光催化剂SrTiO3的制备及其性能的研究

论述用化学液相共沉淀法制备SrTiO_3的最佳条件,及在不同的活化条件下对SrTiO_3光催化性能的影响。此外还研究了掺入过渡金属氧化物对SrTiO_3催化性能的改善。     

Au/ZnO and Au/Fe2O3 catalysts for CO oxidation at ambient temperature: comments on the effect of synthesis conditions on the preparation of high activity catalysts prepared by coprecipitation

The preparation of Au/ZnO and Au/Fe₂O₃ catalysts using two coprecipitation methods is investigated to determine the important factors that control the synthesis of high activity catalysts for the oxidation of carbon monoxide at ambient temperature. In particular, the factors involved in the preparation of catalysts that are active without the need for a calcination step are evaluated. The two preparation methods differ in the manner in which the pH is controlled during the precipitation, either constant pH throughout or variable pH in which the pH is raised from an initial low value to a defined end point. Non-calcined Au/ZnO catalysts prepared using both methods are very sensitive to pH and ageing time, and catalysts prepared at a maximum pH = 5 with a short ageing time (ca. 0–3 h) exhibit high activity. Catalysts prepared at higher pH give lower activity. However, all catalysts require a short operation period during which the oxidation activity increases. In contrast, the calcined catalysts are not particularly sensitive to the preparation conditions. Non-calcined Au/Fe₂O₃ catalysts exhibit high activity when prepared at pH ≥ 5. Calcined Au/Fe₂O₃ prepared using the controlled pH method retain high activity, whereas calcined catalysts prepared using the variable pH method are inactive. The study shows the immense sensitivity of the catalyst performance to the preparation methods. It is therefore not surprising that marked differences in the performance of supported Au catalysts for CO oxidation that are apparent in the extensive literature on this subject, particularly the effect of calcination, can be expected if the preparation parameters are not carefully controlled and reported.     

异丁烯两段催化氧化制甲基丙烯酸催化剂研究 Ⅰ．异丁烯气相氧化制甲基丙烯醛多元复合氧化物催化剂的研究

本文报导用于异丁烯（叔丁醇）选择氧化制ＭＡＬ（甲基丙烯醛）的多元复合氧化物催化剂的研究结果。同共沉淀法制备的催化剂的活性主要决定于其化学组成，同时受到制备条件的影响。最佳催化剂的主要物相组成为ＰｂＯ３，Ｂｉ２ＭｏＯ３．３、ＮｉＭｏＯ４、Ｓｂ２Ｏ３及ａ－Ｆｅ２Ｏ３小颗粒。在３５５℃，１０００～２５００ｈ－１空速范围，叔丁醇：水：空气＝１：３．３：７（摩尔比）的条件下可获得异丁烯转化率达９６％，ＭＡＬ选择性达８９％的结果。     

钯负载锰氧化物基双金属复合氧化物催化氧化羰基化合成碳酸二苯酯

采用共沉淀法分别制备锰掺杂钨、钒、铋3种双金属复合氧化物载体,以氯化钯为活性组分制备负载型催化剂,并用于苯酚氧化羰基化合成碳酸二苯酯（DPC）。通过气相色谱（GC）、X射线衍射（XRD）、氢气程序升温还原（H₂-TPR）、X射线光电子能谱（XPS）等表征手段,对催化剂结构和性能进行表征。结果表明:钨-锰载体随掺杂比例和焙烧温度升高,逐步形成四氧化三锰晶粒,同时钨渗入锰氧化物晶格中,在掺杂比（物质的量比）为1:1、焙烧温度为600 ℃条件下制备的催化剂性能最佳,DPC收率为5.20%;钒-锰载体在焙烧温度为400 ℃、掺杂比为1:5条件下形成二氧化锰晶相,催化剂性能明显提高,DPC收率为10.46%,而较高的焙烧温度会破坏晶型的完整;铋-锰载体在掺杂比为1:5、焙烧温度为400 ℃条件下制备的催化剂催化效果最好,DPC单程收率可达到13.13%。     

Dy_2O_3掺杂对钛酸锶钡陶瓷结构性能的影响

采用草酸盐沉淀法,以硝酸锶、硝酸钡、钛酸丁酯和草酸为原料,Dy2O3为掺杂剂,制得了Ba0.6Sr0.4TiO3粉体,并于1250℃将其烧结成Ba0.6Sr0.4TiO3系电介质陶瓷。利用扫描电镜、X射线衍射及TH2818自动元件分析仪对Dy2O3掺杂量为0.2%~2%的Ba0.6Sr0.4TiO3陶瓷的微观结构和介电性能进行研究。结果表明,Dy2O3的掺杂没有影响到BST陶瓷的主晶相钙钛矿结构,且一定量的Dy3+进入到BST晶格中。BST陶瓷的介电损耗随着掺杂量的增加而逐渐减小,介电常数随着掺杂量的增加呈现先增大后减小的趋势,当掺杂量为0.5%时,介电常数最大,为4 474.48。     

Synthesis and luminescence properties of red phosphor CaO: Eu3+

Ca(NO₃)₂·4H₂O, Eu(NO₃)₃ and H₂C₂O₄·2H₂O were adopted to synthesize CaO: Eu³⁺ with the chemical co-precipitation method, and the effects of the calcination temperature and Eu³⁺ doping concentration on the phosphor structure and its luminescent properties were investigated by TG-SDTA, XRD, and PL-PLE. The results confirm that the Eu³⁺ ions as luminescent centers substitutes Ca²⁺ sites without changing the crystal structure of cubic CaO. The optimum calcination temperature and the optimum concentration of Eu³⁺ are 1 100 ° and 1 mol%, respectively, under which the best crystallinity and highest PL intensity appeared. The maximum emission wavelength is 592 nm (⁵D₀→⁷F₁) which is excited by xenon lamp with the wavelength of 200–280 nm, indicating that the Eu³⁺ ion mainly locates in the symmetric position (O_h) in the crystal lattice of CaO. Funded by the Science and Technology Bureau of Sichun Province(No. 2006J13-059) and Education Bureau of Sichun Province (No. 2006A094)     

铜铈钛复合氧化物的制备及其催化一氧化碳氧化反应的性能

采用共沉淀法制备了不同钛含量的铜铈钛复合氧化物催化剂（Cu0.1CCe0.9-xTixO2,X=0～0．3）,采用微反-色谱评价装置考察了Cu0.1Ce0.9-xTixO2催化CO氧化反应的活性,并采用氮吸附／脱附,X-射线衍射以及程序升温还原等技术对催化剂进行了表征。结果表明,适量Ti（X≤0．15）的加入,提高了Cu0.1Ce0.9-xTixO2催化剂中CuO的分散度,从而提高了其催化活性。而当Ti含量过高（X=0．3）时,Cu0.1Ce0.9-xTixO2催化剂中CuO的分散度反而降低,从而导致其催化活性显著降低。     

纳米掺杂Ag（SnFe）O2电接触合金的研究

利用化学共沉淀、高能球磨技术及热压烧结等方法制备出纳米掺杂Ag（SnFe）O2触头合金，通过X射线衍射（XRD）、透射电镜（TEM）和冷场发射扫描电镜（FESEM）等对合金触头及其燃弧性能进行了分析。结果发现：Fe元素的加入，使Sn02纳米颗粒在550℃以下焙烧制粉和750℃以下块体烧结成型时都未明显长大，保持在20nm左右，制备的触头合金呈现纳米第二相弥散均匀分布在Ag基体中。在模拟电弧侵蚀试验中，该合金电弧阴极斑点铺展在较大区域，形成多点燃弧形貌，有效降低燃弧时间和电弧电流，分散电弧能量，使阴极斑点没有明显的液体喷溅、Ag的蒸发和第二相的分解，同时非晶的纳米第二相与Ag的润湿性更好，可进一步增加熔体粘度，提高耐电弧侵蚀性能。     

强磁场对锰锌铁氧体前驱体纳米颗粒形貌的影响

在共沉淀制备非铁磁性锰锌铁氧体前驱体纳米颗粒的过程中,分别施加零磁场、弱磁场(0.1～0.7 T)和强磁场(10 T),探讨磁场对非铁磁性锰锌铁氧体前驱体纳米颗粒形貌的影响规律.结果表明,当磁感应强度超过某一临界值时,非铁磁性纳米颗粒由球形颗粒向链状颗粒,然后向棒状或者纤维状颗粒转变.在10 T的强磁场下,纳米颗粒长成长径比很大的纤维状,能谱分析结果表明,纤维状颗粒主要为复合铁氧体,而非单一的沉淀产物.随着反应温度增加、溶液滴加时间延长将使纤维直径降低.     

Fe3Se8/Co3Se4/NiSe2/NC复合材料的制备及性能

由于锂资源的价格逐渐攀升,亟需开发价格低廉的电池系统。通过共沉淀法合成FeCoNiCP片状前驱体,再经过包覆多巴胺、退火和在氮气下硒化,制备钠离子电池负极材料Fe₃Se₈/Co₃Se₄/NiSe₂/NC。在0.01~3.00 V充放电,以0.1 A/g的电流循环70次,电极仍有468.38 mAh/g的可逆比容量;在0.1 A/g、0.2 A/g、0.5 A/g、1.0 A/g、2.0 A/g和5.0 A/g的电流下,分别具有363.85 mAh/g、345.88 mAh/g、320.73 mAh/g、308.31 mAh/g、290.33 mAh/g和249.29 mAh/g的可逆比容量。Fe₃Se₈/Co₃Se₄/NiSe₂/NC复合材料较好的电化学性能,可归因于碳导电网络、多金属硒化物和独特的纳米结构的协同作用,缓解了充放电过程中的体积膨胀。