微米级高聚物包埋型金属铁复合粒子的球磨法制备及其磁流变效应

采用球磨法,能成功地直接从高聚物与金属铁的混合研磨中,获得微米级由聚苯乙烯和聚甲基丙烯酸甲酯等高聚物包埋型金属羰基铁复合粒子.详细讨论制备条件包括不同高聚物比例、球磨时间对复合粒子形貌和粒径的影响及其复合粒子的热稳定性,还简要研究了由这些粒子组成的浓有机悬浮溶液的磁流变效应及其粒子的沉降稳定性.     

超细金属铁颗粒的高分子修饰及其悬浮液的磁流变性能

报道以γ射线辐照方法合成出具有良好分散性的高分子复合金属铁粒子.分别选择十二烷基硫酸钠、溴化十六烷基三甲基铵、Tween-80、TritonX-200和OP-10等表面活性剂和有机单体、无机铁颗粒一起制备乳状液,通过对这种含有超细金属铁颗粒乳状液稳定性的比较,以寻求合适的乳化剂.并对以TritonX-200为乳化剂时合成出的高聚物复合铁颗粒进行了XRD、TEM和IP表征.还将实验中所获得的高聚物复合铁粒子与粒径相同的未经修饰的纯铁粒子分别制成了悬浮液,对两者的悬浮性能进行了比较,同时,也将高聚物复合铁粒子制成的悬浮液与Fe3O4-PMMA复合粒子悬浮液两者的屈服应力随磁场变化情况进行比较研究.     

液相脉冲激光烧蚀法制备高熔点的纳米金属粒子

采用液相脉冲激光烧蚀法成功地制备了高熔点的金属Pt、Ru与Ag纳米粒子. 采用SEM、TEM、ED和紫外-可见吸收光谱表征了纳米粒子的特征. 纳米粒子的粒径基本在数个到数十个纳米的大小范围内. 发现含适量PVP(poly(vinylpyrrolidone))的水溶液有利于纳米粒子的制备, 而且还能够提高纳米粒子悬浮液的稳定性. 该制备方法较简单, 在制备高熔点的纳米金属粒子方面有着其它方法所不能比拟的优势.     

氨基改性纤维素纳米晶体的自组装行为研究

采用硫酸水解法制备纤维素纳米晶体(CNC)，然后用环氧氯丙烷、氨水依次对其表面改性得到氨基改性的CNC (CNC-NH_2)，进一步采用蒸发诱导自组装(EISA)法制备CNC-NH_2薄膜.通过偏光显微镜(POM)、原子力显微镜(AFM)、扫描电子显微镜(SEM)和流变测试对CNC-NH_2悬浮液和薄膜的自组装行为进行研究.结果表明，CNC-NH_2为棒状粒子，氨基的引入提高了其热稳定性.随着CNC-NH_2悬浮液浓度增大，手性向列型液晶相逐渐形成，且干燥成膜后仍然能保持织态结构.流变测试表明，CNCNH_2悬浮液显示独特的流变行为，可以观察到明显的相转变浓度和相转变温度.此外，考察了超声时间对CNC-NH_2悬浮液成膜的影响.随着超声时间的延长，CNC-NH_2膜由无色透明向虹彩色转变，且具有虹彩现象的膜对光的特殊波段产生吸收.     

超细α-Fe粒子对磁性粒子浓悬浮体系磁流变性能的增强

报道在磁性粒子浓悬浮体系中加入球磨超细α-Fe粒子对其磁流变性能的影响,主要研究其动态屈服应力的变化,沉降稳定性的改变以及超细粒子对相变结构的可能影响.超细α-Fe粒子的加入,能使磁性粒子浓悬浮体系的抗剪切能力有明显变化,悬浮稳定性增强.对其它几种超细粒子实验结果进行了简要讨论.超细粒子对磁流变性能影响程度取决于加入物与磁性颗粒的重量比例、加入物质的性质以及所加入超细粒子的尺寸.     

氨基改性纤维素纳米晶体的自组装行为研究

采用硫酸水解法制备纤维素纳米晶体(CNC),然后用环氧氯丙烷、氨水依次对其表面改性得到氨基改性的CNC (CNC-NH2),进一步采用蒸发诱导自组装(EISA)法制备CNC-NH2薄膜.通过偏光显微镜(POM)、原子力显微镜(AFM)、扫描电子显微镜(SEM)和流变测试对CNC-NH2悬浮液和薄膜的自组装行为进行研究.结果表明,CNC-NH2为棒状粒子,氨基的引入提高了其热稳定性.随着CNC-NH2悬浮液浓度增大,手性向列型液晶相逐渐形成,且干燥成膜后仍然能保持织态结构.流变测试表明,CNCNH2悬浮液显示独特的流变行为,可以观察到明显的相转变浓度和相转变温度.此外,考察了超声时间对CNC-NH2悬浮液成膜的影响.随着超声时间的延长,CNC-NH2膜由无色透明向虹彩色转变,且具有虹彩现象的膜对光的特殊波段产生吸收.     

氯化钠在球形纳米氧化铈形成过程中的作用

以水合碳酸铈为原料, 以氯化钠作为助磨剂和阻聚剂, 采用机械活化法制备了球形纳米氧化铈, 用XRD法研究了水合碳酸铈与氯化钠质量比、球磨时间、煅烧温度对CeO2粉体晶粒度的影响, 用TEM对最终产物粒子进行形貌观察. 结果表明: 在碳酸铈的球磨过程及其随后的煅烧过程中, 氯化钠的存在起到了很好的助磨和阻聚作用, 所得CeO2为类球形粒子, 分散性较好, 晶粒度约为30～50 nm.     

络合氢化物Ti-NaAlH4的制备与储氢特性

采用Ti粉为催化剂前驱体、预处理Al粉和NaH为合成原料, 通过机械球磨-加氢方法合成出络合氢化物Ti-NaAlH4, 系统研究了球磨保护气氛、球磨时间和氢化加氢压力等制备参数对其储氢性能的影响. 结果表明, 制备方法对Ti-NaAlH4储氢特性有很大影响. 与氩气保护气氛相比, 在氢气气氛中球磨制备的复合物具有更高的吸放氢性能. 在氢气保护气氛下, 随着球磨时间从6 h增至24 h, 复合物的吸氢容量和吸氢速率先增后减, 12 h时达到最佳值, 而复合物的放氢容量和放氢速率则逐渐增高; 进一步延长球磨时间会使颗粒发生团聚, 从而导致吸氢性能下降. 随着氢化加氢压力从7.5 MPa升至13.5 MPa, 复合物的吸氢容量(质量分数)由2.83%逐渐增至4.21%. 复合物球磨后出现的Na3AlH6中间氢化物相表明, 在氢气下掺Ti球磨对NaH和Al的氢化反应起到很好的促进作用.     

纳米尺度的消化熟化及其在单分散纳米材料制备中的应用

近年来，消化熟化方法已经被广泛采用来制备单分散纳米粒子，特别是在制备亚10 nm的小尺寸纳米粒子方面具有显著优势.但是，目前国内尚未发现关于此方法的中文文献报道，影响了部分国内学者对消化熟化方法的认识和应用.因此，从纳米尺度的消化熟化现象的发现过程和机理的提出开始，分析了沉淀反应前驱物、消化熟化剂种类、热处理温度和时间、溶剂类型以及其他因素对消化熟化现象的影响，介绍了基于颗粒表面带电与曲率效应、颗粒表面与配体分子层的相互作用以及消化熟化过程中的竞争反应平衡等因素的理论模型和研究结果，阐述了消化熟化法在制备金属纳米粒子、合金纳米粒子、金属氧化物和硫族化合物量子点以及其他纳米粒子等单分散纳米材料中的应用，最后展望了消化熟化法制备的单分散纳米粒子在纳米组装和多相催化等领域的应用.     

磁性粒子浓悬浮体系沉降稳定性的光学表征

报道一种新的磁性粒子浓悬浮体系沉降稳定性的表征方法.对均匀分散的磁性粒子浓悬浮体系,采用定时光度测量法对其沉降稳定性进行表征,可以得到一定时间内粒子沉降的定量数据.此方法可用于低体积分数磁流变液沉降稳定性的表征.同时,对比分析表明,在磁性粒子浓悬浮体系中加入纳米级TiO2粒子,能使制备的磁流变液稳定性显著增强.     

界面缓蚀剂的吸附稳定性

研究表明：在一定条件下,阳极脱附电位可作为评价缓蚀剂吸附稳定性的一个经验参数：缓蚀剂吸脱附诱导的电化学振荡是缓蚀体系的一种特殊失稳状态,即缓蚀剂吸附过程与电极反应中间吸附态产物耦合的结果;卤素离子的协同作用不仅可以提高某些有机缓蚀剂的吸附复盖度,而且可以增强其吸附稳定性;微分极化曲线是研究吸附稳定性的有效方法。     

Effect of the graphitic degree of carbon supports on the catalytic performance of ammonia synthesis over Ba-Ru-K/HSGC catalyst

A series of high surface area graphitic carbon materials （HSGCs） were prepared by ball-milling method. Effect of the graphitic degree of HSGCs on the catalytic performance of Ba-Ru-K/HSGC-x （x is the ball-milling time in hour） catalysts was studied using ammonia synthesis as a probe reaction. The graphitic degree and pore structure of HSGC-x supports could be successfully tuned via the variation of ball-milling time. Ru nanoparticles of different Ba-Ru-K/HSGC-x catalysts are homogeneously distributed on the supports with the particle sizes ranging from 1.6 to 2.0 nm. The graphitic degree of the support is closely related to its facile electron transfer capability and so plays an important role in improving the intrinsic catalytic performance of Ba-Ru-K/HSGC-x catalyst.     

Electrophoretic deposition of unstable colloidal suspensions for superhydrophobic surfaces

A novel method to fabricate superhydrophobic surfaces using electrophoretic deposition (EPD) is presented. EPD presents a readily scalable, customizable, and potentially low cost surface manufacturing process. Low surface energy materials with high surface roughness are achieved using EPD of unstable hydrophobic SiO(2) particle suspensions. The effect of suspension stability on surface roughness is quantitatively explored with optical absorbance measurements (to determine suspension stability) and atomic force microscopy (to measure surface roughness). Varying suspension pH modulates suspension stability. Contrary to most applications of EPD, we show that superhydrophobic surfaces favor mildly unstable suspensions since they result in high surface roughness. Particle agglomerates formed in unstable suspensions lead to highly irregular films after EPD. After only 1 min of EPD, we obtain surfaces with low contact angle hysteresis and static contact angles exceeding 160°. We also present a technique to enhance the mechanical durability of the superhydrophobic surfaces by adding a polymeric binder to the suspension prior to EPD.     

球磨方式对锂离子正极材料LiFePO4性能的影响

采用高温固相合成法制备橄榄石型的LiFePO₄正极材料，在合成过程中分别采用湿法球磨和干法球磨两种球磨方式。用X-射线衍射，扫描电镜，激光粒度测试等对合成材料进行表征，并对以LiFePO₄为正极的电池进行电化学性能测试。结果表明，相对于干法球磨，湿法球磨制备的LiFePO₄样品具有更好的电化学性能，0.2C放电的首次放电比容量为134.9 mAh·g^-1，并有优良的大电流放电性能及循环性能。这主要是因为采用湿法球磨制备的LiFePO₄材料物相较纯、粒径均匀，与导电添加剂的接触更加紧密，从而提高了LiFePO₄材料电化学性能。     

LaMg_(11)Zr+Ni合金电极电化学性能研究

以LaMg11Zr为母体合金,由机械合金化方法制备LaMg11Zr+200%N i合金,用X射线衍射(XRD)测定球磨时间对非晶相化的影响,20 h合金即可达到完全非晶态化,合金电极化学性能和循环寿命最好.     

Kinetics of bacterial potentiometric titrations: the effect of equilibration time on buffering capacity of Pantoea agglomerans suspensions

Several recent studies have made use of continuous acid-base titration data to describe the surface chemistry of bacterial cells as a basis for accurately modelling metal adsorption to bacteria and other biomaterials of potential industrial importance. These studies do not share a common protocol; rather they titrate in different pH ranges and they use different stability criteria to define equilibration time during titration. In the present study we investigate the kinetics of bacterial titrations and test the effect they have on the derivation of functional group concentrations and acidity constants. We titrated suspensions of Pantoea agglomerans by varying the equilibration time between successive titrant additions until stability of 0.1 or 0.001 mV s(-1) was attained. We show that under longer equilibration times, titration results are less reproducible and suspensions exhibit marginally higher buffering. Fluorescence images suggest that cell lysis is not responsible for these effects. Rather, high DOC values and titration reversibility hysterisis after long equilibration times suggest that variability in buffering is due to the presence of bacterial exudates, as demonstrated by titrating supernatants separated from suspensions of different equilibration times. It is recommended that an optimal equilibration time is always determined with variable stability control and preliminary reversibility titration experiments.     

Colloidal stability of magnetite/poly(lactic acid) core/shell nanoparticles

In this work, we describe an experimental investigation on the colloidal stability of suspensions of three kinds of particles, including magnetite, poly(lactic acid) (PLA), and composite core/shell colloids formed by a magnetite core surrounded by a PLA shell. The experiments were performed with dilute suspensions, so that recording the optical absorbance with time gives a suitable indication of the aggregation and sedimentation of the suspensions. The method allowed us to distinguish very accurately between the different surface and magnetic forces responsible for the structures acquired by particle aggregates. Thus, the pure PLA suspensions are very sensitive to ionic strength and almost unaffected by pH changes. On the contrary, the stability of magnetite systems is mainly controlled by pH. The effect of vertical magnetic fields on the stability of magnetite and magnetite/PLA suspensions is also investigated. The PLA shell reduces the magnetic responsiveness of magnetite, but it is demonstrated that the mixed particles can also form structures induced by the field, despite their lower magnetization, and they can be considered in magnetically targeted biomedical applications.     

非金属与金属的协同作用对镁基储氢合金电化学性能的影响

用机械球磨法分别以Ti、B、复合物TiB对非晶态Mg45Ti3V2Ni50储氢合金进行了表面修饰.实验结果表明,恰当比例的TiB球磨修饰对镁基储氢合金循环稳定性远好于Ti、B同比例单独修饰合金电极的效果.Mg45Ti3V2Ni50与TiB质量比为2∶1的Mg45Ti3V2Ni50-TiB(2∶1)复合合金电极的初始放电容量为529.4mAh·g-1,第50次循环放电容量仍为277.1mAh·g-1.复合物TiB中Ti、B元素之间和复合合金中合金元素与TiB之间产生了金属与非金属的协同作用,导致复合合金新的立体褶皱结构的生成,增强了修饰层与合金间的作用,Mg45Ti3V2Ni50-TiB(2∶1)合金电极表面活性增强,循环稳定性显著提高.     

Experimental study of a dynamic filtration system with overlapping ceramic membranes and non-permeating disks rotating at independent speeds

In a previous paper [Ding et al., J. Membr. Sci. 276 (2006) 232], we have investigated the performance in microfiltration of mineral suspensions of a novel filtration pilot consisting in overlapping ceramic membranes disks rotating at same speed on two parallel shafts. In this paper, we investigate a modification of this concept in which the ceramic disks of one shaft were replaced by non-permeating metal disks of same size rotating at a speed different from that of membranes. We also operated the pilot without disks on the 2nd shaft in order to eliminate membrane overlapping. When using metal disks with radial vanes, permeate fluxes were found to be 50–60% higher than those obtained in the same conditions with the previous design using only ceramic disks. By comparing permeate fluxes in different configurations, membranes on both shafts, membranes on the 1st shaft with and without metal disks on the 2nd shaft, we showed that, at a feed concentration of 200 g L⁻¹, the effect on permeate flux J, of shear rate increment due to membrane overlapping, could be completely offset by the high concentration increase between two adjacent and overlapping membranes. Raising the ceramic disks rotation speed N_c had a larger effect on J than increasing the metal disks speed N_m. For N_c = 32.16 Hz (1930 rpm) and N_m = 2.4 Hz (144 rpm), J reached 1790 L h⁻¹ m⁻² at 310 kPa, versus 1100 L h⁻¹ m⁻² for N_c = 12.3 Hz (738 rpm) and N_m = 22.26 Hz (1336 rpm) (for the same total sum N_c + N_m). Measurements of electrical power consumed by friction on rotating disks showed that the energy spent per m³ of permeate was lowest when using metal disk with vanes rotating at low speed and ceramic disks rotating at high speed.     

Influence of dispersion conditions and nature of the emulsifier on the dispersity and stability of artificial polymer suspensions based on polyetherimide

New methods for producing artificial polyetherimide suspensions in the presence of domestic cationic surfactants, their mixtures, and mixtures of cationic and organosilicon surfactants were proposed. The effect of the polymer concentration in the initial solution and conditions of emulsion dispersion on the stability and particle size of the final polymer suspensions is shown. The colloidal chemical properties of the obtained polymer suspensions are considered. Conclusions about the influence of the nature and concentration of surfactants on the stability of the obtained suspensions are drawn. When using a mixture of cationic and organosilicon surfactants, polymer suspensions stable during production and storage are formed, which is explained by the formation of structural mechanical and electrostatic stability barriers in the surface layers of the particles.