/PU共混水凝胶微球的制备及性能研究

得到性能良好的SA/PU共混微球以用于药物缓控释;方法:利用预聚-扩链-中和-分散法合成阴离子型PU水溶液;将SA水溶液与PU水溶液按质量比为1∶1,1∶2,1∶3,1∶4,1∶5混合,用滴制法制备共混微球;测定了微球的凝胶化、圆整性及溶胀性能.结果表明:用TDI与PEG-6000和PEG-4000反应才能制备出PU水溶液,而只有水溶液才能和海藻酸钠水溶液混合完全得到理想的共混溶液;SA/PU共混微球28h后凝胶化完全,SA微球48h后可凝胶化完全.PEG-6000合成的PU与海藻酸钠共混得到的微球圆整性要好于PEG-4000合成的PU与海藻酸钠共混得到的微球.且随着复合微球中PU的含量增大,微球的圆整性变好;SA/PU复合微球在蒸馏水(pH7)和盐酸(pH1)中均不溶胀,在磷酸缓冲溶液(pH6.86)中快速溶胀,在4～5h后开始崩解.结论:SA/PU复合微球在胃液中保持原状,在肠液中溶胀,可作为药物的缓释载体.     

PDMS-PU/ST复合微球的制备及其性能研究

采用预聚-扩链-中和-分散法合成了端羟基聚二甲基硅氧烷(DHPDMS)改性聚氨酯(PU)水溶液,再将PU水溶液和淀粉(ST)溶液按照不同的质量比进行复合,采用凝聚相分离法制备出PDMS-PU/ST复合微球;考察了PEG分子量、n(-OH)/n(-NCO)、DHPDMS的质量分数,淀粉质量分数对PDMS-PU/ST复合微球的球形、力学强度和降解率的影响。并通过扫描电子显微镜(SEM)和傅立叶变换红外光谱(FT-IR)对微球的表面形态和化学结构进行表征,SEM照片显示复合微球表面光滑且内部有很多致密的管状孔隙,适合用作药物释放载体材料;FT-IR表明硅氧键引入到PU中,且PU和ST之间通过氢键复合。     

聚氨酯/淀粉复合微球的制备及药物释放性能研究

采用预聚-扩链-中和-分散法合成聚氨酯(PU)水溶液,将PU与淀粉(ST)溶液按照不同质量比进行复合,采用凝聚相分离法制备PU/ST复合微球;用傅立叶变换红外光谱(FTIR)、扫描电子显微镜(SEM)对微球进行表征,并以盐酸四环素为模型药物制备载药复合微球,初步研究了载药PU/ST复合微球的药物释放性能.结果表明,微球...     

超声改性淀粉/PVA/SA复合微球的制备及性能研究

用凝聚相分离法制备超声改性淀粉/聚乙烯醇/海藻酸钠(ST/PVA/SA)复合微球,考察了ST、PVA、SA和CaCl2的质量分数、干燥方式对微球形态性能的影响。通过红外光谱对微球进行了结构表征,并测定了微球的含水率、溶胀率、降解率。研究了载药微球在体外的药物释放规律。结果表明,微球的最佳合成条件是ST、PVA、SA和CaCl2的质量分数分别为4%、8%、4%和5%,此条件下微球具有良好的pH敏感性和药物缓释效果。     

超临界流体技术制备吗啡/聚乳酸-聚乙二醇共聚物缓释微球

以L-聚乳酸-聚乙二醇三嵌段共聚物(PLLA-PEG-PLLA)为载体材料,通过超临界流体强制溶液分散技术制备吗啡/聚乳酸-聚乙二醇共聚物(MF/PLLA-PEG-PLLA)的复合微球,考察了PEG分子量的变化对微球性能的影响。通过表面形貌,粒径及粒径分布,载药量,包封率及释放性能来表征复合微球的各项性能;利用气相色谱法测定二氯甲烷和甲醇的残留量;通过溶血实验来评价复合微球的血液相容性。实验表明,所制备的复合微球呈球形或类球形形貌,平均粒径在1.99～6.20μm之间,载药量达到17.92%,包封率最高可至69.57%,复合微球的药物释放呈先突释后缓释的释药模式;二氯甲烷和甲醇的残留量分别为0.0076%和0.0016%;微球溶血率<1%,远小于国家标准5%,证明复合微球具有较好的血液相容性。     

纳米羟基磷灰石/聚氨酯载药微球的制备及性能

通过乳液聚合法制备了负载阿莫西林的纳米羟基磷灰石/聚氨酯(n-HA/PU)载药微球,通过正交设计实验对其制备工艺进行了优化,采用红外光谱、热重分析、扫描电镜等分析了微球的结构和性能,对其体外药物缓释过程进行探讨。研究结果表明,复合微球粒径大小与固含量、聚乙烯吡咯烷酮(PVP)含量、搅拌速度等有关,所制备的微球平均粒径为0.8~1.2mm;载药微球的优化制备工艺条件为:原料配比-NCO∶-OH=2∶1,预聚时间180min,预聚温度80℃,nHA含量3%,固含量7%,搅拌速度600r/min,PVP用量3%,所制备微球的载药量为6.58%,包封率为86.86%。体外缓释结果表明,载药微球的释药行为符合Higuchi动力学,半衰期(t1/2)为22.29h,具有良好的药物缓释作用。     

载当归羧甲基纤维素-海藻酸钠复合微球的制备和表征

采用W/O乳液法,在不同条件下,用Ca2+交联和戊二醛交联制备了羧甲基纤维素(CMC)-海藻酸钠(SA)复合微球。SEM结果显示,当m(CMC)∶m(SA)=1∶5、温度为60℃时,球形较好。采用FT-IR分析了复合微球的化学结构。对复合微球的溶胀率、药物包封率进行表征,结果显示复合微球在磷酸缓冲液中的溶胀率达到700%,且溶胀速度快。该复合微球对当归(ASD)具有较好的缓释作用。     

纳米Fe3O4@茶渣/海藻酸钙磁性复合材料制备及其对亚甲基蓝的吸附性能与吸附机制

采用离子共沉淀技术在茶渣(Tea waste, TW)表面沉积纳米Fe₃O₄粒子(TW@nano-Fe₃O₄),用溶胶凝胶法制备茶渣@纳米Fe₃O₄/海藻酸钙(TW@nano-Fe₃O₄/CA)磁性复合微球,通过SEM、XPS、XRD、振动样品磁强计(VSM)及万能试验机对材料结构和性能进行了表征与测试,并研究了其对水溶液中亚甲基蓝(Methylene blue, MB)的吸附性能与机制。结果表明,TW@nano-Fe₃O₄/CA复合微球磁性响应明显,粒径为1.2~1.7 mm。微球表面粗糙、褶皱,内部为疏松多孔道结构。随TW@nano-Fe₃O₄含量增加,微球粒径增加,磁响应增强,但对MB的吸附量缓慢下降;TW@nano-Fe₃O₄/CA微球对MB的吸附动力学数据与准二级动力学方程拟合较好,等温吸附过程符合Langmuir模型,对MB的吸附过程是自发性和熵减小的放热过程。在303 K下,质量配比为TW@nano-Fe₃O₄∶CA=4∶1的复合微球对MB的Langmuir最大吸附量为272.5 mg·g^-1,比TW提高86.7%,并具有良好的再生与循环使用性能。     

PU/CS复合微球的制备及影响因素

采用预聚-扩链-中和-分散法合成PU水溶液,采用凝聚相分离法制备PU微球;考察PU水溶液合成时的预聚温度、预聚时间、搅拌速度,确定合成PU水溶液的最佳条件;考察PEG分子量、-NCO/-OH比值、PCL的引入、CaCl2浓度、CS浓度及溶解度等因素以确定PU/CS微球成球的最佳条件;对载药复合微球进行药物释放研究,观察微球的降解规律。     

Fe3O4/SiO2/CMCH/CdTe荧光磁性微球的合成与表征

利用St ber法和交联法制备出具有荧光和磁性功能的Fe3O4/SiO2/CMCH/CdTe微球,并对其性能和应用效果进行了分析讨论.首先以正硅酸四乙酯为前躯体,Fe2＋和Fe3＋物质的量的比为1∶2,利用超临界干燥法制备出了Fe3O4/SiO2复合微球;并通过透射电镜对其进行观察,Fe3O4颗粒粒径为10 nm,SiO2层厚度为5 nm;其次羧甲基化的壳聚糖（CMCH）被嫁接在Fe3O4/SiO2表面上;然后利用水热法制备出CdTe荧光颗粒,通过壳聚糖与CdTe之间的静电吸引作用,CdTe被吸附在壳聚糖表面;最后利用戊二醛对壳聚糖的选择性交联作用制备出粒径在200 nm以内,饱和磁化强度为22.16 A.m2/kg,且具有良好荧光性能的Fe3O4/SiO2/CMCH/CdTe微球.荧光光谱分析表明最大发射波长从519 nm红移到528 nm,也证实了荧光颗粒CdTe成功吸附在Fe3O4/SiO2/CMCH表面.在动物实验中,该复合微球也显示出良好的荧光性、磁性及稳定性.     

Percolation and the resistive transition of the critical temperature Tc of Nb3Sn

The relationship between the distribution of the critical temperature, the percolation function, and the resistive transition of the critical temperature is explored for polycrystalline Nb₃Sn. In the neighborhood of the critical temperature, Nb₃Sn is assumed to be a random mixture of superconducting and normal grains. Percolation concepts are applied to a study of the resistivity. A general analysis is made showing that the onset and shape of the resistive transition for composite conductors are determined by the percolation function and the distribution of the critical temperature. An approximate form of the percolation function is determined based on a linear FEM analysis. Example resistive transitions are calculated for an assumed normal distribution of the critical temperature. An argument is presented that relates grain orientation and strain dependence in Nb₃Sn. It is noted that a dependence of the distribution of T_c with strain, in addition to the usual shift in T_c with strain, would be the result of a strain dependence that is a function of grain orientation. The analysis shows the extent to which the slope of the resistive transition is a measure of the distribution of the critical temperature, and therefore a measure of the grain orientation strain sensitivity. Finally, a method is described to determine the percolation function experimentally.     

(La2/3Ca1/3)(Mn(3-x)/3)Fex/3)O3体系磁电阻行为的研究

通过系统地测量（La2/3Ca1/3）（Mn（3-x）／3Fex／3）O3（x＝0、0.1、0．2、0．3的体系样品的电阻率-温度关系以及一定温度下磁电阻率与磁场的关系,发现随x的变化其磁电阻率峰和电阻率峰均发生位移,磁电阻率峰值增大,并伴生磁电阻率峰展宽效应．作者认为由于Fe的替代,引起体系中Mn3 ／Mn4 比率及磁矩的变化,加之外场对磁有序结构的调制作用,从而影响了Mn3 －O－Mn4 的双交换作用,最终导致磁电阻行为发生变化．     

聚乙烯醇/磺化聚醚醚酮/对氨基二苯胺电活性复合膜的制备与性能

以聚乙烯醇(PVA)、磺化聚醚醚酮(SPEEK)和对氨基二苯胺(p-ADA)为原料,通过水溶液流延成膜法制备了PVA/SPEEK/p-ADA电活性复合膜。借助核磁共振谱(1 H-NMR)、红外光谱(FTIR)和X射线光电子能谱(XPS)分别对SPEEK和复合膜的化学结构进行了表征。采用万能材料试验机和电化学综合站分别对复合膜的力学性能和电性能进行分析测试。结果表明,当PVA含量为60%(质量分数)、SPEEK含量为35%(质量分数)、p-ADA含量为5%(质量分数)时复合膜的力学性能最佳,拉伸强度和弹性模量分别达到64 MPa和2 538 MPa,较纯PVA分别提高了52%和122%。电压窗口为-0.8~0.8 V时,PVA-60%/SPEEK-35%/p-ADA-5%复合膜具有明显的电活性,并且该电活性复合膜在外界酸碱环境发生改变时具有变色性。     

Chitosan-collagen/organomontmorillonite scaffold for bone tissue engineering

A novel composite scaffold based on chitosan-collagen/organomontmo-rillonite (CS-COL/OMMT) was prepared to improve swelling ratio, biodegradation ratio, biomineralization and mechanical properties for use in tissue engineering applications. In order to expend the basal spacing, montmorillonite (MMT) was modified with sodium dodecyl sulfate (SDS) and was characterized by XRD, TGA and FTIR. The results indicated that the anionic surfactants entered into interlayer of MMT and the basal spacing of MMT was expanded to 3.85 nm. The prepared composite scaffolds were characterized by FTIR, XRD and SEM. The swelling ratio, biodegradation ratio and mechanical properties of composite scaffolds were also studied. The results demonstrated that the scaffold decreased swelling ratio, degradation ratio and improved mechanical and biomineralization properties because of OMMT.     

Analytical and finite element investigations of shear/compression test fixtures

Insulation systems are critical components of the international thermonuclear experimental reactor (ITER). They must meet the super conducting magnets design requirements, including mechanical strength under combined shear and compressive stresses at cryogenic temperatures. Past cryogenic magnet systems often relied on woven glass/epoxy materials for insulation. An important point is to find a reliable shear/compression test method for these materials. The present work investigates a commonly used shear/compression setup and aims at measuring the reliability of the obtained test results. Therefore, the stress and failure analysis is performed analytically and numerically using the finite element method. The model is based on woven glass fiber reinforced materials which are subjected to combined shear and compressive stresses as well as to thermal loading, that results from cooling from 293 K to the test temperature of 77 K. A short analytical section shows the problems of common failure criteria which are used to describe the interaction of the shear and compression stresses. The numerical—finite element—section is based on three-dimensional linear elastic finite element models under thermo-mechanical loading. The locations of high stress gradients are investigated using an average stress criterion. Three different model geometries (15°, 45°, and 70°) are analyzed and finally compared with respect to their reliability.     

(La2/3Ca1/3)(Mn(3-x)/3)Fex/3)O3体系磁电阻行为的研究

通过系统地测量（La_2/3Ca_1/3）（Mn_{（3-x）／3}Fe_x／3）O₃（x＝0、0.1、0．2、0．3的体系样品的电阻率-温度关系以及一定温度下磁电阻率与磁场的关系,发现随x的变化其磁电阻率峰和电阻率峰均发生位移,磁电阻率峰值增大,并伴生磁电阻率峰展宽效应．作者认为由于Fe的替代,引起体系中Mn³⁺／Mn⁴⁺比率及磁矩的变化,加之外场对磁有序结构的调制作用,从而影响了Mn³⁺－O^－Mn⁴⁺的双交换作用,最终导致磁电阻行为发生变化．     

单分散SiO2/TiO2/SiO2多层复合微球的制备

采用一种以醇盐水解法为基本的生长硅溶胶的方法,制备了粒径为200nm的单分散二氧化硅球形颗粒,并将其作为核心,利用常温连续进料的钛酸丁酯水解的多步法,在二氧化硅核心外经多次包覆形成厚层二氧化钛;在正硅酸 酯的水解和陈化环境下,将上述TiO2/SiO2复合颗粒外再包覆一薄层二氧化硅,形成一种高折射率,可用于组装光子晶体的SiO2/TiO2/SiO2多层复合微球,对该复合微球用重力沉降法、透射电镜法（TEM）、X射线能谱分析法（EDS）进行了表征。其中,重力沉降法是一种将Stokes公式为基础的复合颗粒的粒径与沉降速度关系式所得的一系列数据进行拟合外延,来测定复合颗粒的粒径及包覆厚度的方法。     

Deposition and structural properties of RF magnetron-sputtered ZnO thin films on Pt/Ti/SiNx/Si substrate for FBAR device

This work investigates high-quality bottom electrode and piezoelectric film used in a thin-film bulk acoustic resonator (TFBAR) device. The titanium (Ti) seeding layer and platinum (Pt) bottom electrode were deposited on silicon substrates by DC sputtering using a dual-gun system. Zinc oxide (ZnO) was then deposited onto the Pt bottom electrode by RF magnetron sputtering. Field-emission scanning electron microscopy (SEM), atom force microscopy (AFM) and the four-point probe method showed that the Pt bottom electrode deposited on the Ti seeding layer exhibited favorable characteristics, such as a crystallite size of less than 10 nm, a surface roughness of 0.69 nm and a sheet resistance of 2.27 Ω/□. The ZnO thin film with a highly c-axis-preferred orientation (FWHM = 0.28°) and a roughness of 6.22 nm was investigated by X-ray diffraction (XRD) and AFM analysis, respectively. The bottom electrode with a low resistance and the highly crystalline ZnO thin film will contribute significantly to the favorable characteristics of the FBAR devices.     

LLDPE/HDPE/MMT纳米复合材料的制备及性能研究

以线性低密度聚乙烯(LLDPE)、高密度聚乙烯(HDPE)、有机改性的蒙脱土(MMT)为主要原料,选用乙烯-醋酸乙烯酯接枝马来酸酐(EVA-g-MAH)作为增容剂,采用熔融插层法制备了线性低密度聚乙烯/高密度聚乙烯/蒙脱土(LLDPE/HDPE/MMT)纳米复合材料。通过X射线衍射(XRD)分析蒙脱土在聚乙烯基体中的分散情况,并研究蒙脱土的含量对其在基体中分散效果的影响。TG实验结果表明,蒙脱土的加入使LLDPE/HDPE/MMT纳米复合材料的热稳定性得到很大的提高。由DSC曲线可以得出,加入蒙脱土的复合材料相比于纯聚合物,其熔点和热分解温度都有很大的提高,提高程度与蒙脱土的含量有关。     

High-temperature stability of α-Ta4AlC3

Cold-pressed α-Ta4AlC3 powders were annealed up to 1750 °C to test first-principles predictions of α-β phase-stability reversal at 1600 °C. Up to 1600 °C, the α-Ta₄AlC₃ samples were stable with no indications of any α-β transformation, as shown by the strong characteristic X-ray diffraction peaks of α-Ta₄AlC₃ and the zigzag stacking observed by transmission electron microscopy. These results show that, in this experimental situation, high temperature alone is not sufficient to cause the α-β transformation.