制备条件对气凝胶粉末粒径的影响

利用超声波乳化技术,结合溶胶-凝胶反应制备了间苯二酚-甲醛有机气凝胶粉末和碳化气凝胶粉末。通过大量实验,探讨了制备条件对气凝胶粉末粒径的影响。在粉末干燥前以Zeta电位-粒径分布测试仪对乙醇悬浊液进行分析测试,对有机粉末和碳化粉末用TEM方法进行表征。研究了反应液质量分数、反应温度和时间以及分散剂与反应液体积比对产物粒径的影响。实验表明：制备条件对于制备纳米级的气凝胶粉末影响非常大,通过优化实验条件可以制备出分布较好的气凝胶粉末,超声功率较大容易实现体系均匀混合,反应液在反应过程中温度和时间的控制起着关键的作用,低质量分数的反应液所生成的产物比高质量分数的粒径要小,经碳化后粉末粒径进一步降低。     

铜基氧化物气凝胶的制备与表征

以CuCl2·2H2O为前躯体,环氧丙烷为凝胶促进剂,制得了铜基氧化物气凝胶。通过场发射扫描电镜、高分辨透射电镜、X射线衍射、红外谱图及N2吸附等方法,对气凝胶的结构进行了表征。结果表明：室温下合成的铜基氧化物气凝胶呈现3维网络状结构,其骨架由大量微小晶粒组成,颗粒粒径为几nm;随处理温度的升高,体系中的有机相逐渐被灼烧完全,气凝胶也由3维网络状结构转变为致密结构;气凝胶随温度升高不断变化,并最终生成氧化铜气凝胶。N2吸附结果表明气凝胶具有较高的比表面积,为386 m2/g。     

二氧化硅气凝胶靶丸研制

2003年，低密度二氧化硅气凝胶微球制备技术以及相关的溶胶-凝胶过程的研究取得了一些进展。在黑腔辐射场均匀性以及非对称性研究中，需要实心二氧化硅气凝胶微球作为黑腔内靶丸，必须满足很高的球形度和较低的密度以及小粒径的要求。一般地，为统一起见，可以用非球形参数OOR(out-of-round)表征微球的球形度，OOR越小，表示微球球形度越高。作为ICF靶丸，一般必须满足OOR小于5％。因此，实心二氧化硅气凝胶微球的制备技术附加了有别于普通二氧化硅块状气凝胶的特殊性。     

对苯二酚-甲醛碳气凝胶的制备

 溶胶-凝胶法制备了高HC比（10~40,对苯二酚与催化剂(Na₂CO_{3/sub>)的物质的量之比）的对苯二酚-甲醛有机气凝胶,并经高温碳化处理得到其碳气凝胶。借助有机气凝胶的红外光谱研究了其化学结构,说明其网孔结构形成的可能性;研究了有机气凝胶的扫描电镜图像、比表面积及孔径分布等,并得到碳化前后的一些对比数据：有机气凝胶颗粒大小30~50 nm,碳化后约为10 nm,比表面积从341.77 m²/g增大到452.75 m²/g,密度从0.170 8 g/cm^{3/sup>增大到0.335 6 g/cm3/sup>。}}     

辐射法制备Pd掺杂碳气凝胶粉末

利用辐射还原法,在100, 200, 500 kGy辐射剂量下制备了金属Pd掺杂的碳气凝胶粉末。X射线衍射（XRD）,扫描电子显微镜（SEM）和能谱测试证实了辐射法成功地制备出Pd掺杂的碳气凝胶粉末复合物。SEM照片表明,还原生成的金属Pd相对均匀地分布在所有碳气凝胶颗粒表面。N2吸附数据分析表明:掺入金属Pd后,碳气凝胶粉末比表面积、平均孔径和总孔体积都显著减小。由于被还原金属大多沉积在碳气凝胶粉末表面,不同辐射剂量下制得的掺杂碳气凝胶粉末的比表面积等多孔特征数据相差不大。     

辐射法制备Pd掺杂碳气凝胶粉末

利用辐射还原法,在100, 200, 500 kGy辐射剂量下制备了金属Pd掺杂的碳气凝胶粉末。X射线衍射（XRD）,扫描电子显微镜（SEM）和能谱测试证实了辐射法成功地制备出Pd掺杂的碳气凝胶粉末复合物。SEM照片表明,还原生成的金属Pd相对均匀地分布在所有碳气凝胶颗粒表面。N2吸附数据分析表明:掺入金属Pd后,碳气凝胶粉末比表面积、平均孔径和总孔体积都显著减小。由于被还原金属大多沉积在碳气凝胶粉末表面,不同辐射剂量下制得的掺杂碳气凝胶粉末的比表面积等多孔特征数据相差不大。     

溶剂对块体La基气凝胶性能的影响

采用溶胶-凝胶工艺,以氯化镧（LaCl37H2O）为前驱体,以甲醇和乙醇为溶剂,聚丙烯酸为分散剂,环氧丙烷为凝胶促进剂,分别合成两种性能不同的稀土La基气凝胶。采用扫描电子显微镜、傅里叶红外光谱仪、比表面积与孔径分析仪、力学性能测试仪对不同溶剂制备的两种稀土La基气凝胶的微观结构、成分、比表面积、孔径分布和力学性能进行了研究表征。结果表明,以甲醇和乙醇为溶剂制备的稀土La基气凝胶都具有纳米多孔材料的典型特征,由大量nm量级的球形和长条形颗粒胶连而成,孔洞结构丰富。以乙醇为溶剂制备的稀土La基气凝胶的网络骨架更纤细,孔洞更大,比表面积达到220 m2g-1,密度约为160 mgcm-3,但力学性能较差。而以甲醇为溶剂制备的稀土La基气凝胶的网络骨架更强壮,孔洞更小,比表面积达到95 m2g-1,密度约为350 mgcm-3,力学性能较好。样品性能上的差异可能是由甲醇的极性比乙醇的极性强引起的。     

无催化法制备低密度三聚氰胺-甲醛气凝胶

以三聚氰胺和多聚甲醛为原料,二甲基亚砜为溶剂制备三聚氰胺-甲醛(MF)气凝胶,湿凝胶经超临界干燥,制备出密度最低可达70 kg/m3的MF气凝胶。采用红外吸收光谱、场发射扫描电镜、N2吸附-脱吸附分析和热失重分析表征了MF气凝胶的组成、微结构以及热性能。结果表明:以二甲基亚砜为溶剂制备的MF气凝胶,虽然其微观结构较以水为溶剂的气凝胶差,比表面积及孔径分布均一性均降低,但是其热稳定性有所提高。     

不同酸催化条件下Ta2O5气凝胶的制备

采用溶胶-凝胶技术,以乙醇钽为前躯体,乙醇为溶剂,分别以盐酸、硝酸、硫酸为催化剂,结合CO2超临界干燥技术制备了Ta2O5气凝胶。研究发现:硫酸作催化剂的体系,其胶凝时间远远小于其他体系,且溶剂交换及超临界干燥过程中的收缩开裂现象明显改善;扫描电镜分析结果显示,硫酸为催化剂制备的Ta2O5气凝胶骨架颗粒间存在较严重的团簇现象,比表面积约167 m2/g,明显低于以盐酸、硝酸为催化剂的体系。X射线光电子能谱测试结果显示,Ta2O5气凝胶中无相应的Cl元素或N元素残留,而S元素则基本上滞留在Ta2O5气凝胶中。说明S元素进入了Ta-O-Ta交联结构,正是因为这种结构的引入,Ta2O5气凝胶的收缩龟裂现象得以明显改善并呈现出相对较高的力学性能。     

块状TiO2气凝胶的溶胶-凝胶过程及结构

 对块状TiO₂气凝胶的溶胶-凝胶过程及结构进行了实验研究,结果发现：增加催化剂的量,凝胶化时间缩短,湿凝胶的透明度降低,强度提高;增加前驱体的量,凝胶化时间缩短,湿凝胶的透明度变化不大,强度提高;增加水量,凝胶化时间先缩短后增加,湿凝胶透明度先减小后增加,强度先增加后减小。利用扫描电镜对超临界干燥法制备的不同催化剂量和密度的块状TiO₂气凝胶的结构进行了表征,并对结构与溶胶-凝胶过程之间的联系进行了分析。结果表明：增加催化剂量,由于缩聚反应进行的程度提高,气凝胶粒子粒径较小且总的孔径较大。减小前驱体量,气凝胶粒子粒径增大且结构逐渐疏松。     

The morphology control on the preparation of silver nanotriangles

A seed-mediated growth method was commonly applied to prepare one-dimension nanomaterials. However, some associated particles were unavoidable in the formation of target nanoparticles. Herein, we reported a modified method to prepare silver nanotriangles with higher uniform shape and particle size. The size and morphology of the formed nanoparticles could be controlled by regulating reaction conditions. The results showed that cetyl trimethyl ammonium bromide (CTAB) concentration and seed concentration were related with both the morphology and the particle size. The NaOH concentration, AgNO₃ concentration, and the mole ratio of V_c/Ag⁺ mainly affected the particle size of the formed nanotriangles. The formation of silver nanotriangles may be due to the selective stacking of the new tiny nanoparticles and the oriented growth of silver seed crystals. The oxidizing action of Br⁻/O₂ existing in the CTAB system should be responsible for the final morphology of truncated triangular silver nanoplates.     

Effect of ultrasonic frequency on size distributions of nanosized mist generated by ultrasonic atomization

Ultrasonic atomization is used to produce fine liquid mists with diameter ranges below 100 nm. We investigated the effect of the frequency on the size distribution of ultrasonic mist. A bimodal distribution was obtained for the mist generated by ultrasonic atomization with a wide-range particle spectrometer. The peak diameter decreased with increasing frequency, and the number concentration of the mist increased in the smaller range. We determined the relation between the size distribution of the mist and the ultrasonic frequency, and we proposed a generation mechanism for the ultrasonic nanosized mist based on the amount of water vapor around the liquid column. Increasing the power intensity and density by changing the surface diameter of the ultrasonic oscillator affected the number concentration and size distribution of the nanosized mist. Using this technique, the diameter of the mist can be controlled by changing the frequency of the ultrasonic transducer.     

The tungsten powder study of the dispenser cathode

The intercorrelation of tungsten powder properties, such as grain size, distribution and morphology, and porous matrix parameters with electron emission capability and longevity of Ba dispenser cathodes has been investigated for the different grain morphologies. It is shown that a fully cleaning step of the tungsten powder is so necessary that the tungsten powder will be reduction of oxide in hydrogen atmosphere above 700 °C. The porosity of the tungsten matrix distributes more even and the closed pore is fewer, the average granule size of the tungsten powder distributes more convergent. The porosity of the tungsten matrix and the evaporation of the activator are bigger and the pulse of the cathode is smaller when the granularity is bigger by the analysis of the electronic microscope and diode experiment.     

基于超声波测量技术的颗粒尺寸分布模型的研究

提出了一种利用单颗粒背向散射信号来进行粒径分布估算的超声波测量技术,系统阐述了其 理论基础及基本工作原理。被测颗粒的散射信号幅度与它在探测区中的位置、颗粒尺寸和形状有关。 通过理论分析,建立了一个可用于描述散射信号幅度概率分布与颗粒系尺寸分布之间关系的数学模 型,对该模型的反演计算便可得到颗粒系的尺寸分布信息。为了避免求解过程中的病态系数矩阵问 题,将模型求解转化成了易于解决的最优化问题。仿真实例结果验证了该技术的可行性。     

Influence of ultrasound on nanostructural iron formed by electrochemical reduction

A method for control of particle dimensions of nanostructural amorphous iron powder obtained by electrochemical reduction under the effect of ultrasonic oscillations in reaction medium is described in this paper. Depending on the character of ultrasonic oscillations nanostructural powders were obtained differing both in average dimension and distribution of particle dimensions. In the case of simultaneous sonocation using ultrasonic vibrations with frequencies differing from each other by a factor of ten (20 and 200 kHz), the effect is complex, but includes narrowing of the average particle dimension.     

Effect of different trimethyl silylating agents on the hydrophobic and physical properties of silica aerogels

An essential feature of the ambient pressure dried aerogel manufacturing process is the end-capping of the reactive silanol groups in the silica wet gel. In this report, we have presented the effect of two different trimethyl silylating agents viz. trimethylchlorosilane (TMCS) and hexamethyldisilazane (HMDZ) on the hydrophobic and physical properties of ambient pressure dried silica aerogels. The hydrogels were prepared by sol-gel processing of sodium silicate precursor (Na₂SiO₃) in the presence of acetic acid catalyst followed by vapour passing treatment and different solvent exchanging steps. The silylating agent in hexane was used for end-capping of the silanols present on the silica surface of the gel. To study silylation behavior silylating agent/Na₂SiO₃ molar ratio was varied from 2.4 to 5.6. The aerogels have been characterized by density, % of volume shrinkage, porosity, % of optical transmission, Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Thermo-gravimetric and Differential Thermal Analysis (TG-DTA) and contact angle measurements.     

全谱拟合法研究聚丙烯腈基碳纤维形成过程中晶态结构演变

通过全谱拟合法对碳纤维制备过程中不同阶段纤维的XRD谱图进行处理,得到不同阶段纤维的微观结构参数,研究了聚丙烯腈(PAN)基碳纤维制备过程中晶态结构的演变.全谱拟合法基于晶体衍射的严格物理理论,拟合目标为整个衍射谱,并不是个别衍射峰,所得结果具有更高的可信度.研究结果表明:PAN原丝中的高分子链沿纤维轴高度取向,表观晶粒尺寸为6.5 nm左右;经过预氧化处理,纤维中的有序结构遭到破坏,表观晶粒尺寸锐减.纤维中逐渐形成梯形结构并沿纤维轴取向,从而形成新的有序结构;经过碳化处理后,环状梯形结构转变为碳的层状结 关键词： 碳纤维 晶体结构 XRD 全谱拟合法