反相微乳液中纳米银粉的合成

以次亚磷酸钠还原剂,采用反相微乳液法制备纳米银粉;并借助TEM、X射线衍射和粒度分析仪研究了反应温度、水和表面活性剂的摩尔比、Ag+浓度和助表面活性剂对纳米银粉的粒径大小的影响。结果表明:随着水和表面活性剂的摩尔比的增加,纳米银粉的粒径尺寸随之变大;随着银离子浓度的增大,纳米银粉的粒径变小,当银离子浓度超过0.1 mol/L时,纳米银粒子出现团聚明显的现象,且粒径大小分布范围变大;随着助表面活性剂用量的增加,纳米银粉的粒径先降低,当正己醇的用量超过0.2 mol时,粒径大小反而缓慢增大;反应温度不太高时(20℃,40℃),纳米银粉的粒径分布大致都在20~40 nm之内,当温度高于60℃时,纳米银粉粒径分布不均匀且形状不规则,且出现明显的团聚现象。适宜工艺为:温度为40℃,水和表面活性剂的摩尔比ω=1,Ag+浓度为0.1 mol/L,助表面活性剂(正己醇)的用量为0.2 mol;制备的纳米银粉为面心立方晶系纯相银、分散性好、规则球形形状、粒径分布均匀、平均粒径为22 nm。     

功能材料纳米氧化锌粉体合成

采用直接沉淀法合成纳米氧化锌粉体。考察了锌源、沉淀剂、表面活性剂和反应介质等因素对纳米氧化锌粒径的影响。采用沉降法对产品粒径及粒径分布进行初步测量和判断,并采用SEM和XRD对产品进行表征。结果表明,以硝酸锌和碳酸钠为原料、十二烷基苯磺酸钠为表面活性剂合成的纳米氧化锌粉体,粒径小,粒径分布窄,平均粒径在50～100 nm。     

可生物降解聚乳酸纳米粒的制备及表征

采用乳化 -溶剂蒸发法 ( O/W)制备聚乳酸 ( PLA)纳米粒 ,用透射电子显微镜和激光粒度仪对纳米粒进行了表征 ,纳米粒具有规整的球形且正态分布 ,同时从有机相和水相的体积比、聚合物的浓度、表面活性剂的选择及表面活性剂的浓度等几个因素对纳米粒粒径大小的影响作了较详细地讨论。有机相与水相的体积比从 1∶ 3减小到 1∶ 30 ,纳米粒的粒径从 ( 30 6.2 + 1 1 ) nm减小到( 1 87.1 + 2 .4) nm;聚合物在有机相的浓度从 1 %(质量分数 )增加到 5 %(质量分数 ) ,纳米粒的粒径从 1 94nm增加到 32 1 nm;随着水相中表面活性剂浓度从 0 .5 (质量体积分数 )增大到 3.5 %(质量体积分数 ) ,纳米粒粒径从 2 0 2 nm减小 1 78nm且有一个低的多分散指数。而且还比较了搅拌蒸发法和减压抽提法对纳米粒表面形态的影响     

双微乳液法制备纳米硫酸钡颗粒

在水溶液/Triton X-100/正己醇/环己烷组成的反相微乳液中,以氯化钡和硫酸钠为原料,通过沉淀反应,制备出类球形BaSO_4纳米颗粒,并通过XRD、SEM、TEM、FTIR对其进行表征。考察了三种反应方式、水/Triton X-100摩尔比(R)、反应物浓度以及助表面活性剂/表面活性剂摩尔比(P)对纳米BaSO_4颗粒大小和形貌的影响。同时考察了R对微乳液液滴大小和粒径分布的影响,并通过动态光散射技术(DLS)对微乳液液滴进行测定。实验结果表明:室温条件下,采用双微乳液法,R=17.97,P在2.11~4.22之间是纳米BaSO_4颗粒合成的最佳反应条件,反应物浓度对BaSO_4颗粒的大小和形貌几乎没有影响。在该反应条件下,合成出的类球形BaSO_4粒径为18~22 nm,产率可达87.5%。     

“一步法”合成改性纳米碳酸钙及表征

通过直接沉淀法、微乳液法和水热法合成并改性了纳米CaCO3。3种方法均有表面活性剂的介入,目的在于表面活性剂在控制碳酸钙晶粒生长的同时可使纳米CaCO3表面得到改性。采用X射线衍射(XRD)、红外光谱(FTIR)、透射电镜(TEM)等分析测试方法对产物的物相、形貌及颗粒大小进行表征。结果表明,采用水热法在十二烷基磺酸钠(SDS)和EDTA共同作用下得到粒径为20~50 nm的方解石型纳米CaCO3,通过表面活性剂与纳米CaCO3表面的化学吸附实现表面改性的目的。     

纳米磷酸锌的可控合成

在氧化锌、磷酸固-液反应体系中,以研磨反应代替搅拌反应,辅助表面活性剂对磷酸锌的颗粒尺寸进行可控合成,考察了研磨介质、磨球比例、球料比、固液比、表面活性剂等工艺条件对磷酸锌粒径分布、形貌及团聚状况的影响,并采用SEM、XRD、粒度分布和TEM对纳米磷酸锌做了表征。结果表明,表面活性剂CTAB浓度为9×10^-4 mol/L、研磨时间为3 h、锆球为研磨介质、球料质量比为150:1、Φ10 mm与Φ6 mm磨球质量比为1:4、转速为200 r/min、固液比[氧化锌和（磷酸+表面活性剂）的质量比]为1:1时,可以制备粒径分布为59~79 nm、平均粒径为68 nm、无团聚的粒状纳米磷酸锌。     

金属醇盐水解和均匀沉淀耦合法制备Sb2O3纳米粒子

以SbCl3为原料,用金属醇盐水解和均匀沉淀耦合法制备出了Sb20,纳米粒子,详细讨论了反应温度、表面活性剂、尿素浓度、超声波等实验条件对纳米Sb20,粒径的影响。采用透射电子显微镜(TEM)、X射线衍射仪(XRD)等技术对粒子性能进行了分析。实验结果表明：制备出的Sb20,纳米粒子平均粒径在30nm,单分散性好,粒度分布窄。超声波技术的引入减小了SbzO3纳米粒子的粒径并且提高了分散性。     

氧化还原法制备纳米镍粉研究

以氨水、Ni(NO3)2·6H2O为原料,在氧化还原体系下制备纳米镍粉末。讨论了表面活性剂、加料顺序、干燥方式以及煅烧温度等因素对纳米镍制备的影响;用X射线衍射、透射电子显微镜等对样品的成分、晶体结构、粒度及其分布进行了分析。结果表明:制得的纳米金属镍粉纯度高,粒径分布窄,平均粒径为35nm,粒径范围在30～40nm。     

多元胺醇型表面活性剂对铜晶圆平坦化的影响

研究了一种多元胺醇型非离子表面活性剂对铜化学机械抛光(CMP)液粒径及分散度、抛光速率、抛光后铜膜的碟形坑高度、表面非均匀性和表面粗糙度的影响。抛光液的基本组成和工艺条件为:SiO_2(粒径60~70 nm)5%(体积分数,下同),多羟多胺螯合剂3%,30%(质量分数)过氧化氢3%,工作压力1 psi,背压1 psi,抛头转速87 r/min,抛盘转速93 r/min,抛光液流量300 mL/min,抛光时间60 s,抛光温度23°C。结果表明,表面活性剂的引入可提高抛光液的稳定性。当表面活性剂含量为3%时,抛光速率、抛光后碟形坑高度、表面非均匀性和表面粗糙度分别为614.86 nm/min、76.5 nm、3.26%和0.483 nm,对铜晶圆的平坦化效果最好。     

不同粒径立方纳米CeO_2的可控合成研究

纳米CeO_2由于具有优异的性能而被广泛应用于催化剂、储氢材料、热电材料和气体传感器等领域;其优异的性能不仅与其本身的物理化学性质有关,还取决于材料的粒径大小。因此可控合成不同粒径、形貌规则的纳米CeO_2是研究其性能的先决条件。以Ce(NO_3)_3·6H_2O和NaOH为原料,通过水热法可控合成粒径范围为19.6~59.8 nm的立方纳米CeO_2,并研究了不同实验条件对其粒径的影响。研究结果表明,水热温度、NaOH的浓度和表面活性剂的种类是影响粒径的主要因素,随着水热温度的升高,粒径逐渐增大;随着NaOH浓度的增加,纳米CeO_2的粒径先呈增大的趋势,当NaOH的浓度过高时,纳米CeO_2的粒径又呈减小的趋势;体系中加入不同的表面活性剂对粒径产生不同的影响:聚乙二醇-2000和柠檬酸钠使纳米CeO_2的粒径明显减小,而聚乙二醇-400则产生相反的结果。     

Submicron particle size and polymerization excess surfactant analysis by capillary hydrodynamic fractionation (CHDF)

The particle size distribution of a blend of two polymer latex monodisperse standards, 86 and 238 nm, has been measured by capillary hydrodynamic fractionation (CHDF). The particle size distributions obtained agreed well with the expected particle diameters. The relative amounts of the two standards in the blends were accurately measured at different blend ratios. The particle size distribution of a parenteral lipid sample was successfully measured. A soluble species was fractionated from latex standards smaller than 100nm. This soluble species appears to be excess surfactant used in the preparation of small size monodisperse latexes. The amount of excess surfactant increases as the particle diameter of the standard decreases.     

分散剂和非离子型表面活性剂对悬浮聚氯乙烯树脂颗粒特性的影响

研究了聚乙烯醇(PVA)分散剂和非离子型表面活性剂对悬浮聚氯乙烯(PVC)树脂颗粒特性的影响。结果表明随着PVA醇解度的增加，PVC树脂的颗粒规整性和表现密度增加，孔隙率和吸油率降低；随着非离子型表面活性剂添加量的增加，PVC树脂的平均粒径和吸油率增大。从PVA和表面活性剂在水一油两相分配出发，讨论了PVA醇解度和添加非离子型表面活性剂对PVC树脂的颗粒特性影响机理。     

液相法制备纳米铜粉的研究

以KBH4和CuSO4为原料,采用液相还原法,在以下工艺条件下制备出纳米级铜粉,Cu2+的初始浓度为0.3mol/L,KBH4与Cu2+的摩尔比为0.75,反应温度为40℃,用表面活性剂OP进一步控制产品粒径及其分散性;并对纳米铜粉用XRD、TEM进行了表征。结果表明:本法制备的纳米铜粉呈球形,平均粒径为30 nm,分散性较好,转化率较高。     

Influence of ingredients in water-based polyurethane–acrylic hybrid latexes on latex properties

Polyurethane–acrylic (PU–AC) hybrid latexes were prepared. Main monomers for PU preparation were isophorone diisocyanate, DMPA (dimethylol propanic acid) and polypropylene oxides (PPO) of different molecular weights. Acrylic monomers included butyl acrylate, methyl methacrylate and a crosslinker, trihydroxymethyl propane triacrylates (TMPTA). Several important ingredients in PU–AC latex preparation, such as surfactants, initiator, DMPA and PU/AC ratio, etc., were varied, and their effects on latex properties studied. Compared with surfactant free latexes, a sharp increase in particle size was observed in latexes done with 0.1% of surfactant regardless of the nature of the surfactants used (anionic, nonionic and anionic with long chain of amphiphilic alkylphenyl polyethoxylate). Further increase in surfactant content, however, led to latexes with smaller particle size and narrower particle size distribution when compared between latexes prepared using a same surfactant. When amount of the oil soluble initiator, azobisisobutyronitrile, was increased, AC monomers conversion was increased. It is interesting to observe that PPO with long propylene oxides brought about larger particle size combined with broader size distribution and less charge on particle surface; whereas lower DMPA levels led to latexes also of larger size combined with broader size distribution but more charges on particle surface. AC monomer crosslinker, TMPTA, contributed to reduce particle size, narrower size distribution and lower particle surface charges. By increasing AC amount in PU–AC latex, latex particle size significantly increased accompanied by a remarkable increase in particle surface charges. Mechanisms of particle formation and of DMPA stabilization were discussed in order to understand the experimental results.     

Preparation of water-stable submicron fibers from aqueous latex dispersion of water-insoluble polymers by electrospinning

Submicron polystyrene (PS) fibers were prepared by electrospinning of an aqueous dispersion of PS latex and a small amount of poly(vinyl alcohol) (PVA) and subsequent extraction by water. Depending on particle size, surfactant, ratio of PS:PVA, and applied voltage fibers of different morphology and water stability were obtained. Analysis of latex fibers by TEM revealed hexagonal packaging of particles within the fibers.     

用阴离子Gemini 9 B-6-9 B乳化剂合成苯乙烯-丙烯酸丁酯共聚物纳米乳液

以壬基酚、1,6-二溴己烷、氯磺酸为主要原料合成的阴离子Gemini磺酸盐表面活性剂9 B-6-9 B为乳化剂,苯乙烯(St)、丙烯酸丁酯(BA)为单体,合成了乳胶粒径小于100 nm且分布均匀的苯乙烯-丙烯酸丁酯共聚物纳米乳液,考察了聚合温度、乳化剂用量、引发剂用量、单体配比、单体含量对乳液的影响,探讨了乳胶粒子成核机理。结果表明,随着温度的升高,乳胶粒子的平均粒径减小,转化率与凝胶率增大;随着乳化剂或引发剂用量的增加,乳胶粒子的平均粒径和凝胶率减小,转化率增大;随着软单体比例的增加,乳胶粒子的平均粒径与转化率增大,粒径分布变宽,凝胶率减小;单体用量增大,乳胶粒子的平均粒径与凝胶率增大,转化率降低;乳胶粒子的粒径呈单峰分布,可能是按胶束成核机理形成的。     

有机硅/丙烯酸酯乳液的粒径与分散行为研究

采用半连续乳液聚合法合成了以丙烯酸丁酯和甲基丙烯酸甲酯为成核单体,丙烯酸丁酯(MAA)、甲基丙烯酸甲酯(BA)、丙烯酸(AA)和γ―甲基丙烯酰氧基丙基三甲氧基硅烷为成壳单体的核壳结构乳液。采用马尔文纳米粒度仪等研究了乳液的粒径及其分布与引发剂和乳化剂用量之间的关系,粒径对乳液稳定性的影响以及乳液粒径与温度的关系,通过透射电镜对乳液微粒形态进行了分析。结果表明,乳液的粒径随着引发剂和乳化剂用量的增加而减小,乳液粒径在30～60℃时较为稳定,当引发剂过硫酸铵质量分数为0.55%,乳化剂十二烷基苯磺酸钠质量分数为2%时,制得的乳液粒径在120 nm左右,具有明显的核壳结构和较好的稳定性。     

表面活性剂对聚乙烯醇基薄膜透光性及机理的影响

针对聚乙烯醇（PVA）与表面活性剂能组成复配体系,制备了聚乙烯醇基亲水性薄膜材料,研究了表面活性剂的掺量对聚乙烯醇基薄膜的微观结构、孔隙度、透光性能、PVA结晶度及晶粒尺寸的影响。采用紫外分光光度计考察了各薄膜的透光性;采用扫描电子显微镜观察了聚乙烯醇/表面活性剂的横截面微观结构;采用X射线衍射仪考察了不同表面活性剂的添加量对复合薄膜的晶相组成及PVA晶粒尺寸的影响,结果表明当表面活性剂添加量在6%~10%（质量分数,下同）时,阳离子表面活性剂十六烷基三甲基溴化铵（CTAB）明显地降低聚乙烯醇的结晶度,而阴离子表面活性剂十二烷基苯磺酸钠（SDBS）则没有此效果;CTAB的加入使聚乙烯醇/CTAB体系中PVA晶粒尺寸增大,SDBS的加入使聚乙烯醇/SDBS体系中PVA晶粒尺寸减小。最后对聚乙烯醇与表面活性剂相互作用机理示意图进行了预测。     

Contributions of TMAH Surfactant on Hierarchical Structures of PVA/Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>–TMAH Ferrogels by Using SAXS Instrument

The magnetic hydrogels combining polyvinyl-alcohol (PVA) and Fe₃O₄ (magnetite)–TMAH (tetra-methyl ammonium hydroxide) have been successfully fabricated via a Freezing-thawing route. The magnetite nanoparticles were prepared from iron sands by using coprecipitation method. The transmission electron microscopy image revealed that the magnetite nanoparticles with a reaction temperature of 30 °C had the average particle size of 12 nm in clusters of aggregation. The result was similar to the particle size obtained from X-ray diffraction data analyzed by Scherer equation. Furthermore, synchrotron small angle X-ray scattering data were analyzed by using two lognormal distributions to calculate the distribution of the individual magnetite particles. Meanwhile, Teubner-Strey and Beaucage models were employed to observe the distribution of magnetite particles coated by TMAH as a surfactant. The data analysis showed that the magnetite particles within the magnetic hydrogels formed aggregations with diameters of cluster particles in the range from 13.1 to 31.8 nm. Interestingly, the diameter of clusters particle increased from 13.1 to 31.8 nm along with the increasing concentration of ferrofluids from 1 to 15 wt%. This phenomenon was predicted to result from the effect of TMAH as a surface reactant agent that prevented the aggregation by coating the surface of the magnetite nanoparticles.