Controllable fabrication of carbon aerogels

Nano-pore carbon aerogels were prepared by the sol-gel polymerization of resorcinol (1,3-dihydroxybenzene)(C6H4(OH)2) with formaldehyde (HCHO) in a slightly basic aqueous solution, followed by super-critical drying under liquid carbon dioxide as super-critical media and carbonization at 700 ℃ under N2 gas atmosphere. The key of the work is to fabricate carbon aerogels with controllable nano-pore structure, which means extremely high surface area and sharp pore size distribution. Aiming to investigate the effects of preparation conditions on the gelation process, the bulk density, and the physical and chemical structure of the resultant carbon aerogels, the molar ratio of R/C (resorcinol to catalyst) and the amount of distilled water were varied, consequently two different sets of samples, with series of R/C ratio and RF/W (Resorcinol-Formaldehyde to water, or the content of reactant) ratio, were prepared. The result of N2 adsorption/desorption experiment at 77 K shows that the pore sizes decreasing from 11.4 down tO2.2 nm with the increasing of the molar ratio of R/C from 100 to 400, and/or, the pore sizes decreasing from 3.8 down to 1.6 nm with the increasing of reactant content from 0.4 to 0.6.     

常压制备低密度高比表面积SiO_2气凝胶的工艺研究

以正硅酸乙酯、乙醇、去离子水、盐酸和氨水为原料制备出SiO_2凝胶后,经老化、表面改性、溶剂置换工艺,再通过常压干燥制备出SiO_2气凝胶,研究了表面改性及溶剂置换工艺对SiO_2气凝胶性能的影响.结果表明,随着表面改性次数和改性剂浓度的增加,气凝胶的密度和比表面积降低;溶剂置换对气凝胶的密度和比表面积影响不大.通过优化的工艺制备出的SiO_2气凝胶具有疏水性,与水的接触角约为118°,密度为0.124 g/cm~3,孔隙率94.3%,平均孔径为23.3 nm,比表面积712 m~2/g.     

Electrochemical performances of hydrogen storage alloys treated using a new milling technique

A new self-made additive of amidocyanogen-acetic salt was used in wet bail-grind technique (WBGT) for preparing hydrogen storage alloys, and the effect on the electrochemical performance of the alloy electrode was investigated in detail. It was found that the prepared electrode had perfect electrochemical performances, such as rapid activation, high capability, high-rate discharge (HRD) ability, and good stability. The first discharge capacitance at 0.2 C (throughout this study, n C rate means that the rated capacity of a hydrogen storage alloy (full capacity) is charged or discharged completely in 1/n h) reached 278mAh.g-1 and the discharge capacitance reached the maximum of 322mAh·g-1 only after two charge-discharge cycles. For the dry method, wet method, and WBGT, the high rate discharge (HRD) values (C5C/C0.2C ratio) were approximately 0.59, 0.76, and 0.83, respectively. The stable discharge capacity at 3 C increased from 275mAh·g-1 (dry method) to 295mAh·g-1 (WBGT).     

常压干燥法制备CNTs掺杂TiO2气凝胶

以钛酸丁酯为原料,乙酸为有机配体,甲酰胺为干燥控制化学添加剂(DCCA),采用溶胶凝胶法制备碳纳米管(CNTs)掺杂TiO2复合醇凝胶,并结合常压干燥等后续工艺,制备了CNTs掺杂TiO2块体气凝胶。采用XRD、BET、TEM、SEM、EDS、DSC及FT-IR等对样品进行表征。结果表明:制备态CNTs掺杂TiO2气凝胶晶型为无定型,比表面积为601.7 m2/g;在氮气保护下,经950℃热处理后,比表面积为136.8 m2/g,TiO2以锐钛矿相存在,且均匀密集包覆在CNTs表面,对甲基橙光降解具有较高光催化活性。     

Effect of dehydration on porous structure of monolithic aerogels based on fibrous aluminum oxyhydroxide

Aluminum oxide monolithic aerogels (PMAOs) with specific surfaces of up to 400 m²/g and densities of up to 0.004 g/cm³ were obtained by the direct oxidation of metallic aluminum by water vapors. Studies of the obtained aerogels using the methods of scanning and transmission electron microscopy showed that a freshly prepared aerogel represents the amorphous structure from alumina fibrous with a diameter of about 5 nm. Parameters of a porous aerogel structure were determined from the isotherms of adsorption of nitrogen vapors at 77 K. It is shown that the specific surface area decreases by 50% upon the dehydration of aerogel by temperature pretreatment at 900°C until the phase transition temperature is reached. At the same time, heat treatment at temperatures above 1200°C results in a phase transition at which significant contraction of structure occurs and the specific surface area decreases to 20 m²/g. The number of primary adsorption centers was obtained from comparative plots of water vapor adsorption. It was found that preliminary dehydration only slightly affects the number of primary centers of water adsorption.     

非晶态纳米氢氧化镍电极材料物理特性与电化学性能

采用快速冷冻沉淀法制备出了非晶态纳米氢氧化镍。对制得材料样品进行了XRD，SEM，TEM，DSC和比表面积与孔径分析，将其制成MH-Ni电池正极材料进行充放电性能测试。结果表明：材料粉体为非品态，颗粒粒度为纳米级，类似球形。非晶纳米Ni（OH）2的热分解温度286．4℃低于常规球形Ni（OH）2的热分解温度333.8℃，同时具有较大得比表面积和孔径，分别为76．2089m^2·g^-1和37．7nm。与普通β-Ni（OH）2相比较，非晶态纳米氢氧化镍电极充电电压低，放电电压平台时间长，且高达1．258V，放电比容量为349．85mAh／g，具有较好的循环性能，20次循环后其容量衰减仅为1．28％。     

锂硫电池正极材料Al-ABTC/RGO@S的制备及电化学性能

通过溶剂热法制备了一种高比表面积的铝基金属有机框架（metal organic frameworks,MOFs）材料Al-ABTC。然后通过静电吸附法将Al-ABTC与氧化石墨烯（GO）复合,并载硫得到Al-ABTC/RGO@S复合材料用于锂硫电池。采用 X 射线衍射(XRD)分析了Al-ABTC的晶体结构,采用扫描电镜(SEM)对Al-ABTC、Al-ABTC/GO和Al-ABTC/RGO@S的八面体形貌进行表征,用恒流充放电测试材料的电化学性能。结果表明,Al-ABTC/RGO@S复合电极在0.2 C电流密度下的首次放电容量达到1345.3 mAh g-1,经过200次的循环以后还能达到406.4 mAh g-1的比容量,其平均库伦效率为99.1%。此外电池即使在2 C下,首次放电比容量高达714.7 mAh g-1,经过300次循环以后容量保持在331 mAh g-1,表现出良好的长循环性能。     

CuxBy表面修饰对Mg50Ni50合金循环稳定性的影响

用机械合金化法合成了CuxBy合金和非晶态Mg50Ni50储氢合金.用同样的方法以CuxBy对非晶态Mg50Ni50合金进行表面修饰.探索了不同组成的CuxBy合金、同一组成不同比例(质量比,下同)的修饰对Mg50Ni50合金电极循环稳定性的影响.结果表明:不同组成的CuxBy合金对Mg50Ni50合金的表面修饰,都不同程度地提高了Mg50Ni50合金电极的循环稳定性.同一组成不同比例的修饰,对Mg50Ni50合金电极循环稳定性改性效果差异较大.当Mg50Ni50:Cu0..9B0.1=5:1时,初始放电容量为465 mAh·g-1,第50个循环放电容量为222 mAh·g-1.在保持高放电容量的前提下,有效地提高了非晶态Mg50Ni50合金电极的循环稳定性.     

锂空气电池空气电极层次多孔碳的制备及其性能

在不同表面活性剂浓度下通过溶胶-凝胶自组装方法制备了具有介孔结构的层次多孔碳材料（HPCs）。用场发射扫描电镜（FE-SEM）、透射电镜（TEM）、氮气吸脱附测试和恒流充放电测试对样品进行物理和电化学性能研究。结果表明：所有的HPCs主要为介孔结构并且具有相似的孔径分布。以HPCs为空气电极载体碳材料的锂空气电池具有较高的放电容量。且相似孔径大小的碳材料为载体的锂空气电池放电容量随着碳材料的比表面积增加而增加。在c（CTAB）=0.27 mol/L时制备的HPCs-3样品具有最佳的电化学性能。通过控制放电深度至800 mA·h/g,电池表现出良好的容量保持率,在0.1 mA/cm2电流密度下,首次放电容量为2050 mA·h/g。     

碳气凝胶的纳米结构控制及其在锂离子电池中的应用(英文)

以间苯二酚和甲醛为前驱体,通过溶胶凝胶法制备有机气凝胶,通过高温裂解制备得到碳气凝胶。由于其高的比表面积,低的电阻率,空间网络结构以及化学惰性,碳气凝胶被认为是可充电电池的理想电极材料。研究了碳气凝胶的制备和结构控制,通过SEM,BET,XRD等手段测试其显微结构性质和结构控制。BET测试结果表明有机气凝胶炭化以后,比表面积显著增加,碳气凝胶具有518～621m2/g的较高比表面积。碳电极分别由碳气凝胶、石墨、碳气凝胶和石墨的混合物与黏结剂组成,以锂片为对电极制成纽扣电池。电化学测试结果显示其具有很高的首次放电容量(958.6mAh/g),但是可逆容量只有总容量的30%到40%。并且混合电极的性能优于其他纯电极。     

二氧化硅气凝胶的制备与表征(英文)

二氧化硅气凝胶是目前世界上最轻的人造多孔固体材料。采用硅酸钠为硅源,通过采取老化、溶剂置换、表面改性和分级干燥等一系列措施,常压干燥制得SiO2气凝胶颗粒,并利用红外光谱、比表面分析、扫描电镜等测试方法对其结构、形貌及化学组成进行了分析。研究表明:该样品呈疏水性,孔径较小,比表面积为740m2/g,孔体积为0.89cm3/g,平均孔径为4.8nm。     

Preparation and characterization of CuO-CoO-MnO/SiO2 nanocomposite aerogels as catalyst carriers

CuO-CoO-MnO/SiO₂ nanocomposite aerogels were prepared by using tetraethyl orthosilicate (TEOS) as Si source, and aqueous solution of Cu, Co and Mn acetates as the precursors via sol-gel process and ethanol supercritical drying technique. The gelatination mechanism was investigated by nuclear magnetic resonance (NMR) and X-ray photoelectron spectroscopy (XPS). The microstructure and composition of the CuO-CoO-MnO/SiO₂ nanocomposite aerogels were characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), electron dispersive spectroscopy (EDS) and XPS. The specific surface area, pore size and pore size distribution of the nanocomposite aerogels were determined by the Brunauer-Emmett-Teller (BET) method. The products were analyzed by gas chromatography (GC). The results show that the CuO-CoO-MnO/SiO₂ nanocomposite aerogels are porous, with a particle size distribution of 10–150 nm, a pore size distribution of 2–16 nm, an average pore size of 7.68 nm, and a specific surface area of 664.4–695.8 m²/g. The molar fraction of transition metals in the nanocomposite aerogels is 0.71%-13.77%. This kind of structure is favorable not only to increase the loading of catalysts, but also to make full use of the effect of transition metal oxides as cocatalysts; CuO-CoO-MnO/SiO₂ nanocomposite aerogels can be used as a novel catalyst carrier in the safer and environment-friendly synthesis of diphenyl carbonate and other fields of catalysis.     

原位法制备Ni纳米线/SiO2复合气凝胶催化剂

以正硅酸乙酯和硝酸镍为原料、乙二醇为还原剂,采用溶胶-凝胶法和超临界干燥工艺制备负载金属Ni纳米线的SiO2复合气凝胶.通过BET、XRD、TEM、TPR和H2-TPD等技术,对其物相组成和活性比表面进行表征.结果表明:负载Ni主要以金属Ni单质纳米线的形态均匀分布在SiO2气凝胶三维网络骨架结构上,该纳米线直径为1～5 nm、长度为10～80nm,载体骨架结构上存在尚未还原完全的Ni;随Ni负载量的增加,Ni与载体SiO2之间的相互作用逐渐减弱,催化剂的Ni活性中心点增多;负载Ni纳米线显示出较强的热稳定性.     

Synthesis of Porous LiFePO4/C Composite Materials by CCVD Method

以C2H2为碳源,Fe为催化剂,纳米FePO4为原料,采用催化化学气相沉积法(CCVD)合成多孔LiFePO4/C正极材料。经BET、SEM、CHON有机元素分析仪、XRD等手段对复合材料进行结构分析表征。结果表明,该复合材料具有连续贯通的三维导电网络结构,大的比表面积以及多重孔隙的类球形结构,含碳量为4.42%(质量分数),低于传统碳热还原法所制备的材料。电化学测试表明,该材料在0.1、1、5、10 C倍率下,放电比容量分别为147,141,126,110 m Ah·g-1,高倍率充放电性能大大提高,另外,该材料1 C循环80次后,放电比容量基本没有降低,显示了良好的循环稳定性能。     

Synthesis and performance of Li3Ve(PO4)3/C composites as cathode materials

Carbon-coated Li3V2(PO4)3 cathode materials for lithium-ion batteries were prepared by a carbon-thermal reduction (CTR) method using sucrose as carbon source.The Li3V2(PO4)3/C composite cathode materials were characterized by X-ray diffraction (XRD),scanning electron microscopy (SEM),and electrochemical measurement.The results show that the Li3V2(PO4)3 samples synthesized using sucrose as carbon source have the same monoclinic structure as the Li3V2(PO4)3 sample synthesized using acetylene black as carbon Source.SEM image exhibits that the particle size is about 1 μm together with homogenous distribution.Electrochemical test shows that the initial discharge capacity of Li3V2(PO4)3 powders is 122 mAh·g-1 at the rate of 0.2C,and the capacity retains 111 mAh·g-1 after 50 cycles.     

Preparation of low cobalt high rate discharge hydrogen storage alloy MlNi_(3.85)Co_(0.45) Mn_(0.4)Al_(0.3)X_(0.1)(X=Mg,Si,Sn)

1　INTRODUCTIONInrecentyears,Ni/MHbatterythatisanewgenerationbatterywithhighenergydensitywasrapidlydevelopedafterwardsNi/Cdbattery .WiththeincreasinglymatureofNi/MHbatteryproductiontechnique,itbeginstojointhefieldofhighpowerandgreatcapacitycell,andbecomesgraduallythemostpromisinggreendynamiccellthatwasappliedtoelectromotivemotor .Thehydrogenstoragealloy ,asthekeymaterialofNi/MHdynamiccell,mustbecharacterizedbyitshighspecialcapacity ,highvolt ageplatform ,goodcatalyzeactivity ,longcycl…     

Electrochemical characteristics of CoSnx alloy composite anode forlithium-ion rechargeable batteries

Nano/micro-scaled CoSnx alloy powders synthesized via carbothermal reduction at 800 ℃ with different compositions were characterized for anode materials in Li-ion battery. The synthesized spherical CoSnx particles show a loose nano/micro sized particle structural characteristic, which is apparently favorable for the improvement of cycling stability. The prepared CoSn3 alloy composite electrode exhibits a low initial irreversible capacity of ca.130 mAh·g-1 and a high specific capacity of ca.440 mAh·g-1 at constant current density of 100 mA·g-1 . The relatively large particle size is considered to be the main reason for the lower irreversible capacity of CoSn3 electrode.     

碳纳米管掺杂SiO2气凝胶隔热材料的制备与性能表征

以正硅酸乙酯（TEOS）和碳纳米管（CNTs）为原料，采用溶胶-凝胶法和常压干燥法制备不同碳纳米管（CNTs）含量的SiO2气凝胶隔热材料。采用DET、SEM、XRD等测试方法考察了添加CNTs对SiO2气凝胶比表面积、孔结构特征和密度的影响。结果表明：添加CNTs不仅能够增强SiO2气凝胶的强度，而且能够在很大程度上提高气凝胶的比表面积，使孔结构分布更加均匀。     

Electrochemical hydrogen storage properties of La0.95Mg2.05Ni9 alloy prepared by mechanical alloying

1　INTRODUCTIONTheMg basedhydrogenstoragealloysastheac tivematerialsofmetalhydrideelectrodeshaveattract edattentionbecauseofhighertheoreticalcapacitiesforhydrogenabsorption/desorption ,andthelowerpricecomparedwiththeotherhydrides[17] .Recent ly ,thecharge dischargepropertiesofMg basedalloysatroomtemperaturehavebeengreatlyimprovedbysomeresearchers[813] .Inparticular ,theMg Ni REsystemalloyisoneofthemost promisinghydrides[14 16 ] .Tanakaetal[15] reportedthatthenanocrystallineMg Ni RE(R…     

稀土Y掺杂非晶态纳米Ni(OH)2的结构及其电化学性能研究

以Tween-80/n-C4H9OH/c-C6H12/NiSO4水溶液体系,采用微乳液快速冷冻沉淀法制备出稀土Y掺杂非晶态纳米级氢氧化镍粉体材料.采用XRD、SAED、SEM、TEM、EDS、Raman、IR,粒度分析和比表面等测试方法对所制备的粉体进行了结构形态表征,并对其充放电性能和交流阻抗谱进行测试.结果发现,适量稀土元素Y的掺入使非晶态纳米氢氧化镍的结构缺陷增多、无序性增强,平均粒度减小、比表面积增大,有利于降低其溶液电阻、电荷转移电阻和Warburg阻抗,从而提高其放电比容量.样品作为MH-Ni电池正极材料以0.2 C充放电,终止电压为1.0 V,当掺杂Y的质量分数为4%时,放电比容量达到333.3 mAh/g.