乙二胺改性Co3O4-NiO复合粒子的制备及其超级电容性能研究

利用简单液相共沉淀法制得中间产物Ni(OH)2-Co(OH)2,再经煅烧得到Co3O4-NiO复合粒子;用乙二胺对Co3O4-NiO复合粒子进行改性,改性后Co3O4-NiO微粒分散性提高,形貌为片状,片与片之间相互交叉形成疏松的介孔结构。电化学测试表明Co3O4-NiO电极材料在改性后表现出优良的电化学性能,在电位窗口为0～0.4V时,单电极比电容可达1202F/g,相比改性前提高了171F/g。     

溶胶-凝胶法制备单相Ca2Co2O5粉体

以Co（N03）2.6H2O，Ca（NO3）2.4H2O为原料，柠檬酸为络合剂，利用溶胶-凝胶法（Sol-gel）制备出Ca2CO2O5粉体。采用TG-DSC、XRD和ESEM等测试方法对干凝胶体的热分解过程、样品的物相以及形貌进行了表征。实验结果表明：干凝胶体在700-900℃煅烧，煅烧2h后均能得到单相的Ca2CO2O5粉体，颗粒尺寸分布均匀，范围在1-2μm。在同一配比浓度、同一煅烧时间下，适当提高煅烧温度有利于Ca2CO2O5晶体的生长。     

纳米TiO2/还原石墨烯复合修饰电极用于食品中 柠檬黄的检测

为了检测食品中柠檬黄的含量,利用滴涂法和电化学还原法制备纳米TiO_2/还原石墨烯复合修饰玻碳电极(TiO_2-Er GO/GCE)。采用透射电子显微镜和X射线粉末衍射仪对TiO_2和TiO_2-GO两种修饰电极材料进行表征;通过循环伏安法观察了柠檬黄在不同电极上的电化学行为,并对检测条件如p H值、富集电位、富集时间进行了优化。实验结果表明:TiO_2-Er GO/GCE增大了电极的电化学活性面积,提高了柠檬黄的电化学氧化响应;最优的检测条件为p H值为3.7、富集电位为-0.20 V、富集时间为180 s;在最优的检测条件下,采用线性扫描伏安法检测柠檬黄的线性范围为2.0×10-8~2.0×10-5 mol/L,检测限为8.0×10-9 mol/L(信噪比为3)。     

MnO2纳米棒-还原石墨烯复合修饰玻碳电极用于苋菜红的检测

利用电化学还原法制备MnO₂纳米棒-还原石墨烯复合修饰电极（MnO₂ NRs-ErGO/GCE）用于苋菜红的检测。采用SEM和XRD分别对修饰电极材料进行微观形貌和成分结构表征。通过循环伏安法考察了苋菜红在裸电极、ErGO/GCE和MnO₂ NRs-ErGO/GCE上的电化学行为,并对测定条件如pH值、富集电位、富集时间进行了优化。结果表明,MnO₂ NRs-ErGO增大了GCE电化学活性面积,提高了苋菜红的电化学氧化响应。在最优的检测条件下,MnO₂ NRs-ErGO/GCE线性扫描伏安法检测苋菜红线性范围为2.0×10^-8~1.0×10^-5 mol/L和1.0×10^-5~4.0×10^-4 mol/L,检测限为1.0×10^-8 mol/L。MnO₂ NRs-ErGO/GCE用于真实饮料样品检测,获得满意结果。     

液相包裹法制备Pb(Mg_(1/3)Nb_(2/3))O_3-CoFe_2O_4磁电耦合材料

以无机盐Nb2O5、Mg(NO3)2、Pb(NO3)4、Co(NO3)2、Fe2(NO3)3为原料,柠檬酸和EDTA为络合剂,分别制备了Nb5+、Mg2+、Pb2+、Co2+、Fe3+等离子的络合溶液。采用络合法制备了铌酸镁-铁酸钴先驱体(MgNb2O6-CoFe2O4,简称MN-CFO)。此先驱体在1000℃煅烧1h后,得到纯净的MgNb2O6-CoFe2O4固溶体。采用液相包裹法制备了铌镁酸铅-铁酸钴(Pb(Mg1/3Nb2/3)O3-CoFe2O4)先驱体,在1000℃煅烧1h,Pb(Mg1/3Nb2/3)O3-CoFe2O4先驱体分解为具有铁电相Pb(Mg1/3Nb2/3)O3和铁磁相CoFe2O4的复相组织。研究了10%过量的PbO对煅烧过程中烧绿石相向铁电相的转变作用,并在700℃煅烧5h条件下制备了不含烧绿石相的Pb(Mg1/3Nb2/3)O3-CoFe2O4固溶体。     

超级电容器材料纳米Co3O4的固相法制备及电化学性能

以CoCl2·6H2O和NH4HCO3为原料,通过室温固相反应得到前驱体,将前驱体于350 ℃、空气氛中煅烧3 h,氧化分解得到Co3O4样品.X射线衍射(XRD)、透射电镜(TEM)和红外光谱(IR)分析表明,所得样品为纳米级立方尖晶石相Co3O4.循环伏安和交流阻抗测试结果表明,Co3O4电极在6 mol·L-1KOH水溶液中具有可逆的法拉第反应特性和较好的动力学性能.恒电流充放电结果表明,以Co3O4电极为正极、活性炭(AC)电极为负极、6 mol·L-1 KOH水溶液为电解质组成的碱性Co3O4/AC混合电容器具有较好的大电流充放电性能和循环稳定性.     

基于[C_(10)-mim~+]Br~-固定HRP于Au/石墨烯复合材料电极表面的新型H_2O_2酶生物传感器

利用长链离子液体特殊的性质,用其固定HRP于Au/graphene电极表面(Nafion/HRP/[C10-mim+]Br-/Au/Gr/GCE)组装成H2O2传感器。用透射电镜来表征Au/氧化石墨烯的形貌,金纳米颗粒很均匀的分散在石墨烯表面,并不存在团聚现像。电化学技术检测Nafion/HRP/[C10-mim+]Br-/Au/Gr修饰电极对H2O2的响应情况,显示修饰电极对H2O2有很好的响应,在H2O2浓度2.0×10-6~1.2×10-3 mol/L的范围内,还原电流与浓度存在线性关系(R=0.997),检测限为3.0×10-7 mol/L;另外传感器具有很好的稳定性和选择性,为生物分子的检测提供新方法。     

碱化插层二维过渡金属碳化物的制备及其对铀酰离子的电化学检测

二维过渡金属碳化物(MXenes)具有良好的电化学性能与辐照稳定性, 其在放射性核素电化学检测领域有潜在应用价值。本研究通过碱活化的方式处理碳化钛型MXene(Ti₃C₂T_x), 随后将钾插层的Ti₃C₂T_x(K-Ti₃C₂T_x)负载到玻碳电极(GCE)上得到K-Ti₃C₂T_x/GCE修饰电极。采用XRD、SEM、XPS等手段分别对Ti₃C₂T_x和K-Ti₃C₂T_x进行分析表征, 并进一步研究了K-Ti₃C₂T_x/GCE对痕量铀酰离子(UO₂²⁺)的电化学检测性能。循环伏安(CV)实验结果表明, 相比于GCE电极, K-Ti₃C₂T_x/GCE修饰电极对UO₂²⁺的电化学响应显著增强。进一步使用差分脉冲伏安法(DPV)扫描, 发现pH=4.0时, K-Ti₃C₂T_x/GCE修饰电极对UO₂²⁺在铀浓度0.5~10 mg/L范围内呈现良好的线性检测关系, 本方法的检测限为0.083 mg/L(S/N=3), 稳定性和重复性好。     

牛血清白蛋白对NaxCo2O4化合物形成的影响

探索了一种用于制备纳米片状NaxCO2O4化合物的新的化学合成法-蛋白质吸附法,研究了牛血清白蛋白(BSA)对NaxCo2O4化合物形成的影响.结果表明,BSA在一定浓度范围内可以明显降低胶态前驱体的平均粒子尺寸,BSA浓度的增大抑制了γ-Na0.71Co0.96O2晶体的形成,并对煅烧产物的相组成和形态产生了明显的影响.800°C煅烧得到超薄片状γ-Na0.71Co0.96O2晶体,厚度约200nm,片状方向的等效尺寸在1～5μm之间.与固相法相比, BSA作为吸附剂获得的NaxCO2O4片状晶体的厚度明显减小.     

纳米γ-Fe_2O_3的室温固相反应工艺研究

采用室温固相法合成了γ-Fe2O3的前驱体FeC2O4·2H2O及纳米γ-Fe2O3。以FeSO4·7H2O和H2C2O4·2H2O为原料,先得到了前驱体FeC2O4·2H2O,通过对反应机理的初步探讨,并研究其物质结构、分解过程和合适煅烧温度,最后在400℃下煅烧前驱体3h得到γ-Fe2O3纳米粒子。经热重(TG-DTA)、X射线衍射(XRD)和透射电镜(TEM)测试手段的分析,结果表明:室温固相法合成纳米γ-Fe2O3产物γ-Fe2O3纯净、粒子为纳米级且分布均匀。     

Some physical properties of V2O5-Fe2O3 and V2O5-Fe2O3-Li2O systems

Various methods have been used to study the physical properties of the V₂O₅-Fe₂O₃ and V₂O₅-Fe₂O₃-Li₂O systems, including X-ray, electron microscope, Mössbauer effect, NMR and thermogravimetric measurements. The iron ions are approximately equally distributed in substitutional and interstitial sites in the V₂O₅ lattice. The maximum number of iron ions dissolved in the V₂O₅ matrix corresponds to 4 mol % Fe₂O₃. In all the samples a quantity of Fe₂O₃ which has not been included in lattice is observed. The V₂O₅-Fe₂O₃ and V₂O₅-Fe₂O₃-Li₂O systems are formed from solid solutions mixed with very small Fe₂O₃ particles. The analysis of the charge compensation of iron ions suggests that V₂O₅ is a quasi-amorphous semiconductor. Irradiation of V₂O₅-based samples with an electron beam induces the V₂O₅ platelets to convert to the VO _x phase.     

Structural studies of some V2O5-P2O5-B2O3-Fe2O3 glass systems

X-ray diffraction and infrared measurements were performed on vanadium borophosphate glass containing different amounts of iron ranging from 0–7.5 mol % and heat treated at 300 °C for various times. The structure and phase separation could be determined for each glass composition. V₂O₅ was the main precipitated phase in all heat-treated samples, and its amount was dependent on the heat-treatment time and Fe₂O₃ content. Also FeP was detected in samples heat treated for 24 h. The infrared measurements showed the presence of both V⁴⁺ and V⁵⁺. The symmetry of V₂O ₇ ⁴⁻ and VO ₄ ³⁻ groups was found to increase with increasing Fe₂O₃ content. It was also found that some PO₄ changed to BO₃, forming a non-bridging oxygen.     

Study of structures and properties of ZnO-Sb2O3-P2O5-Na2O glasses

The influence of ZnO substitution by 0–12 wt.% Na₂O on the properties of ZnO-Sb₂O₃-P₂O₅-Na₂O glasses has been investigated. The structure and properties of the glasses with the composition of (13.86-x)ZnO-57.93Sb₂O₃-28.21P₂O_5?x Na₂O (x = 0–12 wt.%) were characterized by infrared spectra (IR), X-ray diffraction and differential thermal analysis (DTA). The results of IR indicated an increase in the intensity of symmetric vibrations of P-O-P bond, which was confirmed by the improvement of water durability with the increasing amount of Na₂O in the range of 0–10 wt.%. Substitution of 10 wt.% Na₂O led to the weight loss of the glass to 5.93 mg/cm^?2 after immersion in deionized water at 50 °C for 24 h. The results of XRD showed that the ability of crystallization decreased, indicating the good thermal stability of the glass. The glass containing 8 wt.% Na₂O had the best properties in every respect and might be an alternative to lead based glasses for the applications, providing further composition improvement.     

Plasma spraying of Al2O3 and Al2O3Y2O3

A microstructural study has been carried out of plasma-sprayed Al₂O₃ and mixed and sintered Al₂O₃Y₂O₃. In order to ascertain the degree of metastability achieved by plasma spraying, these results are compared with a similar experiment utilizing a CO₂ laser for melting and the hammer-and-anvil technique for quenching of the same materials. X-ray diffraction methods were used to determine the obtained phases and crystal structures. In addition, transmission electron microscopy was used to confirm the phases present and to study their morpology. The porosity was studied with both mercury intrusion porosimetry and small angle neutron scattering. The addition of Y₂O₃ is shown to decrease the porosity from 15% to 7.5%. Adhesion is likewise related to the addition of Y₂O₃ and it is seen that adhesion of the mixture is measurably improved over that of pure Al₂O₃. The implication of these results is discussed.     

Crystallization and properties of CaO-P2O2-B2O3 glasses

Glasses were prepared with compositions (50–0.5 x) CaO.(50–0.5 x) P₂O₅ · x B₂O₃ with B₂O₃ contents (x) from 0 to 45 mol%. The glass transformation temperature (T _g), dilatational softening temperature (T _D) and Vickers hardness (H _V) initially increased with x, but showed maxima at about x=20 for T _g and T _D and at about x=35 for H _V. The thermal expansion coefficient decreased with x, levelling off at about 35 mol% B₂O₃. The maximum tendency to crystallize occurred at around 25 mol% B₂O₃. Volume nucleation (and hence glass-ceramic formation) and surface nucleation were obtained for x between 15 and 25 mol%. The first phase to appear was BPO₄, which was probably homogeneously nucleated. Subsequently the 4CaO · P₂O₅ phase was heterogeneously nucleated on the BPO₄. For 10 x 35 only surface nucleation was observed. The kinetics of nucleation were investigated in the 20 mol% B₂O₃ glass. The changes in properties and crystallisation behaviour with B₂O₃ content were related to short-range structural information. Infrared spectra and literature data indicated a threedimensional network of B-O-B and B-O-P linkages in the glasses.