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1.
Platinum nanoparticles supported on graphite nanofibers (GNFs) were prepared by microwave assistant heating polyol process. TEM images showed that microwave prepared Pt nanoparticles supported on GNFs were small and uniform, and the average diameter was about 3.4 nm. Cyclic voltammetric test showed that Pt/GNFs exhibited very high electrocatalytic activity for methanol oxidation.  相似文献   

2.
微乳法制备纳米TiO2 /SiO2的结构及光催化研究   总被引:1,自引:0,他引:1  
Nanosized TiO2 and TiO2/SiO2 particles were prepared by hydrolysis of tetrabutyl titanate (TBOT) and tetraethyl orthosilicate (TEOS) in the TX-100 reverse microemulsion. These particles were characterized by TG-DSC, XRD, FTIR, TEM,N2 adsorption-desorption. Their photocatalytic activity was tested by degradation of methyl orange. The result shows that TiO2/SiO2 nanoparticles are with a monodispersed spherical phase and a uniform size distribution,and TiO2 particles are dispersed on the surface of SiO2. The band for Ti-O-Si vibration in FTIR was observed, the Ti-O-Si bond increased the stability of anatase TiO2, suppressed the phase transformation of titania from anatase to rutile. And due to the addition of SiO2, the average size of titania decreased from 38 nm in pure TiO2 to 5 nm in TiO2/SiO2. It was found, under UV light irradiation, TiO2/SiO2 particles showed higher activity than pure TiO2, and TiO2/SiO2(1/1) particles showed the highest photocatalytic activity on the photocatalytic decomposition of methyl orange, which was influenced by crystal structure, particle size, crystallinity and Surface area Characteristics.  相似文献   

3.
TiO2 membranes were prepared on aluminum-alloy thin plates by electrophoretic deposition and dip coating in a colloid solution of TiO2, respectively. The photocatalytic activity of TiO2 membrane was compared using ethylene as reactant, and the crystal and morphological structure of the membrane were characterized by XRD and SEM. The results showed that a more compact membrane with high loading of TiO2 but lower photocatalytic activity of unit TiO2 mass was obtained by electrophoresis compared with dip coating method. The addition of polyethylene glycol (PEG) to the sol of TiO2 could improve the specific photocatalytic activity (ethylene conversion per unit mass TiO2 and unit area of membrane piece) of the electrophoresis-membrane prepared from the sol, but could not change the specific photocatalytic activity of the dip-coating membrane from the sol. The ethylene conversion on the electrophoresis membrane prepared from the sol containing PEG (50 g·L-1) was 9 times of that on the dip coating membrane. The effect of PEG on the properties of electrophoresis-membrane of TiO2 was attributed to the change of electrokinetic properties of sol. Addition of PEG decreased ζ potential value of the sol and the mobility of the sol particle, increased viscidity of the colloid, thus decreasing both the electrophoresis deposition velocity of colloid particles and the electroosmosis velocity of diffuse layer of colloid particles. These favored the formation of a low compact and porous membrane on the electrode in electric field, and thus increasing the availability of TiO2 in photocatalytic process.  相似文献   

4.
微波辐照方式对CdS和Bi2S3纳米粒子结晶度的影响   总被引:4,自引:0,他引:4       下载免费PDF全文
The effect of traveling microwave irradiation on the crystallinities of CdS nanoparticles and Bi2S3 nanorods was studied. Results showed that as compared with stationary microwave irradiation the crystallinities and the crystal growth of sulfide nanoparticles were improved. Traveling microwave irradiation can supply narrower frequency distribution and stronger power density of irradiation, CdS nanoparticles and Bi2S3 nanorods obtained are better in crystallinities and larger in size than under stationary microwave irradiation.  相似文献   

5.
电沉积HA/TiO2复合涂层的结合强度和热稳定性研究   总被引:6,自引:0,他引:6  
HA/TiO2 composite coating were fabricated via adding TiO2 powder in the electrolyte by electrodeposition. The influence of current density and deposition time on the content of TiO2 in the coating, the influence of the content of TiO2 in the coating on the bonding strength of coating and the influence of sintering temperature on the structure and the bonding strength of coating were investigated. The experiment results show that the content of TiO2 in the coating increase with reducing the current density and prolonging the deposition time, the bonding strength improve with increasing the content of TiO2 in the coating, which can obtain 18.7 MPa when the weight percent TiO2 in the coating attain 72.2 %. The addition of TiO2 in the coating reduces the thermal expansion coefficient of the coating, improves the bonding strength of coating and changes the fracture mechanism of the coating from adhesion failure to cohesive failure. HA in the composite coatings is decomposed by the catalysis reaction of TiO2 at the temperature of sinter 850 ℃. Differential scanning calorimetry and X-ray diffractometry analyses showed that the chemical reaction between HA and TiO2 lead to the product are α-TCP and CaTiO3 at the temperature of sinter 1200 ℃. In order to prevent the coating from decomposing and attain hign bonding strength, the sintering temperature should be less than 820 ℃.  相似文献   

6.
LaNiO3(LNO) thin films were prepared on Pt(111) / Ti / SiO2/ Si substrate by metal-organic decomposition (MOD) method. Pb(Zr,Ti)O3 ferroelectric thin films and their compositionally graded thin films were prepared on LNO / Pt / Ti / SiO2 /Si substrates by Sol-gel method. The composition depth profile of a typical up-graded film was determined by using a combination of Auger Electron Spectroscopy (ASE) and Ar Ion Etching. The results confirm that the processing method produces graded composition changes. XRD analysis showed that the graded thin films possessed composite structure of tetragonal and rhombohedral. The dielectric constants of Up-graded and Down-graded thin films were higher than that of each thin film unit. The dielectric constants were 277 and 269 at 10 kHz, respectively. The loss tangents were 0.019 and 0.018 at 10 kHz, respectively. The Hysteresis loops showed that the remanent polarizations of graded thin films were higher than that of each thin film unit, but the coercive fields were smaller. The remanent polarizations of Up-graded and Down-graded thin films were 30.06 and 26.96 μC·cm-2, respectively. The coercive fields were 54.14, 54.23 kV·cm-1, respectively. The pyroelectric coefficients of Up-graded and Down-graded thin films were 4.62, 2.51×10-8 C·cm-2·K-1 at room temperature, respectively. They were higher than that of each thin film unit.  相似文献   

7.
球形Gd2O3∶Eu纳米发光材料的制备   总被引:1,自引:0,他引:1  
Spherical nanometer Gd2O3∶Eu luminescent materials were prepared by homogeneous precipitation method, and the properties were studied also. TG, FTIR and XRD analysis showed that the precursor was carbonate, the cubic Gd2O3was obtained after calcination. TEM photographs indicated that the samples were spherical and well dispersed with nanometer and submicrometer size of 200~300 nm which is the nanoparticles’ aggregate. The mechanics of agglomerating growth is also discussed. ED photograph showed that the particle was crystalline. The PL analysis exhibited that CTB band of nanometer Gd2O3∶Eu was of 17 nm red shift to bulk materials, and the emission peak was broadened due to the surface and interface effect of nanocrystals.  相似文献   

8.
TiO2 coated SiO2 materials as anode for lithium-ion batteries were synthesized via an in situ hydrolysis of tetraethyl orthosilicate under ultrasonic irradiation using nanometer-sized TiO2 colloids as precursors. The XRD patterns indicate that the as-prepared core/shell particles remain anatase after calcining below 800 ℃. TEM observation shows that the particle size of TiO2 / SiO2 composites is ca. 200 nm, and a homogeneous SiO2 layer is coated on the surfaces of TiO2 particles. FTIR spectra demonstrate that SiO2 could have been coated on the surfaces of TiO2 particles via a chemical bonding. In addition, the first specific charge and discharge capacities of the coated particle electrode were 66.4 mAh·g-1 and 90.7 mAh·g-1, respectively, which indicates that the TiO2 / SiO2 particles are more stable than the monodispersed TiO2. Meanwhile, the new material has good lithium intercalation-deintercalation performances.  相似文献   

9.
铁、氮共掺杂二氧化钛粉末的制备及光催化活性   总被引:24,自引:0,他引:24  
Using TiCl4 as the titanium source, nanoparticles of TiO2 doped with nitrogen(N-TiO2) were synthesized by triethylamine. TiO2 powder codoped with iron and nitrogen(Fe/N-TiO2) were prepared by adsorption-deposition of Fe3+ on N-TiO2 and calcining at 400 ℃ for 2 h. From the XPS results for N1s binding energy at 399.6 eV and 396.6 eV, it is proposed that the partial N atoms as substitution atoms replace for O atoms in TiO2 lattice. The onset of the absorption spectrum of Fe/N-TiO2 has a 45 nm red-shift compared with that of TiO2. The results of photocatalytic degradation of methylene blue solution indicate that Fe/N-TiO2(0.45% Fe3+) has a higher activity. Its photocatalytic activity is about 2 times as high as that of pure TiO2 under UV-light, and 3 times under sunlight. Doping of nitrogen in TiO2 enhances photoresponse in visible light region and doping of Fe3+ reduces the recombination of electrons and holes. Both of the above effects are beneficial for improving the performances of Fe/N-TiO2 photocatalyst.  相似文献   

10.
TiO2-SiO2 nanocomposite particles were prepared in premixed H2 / Air flame, and the morphology and structure of these nanocomposites were characterized by FTIR, XRD, TEM and HRTEM. The morphology of SiO2 / TiO2 nanocomposites was different from that of pure TiO2 or SiO2 nanoparticles, and the chemical bond of Ti-O-Si was found in the nanocomposites indicating that the TiO2 / SiO2 nanocomposites were not merely a physical mixture of TiO2 and SiO2. TiO2 nanocrystalline grains with sizes of 1~2 nm were homogeneously dispersed in the amorphous SiO2 matrix when TiCl4 and SiCl4 were mixed at molecular level in the flame. The particle size and rutile content decreased with increasing of SiO2 molar ratio.  相似文献   

11.
针对银精矿样品复杂,难消解的特点,研究了不同酸溶法和碱熔法对样品的消解情况,建立了硝酸,盐酸,氢氟酸,高氯酸消解银精矿的方法。根据元素灵敏度和抗干扰性,选定各元素的测定波长。通过酸溶样和碱熔样测定结果比对,验证了方法准确性。建立了四酸消解-电感耦合等离子体光谱法测定银精矿中铜、铅、锌、砷、镉、钙、镁、锰含量的方法,元素的线性相关系数均在0.9999以上。通过共存元素干扰实验,确定了银精矿中高含量元素(铜、铅、锌、铁、锑、铋等)对测定元素结果没有影响。方法检出限:Cu 0.0063 mg/L, Pb 0.0159 mg/L ,Zn 0.0090 mg/L,As 0.0192 mg/L, Cd 0.0093 mg/L ,Ca 0.0084 mg/L, Mg 0.0075 mg/L, Mn 0.0081 mg/L。测定下限:Cu 0.0105mg/L,Pb 0.0265 mg/L, Zn 0.0150 mg/L, As 0.0320 mg/L, Cd 0.0155 mg/L, Ca 0.0140 mg/L, Mg 0.0125 mg/L,Mn 0.0135 mg/L。3个样品的相对标准偏差在0.87%~3.56%之间,加标回收率在95.00%~103.56%之间。方法流程短,操作简单,快速,灵敏度和再现性高,结果准确可靠,可以满足银精矿中铜、铅、锌、砷、镉、钙、镁、锰含量的测定。  相似文献   

12.
Single crystals of K3RESi2O7 (RE=Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) were grown from a potassium fluoride flux. Two different structure types were found for this series. Silicates containing the larger rare earths, RE=Gd, Tb, Dy, Ho, Er, Tm, Yb crystallize in a structure K3RESi2O7 that contains the rare-earth cation in both a slightly distorted octahedral and an ideal trigonal prismatic coordination environment, while in K3LuSi2O7, containing the smallest of the rare earths, lutetium is found solely in an octahedral coordination environment. The structure of K3LuSi2O7 crystallizes in space group P63/mmc with a=5.71160(10) Å and c=13.8883(6) Å. The structures containing the remaining rare earths crystallize in the space group P63/mcm with the lattice parameters of a=9.9359(2) Å, c=14.4295(4) Å, (K3GdSi2O7); a=9.88730(10) Å, c=14.3856(3) Å, (K3TbSi2O7); a=9.8673(2) Å, c=14.3572(4) Å, (K3DySi2O7); a=9.8408(3) Å, c=14.3206(6) Å, (K3HoSi2O7); a=9.82120(10) Å, c=14.2986(2) Å, (K3ErSi2O7); a=9.80200(10) Å, c=14.2863(4) Å, (K3TmSi2O7); a=9.78190(10) Å, c=14.2401(3) Å, (K3YbSi2O7). The optical properties of the silicates were investigated and K3TbSi2O7 was found to fluoresce in the visible.  相似文献   

13.
A series of osmium double perovskite oxides, Ln2LiOsO6 (Ln=La, Pr, Nd, Sm), has been prepared as single crystals from acidic molten hydroxide. All four oxides crystallize in the monoclinic space group P21/n (Glazer tilt system #10, aab+), forming a 1:1 ordered rock salt lattice of Li+ and Os5+ cations. Magnetic susceptibility measurements show that these compounds are antiferromagnetic at low temperature with ordering temperatures of 39, 35, 23, and 32 K for Ln2LiOsO6 (Ln=La, Pr, Nd, Sm), respectively.  相似文献   

14.
A particular pathology of certain W5Si3-type A5B3 structures (I4/mcm) appears to arise because of unduly close approaches of the A1-type atoms on the cell faces at , 0, () that occur with the larger and more electropositive A and/or in the presence of smaller B atoms. A structure refinement of binary Ba4.81Pb3 indicates such a marginal stability in that the Ba atoms in the facial Ba0.81 chains exhibit an extreme displacement ellipsoid along . Although Ca5Sn3 and La5Ga3 binaries are unknown in this structure type, five stable ternary derivatives of these have been synthesized via substitution reactions and characterized by single crystal X-ray diffraction means: Ca4Sn3.223(4)Mg0.777, Ca4Sn3Cu1.30(4), Ca4.66(6)Sn3Zn0.704(4), La4.81(1)Ga1.38(2)Al1.62, and La4.762(5)Ga1.5(1)Zn1.5. Only the Ca-Sn-Zn phase exhibits lower symmetry, P4/mbm. The problematic A1 sites exhibit diverse changes in these, whereas the surrounding B2 tetrahedra are largely unaltered. The Ca-Sn results are, respectively: direct Mg/Sn substitution at the Ca1 site; mixed fractional distribution of the smaller Cu at two sites around the A1 position with an unresolved disorder; a pair of apparently independent modes, fractional Ca in the normal position and fractional Zn rectangles thereabout. The two La-Sn phases contain normal Ga,Al (Ga,Zn) tetrahedral chains with pairs of fractional disordered La atoms along , 0, z. Each can be rationalized in terms of a reasonable incommensurate structure. Electronic effects may also be operable.  相似文献   

15.
Single crystals of a series of lanthanide lithium iridium oxides, Ln2LiIrO6 (Ln=La, Pr, Nd, Sm, Eu) with the double perovskite structure have been grown from molten LiOH/KOH fluxes. The compounds crystallize in a distorted 1:1 rock salt lattice of Li+ and Ir5+ cations in the monoclinic space group P21/n. The magnetic susceptibilities of Ln2LiIrO6 (Ln=Pr, Nd, Sm, Eu) are presented.  相似文献   

16.
Singlet-triplet energy gaps in cyclopenta-2,4-dienylidene, as well as its 2- or 3-halogenated derivatives, are compared and contrasted with their sila, germa, stana, and plumba analogues; at HF/6-31G* and B3LYP/ 6-311++G(3df, 2p) levels of theory. Energy gaps (ΔGt-s), between triplet (t) and singlet (s) states, appear linearly proportional to: (i) the size of the group 14 divalent element (M = C, Si, Ge, Sn and Pb), (ii) the angle ∠C-M-C, and (iii) the ΔG(LUMO-HOMO) of the singlet state involved. The magnitude of ΔGt-s, for each 2- and/or 3-substituted species studied, increases with an order of: carbenes < silylenes < germylenes < stanylenes < plumbylenes. This order reverses for the barriers of the ring puckering. The puckering occurs with more ease for every singlet, compared to its corresponding triplet form.Regardless of the group 14 element (M) employed, every 3-halo-substituted species is more stable than the corresponding 2-halo-substituted isomer. For M = Pb, Sn and/or Ge; 3-halo-substituted species have higher ΔGt-s than their corresponding 2-halo-substituted analogues. For M = Si, similar ΔGt-s are found for 2- and 3-halogenated isomers. For M = C, 3-halo-substituted species have lower ΔGt-s than their corresponding 2-halo-substituted analogues.Every cyclic singlet has a larger ∠C-M-C angle, than its corresponding cyclic triplet state, except for 3-halosilacyclopenta-2,4-dienylidenes where triplet has a larger ∠C-M-C angle than its corresponding singlet state.  相似文献   

17.
The crystal structures of five isotypic hexagonal compounds with general formulaMAs4O6 X [M=K, NH4;X=Cl, Br, I; space group: P622;Z=1] were determined from 370 single crystal X-ray data and refined toR values <0.05. The structure type is characterized by neutral charged [As2O3] sheets arranged parallel (00.1). The As atoms of neighbouring two sheets point to each other and the sheets are combined by interlayeredM andX atoms, respectively. TheM atoms are coordinated to twelve oxygen atoms, theX atoms are coordinated to twelve arsenic atoms. In both cases the coordination polyhedron is a hexagonal prism. The compounds were synthesized by thermal treatments of cubic As2O3 and potassium or ammonium haloids in a saturated aqueous solution of potassium acetate resp. ammonia [500 K, saturation vapour pressure].
Die Verbindungen KAs4O6 X (X=Cl, Br, I) und NH4As4O6 X (X=Br, I): Hydrothermalsynthese und Strukturbestimmung
Zusammenfassung Die Kristallstrukturen der fünf isotypen hexagonalen Verbindungen mit der allgemeinen FormelMAs4O6 X [M=K, NH4;X=Cl, Br, I; Raumgruppe: P622;Z=1] wurden anhand von 370 Einkristall-Röntgendaten bestimmt und aufR-Werte <0.05 verfeinert. Der Strukturtyp ist ausgezeichnet durch neutrale [As2O3]-Schichten, die parallel (00.1) angeordnet sind. Die As-Atome zweier benachbarter Schichten weisen jeweils aufeinander zu, und die Schichten selbst werden durch zwischengelagerteM- bzw.X-Atome verbunden. DieM-Atome werden jeweils von zwölf O-Atomen, dieX-Atome von zwölf As-Atomen umgeben. Das Koordinationspolyeder ist in beiden Fällen ein hexagonales Primsa. Die einzelnen Verbindungen wurden unter Hydrothermalbedingungen aus kubischem As2O3 und dem jeweiligen Kalium- oder Ammoniumhalogenid in einer gesättigten wäßrigen Lösung von Kaliumacetat bzw. Ammoniak synthetisiert (500 K, Sättigungsdampfdruck).
  相似文献   

18.
Sulfur/oxygen-bridged incomplete cubane-type triphenylphosphine molybdenum and tungsten-clusters [Mo3S4Cl4(H2O)2(PPh3)3]·3THF (1A), [Mo3S4Cl4(H2O)2(PPh3)3]·2THF (2A), [Mo3OS3Cl4(H2O)2(PPh3)3]·2THF (1B), and [W3S4Cl4(H2O)2(PPh3)3]·2THF (1C) were prepared from the corresponding aqua clusters and PPh3 in THF/MeOH. On recrystallization from THF, procedures with and without addition of hexane to the solution gave 1A and 2A, respectively, while the procedures gave no effect on the formation of 1B and 1C. Crystallographic results obtained are as follows: 1A: monoclinic, P21/n, a=17.141(4) Å, b=22.579(5) Å, c=19.069(4) Å, =96.18(2)°, V=7337(3) Å3, Z=4, R(R w)=0.078(0.102); 1C: monoclinic, P2 1/c, a=12.635(1) Å, b=20.216(4) Å, c=27.815(3) Å, =96.16(1)°, V=7062(2) Å3, Z=4, R(R w)=0.071(0.083). If the phenyl groups are ignored, the molecule [Mo3S4Cl4(H2O)2(PPh3)3] in 2A has idealized CS symmetry with the mirror plane perpendicular to the plane determined by the metal atoms, while the molecule in 1A does not have the symmetry. The tungsten compound 1C is isomorphous with the molybdenum compound 2A. 31P NMR spectra of 1A, 2A, and 1C were obtained and compared with similar clusters with dmpe (1,2-bis(dimethylphosphino)ethane) ligands.  相似文献   

19.
The crystal structures of compounds with nominal compositions Bi6FeP2O15+x (I), Bi6NiP2O15+x (II) and Bi6ZnP2O15+x (III) were determined from single-crystal X-ray diffraction data. They are monoclinic, space group I2, Z=2. The lattice parameters for (I) are a=11.2644(7), b=5.4380(3), c=11.1440(5) Å, β=96.154(4)°; for (II) a=11.259(7), b=5.461(4), c=11.109(7) Å, β=96.65(1)°; for (III) a=19.7271(5), b=5.4376(2), c=16.9730(6) Å, β=131.932(1)°. Least squares refinements on F2 converged for (I) to R1=0.0554, wR2=0.1408; for (II) R1=0.0647, wR2=0.1697; for (III) R1=0.0385, wR2=0.1023. The crystals are complexly twinned by 2-fold rotation about , by inversion and by mirror reflection. The structures consist of edge-sharing articulations of OBi4 tetrahedra forming layers in the a-c plane that then continue by edge-sharing parallel to the b-axis. The three-dimensional networks are bridged by Fe and Ni octahedra in (I) and (II) and by Zn trigonal bipyramids in (III) as well as by oxygen atoms of the PO4 moieties. Bi also randomly occupies the octahedral sites. Oxygen vacancies exist in the structures of the three compounds due to required charge balances and they occur in the octahedral coordination polyhedron of the transition metal. In compound (III), no positional disorder in atomic sites is present. The Bi-O coordination polyhedra are trigonal prisms with one, two or three faces capped. Magnetic susceptibility data for compound (I) were obtained between 4.2 and 350 K. Between 4.2 and 250 K it is paramagnetic, μeff=6.1 μB; a magnetic transition occurs above 250 K.  相似文献   

20.
Single crystals of double-perovskite type lanthanide magnesium iridium oxides, Ln2MgIrO6 (Ln=Pr, Nd, Sm-Gd) have been grown in a molten potassium hydroxide flux. The compounds crystallize in a distorted 1:1 rock salt lattice, space group P21/n, consisting of corner shared MO6 (M=Mg2+ and Ir4+) octahedra, where the rare earth cations occupy the eight-fold coordination sites formed by the corner shared octahedra. Pr2MgIrO6, Nd2MgIrO6, Sm2MgIrO6, and Eu2MgIrO6 order antiferromagnetically around 10-15 K.  相似文献   

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