铝酸钠溶液中钒酸盐的析出行为研究

以氧化铝生产流程中氢氧化铝的洗涤液为原料,研究了苛性碱浓度、反应温度及反应时间对溶液中钒酸盐析出情况的影响。结果表明,钒酸盐的析出率随苛性碱浓度的升高和反应时间的延长而增大,随反应温度的升高而减小。当铝酸钠溶液的苛性碱浓度为200g/L、反应温度为30℃、反应时间为72h时,溶液中的钒元素可减少60%以上。结晶析出的钒酸盐主要为钒酸钠和偏钒酸钠,其晶体结构为八面体。     

Formation and characterization of diamond crystals synthesized by microwave plasma CVD system

Abstract

Diamond crystals have been successfully synthesized on (100) Si wafer using microwave plasma CVD. The growth was conditioned in a flowing system in which the parameters, such as CH₄/H₂ ratio, pressure, temperature and microwave power were varied. Cubo‐octahedra or tetrakaidecahedra are the equilibrium shape of diamond single crystals obtained under all conditions and are therefore the basic unit for the formation of polycrystalline diamond films, mostly through repetitive twinning and secondary growth of diamond crystals on {100} habit planes of cubo‐octahedra. Both X‐ray diffraction and Raman spectroscopy were used to facilitate the analysis of the diamond crystallinity and purity. These qualities are similar to those of natural diamonds.     

温度对电沉积制备Pt-Ni阴极催化剂性能的影响

采用电化学还原法在碳布上电沉积Pt-Ni合金催化剂作为质子交换膜燃料电池阴极。通过循环伏安线性扫描法确定Pt-Ni合金的沉积电位,并在该电位下考察了不同电解液温度下所得催化剂的物理、化学性质及电催化性能。研究表明:在-0.35 V电位下可得到Pt-Ni合金,不同的电解液温度会影响Pt-Ni合金催化剂结构、形貌及组分比,进而影响其催化性能。当电解液温度为50℃时,Pt-Ni合金催化剂具有最佳的催化活性,此时催化剂为较小的球状颗粒,Pt与Ni的原子比接近3∶1,其电化学活性表面积为44.19 m2/g,是电解液温度为70℃下制备的催化剂的1.8倍。适当的温度下电沉积制得的Pt-Ni合金催化剂明显提高了铂对氧还原的催化活性。     

Carbon paste electrodes modified by Pt and Pt-Ni microparticles dispersed in polyindole film for electrocatalytic oxidation of methanol

Electrocatalytic activity of the Pt microparticles dispersed into polyindole (PIn) films obtained by electropolymerization on carbon paste electrodes (CPE) towards methanol oxidation in perchloric acid medium has been demonstrated and investigated using cyclic voltammetry, potentiodynamic polarization, chronoamperometry and impedance spectroscopic techniques. The results show that PIn films obtained on these electrodes serve as good host matrices for the dispersion of Pt microparticles and exhibit good catalytic activity towards the electrooxidation of methanol compared to bulk Pt and CPE modified with Pt. The morphology and composition of the modified and unmodified films were obtained using SEM and EDX techniques. The effect of scan rate, amount of Pt and concentration of methanol, on the activity of the electrode has been tested. The effect of alloying Pt with different amounts of Ni was studied and it was found that when the metals are deposited from a solution containing the metal salts in 1:1 ratio the activity towards methanol oxidation was significantly enhanced.     

Controlled synthesis and properties of palladium nanoparticles

In our research, the preparation processes of Pd nanoparticles (Pd NPs) with different methods by adding a certain amount of silver nitrate, iron chloride or sodium iodide are presented in order to control their size and morphology. Various sizes and shapes of Pd NPs are observed by alcohol reduction. The results show the size and morphology control of Pd NPs with chemical reductions of Pd salts by ethanol and ethylene glycol (EG) that have very different reduction processes. The modified polyol method with the gradual addition of Pd and polyvinylpyrollidone precursors in EG at 160°C has led to control their size and morphology in the 10?nm range using 0.02?M AgNO₃. It is observed that the Pd nanorod is also formed. The main factors that will control the shapes of Pd NPs have been presented to explain their growth and formation mechanisms in a control process.     

Stability of Pt-Ni/C (1:1) and Pt/C electrocatalysts as cathode materials for polymer electrolyte fuel cells: Effect of ageing tests

Carbon supported Pt and Pt-Ni (1:1) nanoparticles were prepared by reduction of metal precursors with NaBH₄. XRD analysis indicated that only a small amount of Ni alloyed with Pt (Ni atomic fraction in the alloy about 0.05). The as-prepared catalysts were submitted to chronoamperometry (CA) measurements to evaluate their activity for the oxygen reduction reaction (ORR). CA measurements showed that the ORR activity of the as-prepared Ni-containing catalyst was higher than that of pure Pt. Then, their stability was studied by submitting these catalysts to durability tests involving either 30 h of constant potential (CP, 0.8 V vs. RHE) operation or repetitive potential cycling (RPC, 1000 cycles) between 0.5 and 1.0 V vs. RHE at 20 mV s⁻¹. After 30 h of CP operation at 0.8 V vs. RHE, loss of all non-alloyed Ni, partial dissolution of the Pt-Ni alloy and an increase of the crystallite size was observed for the Pt-Ni/C catalyst. The ORR activity of the Pt-Ni/C catalyst was almost stable, whereas the ORR activity of Pt/C slightly decreased with respect to the as-prepared catalyst. Loss of all non-alloyed and part of alloyed Ni was observed for the Pt-Ni/C catalyst following repetitive potential cycling. Conversely to the results of 30 h of CP operation at 0.8 V vs. RHE, after RPC the ORR activity of Pt-Ni/C was lower than that of both as-prepared Pt-Ni/C and cycled Pt/C. This result was explained in terms of Pt surface enrichment and crystallite size increase for the Pt-Ni/C catalyst.     

(Ba_(1-x)Sr_x)(Zn_(1/3)Nb_(2/3))O_3微波介质陶瓷微结构对介电性能的影响

采用传统的固相烧结法制备(Ba1-xSrx)(Zn1/3Nb2/3)O3微波介质陶瓷,研究微结构对介电性能的影响.随着系统中Sr2+含量的增多,介电常数和温度系数发生异常呈现非线性变化,这是由于氧八面体的畸变而导致的相转变造成的,相转变的发生相应影响了极化以及极化模式.相转变及氧八面体畸变对介质损耗没有明显的影响,介质损耗受到Sr2+含量及烧结温度的影响较大.     

准八面体CBN单晶的合成研究

通过对原料、触媒及合成工艺的研究，采用国产DS-029B型六面顶压机在4．2—5．3GPa，1350。1470℃的范围内，从hBN-单质触媒体系中合成出近乎完美的黑色八面体和截角八面体立方氮化硼单晶体。确定了该种形态的CBN晶体的生长区域。CBN晶体的尺寸在100—400μm，峰值粒度为125—150μm。对所得的晶体进行考察，发现这种CBN晶体结晶形貌发育比较完整、棱角尖锐、晶粒饱满，并且有较高的抗压强度。上述结果表明所用的单质触媒具有使CBN晶体均匀生长的能力，是一种合成CBN晶体的有效触媒，该种CBN晶体具有较好的破碎强度。     

Decane reforming reaction over Pt,Ir, Pt-Ir and Pt-Ni bimetallic catalysts supported on Y-zeolite

Pt, Ir, Pt-Ir and Pt-Ni bimetallic catalysts supported on NaY- and HY-zeolite were examined as a catalyst for producing gasoline from n-decane via simultaneous reforming and cracking. The catalysts were prepared by calcining and reducing metal-ion-exchanged Y-zeolite with O₂ and H₂ at 300°C., respectively. Thus prepared catalysts were characterized by hydrogen chemisorption and temperature programmed desorption of ammonia. Pt-Ni/NaY and Pt-Ir/NaY bimetallic catalysts offered the improved activity maintenance compared to Pt/NaY monometallic catalyst. The catalysts supported on HY-zeolite showed higher selectivity toward C₅–C₇ and skeletal isomers of C₅–C₇- and C₈–C₁₀ than those of the catalysts supported on NaY-zeolite, which is a desired characteristic for increasing octane value of gasoline these days. However, deactivation with reaction time was much more pronounced on HY-zeolite-supported catalyst. When the catalyst was prcsulfided with H,S, the stability with time on stream was enhanced and the selectivity was quite different from that of the catalyst before presulfiding. The acidity of Y-zeolite and presulfiding of catalyst greatly influenced the activny, selectivity and stability of Pt, Ir, Pt-Ir and Pt-Ni bimetallic catalysts supported on Y-zeolite in n-decane reforming reaction.