Effect of the fold surface of the lamellae on the behavior of the trapped radicals in irradiated polyamide-1010

Two types of macromolecular free radicals -CH2CONHCHCH2- (a) and -CH2C=O (b) trapped in irradiated Polyamide-1010 (PA1010) and PA1010 filled with neodymium oxide (Nd2O3) were characterized by an ESR approach. It was found out that a was mainly trapped in the fold surface of the lamellae and b in the amorphous phase. This result suggested that trapped radicals mainly existed in the noncrystalline phases. The effect of the fold surface area of the lamellae on the behavior of the trapped radicals are discussed in this article. Whether for the specimens with similar crystallinities but different crystallite sizes or for those with the same concentration of neodymium oxide but different crystallinities, radical a exists dominantly in a specimen with a larger fold surface area of the lamellae. Under a certain circumstance, radical a can transform into radical b for a specimen with a larger fold surface area of the lamellae. It means that the fold surface area of the lamellae plays an important role in the transformation of radical a to b. (C) 1998 John Wiley & Sons, Inc.

Synthesis, structure and properties of alpha-Keggin-type of K6H3[ZnW11O40Al]center dot 9.5H(2)O

A new heteropolycomplex, K6H3[ZnW11O40Al] . 9.5H(2)O was prepared and characterized by means of elemental analysis, IR, UV spectroscopy, Al-27 NMR, electrochemistry and X-ray crystallography. The crystal of K6H3[ZnW11O40Al] . 9.5H(2)O is cubic, space group Fm-3m, with lattice constants a=b=c=2. 144 8(2) nm, V = 9.866(2) nm(3), Mo radiation, R = 0.057 8 for 497 independent data with [I>2 delta(I)]. The anion is of alpha-type Keggin structure with C-s symmetry.

Variation of crystallographic parameters in PEEKK with heat treatment temperature

Using the wide-angle X-ray diffraction method, the variation of crystallographic parameters of poly(aryl ether ether ketone ketone) (PEEKK) has been studied in different heat treatment temperatures. All the reflections and their intensities as well as their Miller indices are presented in detail according to an orthorhombic system. The investigation indicates that the unit cell parameters a, b, c and the unit cell volume V systematically decrease with increasing heat treatment temperature. This variation is interpreted by the change of conformation of polymer molecular chains during thermal treatment. The results calculated from the formula of degree of crystallinity (W-c,W-x) for PEEKK, which was derived based on X-ray scattering intensity theory and the graphic multipeak resolution method, are compatible with the density measurement (W-c,W-d) and calorimetry (W-c,W-h) values. (C) 1997 Elesevier Science Ltd.

ESR approach to free radicals trapped in irradiated polyamide-1010

Two types of macromolecular free radicals similar to CH2CONH(C) over dotHCH(2) similar to (a) and similar to CH2(C) over dot = O (b) trapped in irradiated polyamide-1010 (PA1010) and PA1010 filled with neodymium oxide (Nd2O3) were characterized by an ESR approach. It is found that (a) is prevailingly trapped in the fold surface of the lamellae and (b) in the amorphous phase. This result suggests that trapped radicals mainly exist in the non-crystalline phases. The effect of the fold surface area of the lamellae on the behavior of the trapped radicals is discussed in this paper. Whether for the specimens with similar crystallinities, but different crystallite sizes, or for those with the same concentration of neodymium oxide, but different crystallinities, radical (a) exists dominantly in the specimen with a larger fold surface area of the lamellae. Under certain circumstances, radical (a) can transform into radical (b), obviously for a specimen with a larger fold surface area of the lamellae. It means that the fold surface area of the lamellae plays an important role in the transformation of radical (a) to (b). (C) 1997 Elsevier Science Ltd.

Study on the microstructure and properties of nanosized stannic oxide powders

Stannic oxide xerogel was prepared by a forced hydrolysis method using SnCl4 as the precursor. The average grain sizes of the nanosized stannic oxide powders varied with the sintering temperatures. The powders were characterized by several different physico-chemical techniques. TEM was employed for the direct observation on grain sizes, shape and state of aggregation of the particles. XRD technique was used for the determination of the crystalline structure. Microstructural parameters of average crystallite size () and mean-square root microstrain (epsilon(2)>(1/2)) for the samples were calculated from the broadened values of the half-peak intensity of XRD. The atomic ratio between oxygen and tin in the surface region of the particles was estimated through the analysis of XPS. Attributing to lots of oxygen vacancies in the surface region of the nanoparticulates and the 'trapped electrons' in the vacancies, an ESR signal was observed in the sample sintered at 300 degrees C for 2 h. FTIR of the powders showed that intensity of the transverse optical mode of Sn-O stretching vibration increased with the sintering temperature while the bending vibration of O-Sn-O showed a blue shift. For Raman spectra, very important spectral characteristics such as variations of intensity and width of the bands were observed. A new Raman vibrational band located at 572 cm(-1) was identified in the samples of nanosized stannic oxide powders. Variation of these spectroscopic properties were strongly affected by grain size, shape and state of aggregation of the nanosized particulates.

Preparation of Pb-Ca-Na master alloy using molten chloride salt electrolysis

An electrolysis technique for co-deposition of Ca2+ and Na+ at the liquid lead cathode was put forward. The experiment was carried out at an electrolysis temperature below 650 degrees C and had a current efficiency of 98%, which are respectively 100 similar to 300 degrees C lower and 15% similar to 30% higher than those reported both at home and abroad.

STUDY ON THE NON-STIOCHIOMETRIC SNO2-X NANOCRYSTALLINE MATERIAL BY XRD, XPS AND ESR

Nonstiochiometric SnO2-x nanocrystalline material were successfully prepared through Sol-Gel process using anhydrous stannic chloride and iso-propyl alcohol. TEM observation shows that the mean diameter of the powder sintered at 700 degrees C for 2 hours is about 20 nm. By the investigation of XRD and ESR, we can conclude that the sample sintered at 300 degrees C for 2 hours was amorphous and it grew into nanocrystalline with the oxygen vacancies and defects when sintered at 700 degrees C for 2 hours. Using these conclusion, the ESR signals and the difference between the two SnO2-x samples are explained.

THERMAL BEHAVIORS OF INTRINSIC POLYANILINE AND ITS DERIVATIVES

Thermal properties of polyaniline (PAn), polytoluidine(POT) and polyanisidine(PAs) were examined by TG and DSC techniques. The weight-uptake of POT at 200-300 degrees C was observed and carefully discussed.

大豆杂种后代过氧化物酶同工酶谱类型及其与亲本关系的分析

采用聚丙烯酰胺凝胶垂直板电泳方法分析有亲缘关系的37个品种(包括15个品种的亲本来源)萌发6天的大豆子叶POD同工酶谱。结果表明,不同品种POD同工酶谱共显示5～10条酶带,分A、B、C三区。以B区酶带色度深浅及数目变化为分类标准,可分为四种酶型:PB_1型、PB_2型、PB_3型和PB_4型。根据此酶型分析了每一个组合的品种与其两亲本。其中6个品种呈现偏父本酶型,6个品种呈现新酶型,2个品种的酶型与父母相同,1个品种呈现偏母本酶型。同时测定了13个组合的36个品种的POD比活力,结果指出:后代品种POD比活力都低于或介于父母本之间,后代比双亲POD比活力有逐渐降低的趋势。

含酚酞侧基聚芳醚砜的辐射交联

研究了含酚酞侧基聚芳醚砜(PES-C)的辐射效应,发现在真空下通过γ射线辐照,PES-C发生交联。而且在高温下PES—C的辐射交联程度比在常温下的高。在25℃下,PES-C的凝胶化剂量为6.6×10~5Gy。而在300℃下,PES-C的凝胶化剂量为6.0×10~4Gy。

Sn-Mo混合氧化物的缺陷结构及催化性能的研究

本文以1-丁烯在水蒸汽存在下选择性氧化制甲乙酮为典型反应,利用 XRD,ESR,IR,XPS,TEM 和 SEM 研究了 Sn-Mo 氧化物的结构与活性的关系.制备了8个样品,A,B,C,D,E,F,G 和 H 的 Mo/(Mo+Sn)分别为0,0.1,0.2,0.4,0.6,0.8,0.9,1.0.根据结构特征,可将 Sn-Mo 氧化物分为三组:第Ⅰ组 Mo/(Mo+Sn)≤0.2;第Ⅱ组0.2

RBa_2Cu_3O_(7-δ)的结构和某些性质的变化趋势

本文用X射线衍射、碘量法,扫描电镜等手段系统地研究了RBa_2Cu_3O_7-δ[R=La、Nd、Sm、Gd、Dy、Er、Yb、(DyYb)]化合物的结构和某些性质(如氧含量、Cu~(3+)/Cu~(2+)等)随稀土离子半径的变化规律。发现随着稀土离子半径的减少,晶胞参数(a、b、c、v)几乎线性降低,Cu~(3+)/Cu~(2+)(％)、氧含量(7-δ)、正交畸变(a-b)几乎线性增加,XRD图谱中001峰加强,SEM像中晶形更加完整。

银对提高YBa_2Cu_3O_(7-y)超导体临界电流密度J_c的作用

对YBa_2Cu_3O_(7-y):Ag_x超导体的性质进行了研究。该体系有较低的正常态电阻。XRD分析表明,在x<0.2时,该体系为正交结构。随Ag含量的增加,123相的α轴与b轴无明显改变,而c轴增加。X=1.5时,c轴增加了0.33％,表明有部分Ag进入123相晶胞。SEM研究表明,YBa_2Cu_3O_(7_y):Ag_x超导体晶粒细化均匀,晶粒间形成网状结构,改善了弱连接,使其临界电流密度J_c从50A/cm~2提高到572A/cm~2。

未掺杂和掺铬、铒ZrO_2-Y_2O_3晶体的光谱性质

研究了未掺杂及掺杂铬和铒ZrO_2-Y_2O_3(88:12mol%)晶体室温下的吸收和发光光谱。未掺杂晶体吸收和发光带是由色心引起,~(60)Co γ射线辐照前后其电子顺磁共振证实单电荷(Y_(Zr),Vo)′络合在点阵中存在。掺杂晶体的吸收、激发和发光光谱带相应于各自Cr~(3+)和Er~(3+)离子能级跃迁。使用3d~3电子久期方程计算3Cr~(3+)在立方场下库仑相互作用参数B、C和内晶格场参数D_q。

三出口萃取工艺动态过程研究

本文根据总萃取比恒定的三出口萃取工艺(A/B/C)中各组份的动态物料平衡,采用 FORTRAN 语言编写了串级萃取动态模拟计算程序,并进行了正常启动和回流启动两种动态过程的实例计算。结果表明,各组份在级体内总量及各出口产品纯度等均随串级排数增多而逐渐趋近于静态模拟计算结果。采用回流方法启动时,可显著缩短达到稳态所需的时间,大大减少启动过程中的非合格产品。本文还根据多个萃取体系的动态模拟结果,分别对萃取段或洗涤段开设第三出口的工艺介绍了回流启动方法。