炭气凝胶微球的制备及在锂离子电池负极材料中的应用

以间苯二酚和甲醛为原料,在催化剂和表面活性剂的作用下经溶胶-凝胶、超临界干燥、炭化等过程合成一种新型的炭气凝胶微球。采 用扫描电镜(SEM)、X-射线衍射(XRD)、低温氮吸附（BET）和充放电测试等表征了炭气凝胶微球微观形貌、结构和电化学性能。结果表明:炭气 凝胶微球具有纳米网络结构（孔径集中分布在3.5nm左右）,微球直径≤40μm,比表面积为555m²/g。电化学性能表现出很大的首次不可逆容量 损失,这主要与材料大的比表面积有关。但在首次循环后,具有良好的循环性能,循环20次后可逆充电容量为281mAh/g,循环效率达到100％ 。     

MTES疏水改性SiO2气凝胶修饰活性炭复合材料的制备及结构表征

采用原位聚合法,以正硅酸四乙酯(TEOS)为原料、甲基三乙氧基硅烷(MTES)为疏水改性剂,活性炭为载体,制备疏水SiO2气凝胶修饰活性炭复合材料。采用接触角分析仪、N2吸附法、傅里叶红外光谱仪(FT-IR)、扫描电子显微镜(SEM)对疏水SiO2气凝胶修饰活性炭复合材料的表面特性和结构进行表征。结果表明:所制备的疏水SiO2气凝胶修饰活性炭复合材料的接触角为156°、比表面积为759.2 m2/g、孔体积为4.38 cm3/g,最可几孔径是32nm,孔径主要分布为1～50 nm,疏水SiO2气凝胶均匀地分散于活性炭表面。     

Synthesis and characterization of wormhole-like mesoporous Ce0.6Zr0.35Y0.05O2 solid solutions

Nanoparticles of Ce0.6Zr0.35Y0.05O2 (CZY) solid solution have been prepared by the CTAB (hexadecyl-trimethyl ammonium bromide), CTAB-EG (ethylene glycol) templating, and CTAB-EG-NaCl (in which the pores of the precursor synthesized by the CTAB-EG method is filled by a certain amount of NaCl) method, respectively. The physical properties of these materials were characterized by means of tech-niques such as X-ray diffraction (XRD), high resolution scanning electron microscopy (HRSEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and N2 adsorp-tion-desorption measurements. The CZY samples synthesized by the above three methods display wormhole-like mesoporous morphology and cubic crystal structures. The materials are narrow in pore size distribution (averaged pore diameter = 5.3―7.1 nm), high in surface areas (95―119 m2/g), and large in pore volumes (0.16―0.18 cm3/g). It has been demonstrated that the introduction of NaCl is capable of retaining the pore structures of solid nanomaterials at high-temperature calcination.     

Mn_2O_3/CRF复合材料的制备及其在超级电容器中的应用

通过采用沉淀法在碳气凝胶表面负载金属氧化物三氧化二锰,制备得到Mn_2O_3/CRF复合材料。采用X射线衍射及电镜扫描等技术对所制备的复合材料进行结构形貌表征。实验结果发现碳气凝胶具有多重片层结构且孔隙发达。通过调节锰盐的含量考察三氧化二锰负载量对复合材料电化学性能的影响作用。采用循环伏安法及充放电测试对材料的电化学性能进行测试,结果表明Mn_2O_3/CRF复合材料具有良好的电容性及较好的可逆性。当Mn_2O_3含量达15%时复合材料的比电容最大,可达118.5 F/g。通过充放电测试1000次后发现该电极的比电容依然能够保持在一稳定值上,具有较好的稳定性。     

SiO2气凝胶的常压制备与表面改性

以水玻璃为硅源,甲酰胺为催化剂,乙二醇为干燥控制化学添加剂(DCCA),采用溶胶-凝胶法常压下干燥制备了硅石气凝胶粉体.研究发现:微过量的甲酰胺,有利于高孔隙率气凝胶的合成;过量的乙二醇的引入不利于低密度气凝胶的形成;pH值对合成气凝胶的性质也有较大的影响.经二甲基二乙氧基硅烷(DMDEOS)表面改性处理后的气凝胶表现出了很好的疏水性能.采用傅里叶变换红外分析(FTIR)、热重分析(TG)、示差扫描量热分析(DSC)等对疏水型气凝胶的结构和性能进行了研究.     

Influence of pore size optimization in catalyst layer on the mechanism of oxygen transport resistance in PEMFCs

In PEMFC, the oxygen transport resistance severely hinders the cell from achieving high performance. In this paper, pore-forming agent was used to optimize the pore size distribution of the catalyst layer (CL), and to study its effect on the mechanism of oxygen transport resistance, including molecular diffusion resistance, Knudsen diffusion resistance, and local O₂ resistance in CL. The results showed that with the pore formation the cell performance had a significant improvement at high current density, mainly due to its better oxygen transport properties, especially under low platinum conditions. The addition of pore-forming agent moved the pore diameter toward a larger pore diameter with a range from 70 to 100 nm, and also obtaining a higher cumulative pore volume. It was found that the increase of the cumulative pore volume and larger pore size were conducive to the diffusion of oxygen molecules in CL, and the resistance caused by which was the dominant part in total transport resistance. Further tests indicated that the improvement of molecular diffusion resistance was much larger than that of Knudsen diffusion resistance in the catalyst layer after pore formed. In addition, the optimized pore structure will also get a higher number of effective pores, which resulted in an increased effective area of the ionomer on the Pt surface. The higher effective area of the ionomer was particularly beneficial for the reduction of local O₂ resistance with low Pt loading.     

Influence of deposition time on the morphology and optical properties of SiO<Subscript>2</Subscript>-ZnO composite photonic crystals

SiO2 photonic crystal were successfully prepared by vertical deposition and then used as a template to fabricate SiO2-ZnO composite photonic crystals on ITO substrates by electrodeposition and subsequent calcination. A number of different deposition times were used. The morphologies of the silica opals and SiO2-ZnO composite photonic crystals were investigated by scanning electron microscopy. It was found that ZnO particles grew randomly on the surfaces of the silica spheres when the deposition time was short. As the deposition time was increased, the ZnO particles grew evenly on the surfaces of the silica spheres so that the interstitial space of the silica template was filled with ZnO particles. Reflectance spectra of the SiO2-ZnO composite crystals revealed that all of the fabricated photonic crystals exhibit a photonic band gap in the normal direction.     

Immobilization of 12-phosphotungstic heteropolyacid on amine-functionalized SiO<Subscript>2</Subscript> for tetrahydrofuran polymerization

The 12-phosphotungstic heteropolyacid (HPW) was immobilized on the surface of a silica carrier modified by the amine groups of organosilane γ-aminopropyl triethoxysilane (APTES), and its catalytic performance was investigated for tetrahydrofuran (THF) ring-opening polymerization. This amine-functionalized catalyst exhibited better activity, and the polytetramethylene ether glycol (PTMG) yield was 63.7%. The 12-phosphotungstic heteropolyacid supported on aminopropyl-functionalized SiO₂ support (HPW/SiO₂-APTES) was reused four times and showed a good maintenance of activity which was better than that of the conven-tional catalyst HPW supported on SiO₂ (HPW/SiO₂). These results were obtained using infrared spectroscopy, nuclear magnetic resonance spectroscopy, nitrogen adsorption and X-ray diffraction. HPW on the HPW/SiO₂-APTES catalyst exhibited higher dispersed state and maintained a more stable structure than that of the HPW/SiO₂ sample.     

硅气凝胶制备及其作为催化剂载体在甲烷部分氧化反应中的应用

采用超临界干燥(SCD)法和以溶剂置换、表面改性为基础的常压干燥(APD)法分别制得二氧化硅气凝胶.采用N2低温物理吸附脱附法、红外光谱(FT-IR)、X射线衍射(XRD)实验和扫描电子显微镜(SEM)等手段对两种方法制备的气凝胶的理化性能进行了表征.结果表明:SCD法和APD法制备的二氧化硅气凝胶的比表面积分别为1 016和846 m2/g,最可几孔径分别位于孔径大小14.5和11.5 nm处.SCD法制备的二氧化硅气凝胶的孔径分布范围和较大孔的数量均较APD法制备的要宽和多.而以两种方法制备的二氧化硅气凝胶为载体,硝酸镍为镍源,采用浸渍法制备的二氧化硅气凝胶负载镍催化剂中,镍均以极微小的颗粒形式高度分散于二氧化硅气凝胶载体上.对甲烷部分氧化(POM)制合成气反应,用两种方法(SCD和APD)制备的二氧化硅气凝胶载体为基础的负载镍催化剂对产物一氧化碳和氢气的选择性相差不大,但甲烷转化率则呈现明显的差异.     

Preparation and radar-absorbing properties of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/TiO<Subscript>2</Subscript>/Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>/Yb<Subscript>2</Subscript>O<Subscript>3</Subscript> composite powder

Al₂O₃/TiO₂/Fe₂O₃/Yb₂O₃ composite powder was synthesized via the sol-gel method. The structure, morphology, and radar-absorption properties of the composite powder were characterized by transmission electron microscopy, X-ray diffraction analysis and RF impedance analysis. The results show that two types of particles exist in the composite powder. One is irregular flakes (100-200 nm) and the other is spherical Al₂O₃ particles (smaller than 80 nm). Electromagnetic wave attenuation is mostly achieved by dielectric loss. The maximum value of the dissipation factor reaches 0.76 (at 15.68 GHz) in the frequency range of 2-18 GHz. The electromagnetic absorption of waves covers 2-18 GHz with the matching thicknesses of 1.5-4.5 mm. The absorption peak shifts to the lower-frequency area with increasing matching thickness. The effective absorption band covers the frequency range of 2.16-9.76 GHz, and the maximum absorption peak reaches -20.18 dB with a matching thickness of 3.5 mm at a frequency of 3.52 GHz.     

环境气压干燥新工艺快速合成SiO2气凝胶研究

以廉价的水玻璃为硅源,用乙醇（EtOH）／三甲基氯硅烷（TMCS）／庚烷混合溶液浸泡水凝胺,使对水凝胶的溶剂交换和表面改性在一步完成,在环境干燥条件下合成了SiO2气凝肢．所合成的SiO2气凝肢为轻质透明的块状固体,密度为0．128～0．165g／cm^3,孔隙率92．4％～94．2％．利用FT—IR、SEM、TEM和BET吸附对气凝肢的微观结构和形貌进行了研究,结果表明,气凝胶为纳米介孔结构,粒子直径和孔径分布均匀,断面呈现明显的蜂窝状结构,孔径13nm左右,比表面积约618m^2／g,表面带有较多的Si—CH3基团．     

Effect of reinforcement content on the adhesive wear behavior of Cu10Sn5Ni/Si3N4 composites produced by stir casting

The main objective of this paper was to fabricate Cu10Sn5Ni alloy and its composites reinforced with various contents of Si₃N₄ particles (5wt%, 10wt%, and 15wt%) and to investigate their dry sliding wear behavior using a pin-on-disk tribometer. Microstructural examinations of the specimens revealed a uniform dispersion of Si₃N₄ particles in the copper matrix. Wear experiments were performed for all combinations of parameters, such as load (10, 20, and 30 N), sliding distance (500, 1000, and 1500 m), and sliding velocity (1, 2, and 3 m/s), for the alloy and the composites. The results revealed that wear rate increased with increasing load and increasing sliding distance, whereas the wear rate decreased and then increased with increasing sliding velocity. The primary wear mechanism encountered at low loads was mild adhesive wear, whereas that at high loads was severe delamination wear. An oxide layer was formed at low velocities, whereas a combination of shear and plastic deformation occurred at high velocities. The mechanism at short sliding distances was ploughing action of Si₃N₄ particles, which act as protrusions; by contrast, at long sliding distances, direct metal-metal contact occurred. Among the investigated samples, the Cu/10wt% Si₃N₄ composite exhibited the best wear resistance at a load of 10 N, a velocity of 2 m/s, and a sliding distance of 500 m.     

CO_2超临界干燥制备SiO_2气凝胶及其表征

以正硅酸乙酯为原料,应用溶胶—凝胶两步催化法制备SiO2醇凝胶,醇凝胶用CO2超临界干燥后得到SiO2气凝胶.以比表面积和密度为评价标准,以CO2流量、超临界温度、干燥时间和超临界压力为实验因素,设计了四因素三水平的正交实验,研究CO2超临界干燥的工艺条件,并运用SEM、TEM、BET、FTIR对SiO2气凝胶结构、形貌及化学组成进行分析.结果表明：优化的工艺条件为CO2流量12 kg.h-1,干燥压力13 mPa,超临界温度45℃,干燥时间6 h.制得SiO2气凝胶的比表面积为927.37 m2.g-1,密度是0.195 6 g.cm-3,由球形纳米颗粒堆积而成,颗粒尺寸范围在0～20 nm左右,孔径分布主要集中在10 nm左右,是典型的纳米孔材料.     

Solid FeS lubricant:a possible alternative to MoS2 for Cu-Fe-based friction materials

Molybdenum disulfide (MoS₂) is one of the most commonly used solid lubricants for Cu-Fe-based friction materials. Nevertheless, MoS₂ reacts with metal matrices to produce metal sulfides (e.g., FeS) and Mo during sintering, and the lubricity of the composite may be related to the generation of FeS. Herein, the use of FeS as an alternative to MoS₂ for producing Cu-Fe-based friction materials was investigated. According to the reaction principle of thermodynamics, two composites-one with MoS₂ (Fe-Cu-MoS₂ sample) and the other with FeS (FeS-Cu₂S-Cu-Fe-Mo sample), were prepared and their friction behaviors and mechanical properties were compared. The results showed that MoS₂ reacted with the Cu-Fe matrix to produce FeS, metallic ternary sulfides, and Mo when sintered at 1050℃. The MoS₂-Cu-Fe and FeS-Cu₂S-Cu-Fe-Mo samples thereby exhibited similar characteristics with respect to phase composition, density, hardness, and tribological behaviors. Micrographs of the worn surfaces revealed that the stable friction regime for both composites stemmed from the iron sulfides friction layers rather than from the molybdenum sulfides layers.     

二甲基硅油/硅溶胶共前驱体法制备二氧化硅气凝胶微球

由于二氧化硅气凝胶具有低密度、高孔隙率、高比表面积、低导热系数等特点,引起了人们的广泛关注。但是,其较差的机械性能和较高的制备成本一直限制二氧化硅气凝胶的应用和推广。采用带有活性端基的二甲基硅油和硅溶胶制备共前驱体溶液,以微乳液法和滴定法分别制备了不同尺寸的二氧化硅气凝胶微球,并探究了甲基含量对其性能的影响。实验结果表明,相对于滴定法,微乳液法制备的气凝胶粒径分布范围较宽,在硅溶胶与硅油体积比相同时,两种方法所制备的气凝胶微球具有相近的比表面积、堆积密度及导热系数;滴定法制备的气凝胶随着甲基含量减少,气凝胶微球的比表面积减小,堆积密度增大,接触角减小,导热系数增大,机械强度增大。     

3,4-dichlorotoluene ammoxidation to 3,4-dichlorobenzonitrile over VPO/SiO<Subscript>2</Subscript> catalyst

Ammoxidation of 3,4-dichlorotoluene (DCT) to prepare 3,4-dichlorobenzonitrile (DCBN) over silica supported vanadium phosphorus oxide catalysts has been studied. On the VPO/SiO₂ catalyst, the influence of the reaction temperature, the molar ratio of air/DCT, the molar ratio of NH₃/DCT in the feed gas and the space velocity (v ₁) on the conversion, yield and selectivity was observed. The most appropriate reaction condition is: reactionT=673 K,n(DCT):n(NH₃):n(air)=1:7:30 andv ₁=250 h⁻¹. At this optimum reaction condition, the conversion of DCT is 97.8%; the molar yield of DCBN is 67.4%. It was found that the addition of element phosphorus can improve the yield of DCBN compared with VO/SiO₂ catalyst. Foundation item: Supported by Youth Chen-Guang Project of the Committee of Science and Technology of Wuhan (20015005042) Biography: Huang Chi(1972-), male, Ph D, Lecture, research direction: ammoxidation.     

干燥溶剂介质对常压制备SiO2气凝胶的影响

以正硅酸乙酯和乙醇等为原料,通过溶胶-凝胶、表面修饰及溶剂置换等后续工艺,实现常压干燥法制备块状SiO2气凝胶,并考察干燥溶剂介质对气凝胶常压制备的影响。研究结果表明:采用混合溶剂干燥的SiO2气凝胶性能较单一溶剂更佳,以正己烷和甲苯混合溶剂制备的SiO2气凝胶性能最优,具有低表观密度(0.102 7 g/cm3)、高比表面积(928.4 m2/g)、大孔容(3.295 cm3/g)及疏水性良好等特性。     

SiO2气凝胶的溶胶-凝胶/共沸蒸馏法制备及表征

以工业水玻璃为硅源,采用溶胶-凝胶和共沸蒸馏的方法在常压下制备SiO2气凝胶,研究制备条件对SiO2气凝胶性能的影响.结果表明,当溶液体系的pH值为4.5,添加2 mL甲酰胺作为干燥控制化学添加剂(DCCA),并以正丁醇与凝胶中的水为共沸蒸发介质时,所制备的SiO2气凝胶具有典型的气凝胶结构特征,经分析SiO2气凝胶的...     

Structural and electrical properties of HCl-polyaniline-Ag composites synthesized by polymerization using Ag-coated (NH4)2S2O8 powder

Ag nanoparticles were sputter-deposited on ammonium persulfate ((NH₄)₂S₂O₈) powder to obtain (NH₄)₂S₂O₈-Ag powder, which was used to synthesize the HCl-doped polyaniline-Ag (HCl-PANI-Ag) composite via a polymerization procedure. The Ag nanoparticles were dispersed in the HCl-PANI matrix, and their sizes mainly ranged from 3 to 6 nm. The Ag nanoparticles did not affect the structure of emeraldine salt in the composite, and they increased the ordered crystalline regions in the HCl-PANI matrix. The HCl-PANI-Ag composite had a conductivity of (6.8 ±0.1) S/cm, which is about four times larger than that of the HCl-PANI. The charge transport mechanism in the composite is explained by the three-dimensional Mott variable-range hopping (3D-Mott-VRH).     

Three-dimensional tubular carbon aerogel for supercapacitors

A three-dimensional elastic carbon nanotube aerogel is fabricated via a simple solution-based strategy using Te nanowires as templates, which can be recycled. The pipe diameter and wall thickness of the carbon nanotube are strongly dependent on the diameter of the Te nanowires and carbon source. The obtained free-standing carbon nanotube aerogel with a large specific surface area (up to 1865 m2?g-1) is promising as an electrode material for supercapacitors. After combination with MnO₂, the capacitor exhibits a specific capacitance of 360.4 F?g-1 at a current of 1 A?g-1 and retention of 97% after 2000 cycles. The high power capabilities and good stability make it a promising candidate as an electrode for supercapacitors.