熔盐法制备片状Bi_(2.5)Na_(3.5)Nb_5O_(18)晶体

以分析纯Bi2O3、Na2CO3和Nb2O5为原料,以NaCl为熔盐,采用熔盐法合成出片状Bi2.5Na3.5Nb5O18(简称BNN5)晶体。研究了合成温度、保温时间和熔盐含量对BNN5晶体形貌的影响。结果表明:随着合成温度的提高、保温时间的延长和熔盐含量的增加,BNN5粉体的尺寸逐渐增大。当熔盐与总反应物的质量比为1∶1,在1100℃下保温3 h时,可以制备出片状的BNN5晶体,其边长为12~24μm,厚度为0.5~2μm,有望成为外延生长001NaNbO3片状晶体的理想模板。     

织构化K0.5Na0.5NbO3无铅压电陶瓷的性能研究

以分析纯Na2CO3、Bi2O3和Nb2O5为原料,以NaCl为熔盐,采用二次熔盐法和拓扑化学反应法合成各向异性片状NaNbO3粉体.以该片状NaNbO3粉体为模板品粒,以固相法合成的NaNbO3和KNbO3粉体为基料,采用流延工艺制备出较高取向度的织构化K0.5Na0.5NbO3(KNN)无铅压电陶瓷,系统研究了模板含量、烧结温度和保温时间等工艺参数对织构化KNN陶瓷显微结构和压电性能的影响规律.研究结果表明:随着模板含量的增加,陶瓷的取向度逐渐增加,当模板含量为15 wt%时,陶瓷的取向度可达0.69,当模板含量为10 wt%,1100 ℃下保温5 h烧结,可以获得具有一定织构度(f=0.58)的KNN陶瓷,并表现出优异的压电性能,d33=128 pC/ N.     

两步熔盐法制备片状NaNbO_3晶体

以分析纯Bi2O3、Na2CO3和Nb2O5为原料,采用两步熔盐法合成出片状NaNbO3。首先以NaCl为熔盐,在1100℃保温3 h合成出片状中间体Bi2.5Na3.5Nb5O18(简称BNN5)晶粒;然后以BNN5为模板晶粒,以NaCl为熔盐,在950℃保温3 h制备出片状NaNbO3。通过XRD和SEM分析表明:所制备的NaNbO3晶体为纯钙钛矿相,NaNbO3晶粒呈各向异性片状,其边长约为12μm,厚约为0.6μm,并探讨了BNN5转变为片状形貌NaNbO形成机理。     

熔盐法制备铌酸钾钠粉体的研究

以分析纯Na2CO3,K2CO3和Nb2O5为原料,以Na2CO3-K2CO3(摩尔比1:1)为熔盐,采用熔盐法在700～850℃保温4h合成了Na0.5K0.5NbO3粉体。研究了合成温度、熔盐含量对粉体形貌的影响。XRD分析结果表明:通过熔盐法可以在700℃下合成纯钙钛矿结构的Na0.5K0.5NbO3粉体;SEM分析显示:随着合成温度的升高,粉体形貌从圆球状转变为立方状,进一步提高合成温度,粉体形貌开始变得不规则;此外,合成粉体的尺寸随着熔盐含量的增加而增大,且粉体团聚现象明显减弱。以熔盐法合成的Na0.5K0.5NbO3粉体为原料,采用传统固相烧结法制备Na0.5K0.5NbO3陶瓷,经1060℃烧结后,Na0.5K0.5NbO3陶瓷具有优异的压电性能和介电性能,其中压电常数d33=124pC/N,介电常数εT/ε=345,居里温度T达402℃。     

非线性光学晶体Na3La9O3(BO3)8的生长研究

以Na3CO3和H3BO3为助熔剂,Na3CO3和H3BO3摩尔比为7/6,熔质Na3La9O3(BO3)8和助熔剂摩尔比为1/10～1/14,采用顶部籽晶生长方法,生长Na3La9O3(BO3)8晶体,晶体尺寸为30×18×8mm3.本文讨论了籽晶方向对Na3La9O3(BO3)8晶体生长的影响,(100)方向比(001)方向更有利于晶体生长.     

水热法合成微米级棒状SnO2

本文采用水热法,以SnCl4.5H2O和ZnO为前驱物,6mol/L KOH作矿化剂,低温180℃反应12h,高温430℃反应24h,合成了微米级棒状SnO2。测量了合成材料的X射线衍射谱(XRD),利用透射电镜(TEM)和扫描电镜(SEM)对晶体的形貌进行了表征。实验结果表明,在低温180℃时首先合成了ZnSnO3,提高温度到430℃,利用ZnSnO3高温分解的特性提供了SnO2晶体生长的溶质条件,使SnO2晶体持续生长,合成了微米级SnO2,晶体直径可达0.3~0.5μm,长度约为3~10μm。通过在酸性溶液中浸泡生成物,可以获得纯SnO2晶体。     

熔盐法制备针状莫来石晶体的研究

本文采用Al2(SO4)3·18H2O和SiO2为原料,以K2SO4,Na2SO4为熔盐,用熔盐法合成了针状莫来石晶体.研究了不同合成温度、熔盐用量和保温时间对合成莫来石晶体的影响,分析了熔盐法合成针状莫来石的反应机理.研究结果表明:以K2SO4为熔盐,熔盐与反应物总量质量比为1: 1,合成温度为1000 ℃,保温时间为3 h时可以合成针状莫来石晶体,针状莫来石的生成符合L-S液固生长机理.     

水热法生长棒状MnOOH和MnO2晶体

以高锰酸钾(KMnO4)和硫酸铵((NH4)2SO4)为主要原料,在150℃反应16h,水热法生长了棒状MnOOH晶体,然后以合成的棒状MnOOH晶体为前驱物,在硫酸溶液中,130℃水热反应12h,生长了棒状MnO2晶体。探索了KMnO4和(NH4)2SO4的用量以及反应温度对合成棒状MnOOH晶体的影响。利用X射线粉末衍射(XRD)、透射电子显微镜(TEM)和选区电子衍射等(SAED)等手段对产物进行了表征。结果表明,产物MnOOH为单斜结构的纯相,呈现棒状形貌,其平均直径约为72nm,长度近9.2μm,显示单晶特性;产物MnO2为四方结构的纯相,呈现棒状形貌,其平均直径约为83nm,长度达11μm,显示单晶特性。     

水热法合成掺Mn橙色刚玉晶体

本文采用水热法，在430℃、40MPa的压力下合成出了纯α-Al2O3晶体。在同样的条件下，通过掺人Mn(NO3)2合成了掺Mn橙红色刚玉晶体。掺人Mn(NO3)2时，合成产物有两种晶体，一种是无色刚玉晶体，体积较小，为六棱柱状，直径30～40μm，高为30～40μm。另一种晶体为橙红色掺Mn刚玉晶体，其外形轮廓近乎球形，晶体表面有十分粗糙的生长阶梯，台阶高度为2～5μm，晶体高200～300μm，直径200～300μm。     

Na3La9O3(BO3)8的晶体结构

以Na2CO3-H3BO3为助熔剂,用顶部籽晶法生长出Na3La9O3(BO3)8单晶。测定了Na3La9O3(BO3)8晶体结构,结果表明:该晶体属六方晶系,空间群:P62m,晶胞参数为a=b=0.89229(13)nm,c=0.87366(17)nm,α=β=90°,γ=120°,Z=1,V=0.60240(17)nm3,密度为5.066g/cm3。晶体结构中的硼氧基团是平面的BO3基团,BO3基团相互独立,通过与Na(1)O6、La(1)O9和La(2)O8的配位多面体连结形成层状结构,所有层平行于(001)面。描述了NaLaO(BO)晶体在非线性光学材料领域的应用前景。     

Synthesis, spectroscopy, and X-ray structures of fac-(CO)3(dppe)MnSC(S)H, fac-(CO)3(dppe)ReSC(S)H, fac-(CO)3(dppp)ReSC(S)H, and fac-(CO)3(dppb)ReSC(S)H

The monodentate dithioformato complexes, fac-(CO)₃(dppe)MnSC(S)H (1), fac- (CO)₃(dppe)ReSC(S)H (2), fac-(CO)₃(dppp)ReSC(S)H (3), and fac-(CO)₃ (dppb)ReSC(S)H (4), where dppe is 1,2-bis(diphenylphosphino)ethane, dppp is 1,3-bis(diphenylphosphino)propane, and dppb is 1,4-bis(diphenylphosphino)butane, were synthesized from the treatment of the corresponding hydrides, fac-(CO)₃ (P-P)MSC(S)H with CS₂. Compounds 1–4 crystallize in the monoclinic crystal system: for 1, space group = P2₁/c, a = 15.3139(3) Å, b = 9.7297(4) Å, c = 19.0991(6) Å, = 105.928(1), V = 2736.5 ų, Z = 4; for 2, space group = P2₁/c, a = 15.6395(8) Å, b = 9.8182(5) Å, c = 19.4153(11) Å, = 106.741(1), V = 2854.9(3) ų, Z = 4; for 3, space group = P2₁/n, a = 11.3570(10) Å, b = 19.465(2) Å, c = 15.5702(14) Å, = 104.776(2), V = 3328.3(5) ų, Z = 4; and for 4, space group = C2/c, a = 32.078(2) Å, b = 10.4741(6) Å, c = 19.0608(9) Å, = 94.315(2), V = 6386.1(6) ų, Z = 8.     

Crystal and molecular structures oftrans-dichloro-(ethylene) (4-methylpyridine)platinum(II) andtrans-dichloro(ethylene) (2,4,6-trimethylpyridine)platinum(II)

The crystal and molecular structures oftrans-[PtCl₂(C₂H₄)(4-MeC₅H₄N)] (I) andtrans-[PtCl₂(C₂H₄)(2,4,6-Me₃C₅H₂N)] (II) have been determined by single-crystal x-ray methods.I crystallizes in space groupP2₁/c witha= 4.991(1), b=21.658(3), c=10.675(3) Å, =110.17(2) °,Z=4;II is orthorhombic (Pbca) witha=10.295(6),b=12.393(8),c=20.370(10) Å,Z=8.Full-matrix least-squares refinements have given finalR factors of 0.053 (1520 reflections) forI and 0.042. (1412 reflections) forII. The intensities were recorded by counter methods, and only those reflections havingI>3(I) were used in the analyses.In both complexes, platinum is four-coordinate with the two chlorine atoms, the double bond of the ethylene, and the nitrogen atom of the substituted pyridine. The two structures are discussed in terms of the arrangement of the pyridine ligand with respect to the PtCl₂(C₂H₄) moiety.     

Molecular structure and spectral characteristics of bis(S-methyl-N-(2-pyridyl)methylendithiocarbazato)nickel(II), (Ni(NNS)2)

A nickel(II) complex of the pyridine-2-aldehyde Schiff base of S-methyldithiocarbazate (HNNS) has been synthesized and characterized by means of elemental analysis, IR and UV-vis spectra. The crystal structure of the complex has been determined by single-crystal X-ray diffraction. The complex crystallizes in the monoclinic, space P2₁/c, with a = 14.092(2), b = 16.886(2), c = 8.857(2)Å; = 105.78(3) °, V = 2028.2(6) ų, and Z = 4. The nickel atom is octahedrally coordinated by two uninegatively charged tridentate Schiff base in a mer-configuration via the pyridine nitrogen atom, azomethine nitrogen atom, and mecaptide sulfur atom.     

Triaquocalcium(18-crown-6) heptaiodopentacuprate(I), triaquostrontium(18-crown-6) heptaiodopentacuprate(I), and triaquozinc(18-crown-6) heptaiodopentacuprate(I)

Ca(H₂O)₃(18-crown-6)Cu₅I₇ (I), Sr(H₂O)₃(18-crown-6)Cu₅I₇ (II), and Zn(H₂O)₃(18-crown-6)Cu₅I₇ (III) are isostructural solids with a polymeric array of Cu₅I₇ stoichiometry. The repeat unit may be understood as a distorted tetrahedron of four copper(I) atoms, bridged on two faces and three edges by iodide atoms, bridged on an additional edge by an I–Cu–I sequence and linked in polymeric series by this copper atom and one of the face-bridging iodide atoms. The three solid materials display no emission in the visible when excited in the ultraviolet. Comparison with other polymeric cuprous iodide materials that do emit suggests that the quenching of the expected emission may stem from short Cu–Cu interactions (2.4–2.5 Å) that represent a bonding interaction.     

Crystal structure of triphenylphosphine-(1-(di(trifluoromethyl)-hydroxymethyl)-cyclopentadienyl)-(1,2-di(carboxymethyl) ethylene-1-yl) ruthenium (0)

The structure of triphenylphosphine — (1 — (di(trifluoromethyl) — hydroxymethyl) — cyclopentadienyl) — (1,2 — di(carboxymethyl)ethylene — 1 — yl) — ruthenium (0) has been studied by single-crystal X-ray diffraction techniques. This compound, [C₅ H₄(CF₃)2 COH] Ru(PPh₃)C2(CO₂Me)₂H, crystallizes in the triclinic space groupP¯1 witha =10.131,b= 15.107,c= 10.798 Å, = 102.14, = 107.04, = 89.64° andZ = 2. The structure was refined by block-diagonal least-squares methods to a finalR value of 0.042, including hydrogen atoms. The compound contains a dicarboxymethylethylene ligand coordinated to ruthenium both through a ketonic oxygen and through a metal--carbon -bond. An intramolecular hydrogen bond is observed. Details of the structure are reported, and the structures of several Ru(0) complexes are compared.     

Structure of (chloranilato)bis(tri-n-butylphosphine)palladium(II)

(Chloranilato)bis(tri-n-butylphosphine)palladium(II), [Pd(C₆Cl₂O₄){P(C₄H₉)₃}₂] (chloranilic acid=2,5-dichloro-3,6-dihydroxy-p-benzoquinone): FW=718.02,P2₁/c,a=21.729(6),b=17.293(5),c=21.010(9) Å,=112.62(3)°,V=7287.42 ų,Z=8,D _c=1.309mg m^–3, Mo, =0.710730 Å,=0.76 mm^–1,F(000)=3008, finalR=0.087, 2594 observed reflections. Palladium is ligated by a distorted square planar P₂O₂ coordination sphere in the title compound. The two molecules per asymmetric unit differ in the arrangement of phosphine n-butyl chains, yielding two unique metal centers.     

Structure of (N-(2-hydroxyphenyl)-salicylaldiminopiperidino) Ni(II) complex

The crystal and molecular structure of the title complex, C₁₈H₁₉N₂O₂Ni, has been determined by direct methods. The compound crystallizes in the monoclinic crystal system witha=22.973(1),b=5.212(1),c=27.076(1)Å, β=106.46(1)°, space groupC2/c,V=3109.1(6)ų, Z=8, andD _x=1.51g cm^?3. The nickel atom is in a slightly distorted square-planar environment of two oxygens [Ni(1)?O(1) 1.824(3) and Ni(1)?O(2) 1.856(3)Å] and two nitrogens [Ni(1)?N(1) 1.849(3) and Ni(1)?N(2) 1.932(3)Å] with O?Ni?N angles between 85.7(1) and 97.1(1)°. The nickel atom is 0.006 Å out of the plane of its ligands.     

X-ray crystal structures ofcis-bis(diphenylphosphinamide)tetracarbonylmolybdenum(0) andtrans-bis(N-methyl diphenylphosphinamide)tetracarbonylmolybdenum(0)

The X-ray crystal structures ofcis-Mo(CO)₄(Ph₂PNH₂)₂,I, andtrans-Mo(CO)₄(Ph₂PNHMe)₂,II, are presented. ComplexI crystallizes in the monoclinic space groupP2₁/c(a=13.433(1),b=12.2719(8),c=17.318(2)Å;=109.79(1)°;V=2686.1(8)ų;Z=4). ComplexII crystallizes in the triclinic space groupP¯1 (a=6.9986(8),b=10.328(1),c=11.241(2)Å,=107.58(1)°,=91.76(1)°, =101.28(1)°,V=756.1(4)ų,Z=1). The molybdenum coordination geometry in each complex is a slightly distorted octahedron. The molybdenum-carbon bond lengths for the carbonyls trans to phosphorus in complexI are shorter than those the carbonyls trans to other carbonyls. The average molybdenum-phosphorus distance inI (2.525(5)Å) is similar to those in other diphenylphosphinamide complexes and longer than the molybdenum-phosphorus distance inII in 2.4585(7)Å). The distance between two nitrogen atoms incis Mo(CO)₄(Ph₂PNH₂)₂ (3.74(3)Å) is significantly larger than the sum of their van der Waals radii (3.10 Å) indicating that the two nitrogens are not hydrogen bonded.     

Crystal structure of aquo (hydroxo) (ethylenediaminetetraacetato) sodium(I) tin(IV), NaSn(OH)(edta)(H2O)

NaSn(OH)(edta)(H₂O) is monoclinic, space groupP2₁/c, witha=9.747(3)Å,b=9.121(3)Å,c=16.430(6)Å, =98.69(4)°, ų, andZ=4. The coordination environment of Sn(IV) is a capped octahedron. Sn–O distances range from 1.990(6)Å to 2.351(7)Å. Na(I) is five coordinated to three different edta molecules. Na–O distances range from 2.283(9)Å to 2.414(7)Å. The edta ligand presents the E, G/R conformation. The crystal structure is composed of sheets parallel to (001): inside a sheet Sn(OH)(edta) molecules are connected to each other by the Na(I) interactions.     

La_(0.5)Sr_(0.5)CoO_3/Pb(Zr_(0.4)Ti_(0.6))O_3/La_(0.5)Sr_(0.5)CoO_3铁电电容器的结构和性能研究

采用磁控溅射法和脉冲激光沉积法,在SrTiO3(001)衬底上制备了La0.5Sr0.5CoO3(70 nm)/Pb(Zr0.4Ti0.6)O3(70 nm)/La0.5Sr0.5CoO3(70 nm) (LSCO/PZT/LSCO)铁电电容器异质结.X射线衍射结果表明:LSCO和PZT薄膜均为外延结构.在5 V的外加电压下, LSCO/PZT/LSCO电容器具有较低的矫顽电压(0.49 V),较高的剩余极化强度(41.7 μC/cm2 )和较低的漏电流密度(1.97×10-5 A/cm2),LSCO/PZT/LSCO电容器的最大介电常数为1073.漏电流的分析表明:当外加电压小于0.6 V时,电容器满足欧姆导电机制;当外加电压大于0.6 V时,符合空间电荷限制电流(SCLC)导电机制.