电化学合成系列锡配合物及纳米SnO2的制备

采用锡金属为"牺牲"阳极,首次在无隔膜电解槽中,电化学一步法制备了纳米SnO₂前驱体锡配合物Sn(OEt)₄, Sn(OBu)₄, Sn(OCH₂CH₂OCH₃)₄, Sn(OEt)₂(acac)₂, Sn(OBu)₂(acac)₂, Sn(OCH₂CH₂OCH₃)₂(acac)₂[acac为乙酰丙酮基],产物通过红外光谱(FT-IR)、拉曼光谱和核磁共振进行表征.同时采用含Sn(OR)₂(acac)₂>的电解液直接水解制备纳米SnO₂粉体,纳米SnO₂通过X射线粉末衍射(XRD)和透射电子显微镜(TEM)进行表征.实验表明,电解时防止阳极钝化,控制温度在40～60℃之间,采用有机胺溴化物为导电盐,可以提高电合成效率;电解合成Sn(OCH2CH₂OCH₃)₄, Sn(OEt)₂(acac)₂, Sn(OBu)₂(acac)₂, Sn(OCH₂CH₂OCH₃)₂(acac)₂的电流效率比Sn(OEt)₄, Sn(OBu)₄高,适宜作为溶胶-凝胶(Sol-gel)法制备纳米SnO₂的原料,制备得到的纳米SnO₂经600℃煅烧后呈球形单分散结构,晶型为四方锡石型,平均粒径在(10±0.4) nm左右.     

在乙二醇溶液中原位法制备纳米SnO2

乙二醇;锡配合物;溶胶 凝胶;纳米SnO2     

纳米SnO2@TiO2的制备及其光催化性能

以SnCl4和Ti(OBu)4为原料,采用活性层包覆法制备了SnO2@TiO2包覆型复合光催化剂,并用XPS、IR、XRD、TEM和BET等手段进行了表征,以二甲基二氯乙烯基磷酸酯（简称DDVP）稀释液为模拟废水,考察了SnO2@TiO2的光催化活性及降解液初始浓度对反应动力学的影响.结果表明：包覆粒子由锐钛矿型TiO2和金红石型SnO2组成;与纯SnO2、TiO2相比,SnO2@TiO2包覆粒子的光催化活性明显提高,DDVP稀释液被光催化降解属于零级反应,但反应表观速率常数与降解液初始浓度成正比.     

SnO2纳米薄膜的制备、显微结构及气敏性能

SnO2纳米薄膜的制备、显微结构及气敏性能;SnO2薄膜;溶胶-凝胶法     

在乙二醇甲醚溶液中合成NiTiO_3超细粉末

在无隔膜电解槽中,加入0.035mol/L（Bu4N）Br的乙二醇甲醚溶液,保持电解温度40℃、电流密度30mA/cm2时,先电解钛片6h,再电解镍片3h,制得镍、钛醇盐配合物,电流效率为95.1%。采用红外、拉曼光谱对其进行了表征。结果表明,前驱体结构为NiTi（OCH2CH2OCH3）6,可以有效克服团聚现象。水解...     

不同形态SnO2纳米晶的制备

In this paper, we report our research on morphologically selective synthesis of nanocrystalline SnO2 by the combination of hydrothermal preparation and calcinated process. We firstly prepared SnO2 nanocrystals by the hydrothermal method at 140 ℃ for 3 h, using SnCI4 as the reactant. With the initial pH of 1.8 or 1.34, we prepared uniform and well-dispersed SnO2(tetragonal) nanocrystals, with similar size of about 3 nm, as determined by TEM. However, after being calcinated at 500 ℃ for 2 h, specimen 1 prepared at pH＝1.8 showed the rod-like shape with an average size of 5 nm×20 nm, while the other one(specimen 2)prepaed at pH＝1.34 showed a granular shape with an average size of 10 nm. XRD experiments showed that specimen 1 had a new diffraction peak after calcination, which was contributed by the (023) face of orthorhombic SnO2. The experiment results indicated that the morpholgy of SnO2 nanocrystals after calcination was closely related to the initial acidity of the reaction solution, possibly due to the difference in surface properties, e.g. the difference in crystalline faces exposed to the surface of particals, under different hydrothermal conditions.     

水热法制备SnO2/α-Fe2O3纳米复合材料

用α-Fe2O3纳米粒子作为前驱物,以SnC l4和NaOH作为反应试剂,通过简单的水热法制备了SnO2/α-Fe2O3纳米复合材料。SnO2/α-Fe2O3纳米复合材料具有有趣的形貌:直径约为20nm的SnO2纳米棒以α-Fe2O3纳米粒子为中心向四周辐射生长。利用X-ray粉末衍射(XRD),透射电镜(TEM)和扫描电镜(SEM)等测试手段对样品的成份、结构、形貌和尺寸进行了表征,初步探讨了SnO2/α-Fe2O3纳米复合材料的形成机理。     

复合纳米微粒Rh3+/TiO2/SnO2的合成、表征及光催化降解4-(2-吡啶偶氮)间苯二酚的研究

采用溶胶 凝胶法制备复合纳米微粒Rh³⁺/TiO₂/SnO₂作系列光催化剂,运用BET、XRD等技术对样品进行了表征.讨论了影响污染物4 (2 吡啶偶氮)间苯二酚(PAR)光催化降解率的主要因素,实验结果表明:以Rh³⁺/TiO₂/SnO₂为复合光催化剂,当m(TiO₂)∶m(SnO₂)=56:44,ω(Rh³⁺)=2.0%,催化剂用量为1.0 g,通入空气的流量为10.0 L/min,试液的质量分数为2.0×10^-6,pH=7.0时,光照2h,PAR的降解率达到96.2%.     

SnO2纳米粒子的制备与表面改性

以SnCl4·5H2O和氨水为原料,用水热法制备了粒度均匀的SnO2纳米粒子,并用γ-氨丙基三乙氧基硅烷(KH-550)对其进行了表面改性. 用X射线衍射(XRD)、透射电子显微镜(TEM)、纳米粒度/Zeta电位测定和元素分析测试技术对粒子进行了表征. 研究结果表明,所制得的SnO2纳米粒子为四方晶系金红石型结构,改性后的纳米粒子均一性进一步提高,粒径分布在8～20 nm,能形成稳定的分散体系.     

CeO2/SnO2纳米材料的制备与气敏性能研究

本文应用溶胶-凝胶法制备了7种不同成分和煅烧温度的CeO2/SnO2材料,应用X射线衍射方法对其中的3种进行了结构表征和粒度分析,运用自组装的气敏性能设备检测了该7种不同成分的CeO2/SnO2材料的气敏性能,简要分析了其气敏机理。结果表明:掺杂CeO2有利于SnO2晶粒的细化;掺杂CeO2和La2O3可改变或提高SnO2气敏材料对某些气体的气敏性能;煅烧温度在600℃~800℃之间,掺杂2?O2的CeO2/SnO2气敏材料,随煅烧温度上升,气敏性能下降;煅烧温度600℃、掺杂5?O2的CeO2/SnO2气敏材料,对乙醇具有较高的灵敏度和选择性,具有开发应用价值;CeO2/SnO2气敏材料的气敏机理为表面电导控制型。     

电化学溶解钛金属直接水解法制备纳米TiO_2

纳米材料是目前材料科学的热点 .TiO2作为一种重要的无机功能材料 ,具有温敏、气敏、光催化等功能 ,广泛用于光电材料、涂料、传感器、介电材料、催化剂及载体等重要领域 .由于其各种应用都与粉体的性能有直接关系 ,因此研究纳米 TiO2的制备方法具有重要的实际意义 [1].近年来 ,纳米 TiO2粉体制备方法有了很大的发展 ,如 TiCl4气相水解沉淀法 [2],乳浊液法和 Ti(OC4H9)4水解沉淀法 [1],喷雾热解法 [3],放电爆炸法 [4],反应电极埋弧法 [5],溶胶凝胶 (Sol gel)法 [6]等 ,其中溶胶凝胶法是制备纳米材料的有效方法 .但这些方法存在…     

电化学溶解钛金属直接水解法制备纳米TiO2

Metallic titanium was electrochemically dissoluted in absolute ethanol in the presence of Et4N•Br(as electro conductive additive),The electrolyte solution was then directly hydrolysized to obtain nanocrystalline TiO2.The powder obtained was calcined at 720℃ for 1 h.FT IR,Raman spectra,XRD and TEM were used to investigate the structure and particle size of the powder.Studies showed that the nanocrystalline TiO2 prepared by this method was of monocline structure with high textural stability and narrow size distribution of 10－20 nm,and its Raman spectra showed a shift of about 25 cm－1.The experiments also showed that the product yield could be improved by controlling the temperature under 50－60℃,selecting R4N•Br as conductive additive and preventing titanium anode from being passivated.The electrochemical dissolution of metal anode may be recommanded as a promising technique for the synthesis of nanomaterials.     

Synergistic Effect of Oxalate and Ethylene Glycol on the Formation of SnO2 Rods

SnO₂ rods have been synthesized by using tin (II) chain‐like complexes as precursors in which oxalate and ethylene glycol act as co‐ligands. On the basis of experimental analysis, a reasonable formation mechanism of rods is discussed, which is further supported by Fourier transform infrared spectroscopy (FT‐IR). These results show that the synergistic effect of oxalate group and ethylene glycol plays an important role in the formation of long SnO₂ rods.     

A Novel Electrochemical Sensor for β2‐Agonists with High Sensitivity and Selectivity Based on Surface Molecularly Imprinted Sol‐gel Doped with Antimony‐Doped Tin Oxide

A novel strategy to improve the sensitivity of molecularly imprinted polymer (MIP) sensors was proposed for the determination of β₂‐agonists. The imprinted sol‐gel film was prepared by mixing silica sol with a functional monomer of antimony‐doped tin oxide (ATO) and a template of β₂‐agonists. ATO, which was embedded in the surface of the molecularly imprinted sol‐gel film, not only provides the excellent conductivity for biosensor but also increases the stability and the surface area of the MIP film. The imprinted sensor was characterised by field emission scanning electron microscope, fourier transform infrared spectroscopy and electrochemical methods. Under the optimal experimental conditions, the peak current was linear with the logarithm of the concentration of clenbuterol (CLB) in the range of 5.5 nM–6.3 µM, and a detection limit of 1.7 nM was obtained. Meanwhile, the electrochemical sensor showed excellent specific recognition of the template molecule among structurally similar coexisting substances. Furthermore, the proposed sensor was satisfactorily applied to determine β₂‐agonists in human serum samples. The good results indicated that highly effective molecularly imprinted sol‐gel films doped with ATO can be employed for other analytes.     

球型Ni(OH)2表面包覆Y(OH)3及其高温充放电性能

应用共沉淀的方法在球型Ni(OH)₂的表面包覆了一层Y(OH)₃,并研究了包覆不同含钇量后的球型Ni(OH)₂的高温充放电性能。研究结果表明:包覆Y(OH)₃的球型Ni(OH)₂具有良好的高温充放电性能。其中1C充放电条件下,包覆量为0.3%的Ni(OH)₂较好,0.2C充放电条件下,包覆量为1%的Ni(OH)₂较好。     

A Facile Procedure for the oxidative Coupling of 2-Naphthol and 2-Naphthalenethiol in Solid State

l,lLBi-2-naPhtholshavebeenwidelyappliedasimportantchiralauxiliariesandligands..tinorganicchemistry'.TheconversionofthiolstothecorrespondingdisulphidesisofintCrestbothfromabiological'andpracticalpointofview.ForthesynthesisofbinaPhtholsanddisulphides,theoxidativecouplingofnaphtholsandthiolshaslongbeenarecognisedmethodofchoice.Variousoxidantscanbringaboutthecouplingofnaphthols'andthiols4insolution,buttheyoftenleadtolowyieldsorsufferfromdisadvantagesduetotheinsolubilityofoxidant,naPhthoIandthiol…     

Melamine-(H_2SO_4)_3 and PVP-(H_2SO_4)_n as solid acids:Synthesis and application in the first mono-and di-nitration of bisphenol A and other phenols

Melamine and poly vinylpyrrolidone（PVP） reacted with neat sulfuric acid readily to form two new organic solid acids namely melamine-（H₂SO₄）₃ and PVP-（H₂SO₄）_n.These solid acids were used for the first nitration of bisphenol A as well as other phenols in the presence of NH₄NO₃.Mono- and di-nitro bisphenol A have been characterized with IR and ¹H NMR techniques.     

磷酸钒钠Na_3V_2(PO_4)_3电化学储能研究进展

锂离子电池在全球范围内的广泛应用加剧了对锂资源的消耗,其成本和原料将限制其未来发展。钠与锂具有相似物理化学性质,并且储量丰富。根据锂离子"摇椅式"电池原理,富钠离子化合物可类似富锂离子正极材料,提供可脱嵌的钠离子及结构。钠离子较锂离子大,其可逆脱嵌反应要求材料结构具有较大的容钠位与离子迁移通道。聚阴离子体磷酸钒钠Na_3V_2(PO_4)_3属于钠离子超导体(NASICON)材料,其NASICON结构骨架形成了稳定的容钠位,并且开放的三维离子迁移通道利于提高钠离子的扩散。Na_3V_2(PO_4)_3作为电池正极材料,具有理想的比容量、电压平台与循环稳定性,从而受到了广泛关注。本文首先介绍了Na_3V_2(PO_4)_3结构特点,其次结合团队已有的工作基础对Na_3V_2(PO_4)_3在钠离子电池、混合离子电池、水系电池,混合超级电容器等体系中的应用与反应机理进行了阐述;总结了基于Na_3V_2(PO_4)_3设计的复合材料与结构并探讨了Na_3V_2(PO_4)_3可能存在的问题与未来发展趋势。     

新型特效钠离子吸附剂Li1+xLaxZr2-x(PO4)3的制备和性能研究

采用高温固相法合成了新型特效Na离子吸附剂Li1 xLaxZr2-x(PO4)3.对不同条件下合成的吸附剂进行了XRD结构分析以及SEM分析和IR分析,并对其吸附性能进行了测定.XRD结构分析表明,当x≤0.4时均能得到与LiZr2(PO4)3相同的晶体结构.SEM分析表明,合成的吸附剂分散性好,粒径范围在5～20μm之间.吸附性能测定结果表明,少量La的加入使Li1 xLaxZr2-x(PO4)3对Na离子产生了特效吸附作用,La离子掺杂是改善LiZr2(PO4)3吸附性能的一条有效途径,当x=0.4时,在pH值为10.0～11.0条件下,Li1 xLaxZr2-x(PO4)3的吸附容量达到48.3mg/g.