医用放射性核素的载体--磁性壳聚糖微球的制备

采用乳化交联法制备了可附载放射性核素的磁靶向药物载体--磁性壳聚糖微球,磁性微球中的纳米磁性Fe3O4粒子由FeSO4和FeCl3通过碱溶液的共沉淀法制备而得,借助SEM、IR及激光粒度仪等对微球的粒径、粒径分布和形貌进行了表征.结果表明在壳聚糖溶液质量分数为1.5%,Fe3O4与壳聚糖的质量比为1∶2,悬浮介质的搅拌速度为1 200r/min等条件下制得的磁性壳聚糖微球的粒径在(40±20)μm,且呈规则的球形,可满足放射性核素载体的基本要求.     

Fe_3O_4/TiO_2复合微粒电流变液的制备及其电流变性能

采用溶胶-凝胶法在经表面羟基活化处理的纳米Fe_3O_4颗粒表面包覆无定型态TiO_2,并用极性分子丙烯酰胺掺杂改性TiO_2包覆层,得到了Fe_3O_4/TiO_2核壳复合微粒,然后将其分散到甲基硅油中配制成复合微粒电流变液;研究了复合微粒的物相和微观形貌,以及电流变液的电流变性能。结果表明:TiO_2能够均匀紧密地包覆于纳米Fe_3O_4颗粒表面,并且包覆4次TiO_2,搅拌时间为4h,丙烯酰胺质量分数为25%时,制得的复合微粒电流变液的电流变性能最好,其剪切强度可达41.9kPa。     

三聚氰胺磁性分子印迹的合成与应用

以三聚氰胺为模板分子,甲基丙烯酸(MAA)为功能单体,乙二醇二甲基丙烯酸酯(EGDMA)为交联剂,以自制Fe_3O_4磁性纳米粒子为载体合成具有特异性识别三聚氰胺的磁性分子印迹聚合物微球。采用扫描电镜(SEM)扫描并分析聚合物微球的表面结构和颗粒大小。结果表明,三聚氰胺分子印迹聚合物与Fe_3O_4磁性纳米粒子成功偶联,结合高效液相色谱分析技术对该分子印迹聚合物的吸附性能及选择性进行分析,结果表明该分子印迹聚合物对三聚氰胺有特异性吸附,并建立了基于磁性分子印迹聚合物前处理技术的三聚氰胺高效液相色谱法,实现了磁性分子印迹技术在牛奶样品中三聚氰胺的检测。     

水热法合成COFe_2O_4纳米颗粒及其磁性能

采用水热法制备尖晶石CoFe_2O_4纳米颗粒,通过改变合成温度(140～200℃)和原料中钴的含量,借助X射线衍射仪、场发射扫描电子显微镜、透射电镜和振动磁强计等研究上述两个因素对合成颗粒结构、形貌及磁性能的影响,并从机制上加以解释。结果表明:水热法合成的CoFe_2O_4纳米颗粒平均粒径在30～40nm之间,提高原料中钴的含量有利于去除α-Fe_2O_3相;随合成温度的升高,该颗粒的饱和磁化强度持续增大,最高为59.694Am~2·kg~(-1),矫顽力先升后降,最高可达1273.28A·m~(-1)。     

Fe_3O_4/MnO_2磁性复合颗粒的制备及表征

以纳米Fe3O4颗粒为核,分别采用液相沉积法和溶胶一凝胶法两种方法将MnO2包覆在其上制备了Fe3O4/MnO2磁性复合颗粒,并借助XRD、TEM、FTIR和VSM等手段分别对纳米Fe3O4颗粒和两种复合颗粒进行表征.结果表明:采用液相沉积法进行包覆可生成以多个纳米Fe3O4颗粒为核、粒径约为200 nm的近球形Fe3O4/MnO2磁性复合颗粒,其饱和磁化强度为24.4 kA·m-1;采用溶胶-凝胶法进行包覆则生成以单个纳米Fe3O4颗粒为核、粒径约为50 nm的磁性复合颗粒,包覆层为絮状MnO2,其饱和磁化强度为16.5 kA·m-1.     

可见光响应TiO_2/Bi_4Ti_3O_(12)复合粉的制备及表征

以熔盐法制备的微米级片状TiO_2/Bi_4Ti_3O_(12)为基体,采用Ti(SO4)2水解结合后续热处理的方法制备了TiO2/TiO_2/Bi_4Ti_3O_(12)复合粉,研究了原料配比对复合粉晶体结构、形貌以及光催化降解脱色效果的影响。结果表明:该复合粉的形貌为微米级片状TiO_2/Bi_4Ti_3O_(12)表面分布着纳米级的TiO_2颗粒;当原料中铋、钛物质的量比低于1∶6时,复合粉对亚甲基蓝具有良好的吸附脱色效果,钛含量过多时会导致水解产物的团聚,降低复合粉的比表面积,使其脱色效果变差;当铋、钛物质的量比为1∶4时,复合粉的比表面积为13.444 m~2·g~(-1),可见光光照4h以内,对亚甲基蓝的脱色率达到85%,其光催化降解脱色速率高于TiO_2/Bi_4Ti_3O_(12)的。     

304不锈钢在不同温度硝酸熔盐中的腐蚀行为

采用腐蚀动力学方法,结合腐蚀表面形貌观察和微区成分分析,研究了304不锈钢在不同温度(400,450,500,565℃)60%NaNO_3+40%KNO_3(质量分数)熔盐中的腐蚀行为。结果表明:试验钢在该熔盐中的腐蚀速率随着温度升高而增大,在565℃下的腐蚀速率达到99.6×10~(-5 )mg·cm~(-2)·h~(-1);在400℃下试验钢表面只有极少量氧化腐蚀产物,在450℃和500℃下表面生成少量的Fe_2O_3,在565℃下表面形成以Fe_2O_3和(Fe,Cr)_3O_4为主的氧化腐蚀产物;随着温度升高,试验钢表面Fe_2O_3含量增加,氧化腐蚀程度加重。     

复合电沉积制备纳米钡铁氧体/钴镍合金磁性镀层

采用复合电沉积技术制备了纳米钡铁氧体(BaFe_(12)O_(19))/钴镍合金磁性镀层,研究了纳米钡铁氧铁颗粒对镀层表面形貌及磁性能的影响和镀液中BaFe_(12)O_(19)颗粒含量、电流密度、镀液温度、施镀时间等电沉积工艺参数对复合镀层矫顽力和最大磁能积的影响。结果表明:镀液中加入纳米钡铁氧体颗粒通过优化电沉积工艺可以制备出磁性复合镀层,可明显提高镀层的最大磁能积和矫顽力;以上四种工艺参数对镀层的最大磁能积和矫顽力有明显影响,但影响规律各不相同。     

镁合金表面的搅拌摩擦加工改性

采用搅拌摩擦加工技术通过加入Al_2O_3颗粒对AZ31镁舍金进行表面改性,研究了表面复合层的显微组织、力学性能及加工速度对显微组织的影响规律。结果表明:采用该技术可在合金表面成功制备出Al_2O_3/AZ31表面复合层,当搅拌头的旋转速度为1 500 r·min~(-1)、加工速度为23.5 mm·min~(-1)时,Al_2O_3颗粒均匀地分布在镁合金基体上,且与基体结合较好;Al_2O_3颗粒对再结晶晶粒的晶界起到钉扎作用,可显著细化晶粒;得到的表面复合层的显微硬度为55 HV,比母材硬度提高41%,细晶强化和颗粒强化对硬度的提高起着主要作用。     

高速铁路轴箱轴承纳米润滑脂摩擦学性能试验研究

以WS2和Si3N4纳米颗粒作为高速客车轴箱轴承润滑脂添加剂,依据完全析因试验方案,合成了高速客车轴箱轴承纳米润滑脂。采用四球摩擦磨损试验机对其抗磨减摩和抗极压性能进行了研究,使用扫描电子显微镜(SEM)分析了钢球磨斑表面形貌,运用双因素方差分析法探究了WS2-Si3N4复合纳米颗粒对纳米润滑脂润滑性能影响。研究表明:当WS2添加量为1.5%,Si3N4添加量为0.1%时,合成的纳米润滑脂PB值最大,摩擦因数最低,钢球磨斑形貌平整光滑;WS2和Si3N4纳米颗粒均可提高纳米润滑脂的润滑性能,对复合纳米润滑脂润滑性能的提高交互作用显著。     

Water-Based Lubrication of Hard Carbon Microspheres as Lubricating Additives

Because of their superior physical and chemical stability, carbon microspheres have been identified as promising lubricating additives. In this paper, hard carbon microspheres with diameters ranging from approximately 130 to 250 nm were prepared through a hydrothermal method using glucose as the carbon source. The as-prepared carbon microspheres were characterized by a series of complementary techniques including field emission scanning electron microscopy, Fourier-transform infrared spectroscopy, Raman spectroscopy, and X-ray diffraction. It was found that the as-prepared carbon microspheres were spherical with graphitic structure. The effects of applied load, concentration, and particle size of the carbon microspheres as water-based lubricating additives against an opposing smooth silicon surface were systematically studied using a UMT tribometer and a 3D noncontact interferometric microscope. The results showed that carbon microspheres can effectively reduce friction and wear on a smooth silicon surface and the optimal performance was obtained at an applied load of 100 mN, a concentration of carbon microspheres of 0.1 wt% and an average particle size of 200 nm. The superior performance of carbon microspheres as water-based lubricating additives was attributed to having the particles dispersed as individual particles (as opposed to clusters) and also having sufficient physically and chemically stable particles within the contact region which allowed for a rolling friction mechanism to reduce friction.     

Nanoparticle embedded chitosan film for agglomeration free TEM images

Transmission electron microscopy (TEM) is a very useful and commonly used microscopy technique, used especially for the characterization of nanoparticles. However, the identification of the magnetic nanoparticle could be thought problematic in TEM analysis, due to the fact that the magnetic nanoparticles are usually form aggregates on the TEM grid to form bigger particles generating higher stability. This prevents to see exact shape and size of each nanoparticle. In order to overcome this problem, a simple process for the formation of well‐dispersed nanoparticles was conducted, by covering chitosan film on the unmodified copper grid, it was said to result in aggregation‐free TEM images. It is also important to fix the magnetic nanoparticles on the TEM grids, due to possible contamination of TEM filament which is operated under high vacuum conditions. The chitosan film matrix also helps to protect the TEM filament from contact with magnetic nanoparticles during the imaging process. The proposed procedure offers a quick method to fix the nanoparticles in a conventional copper TEM grid and chitosan matrix prevents agglomeration of nanoparticles, and thus getting TEM images showing well‐dispersed individual nanoparticles.     

Analysis of networks based on styrene and divinylbenzene containing iron anchored using variable pressure scanning electron microscopy

There is great demand for the development of composite materials containing small metal or metal oxides particles, owing to their variable properties and wide application. However, microscopic evaluation of these materials using high‐vacuum scanning electron microscopy is difficult because the samples must undergo a series of preparation steps to reach a high image quality and to avoid becoming shrunk inside the microscope vacuum chamber. Thus, in this study, we used variable pressure scanning electron microscopy to evaluate the morphology and iron distribution on the surface of magnetic microspheres based on poly(styrene‐co‐divinylbenzene). These materials were obtained by suspension copolymerization of styrene and divinylbenzene in the presence of fine iron particles. Energy‐dispersive X‐rays were also used to analyse distribution of the iron particles. The results indicate that, under the conditions used, magnetic microspheres with a relatively narrow size distribution were formed. Moreover, the micrographs show that agglomerated iron particles appeared only on the microsphere surface.     

Preparation of smallest microparticles of poly-D,L-lactide by modified precipitation method: influence of the process parameters

Biodegradable microspheres such as those made of poly-D,L-lactide (PDLLA) are widely investigated delivery systems for drugs or antigens. The aim of this study was to examine experimental conditions in order to produce PDLLA microspheres with the best properties for controlled and sustained drug delivery by the modified precipitation method. For this purpose, the following parameters were varied: co-solvent (methanol or ethanol), the concentration of stabilizer polyvinyl alcohol (PVA), chloroform-to-water ratio and the speed and time of homogenization. Scanning electron microscopy (SEM) and stereological analysis were used to characterize the particles. The average size and morphology of the microspheres varied substantially with preparation conditions from 8.44-1.25 microm. Results showed that the smallest particles were obtained with methanol, 1% PVA and with 10 min of homogenization at 21,000 rpm.     

基于微喷射技术的药物微粒制备研究简

从数字化微量喷射原理出发,介绍了微量喷射实验系统的结构和控制平台设计;通过微阵列喷点实验,测试了数字化微量喷射实验系统点制阵列和制备微粒的可行性;以聚乳酸-羟基乙酸共聚物（PLGA）为微球／微囊壳材、阿莫西林为主药、聚乙烯醇和吐温作为表面活性剂,应用数字化微喷射技术,并采用内径40um的喷头制备了PLGA微球以及阿莫西林-PLGA微囊;利用单因素法和正交试验法研究了PLGA溶液浓度、驱动电压、喷射频率和搅拌器转速对PLGA微球及阿莫西林-PLGA微囊平均粒径和粒径分布的影响,并得出最优解：同时对微球／微囊表征进行了分析。     

微球材料作为润滑添加剂的摩擦学性能研究——粒径分布的影响

以未处理空心微球材料为原料制备粒度分布均匀集中的空心微球材料,用硅烷偶联剂对其进行表面改性处理,使其具有良好的亲油性。用HQ-1环块试验机在高速低载荷和低速高载荷2种工况下,测定了所制备的空心微球材料作为500SN基础油添加剂的摩擦磨损性能。结果表明:经处理后的空心微球材料可以显著提高500SN基础油的抗磨减摩性能;经处理后的空心微球材料的抗磨减摩性能好于未处理空心微球材料,表明粒径分布对摩擦学性能有显著影响。     

脉冲磁场辅助磁性复合磨粒化学机械抛光技术及其加工试验研究

提出一种脉冲磁场辅助新型磁性复合磨粒化学机械抛光技术。该技术利用磁性聚合物微球与SiO2磨粒组成的复合磨粒抛光液,在脉冲磁场辅助作用下,实现磨粒尺寸对硬质抛光盘微观形貌依赖性小、磨粒易进入抛光区域、材料去除率较高的抛光。设计了“之”字形的对位式结构电磁铁,模拟计算表明其磁感应强度沿抛光平面分布均匀,磁性微球受到的磁力一致性好。磁性微球在抛光系统中的受力分析表明：磁性微球受磁力作用时有利于复合磨粒从近抛光区进入抛光区,以二体磨损的方式去除加工表面;磁性微球不受磁力作用时,复合磨粒随抛光液的流动而移动,避免大量聚集形成磁链。以表面粗糙度Ra=1.1μm的硬质抛光盘进行硅片抛光试验,施加不同频率和占空比的脉冲磁场前后,硅片的去除率从137nm/min提高到288nm/min,频率5Hz、占空比50%时获得最大值,硅片表面粗糙度由抛光前Ra=405nm减小到Ra=0.641nm。     

磁性复合磨粒化学机械抛光技术及其加工试验研究

提出一种新型的磁性复合磨粒化学机械抛光技术。该技术利用磁性聚合物微球与SiO2磨粒组成的复合磨粒抛光液,在辅助磁场的作用下,实现了一种磨粒尺寸与硬质抛光盘微观形貌依赖性小、材料去除率较高的抛光工艺。建立直径8 mm、高度不等的稀土钕铁硼永磁体以点阵形式组合形成的4类辅助磁场。仿真计算表明,柱状下凹磁极的磁场磁力HdH/dz分布均匀,磁性微球受到的磁力一致性好。对磁性微球在抛光系统中的受力分析表明,磁性微球受到的磁力有助于复合磨粒从近抛光区域进入抛光区域,磁性复合磨粒能以二体磨损的方式划擦去除加工表面。以表面粗糙度Ra 0.5μm的硬质抛光盘进行硅片抛光试验,施加辅助磁场前后,硅片的材料去除率从66 nm/min提高到179 nm/min,硅片表面粗糙度由抛光前Ra 405.860 nm减小到Ra 0.490 nm。     

Three-dimensional dynamic morphometry on a diffraction pattern in the focal plane

A new type of morphometry, which shortens the scanning time of precise observation by confocal microscopy, has been investigated. To analyse the 3-D distribution of active sites on a living cell, microspheres of the same size were immunologically marked on specific sites on a cell. Incident coherent light was scattered on the microspheres and the scattered light from each microsphere superimposed upon each other giving a diffraction pattern of the examined cell. Several series of interference fringes were generated on the diffraction pattern, according to the phase difference of the microspheres. These interference fringes on the 2-D diffraction pattern enable the (relative) 3-D positions of the microspheres to be determined. 3-D dynamic morphometry on a 2-D diffraction pattern with interference fringes speeds up imaging in confocal microscopy.     

乙酰丙酮法测定壳寡糖的含量

目的建立一种用于壳寡糖含量检测的乙酰丙酮-分光光度检测方法。方法采用浓盐酸将含有壳寡糖的样品彻底水解,用6 mol/L的氢氧化钠将水解液调成中性,采用乙酰丙酮法于525nm处测定吸光度,代入回归方程,测定壳寡糖含量。结果壳寡糖含量在0.02～0.12 mg/mL浓度范围内时,其含量与吸光度之间呈良好线性关系,r2=0.999。该方法的加样平均回收率为99.25%,精密度和稳定性试验的相对标准偏差RSD分别为0.346%和0.145%,。结论该方法灵敏、准确、简便,可作为一般生产企业进行壳寡糖含量的常规测定。