间苯二酚-甲醛碳气凝胶粉末的性能研究

间苯二酚-甲醛有机气凝胶粉末经过高温碳化处理得到其碳气凝胶粉末.利用全自动吸附仪进行了液氮温度下有机气凝胶粉末和碳气凝胶粉末的N2吸附孔结构表征,主要研究了有机气凝胶碳化前后孔径分布的变化.并采用透射电镜(SEM)和X射线衍射(XRD)对粉末进行分析,结果表明,经碳化后其比表面积有较大的提高(＞500m2/g),粉末粒径减小(＜100nm).     

Sol-gel法制备纳米晶镍锌钴铁氧体/二氧化硅复合颗粒的研究

开发了用溶胶-凝胶法制备纳米晶镍锌钴复合铁氧体颗粒的技术,并对溶胶-凝胶工艺的影响因素进行了研究探讨.用扫描电镜(SEM)、电子探针(EPMA)和X射线衍射(XRD)对样品进行了表征,得到球状分布的纳米晶镍锌钴铁氧体/二氧化硅复合颗粒,并优化了制备工艺.     

溶胶-凝胶燃烧合成制备NiO纳米颗粒的研究

研究了以硝酸镍和柠檬酸为原料溶胶-凝胶自燃烧法制备氧化镍纳米颗粒的最佳工艺条件及配比.用热重分析(TG-DSC)、扫描电镜(SEM)和X射线衍射(XRD)对反应物、反应过程、产物氧化镍等进行了表征.研究了溶胶-凝胶pH值、原料配比对产物的影响并对反应机理进行了初步探讨.通过调整柠檬酸与硝酸镍的配比来避免镍的出现.本方法设备简单,操作方便易行.     

超级电容器MnO2/CRF复合电极材料的制备及性能的研究

以间苯二酚(R)和甲醛(F)为原料,碳酸钠(C)为催化剂,制备碳气凝胶(CRF),并以KMnO4和Mn(CH3COO)2·4H2O为原料,采用了化学沉淀法制备MnO2/CRF复合材料.用N2吸附、X射线衍射(XRD)和扫描电镜(SEM)对所制备的MnO2、CRF和MnO2/CRF复合材料进行了表征,结果表明碳气凝胶具有珍珠串式的无序多孔网络结构,所制备的MnO2为纳米级颗粒,复合材料为纳米级粉体.并对不同配比的MnO2/CRF复合材料的电化学性能进行了研究.循环伏安、恒流充放电实验表明了所制备的MnO2/CRF复合电极材料具有良好的可逆性和充放电性能.当MnO2含量为60%时,MnO2与碳气凝胶复合制成的新型电极材料具有226.3F/g的比电容,比碳气凝胶电极的比电容提高了1倍.此外,对复合电极的循环寿命进行了研究,表明复合电极具有良好的循环充放电性能.     

柠檬酸盐凝胶法制备纳米氧化镍的研究

优化了柠檬酸盐凝胶法制备纳米氧化镍粉体的工艺条件.采用傅立叶红外光谱(FTIR)、热分析(TG/DTA)、X射线衍射(XRD)、扫描电镜(SEM)和BET法对柠檬酸镍络合物的形成,凝胶热分解过程,产物的形貌、粒径和比表面积大小以及同材料配比、热处理温度、热处理时间之间的关系进行了研究,确定了制备纳米氧化镍的最佳工艺条件(柠檬酸与镍离子摩尔比1.2:1.0,400℃热处理1h),并在此条件下成功制备了粒径达30nm,比表面积达181.29m²/g的NiO粉体.通过热力学计算,解释了在凝胶热分解过程中金属镍相出现的可能原因.     

KOH活化碳气凝胶对水中亚甲基蓝的吸附性能研究

以间苯二酚和甲醛为原料水热制备有机气凝胶,在碳化过程中使用KOH作活化剂制备出孔结构丰富的碳气凝胶。采用扫描电镜(SEM)、X射线衍射(XRD)及N2吸脱附法等手段对材料的结构及形貌表征,考察了活化剂用量、染料初始浓度、接触时间等因素对亚甲基蓝在碳气凝胶上吸附的影响,并进行了吸附类型和吸附动力学研究。结果表明:活化剂的加入使碳气凝胶材料的孔结构更加丰富,当活化剂与有机气凝胶的质量比达到2∶1时,其吸附性能最佳。碳气凝胶去除亚甲基蓝的吸附行为符合二级动力学模型。吸附类型为Langmuir吸附模型。     

纳米羟基磷灰石粉体的生物活性的研究

采用溶胶-凝胶法制备羟基磷灰石陶瓷材料.通过控制工艺参数:pH>9,Ca/P=1.67,烧结温度为1100℃及烧结时间2h,合成出纯度较高纳米粒径的羟基磷灰石粉体.通过羟基磷灰石对不同氨基酸的吸附强度,选取显著吸附的氨基酸进行紫外分光光度法、X射线衍射(XRD)物相分析和X射线衍射谱(XDS)分析,研究羟基磷灰石粉体的结构和吸附氨基酸的生物活性.结果表明:羟基磷灰石能吸附氨基酸,吸附位点是PO43-基,而不是Ca2+.提出羟基磷灰石吸附具有不同电位的氨基酸的作用机理.     

块状纯氧化铜气凝胶的制备研究

以无机铜盐CuCl2的醇溶液为前驱体，采用聚丙烯酸（PAA）为分散剂，环氧丙烷为凝胶促进剂，通过溶胶-凝胶工艺（sol-gel process）制备了铜基醇凝胶，再经CO2超临界流体干燥工艺得到浅绿色块状初始铜基气凝胶，最后经过热处理获得黑色块状纯氧化铜气凝胶样品，其平均密度约为300mg／cm^3。用扫描电子显微镜（SEM）对气凝胶的微结构进行分析可知，最终获得的气凝胶样品主要由百纳米级的矩体颗粒堆砌而成。X射线衍射（XRD）分析表明初始样品具有典型的无定形结构，其主要的结晶成份为斜方晶Cu^2＋ 2 Cl（OH）3，而X射线荧光光谱（XRF）测试结果表明其Cu与Cl的元素比为3．55：1，高于Cu^2 ＋2 Cl（OH）3中两元素的化学计量比，结合化学原理分析可知，其未结晶成分主要为水合氢氧化铜。而XRD的测试结果表明，经过500℃热处理后的样品成分主要为单斜晶氧化铜。     

热处理温度对复合SiO2隔热多孔陶瓷材料性能的影响

以SiO_2微粉、SiO_2气凝胶、石英纤维为主要原料,通过改变原料配比,采用半干法成型制备了SiO_2复合隔热多孔材料,通过X射线衍射分析(XRD)、扫描电子显微镜(SEM)等测试方法,研究了不同烧结温度(400~1000℃)对复合SiO_2隔热多孔陶瓷的物相组织、显微结构及物理性能的影响。结果表明当烧结温度升高至800℃时,试样保持着最佳的综合性能:其显气孔率为43.33%、体积密度为1.22g/cm3、抗折强度为2.05MPa、耐压强度为17.30 MPa,试样中均匀分布着大量呈球型、孤立的亚微米级气孔。     

掺镍碳气凝胶的特性研究

以间苯二酚-甲醛为原料,添加水溶性镍盐,利用溶胶-凝胶法制备了具有纳米多孔结构的掺镍碳气凝胶.通过X射线衍射及透射电镜表征了掺镍碳气凝胶的结构.用比表面积测试及孔径分布测试等手段研究了碳气凝胶的多孔特性,研究表明纯碳气凝胶的比表面积为487.3m2/g,掺杂后提高到593.3m2/g.掺镍碳气凝胶的电导率比未掺杂样品有很大的提高.     

碳气凝胶载铂催化剂对甲醇的电催化氧化性能

以用溶胶凝胶法制备的碳气凝胶(CA)作为催化剂载体,用间歇微波法制备了碳气凝胶载铂催化剂。用电感耦合等离子光谱仪(ICP)测定了催化剂中Pt的含量,用透射电镜(TEM)和X射线衍射(XRD)对催化剂的形貌、粒径分布以及颗粒粒度进行了表征。结果表明,碳气凝胶载铂催化剂粒子分布均匀、粒径集中,平均粒经为4 nm.用能量散射X射线能谱(EDX)分析了催化剂的化学成分,用循环伏安法、线形扫描伏安法和计时电流法对催化剂的电化学性能进行了表征.结果表明,以碳气凝胶为载体的催化剂比以活性炭为载体的催化剂具有更高的催化活性。     

单分散镍碳复合纳米球和碳微球的制备

以脱油沥青(deoiled asphalt)为碳源,采用化学气相沉积法(CVD)制备碳微球,其裂解后的残渣经真空热处理制得单分散镍碳复合纳米球.用场发射扫描电镜(FESEM)、高分辨透射电镜(HRTEM)和X射线衍射仪(XRD)对产物进行表征.结果表明,碳微球高纯,属无定型碳结构,大小分布在1～2μm范围内;镍碳复合纳米球为准球形核壳结构,核为镍,壳为碳,尺寸在10～30nm范围,晶化程度较高,结构较完善.     

Preparation of nanostructured NiFe2O4 catalysts by combustion reaction

Nanosize nickel ferrite powders (NiFe₂O₄) have been prepared by combustion reaction using nitrates and urea as fuel. The resulting powders were characterized by X-ray diffraction (XRD), nitrogen physical adsorption (BET), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and catalytic activity. The results showed nanosize nickel ferrite powders with high specific surface area (55.21 m²/g). The powders showed extensive XRD line broadening and the crystallite size calculated from the XRD line broadening was 18.0 nm. The nickel ferrite powder presented significant activity as catalyst for the water gas shift reaction, over the temperature range of 250–450 °C.     

Preparation and characterization of LiNiVO4 powder and non-stoichiometric LiNixVyOz films

Inverse spinel type structured oxide, LiNiVO₄, was synthesized by using solid-state method and the crystalline powder was characterized by Rietveld refinement and X-ray photoelectron spectroscopy. Non-stoichiometric lithium nickel vanadate thin films were prepared by physical vapour deposition technique. The amorphous films were characterized by Rutherford back-scattering spectroscopy (RBS), nuclear reaction analysis (NRA), Auger electron spectroscopy (AES), X-ray diffraction (XRD), scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM) analytical methods. Films crystal growth at various temperatures was also studied by XRD and SEM. The HRTEM analysis of sputtered film shows nanocrystalline domains of NiO and LiNiVO₄ phases with characteristic lattice parameters of the host compound and the results correlate well with the XRD data. Electrochemical properties of the films were discussed.     

Study of correlation of structural and surface properties with electrochemical behaviour in carbon aerogels

Carbon aerogel is a promising material for electrochemical double layer capacitors. In this paper carbon aerogels prepared by subcritical drying method are investigated for the change in the structure and surface properties at different pyrolysis temperatures. The important relations between structure, morphology, surface area and electrical properties were studied using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), surface area measurement and cyclic voltametry. It is shown that structure and the surface functional groups play important role in enhancement of electrochemical capacitance. The specific capacitance achieved was 114 F/gm which is quite large value for subcritically prepared carbon aerogels without any kind of activation process.     

Synthesis and characterization of NiO nanoparticles and their PMMA nanocomposites obtained by in situ bulk polymerization

A nickel oxide (NiO) precursor was prepared using Pechini method. The NiO nanoparticles were prepared by calcination of NiO precursor at temperatures ranging from 300 to 700 °C. The resulting NiO nanoparticles were characterized by X-ray photoelectron spectroscopy, X-ray diffraction (XRD), and transmission electron microscopy. To hamper NiO nanoparticles aggregation, the NiO nanoparticles surface was treated using (3-mercaptopropyl)-trimethoxysilane as a coupling agent. Next, nanocomposites of poly(methyl methacrylate) and modified NiO nanoparticles were successfully prepared by in situ bulk polymerization with 2,2′-azobis(isobutylonitrile) as initiator. The obtained nanocomposites were characterized by XRD and thermogravimetric analysis. L. A. García-Cerda is on sabbatical leave at UT-Dallas, USA.     

Large-scale and shape-controlled synthesis and characterization of nanorod-like nickel powders under microwave radiation

The nanorod-like nickel powders were fabricated via hydrothermal liquid phase reduction route under microwave irradiation with hydrazine hydrate as a reducing agent as well as polyvinyl alcohol as a dispersant and/or structure directing agent. The morphology and structure of as-prepared products could be easily tuned by adjusting process parameters such as pH value and microwave irradiation time. The resulting materials were characterized by X-ray diffraction (XRD), scanning electron microscope, transmission electron microscopy and selected-area electron diffraction (SAED). The results demonstrated that pure nickel powders with face-centered cubic (fcc) structure were prepared at relatively mild condition and no characteristic peaks of nickel oxide in the XRD pattern were found. The phenomenon of lattice expansion for Ni powders was explained in details according to the XRD theory. As-prepared Ni sample was of obvious shape anisotropy with length diameter ratio of 5. Magnetic measurements shown that the magnetic properties of nanorod-like (fcc) Ni powders were quite different from those of hexagonal closed-packed (hcp) Ni nanoparticles. Furthermore, it had more strong ferromagnetic properties than that of Ni powders both bulk and nanoparticles.     

Electrohydrodynamic atomization (EHDA) assisted wet chemical synthesis of nickel nanoparticles

In this study nickel nanoparticles were prepared via chemical reduction of nickel acetate using sodium borohydride using electrohydrodynamic atomization (EHDA) technique. This technique was used to spray a finely dispersed aerosol of nickel precursor solution into the reductive bath. Obtained particles were characterized by means of X-ray diffraction (XRD), UV–Visible spectroscopy, and transmission electron microscopy (TEM). Results confirmed the formation of nickel nanoparticles and showed that applying EHDA technique to chemical reduction method results in producing smaller particles with narrower size distribution in comparison with conventional reductive precipitation method.     

半透明抗紫外纸涂层纳米粉体的制备

采用浸渍法制备了Ce4+掺杂纳米TiO2纳米粉体,并用TEM,XRD和UV-Vis光谱等手段对其进行了表征.结果显示,纳米材料可有效吸收紫外线,并具有半透明性质.以PVP为表面活性剂,在相纸表面涂布,涂覆层均匀光滑,表面光泽度78%,油墨吸收时间约为4.2s.     

多孔壳/磁核结构光催化剂的制备及表征

以聚氧乙烯-聚氧丙烯-聚氧乙烯三嵌段共聚物(P123)为结构导向剂,钛酸丁酯(TBOT)为钛源,SiO2/NiFe2O4为核,制备了具有多孔结构可磁分离的Ti O2/SiO2/NiFe2O4光催化剂。采用N2吸附-脱附、TEM、HRTEM、SEM、XRD和VSM等手段对样品进行分析表征。样品颗粒呈球形,分布均匀,平均粒径约为40nm,具备良好的磁分离性能。以硝基苯为模拟物测定其光催化活性,UV光照条件下,240min内硝基苯污染物降解完全,表明该光催化剂具有良好的光催化活性。