间苯三酚-甲醛气凝胶及其碳气凝胶的制备与表征

 以间苯三酚(P)和甲醛(F)为原料，经溶胶-凝胶、溶剂交换、超临界干燥和碳化等过程制备出了间苯三酚-甲醛气凝胶(PF)及其碳气凝胶(CPF)。测试结果表明气凝胶具有比较高的比表面积、是一种连续nm级3维网络结构的多孔材料；碳化后密度和平均孔径增大，比表面积基本无变化，且仍然维持气凝胶的网络结构。催化剂摩尔比决定气凝胶的微观结构，反应物质量分数控制着气凝胶密度。通过优化制备条件，可以制备出能满足惯性约束聚变(ICF)靶需要的不同结构和不同密度的气凝胶。     

有机气凝胶的超声法制备

 在间苯二酚类有机气凝胶的制备工艺中引入超声波技术，缩短了有机气凝胶制备周期。实验发现：反应物质量分数为10%的溶液在超声作用下的凝胶时间减少8%～17%，超声波能有效抑制凝胶过程中的氧化作用。在反应初始阶段，通过激光粒度仪测量稀溶液反应，发现超声波作用下的凝胶核生长速度是普通加热的凝胶核生长速度的87倍左右。微量水分测定仪的数据表明，低强度超声波可以上万倍地加快凝胶样品的溶剂交换速率。     

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>。}}     

分散剂对RF凝胶掺钛过程的影响

 以间苯二酚、甲醛和经分散的纳米钛粉为反应前体，利用物理掺杂方法研究了掺钛RF凝胶的制备工艺，并在凝胶过程中以zeta电位 粒径分布测试仪对溶液的粒径分布进行分析测试。实验发现六偏磷酸钠对纳米钛粉的分散性最好，掺杂后凝胶时间明显缩短；分散剂种类和用量对凝胶时间有较大影响，其用量为纳米钛粉量的50~100倍为宜。     

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。     

隔热材料的纳米成型与性能分析

经不同工艺和过程制备二氧化硅气凝胶,初步摸索出制备温度、溶剂、催化剂、反应时间最佳参数.在分析气凝胶干燥开裂的原因后,以三甲基氯硅烷(TMCS)为表面修饰剂,正己烷为干燥介质的表面改性工艺,一定程度控制了气凝胶的干燥收缩和开裂.在室温、常压下的通过不同的改性方案制备出四种不同气凝胶样品,揭示了改性条件、干燥温度对于气凝胶孔隙分布、微观结构的影响.     

镍掺杂三聚氰胺-甲醛气凝胶的浸渍-还原法制备

以PdCl2为活化敏化液,水合肼为还原剂,采用化学浸渍-还原法在常温下制得了磁性金属Ni掺杂三聚氰胺-甲醛(MF)气凝胶,为金属掺杂气凝胶的制备寻得了新的途径。利用X-射线粉末衍射仪(XRD)、扫描电镜(SEM)、透射电镜(TEM)等对Ni掺杂MF气凝胶进行表征,SEM和TEM均表明,经浸渍-还原处理后的MF气凝胶骨架中较均匀地分布着粒径约100nm的金属Ni颗粒,其中部分颗粒生长连结形成较大团簇。N2吸-脱附实验数据显示,掺入金属Ni后,MF气凝胶的比表面积、总孔体积、微孔体积均减小,表明浸渍-还原处理后得到的金属Ni颗粒均匀分布于MF气凝胶孔隙中,其中少量大孔的出现是由形成团簇的Ni颗粒填充了部分纯MF气凝胶的孔隙撑开了孔隙结构所致。     

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。     

纳米多孔碳气凝胶的储氢性能

 以间苯二酚和甲醛为原料,采用溶胶-凝胶工艺,结合高温碳化和溶剂替换常压干燥技术,制备了碳气凝胶。通过改变间苯二酚与碳酸钠的物质的量比和反应物间苯二酚与甲醛的质量分数,实现对碳气凝胶孔洞结构的控制。制备了钯掺杂碳气凝胶。以透射电镜、X射线衍射谱证实了钯元素以纳米单质颗粒形式存在于碳气凝胶的骨架结构中。对掺杂碳气凝胶进行了活化工艺的后处理,成功提高了比表面积有2倍之多,获得了比表面积为1 273 m²/g的钯掺杂碳气凝胶。氢吸附性能研究结果表明：最优活化工艺所得的碳气凝胶样品（3 212 m²/g）在92 K,3.5 MPa条件下的饱和储氢质量分数为3%,此样品在303 K,3.2 MPa时的储氢质量分数为0.84%。对钯掺杂碳气凝胶的常温（303 K）氢吸附测试表明,掺杂后碳气凝胶的总储氢质量分数下降了,但单位比表面积的储氢质量分数提高了。     

红外光谱技术在纳米NiFe2O4制备过程中的应用

采用溶胶 凝胶法制备NiFe2 O4 纳米粉末 ,并经不同温度热处理 .测定了制备过程中各阶段的红外吸收光谱和不同温度处理样品的红外漫反射光谱 .结果表明 ,红外吸收光谱较好地反映了溶胶 凝胶法制备NiFe2 O4 纳米粉末过程中结构的变化 ,为确定热处理温度提供了实验依据 ,彻底消除有机物 ,热处理需在 40 0℃以上 ;红外漫反射谱可以较好地反映粉末的尺寸效应和形态效应 ,粉末粒径越小 ,漫反射函数 (K M)值越大 ;当粒径达到一定尺寸时 ,红外漫反射的尺寸效应消失     

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。     

纳米TiO2光催化剂防团聚的光谱研究

本文用溶胶 凝胶过程超临界CO2 萃取制备纳米二氧化钛气凝胶 ,用FT Raman ,FTIR ,FS分别对初生态气凝胶粒子、在常态下以气凝胶形式保存了 36 0天的TiO2 纳米粒子及以初生态气凝胶的粉体保存了36 0天的TiO2 粒子进行表征 ,以光催化降解甲基橙为模型反应 ,结果表明 ,在常态下以气凝胶形式保存纳米TiO2 粒子能有效地防止由纳米TiO2 表面超亲水性引起粒子间的团聚 ,保持了初生态粒子的光催化活性。     

超低密度SiO2气凝胶的制备及成型研究

 以正硅酸乙酯(TEOS)为硅源，采用酸碱二步催化溶胶-凝胶法，结合超临界干燥技术制备了超低密度SiO₂气凝胶,最低密度为3.4 mg/cm³；进一步结合成型工艺，在解决了模具设计和脱模技术后制备了具有不同密度的柱状和微型套筒样品，密度10～50 mg/cm³。研究了水、催化剂、稀释剂对二步溶胶-凝胶过程的影响，获得了制备低密度SiO₂气凝胶的最佳条件。利用扫描电镜、孔径分布及比表面积测试仪等对SiO₂气凝胶微结构进行了研究。结果表明，获得的超低密度SiO₂气凝胶具有较好的纳米网络，平均孔径18.9 nm，还具有高比表面积898 9 m²/g。     

Some comments on superfluid 3He placed in globally deformed aerogel

New experimental results focused on the behavior of the superfluid A-like phase placed in globally deformed aerogel environment are considered. We compare experimental data collected by using optically attested axially stretched silica aerogel, on the one hand, and “nematically ordered” aerogel consisting of nearly parallel Al₂O₃ · H₂O polymer strands, on the other. In the case of axially stretched silica aerogel the point of view was adopted according to which the orbital anisotropy axis l? is long-ranged. The experiments were carried out by pulsed NMR techniques in keeping the direction of an externally applied magnetic field normal to aerogel stretching axis. We have generalized the dipole-locked configuration for arbitrary angle of inclination of the magnetic field with respect to aerogel stretching axis. The experimental data collected in using “nematically ordered” aerogel cannot be reconciled with above-mentioned results.     

Low-temperature instability of uniform spin precession in the <Emphasis Type="Italic">B</Emphasis> phase of pure <Superscript>3</Superscript>He and <Superscript>3</Superscript>He in an aerogel

The magnetic-field dependences of the threshold temperature of the low-temperature instability of uniform spin precession in pure ³He-B and ³He-B in an aerogel have been determined for the bulk mechanism. These dependences appear to be different. The theoretical dependence of the threshold temperature for the pure case has been compared with the experimental dependence. The threshold temperature of the instability for ³He in the aerogel has been estimated for typical experimental conditions.     

Visible,near-infrared and infrared optical properties of silica aerogels

Silica aerogel is an excellent thermal insulation material with a low thermal conductivity and a high porosity and has attracted great concern in applications. This paper was to experimentally investigate the optical properties of optically thick silica aerogel in the visible, near-infrared and infrared spectrum region. The fiber-loaded silica aerogel sample was prepared through sol–gel technique and supercritical drying process. Silica fibers were added into the aerogel during the preparation procedure to strength the skeleton of aerogel. As a comparison with the fiber-load silica aerogel, a silica fiber composite sample with the same chemical component and different physical structure was also prepared. A simplified two-flux model neglecting the boundary effect was used to describe the radiation propagation characteristics inside the samples. The spectral normal-hemispherical reflectances, transmittances, and normal emittances of silica aerogel and silica fiber samples were measured and compared in the wavelengths of 0.38–15 μm. Then the spectral optical constants of samples were determined using the experimental data. The spectral absorption and scattering coefficients of silica aerogel were within (0.01 cm⁻¹, 31.0 cm⁻¹) and (1.4 cm⁻¹, 25.8 cm⁻¹). The results showed that the spectrum region where the scattering coefficient is low usually corresponds to a high absorption coefficient. In addition, the total radiation properties of samples were predicted at high temperatures. The analysis of optical properties of silica aerogel is necessary to provide valuable data in applications.     

Sol-gel synthesis of nanocomposite crystalline HMX/AP coated by resorcinol-formaldehyde

This work aims to improve the performance of composite explosive by using the sol-gel method to mix high explosive and oxidizer in nanoscale. Nanocomposite materials of HMX and AP were prepared by using resorcinol-formaldehyde (RF) as binder. Its structure was characterized by scanning electron microscopy (SEM), BET method, X-ray powder diffraction (XRD), and DSC. SEM images indicate that HMX/AP/RF aerogel has a laminate-like structure with uniform pores. The XRD results show that the mean crystal size of HMX is less than 100 nm; HMX and AP are mixed uniformly in nanoscale. The specific surface area of HMX/AP/RF is 27 m²/g and much less than that of RF aerogel. The mesopores and micropores of HMX/AP/RF aerogel mainly focus in the range of 2-20 and 0.6-1.6 nm, respectively. DSC analysis indicates that the thermal decomposition temperature of HMX/AP/RF is reduced compared to that of original HMX.     

Effects of particle size of silica aerogel on its nano-porous structure and thermal behaviors under both ambient and high temperatures

Silica aerogel as the most commonly used aerogel has attracted increasing attention from both academia and industries due to its extraordinary performances and potentials. Through this study, influences of the particle size (38–880 μm) on its nano-porous structure and thermal behaviors were addressed based on a series of experimental tests under both ambient and high temperatures (i.e., 1000 °C). It was known from the experimental results that the fractional densities of samples with particle sizes of 270–880 μm were similar, which were about 40% of the sample with a particle size of 38 μm. The ratio of densification was found decrease to about 10–40% when heating time increased from 10 to 90 min. For those samples with 150 μm or finer particles, SiC crystal with 70.8 nm particles was generated, and the pore shape was slit in the silica aerogel. The Brunauer–Emmett–Teller (BET) surface area, cumulative pore volume, and average pore diameter of those heated samples with over 75 μm diameter were about 40%, 20%, and 50% of those unheated (virgin) samples, respectively. Virgin samples showed 18% lower thermal conductivity for 75 μm particles compared to that of 38 μm, while for the heated samples, 38 μm particles showed a 28% lower thermal conductivity than that with 880 μm. Mixture of silica aerogel and other inorganic material particles are recommended for high-temperature applications, while the silica aerogel with different-sized particles are observed better for applications under ambient temperature.     

Nonlinear NMR in a superfluid B phase of <Superscript>3</Superscript>He in aerogel

The properties of liquid ³He in a low-density aerogel preliminarily covered with a few monolayers of ⁴He were studied by pulsed and nonlinear CW NMR techniques. It was found that an NMR frequency shift from the Larmor value exhibits a sharp increase at a magnetization tilting angle exceeding 104°. Nonlinear CW NMR signals related to the formation of a macroscopic region featuring homogeneous precession of the magnetization (homogeneous precession domain) were observed. The experimental results confirm that the low-temperature superfluid ³He phase in the aerogel is analogous to the B-phase in bulk ³He and indicate that the spin supercurrents play an important role in the spin dynamics of superfluid ³He in aerogel.     

EPR study of ordered Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-based aerogel

Samples of oriented aerogel based on aluminum oxide are studied by the electron paramagnetic resonance (EPR) technique under steady-state and pulse conditions. At least two types of paramagnetic centers interacting with Al nuclei on the surface of aerogel are revealed. Their spectra are characterized by the presence or absence of superhyperfine structure in the EPR spectra, respectively. The X-ray irradiation at room temperature gives rise to the formation of additional long-lived paramagnetic centers of the second kind. Their characteristic decay times for the “fast” and “slow” processes are determined. The interaction of induced paramagnetic centers with protons located on the surface of aerogel is revealed.