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(LaCl3·7H2O)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220m2·g-1,密度约为160mg·cm-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95m2·g-1,密度约为350mg·cm-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。     

浸渍过程对纳米纤维素/二氧化硅复合气凝胶结构与性能研究

纳米纤维素(CNF)气凝胶兼具传统气凝胶的优异特性和自身优良的生物相容性和可降解性,在很多领域应用前景广阔。然而纤维素自身的超亲水性严重限制了其更广泛的应用,为改善纤维素气凝胶的亲水性能,提高其综合应用性能,采用简单浸渍法在纤维素气凝胶基体中引入二氧化硅(SiO₂)颗粒制备纳米纤维素/二氧化硅复合气凝胶,利用傅里叶红外光谱仪(FTIR)分析纤维素气凝胶和复合气凝胶的化学结构;用扫描电镜(SEM)观察气凝胶的微观结构;测定气凝胶的物理、力学性能和接触角。结果表明,复合气凝胶在3 340 cm-1处-OH吸收峰较纤维素气凝胶均有所减弱,表明SiO₂的引入促使Si-OH形成,也降低了气凝胶的亲水性,同时有Si-CH₃和Si-O-Si吸收振动峰出现,表明三甲基氯硅烷(TMCS)的改性作用以及纤维素与SiO₂颗粒之间形成稳定化学键连接。浸渍时间影响硅含量,进而影响气凝胶的密度、比表面积和孔隙率。当浸渍时间为10 min时制备的复合气凝胶性能较好,其微观结构分布均匀,具有疏水性能,接触角可达152°,同时气凝胶仍具有较好的力学性能和较低密度,其压缩模量和压缩性能分别为5.91和1.38 MPa,密度为0.1 g·cm-3。     

种子法制备金掺杂二氧化硅气凝胶

 采用羟胺种子法合成了金掺杂二氧化硅气凝胶。采用紫外 可见光分光光度计研究了还原过程中体系的变化情况。使用透射电镜（TEM）研究了气凝胶的微观结构，气凝胶的比表面积和孔径分布由BET-BJH方法测试。结果表明通过种子法可以制备金掺杂质量分数0.01%~1.00%，密度25～50 mg／cm³，比表面积达800 m²/g以上的SiO₂气凝胶样品。     

氮掺杂碳气凝胶电极材料的制备及性能

以三聚氰胺（M）、间苯二酚（R）和甲醛（F）为原料,经溶胶-凝胶法、超临界干燥和高温碳化制备了系列的氮掺杂碳气凝胶（NCAs）。X射线光电子能谱(XPS)分析表明,氮元素成功地引入到碳气凝胶中,并且可以通过调节三聚氰胺掺杂量来控制氮掺杂量;扫描电子显微镜（SEM）和N2吸附测试显示出不同氮掺杂量的碳气凝胶的微观结构差异较大,随着氮含量的增加,比表面积有先减后增的趋势;在6 mol/L KOH溶液中进行的恒流充放电和循环伏安测试表明,引入氮元素能够极大地改善碳气凝胶的电化学性能,最高比电容量达176 Fg-1,并且凝胶具有良好的电容特性和可逆性。     

多面体低聚倍半硅氧烷-ZrO2复合气凝胶的制备与表征

以官能团化的多面体低聚倍半硅氧烷（POSS-［C2H4Si(OEt)3］8）和正丁醇锆为原料,以乙醇作为溶剂,通过溶胶-凝胶及二氧化碳超临界干燥成功制备了三种不同锆含量POSS-ZrO2的复合气凝胶。并用傅里叶变换红外光谱分析仪（FTIR）、扫描电镜（SEM）、X射线衍射仪（XRD）和比表面吸附仪（BET）对其进行表征。结果表明:该气凝胶中有SiOZr键,并且所得气凝胶都是无定型的,其比表面积随着锆含量的增加而变小,最高可达491 m2/g,并且其孔径分布都比较广。     

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。     

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。     

超低密度SiO2气凝胶的制备研究

超低密度的SiO2气凝胶是一种经典的三维网状纳米多孔材料,已经广泛应用于如保温隔热、吸附等多种领域。以四甲氧基硅烷(TMOS)为硅源,采用酸碱两步法,利用乙醇超临界干燥技术制备了超低密度的SiO2气凝胶,分别利用SEM\TEM\BET等表征手段对该气凝胶进行了一系列的研究,发现当其密度为0.6 mg/cm3时,气凝胶拥有最佳的综合性能。该种气凝胶具有超低密度、高比表面积、加工成型性好、制备周期短等优点,有望在激光惯性约束聚变实验中作为冷冻靶发挥巨大的作用。     

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。     

碳气凝胶及活化碳气凝胶电极材料制备与性能

 以间苯二酚(R)-甲醛(F)为原料,制备了有机气凝胶和碳气凝胶,并对其进行二氧化碳活化。X射线衍射(XRD)测试表明,二氧化碳渗入到碳气凝胶网络结构发生反应,造成(002)峰和(100)峰减弱;扫描电子显微镜(SEM)测试表明,活化没有破坏碳气凝胶的骨架结构,而是增加了大量的nm尺度微孔,从而大大提高了碳气凝胶的比表面积和微孔比例。在1 mol/L KOH电解液中进行了循环伏安和计时电位扫描测试,电极材料电化学性能稳定,具有较好的可逆性,在1 mA/s电流密度下进行充放电测试,得到活化前电极比电容为103 F/g,活化后由于比表面积的增加,比电容达到371 F/g,是一种理想的电化学电极材料。     

High specific surface area TEOS-based aerogels with large pore volume prepared at an ambient pressure

The experimental results on the synthesis of tetraethoxysilane (TEOS)-based silica aerogel with high specific surface area and large pore volume, via ambient pressure drying (APD) route, are reported. The silica aerogels were prepared by the acid-base sol-gel polymerization of TEOS precursor followed by the drying of the alcogels at an ambient pressure. The solvent present in the alcogel (i.e. ethanol) was replaced by a non-polar solvent such as hexane prior to the surface modification step. In order to minimize the drying shrinkage, the surface of the gels was modified using trimethylchlorosilane (TMCS) before the APD. The FTIR spectra of the surface modified aerogels showed Si-CH₃ peaks at 2965 and 850 cm⁻¹. The effect of the base catalyst (NH₄OH) addition to the sol, at different time intervals (T), on the physical and textural properties of the resulting aerogels has been investigated. It has been observed that the surface area and the cumulative pore volume of the aerogels enhanced considerably from 819 to 1108 m² g⁻¹ and 2.65 to 4.7 cm³ g⁻¹, respectively with an increase in the T value from 6 to 48 h. Silica aerogels with very low bulk density (0.06 g cm⁻³), extremely high specific surface area (1108 m² g⁻¹) and large cumulative pore volume (4.7 cm³ g⁻¹) could be synthesized by drying the alcogels at the ambient pressure. The aerogels were mesoporous solids with the average pore size ranging from 12 to 17 nm. The results have been discussed by taking into consideration the hydrolysis and condensation reactions during the sol-gel polymerization of the TEOS precursor.     

间苯三酚-乙醛有机气凝胶的制备与表征

 以碳酸钠为催化剂,乙醇为溶剂,间苯三酚 乙醛为反应前躯体,经溶胶 凝胶、交联老化、二氧化碳超临界干燥制备出间苯三酚-乙醛(PA)有机气凝胶。扫描电镜观察和N2吸附测试结果表明：气凝胶具有较高的比表面积,是一种连续nm级３维网络结构的多孔材料,其比表面积为1 210 m²/g,平均孔径为11 nm,与传统有机气凝胶相比,提高了比表面积,一定程度上实现有机气凝胶的扩孔。     

Aerogel–copper nanocomposites prepared using the adsorption of a polyfluorinated complex from supercritical CO2

A supercritical deposition method has been used to synthesize aerogel?Ccopper nanocomposites. Carbon, resorcinol?Cformaldehyde, and silica aerogels (CAs, RFAs, and SAs) were impregnated with a new polyfluorinated copper precursor (CuDI6), which has a high solubility in supercritical carbon dioxide (scCO₂). Adsorption isotherms of CuDI6 onto various aerogels from scCO₂ were determined at 35?°C and 10.6?MPa using a batch method which is based on the measurement of the fluid phase concentration. The relative affinity between CuDI6 and different aerogels changed in the following order: CA?>?RFA?>?SA. The effect of temperature on the adsorption isotherms for the CuDI6?CCO₂?CCA system was also studied at 35 and 55?°C and at a CO₂ density of 736.1?kg/m³. The CuDI6 uptake at a particular CuDI6 concentration increased with increasing temperature. Adsorbed CuDI6 was found to convert into Cu and Cu/Cu₂O nanoparticles on the aerogel supports after chemical or thermal treatments at ambient pressure and at temperatures ranging from 200 to 400?°C.     

Study of deposition patterns of plating layers in SiC/Cu composites by electro-brush plating

SiC reinforced copper composite coatings were prepared by electro-brush plating with micron-size silicon carbide (SiC) ranging from 1 to 5 μm on pure copper sheet in this paper. The micro-structural characterizations of SiC/Cu composite coatings were performed by optical microscope and Scanning Electron Microscope (SEM) coupled with spectrometer, to study co-deposition mechanism of SiC/Cu. It was found that there were three different patterns of SiC deposition in plating layers during electro-brush plating process, i.e. the particles could deposit inside copper grains, in grain boundaries, or in holes of the surface. To investigate deposition mechanism of each pattern, size of SiC and copper grains was compared. By comparison of size of copper grains and hard particles, SiC were either wrapped in copper grains or deposited in grain boundaries. Moreover, electro-brush plating layers at different brush velocities and current densities were obtained respectively, to analyze the microstructure evolution of the composite coatings. The hardness of plating layers was measured. The results indicated at the current density of 3 A/dm², the SiC/Cu coating was compact with SiC content at a high level and the hardness reached a maximum.     

锌基复合气凝胶的微观结构

以ZnCl2为前躯物,不同相对分子质量的聚丙烯酸为模版剂,环氧丙烷作为催化剂,超临界干燥成功制得了锌基复合气凝胶。运用场发射扫描电镜、高分辨透射电子显微镜和N2等温吸附测试对气凝胶的微观结构进行了表征。结果表明,制备的锌基复合气凝胶呈现三维网络状结构,其三维结构是由大量微小颗粒组成,颗粒的粒径为nm量级,为介孔材料。选用相对分子质量为1800的聚丙烯酸作为模版剂制备的气凝胶的微观结构最好,无明显的塌陷和团聚现象,其比表面积为236 m2/g,平均孔径分布在11 nm左右,总的孔体积为0.179 cm3/g。     

Studies of the microstructure of a superconducting Nb<Subscript>3</Subscript>Sn-Band obtained from (Cu/Nb)/Cu12Sn nanocomposite

A multilayer layer from the superconducting compound Nb₃Sn was obtained by the thermal treatment of composite (Cu/Nb)/Cu12Sn conductor consisting of Cu-12% Sn and Cu/Nb interlayers consisting in turn of nanosized copper and niobium layers. The conductor was coated with copper from the outside, which served as a stabilizer. The microstructure of the cross section of the composite band in dependence on the volume ratio of Cu/Nb and bronze interlayers and the microstructure of the Cu/Nb interlayers themselves in dependence on the annealing temperature were investigated. The optimum ratio of composite components was as follows: t _Nb N _Nb ≈ 0.288t _CuSn N _CuSn, where t and N are the thickness and number of the niobium and bronze layers, respectively. Trying to maintain the optimum design of the conductor forced us to increase the bronze volume content relative to the content of Cu/Nb interlayers, which had a negative impact on the composite microstructure. This resulted in disruptions of Cu/Nb interlayers. A technique has been developed for producing the (Cu/Nb)/Cu12Sn composite as a precursor to the band from the Nb₃Sn compound with allowance for the first experiment’s shortcomings.     

γ-射线辐射还原法制备金属铜掺杂MF气凝胶

采用γ射线辐射还原法,在不同总吸收剂量条件下制备了金属Cu掺杂三聚氰胺-甲醛(MF)有机气凝胶复合材料。利用X-射线衍射仪(XRD)、电感耦合等离子体吸收光谱(ICP-AES)仪和扫描电子显微镜,测试证实了辐射还原法能成功地在MF气凝胶中还原出金属Cu。扫描电子显微镜(SEM)图谱表明在100kGy和200kGy的总吸收剂量下,在MF气凝胶中还原的金属Cu粒子的粒径较小,不会形成金属团聚区,而在较高的总吸收剂量下(大于200kGy),在MF气凝胶中还原的Cu会形成金属团聚区。N2吸附测试表明,还原的金属Cu会堵塞MF气凝胶的一部分微孔和一部分介孔,从而使样品的比表面积和吸附量降低。随着总吸收剂量不断增加,经辐照后样品中金属Cu的含量也不断增加,同时还会影响还原出金属Cu的分布和形貌。     

Kinetics study for photodegradation of methylene blue dye by titanium dioxide powder prepared by selective leaching method

The kinetics of photodegradation of methylene blue (MB) dye by titanium dioxide (TiO₂) powder were investigated using elementary reactions. TiO₂ powders were prepared by a selective leaching method consisted of processes of CaHPO₄ precipitation, heat treatment, and acid leaching to obtain high crystalline anatase. The obtained TiO₂ samples had wide ranges of specific surface areas (5–23 m²/g) and densities of Ti³⁺ defects (90–480×10¹²spin/g) without a significant change in the anatase phase ratio ranging 0.86–0.91 in mass ratio. The MB photodegradation rate was expressed as functions of specific surface area and density of Ti³⁺ defects under the experimental condition that the photodegradation rate was proportional to UV irradiation intensity and the adsorbed MB amount was proportional to specific surface area. A proposed equation for calculation of photodegradation ate demonstrated greater effect of specific surface area than density of Ti³⁺ defects for MB photodegradation.     

Ag-Cu离子注入玻璃后不同气氛退火的光吸收研究

采用MEVVA源（metal vapor vacuum arc ion source）引出的强束流脉冲Ag,Cu离子先后注入到SiO₂玻璃，x射线光电子能谱仪（XPS）分析显示Ag，Cu大多仍为金属态，有部分氧化态Cu存在.透射电镜观察分析和光学吸收谱都表明在衬底中形成了纳米合金颗粒.结合有效媒质理论，得到模拟的光学吸收谱，与实验结果基本符合，较好地验证了以上结论.样品退火后颗粒发生分解，分解的颗粒在氧化气氛下被氧化，且有部分向样品表面蒸发；在还原气氛下氧化态元素被还原并成核生长.故 关键词： 离子注入 纳米颗粒 退火 光学吸收率