X-RAY SCATTERING STUDIES ON NYLON-1010

From Wide-Angle X-ray Scattering (WAXS) pattern of uniaxially orientated fibers, the crystal structure of Nylon-1010 was determined. The Nylon-1010 crystallizes in the triclinic system, with lattice dimensions: a=4.9A, b=5.4A, c=27.8, α=49 °, β=77 °,γ=63.5 °, the unit cell contains one monomeric unit and the space group is P. The degree of crystallinity of polymer was deter mined as about 60%, using Ruland's method.The structures of Nylon-1010 with different draw ratio have been investigated by using Small-Angle X-ray Scattering (SAXS). The results indicate that the draw ratio of samples has a significant effect on microstructure of Nylon-1010. The long period and thickness of amorphous layer obviously increase but the invariant, average lameUar and interphase zone show almost independent of draw ratio, long period increases because amorphous layer increases with draw ratio. The electron density fluctuation values increased with draw ratio, but inner surface O_s is drecreased.     

Co[(C_2H_5O)_2PS_2]_3·1/2H_2O的合成和分子结构

用光谱法研究了双-(O,O'-二硫代磷酸酯)合钴(Ⅱ)的氧化过程。用电子光谱、光电子能谱、差热-热重分析和质谱等对氧化产物进行了表征。并用X射线衍射法测定了晶体结构。晶体属三斜晶系,空间群为P_1~-,晶胞参数为:α=9.805(1),b=9.812(2),c=14.271(2),α=89.46(2)°,β=89.42(1)°,γ=86.95(2)°,V=1370.9~3,Z=2,D_c=1.509 g·cm~(-3),F(000)=645 e。Co(Ⅲ)与三个二硫代磷酸酯形成六配位的八面体配合物。     

苯甲腈 Stephen 反应中间物的晶体结构

苯甲腈的 Stephen 反应中间物,[C_6H_5CH=NH]_2SnCl_6,的空间群为(?)—1。三斜晶胞的参数为α=7.41(?),b=7.84(?),c=10.45(?),α=86°54′,β=95°,γ=122°6′。晶胞中含有1个{[C_6H_6CH=NH]_2SnCl_6}。从 Patterson 函数 P(u,w)和 P(v,w)中引出重原子锡和氯的参数,并根据这些参数计算电子密度分布函数ρ(x,y),ρ(x,z)和ρ(y,z)。后者给出整个结构的模型和参数。结构分析的结果指出,苯甲腈 Stephen 反应中间物为一由[C_6H_5CH=NH_2]~+和[SnCl_6]~(2-)所组成的离子化合物。氯锡酸离子具有八面体构型,而苯甲醛亚胺离子为一共面的共轭体系。这二种离子间还形成 N—H…Cl 型的氢键。     

新型超分子化合物(H3NCH2CH2NH3)2[(HPO4)2Mo5O15]的晶体结构

首次通过水热方法合成了新型超分子化合物(H3NCH2CH2NH3)2[(HPO4)2Mo5O15]的晶体结构,并通过X衍射进行了结构表征,晶体学数据为:单斜晶系,C2/c空间群,a=1.766 6(4)nm,b=1.003 4(2)nm,c=1.376 7(3)nm,α=90°,β=96.90(3)°,γ=90°,ν=2.422 7(8)nm3,Z=4,R=0.043 1,wR2=0.128 7.     

乙二胺双缩5-氯水杨醛Sclliff碱铜配合物的合成及晶体结构

合成了N,N′-二(5-氯水杨醛)缩乙二胺合铜配合物([Cu(5-ClSalen)]),用单晶X射线衍射法测定了晶体结构.其晶体属三斜晶系,空间群P-1,晶胞参数a=0.83285(1)nm,b=0.95170(4)nm,c=1.09304(4)nm,α=115.130(2)°,β=94.694(2)°,γ=101.127(2)°,V=0.75642(4)nm3,分子式C16H12Cl2CuN2O2,Mr=398.72,Z=2,Dc=1.751g/cm3.在配合物中,Cu处于两个氮原子和两个酚氧原子形成的平面四方场中.     

烟酸钆与邻菲咯啉三元配合物的研究

合成烟酸钆与邻菲咯啉三元配合物,用化学分析、红外光谱、电导和热谱确定其组成为Gd(Phen)_2L_3·3H_2O。其晶体结构分析属三斜晶系,晶胞参数α=9.031,b=12.857,c=17.747;α=84.923°,β=80.564°,γ=84.706°。钆三元配合物抑菌能力大于烟酸钆和邻菲咯啉。     

Schiff碱Cu(II)配合物的结构、光谱及电化学性质

为了探讨配合物结构对性质的影响，合成了两个Schiff碱的铜配合物{[Cu(II) (L1)]ClO_4(1)和[Cu(II)(L2)-(H_2O)_2](BF_4)_2(2)}，并用红外、质谱和元素分 析对它们进行了表征，用X射线衍射方法测定了它们的昌体结构。实验结果表明： 配合物1和2均属三斜晶系，P1空间群。1的晶胞参数为a = 1.1147(6)nm, b = 1. 1481(7)nm, c = 0.770(3)nm; α = 98.81(4) °,β=106.94(4)°γ= 66.49(4)° ;V=0.8715(8)nm~3,Z=2,R=0.044.2的晶胞参数为a=1.0819(4)nm, b = 1.4095(6) nm, c = 1.0192(4)nm; α=96.54(4)°,β=106.18(3)°,γ=80.51(3)°;V=1. 4681(5)nm~3, Z=2, R = 0.068.此外，配合物1的Cu-O(1)键长[0.1880(5)nm]和可 见吸收波长(λ_(max)=557nm)比2[0.1982(6)nm,λ_(max)=605nm]短。配合物2在- 0。80～-1.20V范围内出现两个氧化和两个还原过程。     

新型双锂盐络合物的合成及其单晶结构的测定

报道了一种新的双锂盐络合物的合成及其X衍射单晶结构，该络合物含有2个 Li原子、一个（i-Pr2C6H3)2-dad配体及2个DME分子[triclinic,P-1,α=1.3478(4) ,b=1.5158(3),c=1.0730(3)nm,α=100.668(3)°,β=113.416(3)°，γ=97.128(3) °,Ⅴ=1.790(1)nm^3,Dc=1.06g/cm^3,Z=2,R/Rω=0.058/0.057]。     

有机锡氧羧酸簇合物[PhCH_2Sn(O)(O_2CCH=CHAr)]_6的合成、表征和[PhCH_2Sn(O)(O_2CCH=CHPh)]_6的晶体结构

利用(PhCH_2)_3Sn]_2O与ArCH=CHCO_2H反应，合成6个新的[PhCH_2Sn(O) (O_2CCH=CHAr)]_6簇合物。通过元素分析、红外光谱和X射线单晶衍射对其结构进 行了表征。用X射线单晶衍射测定了[PhCH_2Sn(O)(O_2CCH=CHPh)]_6的晶体结构， 结果表明，该簇合物为三斜晶系，空间群P1, a = 1.6771(3) nm, b = 1.8020(4) nm, c = 2.1073(4) nm, α = 108.111(3)°β = 103.614(3)°,γ = 104.679 (3)°,Z = 2, V = 5.5033(18) nm~3, D_c = 1.350 g/cm~3, μ = 1.396 mm~(-1) , F(000) = 2208, R = 0.0606, wR = 0.698。该化合物为鼓型簇状结构，锡原子 呈畸变的八面体构型。     

分子导体(PyH)[Ni(dmit)_2]_2的合成、结构与导电性

合成了一种新的导电分子晶体(PyH)[Ni(dmit)_2]_2 (Py = pyridine, dmit = (C_3S_5)~(2-) = 4,5-dimercapto-1,3-dithiole-2-thione)，用元素分析、红 外光谱对其进行了表征，并用四圆X射线衍射方法确定了结构，该晶体属于三斜晶 系，P-1空间群；晶胞参数为: a = 0.59227(4) nm，b = 0.82279(6) nm, c = 1. 67535(9) nm, α = 90.233(5)°, β = 92.107(5)°, γ = 104.654(6)°; V = 0.78925(9) nm~3, Z = 1. (PyH)[Ni(dmit)_2]_2晶体中，导电组元[Ni(dmit)_2] ~(-0.5) 沿b轴方向形成具有二聚体结构的柱状堆积，在(001)面形成以肩并肩分子 间的S…S强相互作用为特征的二维导电层，这种二维导电层上的室温电导率为0. 13 Ω~(-1)·cm~(-1)，在c轴方向，(PyH)~+与[Ni(dmit)_2]~(-0.5)之间除库仑作 用外，还存在N-H…S，C-H…S氢键相互作用。单晶(001)面上变温电阻的测定结果 表明，在90 K到室温的温度范围内，(PyH)[Ni(dmit)_2]_2具有半导体导电行为， 导电激活能为0.15 eV。     

THE DEGREE OF CRYSTALLINITY OF NYLON-1010 BY WAXD

Based on the X-ray scattering intensity theory and using the atomic scattering factorapproximate expression,the correction factors for three main crystalline peaks and an amorphouspeak of Nylon-1010 were calculated and the formula of degree of crystallinity of Nylon-1010 wasderived by graphic multipeak resolution method. The results calculated are compatible with the density measurement and calorimetry.     

Structural data and thermal studies on nylon-12,10

The structure and morphology of Nylon-12, 10 lamellar crystals has been investigated using transmission electron microscopy, selected area electron diffraction, and x-ray diffraction. Additional data have been obtained from uniaxially oriented fibers. The unit cell parameters of two crystalline structures have been determined. They are similar to those usually found in other polyamides (α and β form). Calorimetric (DSC) studies on nylon 12, 10 were also carried out. Melting curves indicate that changes in the internal structure occur when scanning speeds less than 80°C min^?1 are used. ©1995 John Wiley & Sons, Inc.     

Crystal structure of an alternating copolymer of ethylene and tetrafluoroethylene

The unit cell of an alternating copolymer of ethylene and tetrafluoroethylene was determined by x-ray diffraction. In spite of uncertainties due to irregularities in the chain structure and a low level of crystallinity, a reasonable unit cell and structure was derived which gives a calculated crystalline density of 1.9 g/cm³. The unit cell is believed to be either orthorhombic or monoclinic with the following parameters: a = 9.6 Å, b = 9.25 Å, c = 5.0 Å, (γ = 96°). The molecular conformation is that of the extended zigzag, and the molecular packing appears to be orthorhombic, each molecule having four nearest neighbors with the CH₂ groups of one chain adjacent to the CF₂ groups of the next.     

热致液晶乙基纤维素与尼龙－1010共混物的研究

在自制单螺杆小型挤出机上通过熔融共混的办法，制备了不同配比（５／９５—２５／７５）的ＥＣ／Ｎｙｌｏｎ—１０１０共混物．用ＷＡＸＤ、ＤＳＣ、毛细管流变仪、力学性能测试等方法对共混物进行了研究．发现共混后尼龙－１０１０的形态结构有明显改变，其强度、模量都有提高，在高剪切速率下，共混物粘度大大降低．配比为１５８５时，这些性能的改进尤为明显．     

热致液晶乙基纤维素与尼龙－1010共混物的研究

在自制单螺杆小型挤出机上通过熔融共混的办法，制备了不同配比（５／９５－２５／７５）的ＥＣ／Ｎｙｌｏｎ－１０１０共混物，用ＷＡＸＤ、ＤＳＣ、毛细管流变仪，力学性能测试等方法对共混物进行研究，发现共混后尼龙－１０１０的形态结构有明显改变，其强度、模量都有提高，在高剪切速率下，共混物粘度大大降低，配比为１４／８５时，这些性能的改进尤为明显。     

Solid-state polymerization of diacetylene: 1,11,13,23-tetracosatetrayne

The solid-state polymerization of a diacetylene, 1,11,13,23-tetracosatetrayne, was studied using x-ray powder diffraction and electron diffraction. It is shown that the material exhibits polymorphism. Thermochromic transitions, which are generally observed for diacetylenes, are related to the particular crystalline phase using x-ray powder diffraction. The unit cell dimensions and space group of one polymorph were determined by electron diffraction analysis: a = 20.83 Å, b = 4.84 Å, c = 10.08 Å, β = 92.4°, space group: P2₁/n. © 1995 John Wiley & Sons, Inc.     

Crystalline structure and morphology of biaxially oriented polyamide‐11 films

The effect of the uniaxial and biaxial stretching and subsequent solution annealing of extrusion‐cast polyamide‐11 films on the crystalline structure and morphology was investigated with differential scanning calorimetry, wide‐angle X‐ray diffraction (WAXD), Fourier transform infrared spectroscopy, and small‐angle X‐ray scattering (SAXS). The extrusion‐cast polyamide‐11 films exhibited elevations in the glass‐transition and cold‐crystallization temperatures with a constant crystallinity and a constant melting point during aging under room conditions (20–26 °C and 20–31% relative humidity). WAXD and SAXS suggested that chain‐folded lamellae of coexisting α‐ and β‐crystals existed in all the stretched polyamide‐11 films. WAXD pole figures indicated that hydrogen bonds in the hydrogen‐bonded sheets of these two crystalline forms apparently formed between antiparallel chain molecules. The unit cell parameters [a = 9.52 Å, b = 5.35 Å, c = 14.90 Å (chain axis), α = 48.5°, β = 90°, and γ = 74.7° for a triclinic α form and a = 9.52 Å, b = 14.90 Å (chain axis), c = 4.00 Å, α = 90°, β = 67.5°, and γ = 90° for a monoclinic β form] for polyamide‐11 crystals were proposed according to the results of this study and the results of previous investigators. The unit cell parameters of the stretched extrusion‐cast polyamide‐11 films varied, depending on the stretching conditions (the stretch temperature and stretch ratio). As the stretch temperature and stretch ratio were increased, the crystal became more similar to the form described previously and was accompanied by an increase in the long spacing of crystalline lamellae. Annealing the stretched films in a boiling 20% formic acid solution made slightly more perfected crystals. The hydrogen‐bonding α(010) + β(002) planes, which are nearly parallel to both amide group planes and zigzag methylene sequence planes of the biaxially stretched films were found to be parallel to the film surface. © 2002 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 40: 2624–2640, 2002     

Préparation Chimique,Caracterisation Cristallographique,Etudes Thermique et Vibrationnelle du Cyclotriphosphate Hexahydraté de Manganèse et de Tetra-Argent,MnAg 4 (P 3 O 9 ) 2 .6H 2 O

The cyclotriphosphate hexahydrate of manganese and silver, MnAg 4 (P 3 O 9 ) 2 .6H 2 O, was prepared by Boullé's process. MnAg 4 (P 3 O 9 ) 2 .6H 2 O crystallizes in the triclinic system, P-1, Z = 1 and its structure was determined by Rietveld's method. The refinement of 54 parameters by this method, using 1752 independent reflections leads to Rw p = 0.098, R p = 0.065 and R B = 0.033 on the basis of its isotype NiAg 4 (P 3 O 9 ) 2 .6H 2 O. The unit cell parameters of this salt are the following a = 8.824(1)Å, b = 8.485(1)Å, c = 6.609(1)Å, f = 90.30(1)°;, g = 92.89(1)°; and n = 107.28(1)°;. The thermal behavior of this new compound was studied, between 25 and 600°;C, under atmospheric pressure by infrared spectrometry, X-ray diffraction, thermal analyses TGA and DTA coupled. This study allows us the identification and the crystallographic characterization of a new phase, MnAg 2 (PO 3 ) 4 isotype of ZnRb 2 (PO 3 ) 4 , obtained between 350 and 450°;C, mixed with the long-chain polyphosphate of silver AgPO 3 . The kinetic characteristics of the dehydration of MnAg 4 (P 3 O 9 ) 2 .6H 2 O and the thermal phenomena accompanying this dehydration were determined and discussed on the basis of the proposed crystalline structure. The vibrational spectrum of the, MnAg 4 (P 3 O 9 ) 2 .6H 2 O, was examined and interpreted in the domain of the stretching vibrations of the P 3 O 9 rings, on the basis of the proposed crystalline structure and in the light of the calculation of the thirty fundamental IR frequencies for the idealized D 3h symmetry.     

马来酸酐改性聚乙烯／尼龙1010共混体系的结晶行为

在尼龙-1010与马来酸酐改性聚乙烯共混体系中,马来酸酐起结晶成核剂的作用,可显著加快共混物中尼龙-1010组份的结晶。共混物的混容性也略有改善。