盐浓度与海藻酸钠/磷虾蛋白复合体系性能的相关性

采用湿法纺丝技术制备了海藻酸钠/磷虾蛋白(SA/AKP)复合纤维, 通过傅里叶变换红外光谱(FTIR)分析了SA/AKP复合体系的氢键相互作用, 用X射线衍射仪、 流变仪及SEM研究了盐(NaCl)浓度对复合体系的结晶、 流动性和形态结构的影响. 结果表明, SA/AKP复合体系中存在分子内和分子间氢键, 分子间氢键的强度随复合材料中盐浓度的增加而增强. 盐浓度的增加导致SA/AKP复合材料的结晶度增加, 流动黏度先降低后增加, 力学性能先增加后降低. SA/AKP纤维的SEM照片显示结晶的盐与纤维分离, 并且复合纤维表面沟槽结构逐渐减少, 表面更加致密光滑. AKP在SA/AKP复合体系中呈完全取向状态.     

预沉积Ge对Si(111)衬底上SSMBE外延生长SiC薄膜的影响

利用固源分子束外延(SSMBE)生长技术, 在Si(111)衬底上预沉积不同厚度(0、0.2、1 nm)Ge, 在衬底温度900 ℃, 生长SiC单晶薄膜. 利用反射式高能电子衍射仪(RHEED)、原子力显微镜(AFM)和傅立叶变换红外光谱(FTIR)等实验技术, 对生长的样品进行了研究. 结果表明, 预沉积少量Ge(0.2 nm)的样品, SiC薄膜表面没有孔洞存在, AFM显示表面比较平整, 粗糙度比较小, FTIR结果表明薄膜内应力比较小. 这说明少量Ge的预沉积抑制了孔洞的形成, 避免衬底Si扩散, 因而SiC薄膜的质量比较好. 没有预沉积Ge的薄膜, 结晶质量比较差, SiC薄膜表面有孔洞且有Si存在. 然而预沉积过量Ge (1 nm) 的样品, 由于Ge的岛状生长,导致生长的SiC表面粗糙度变大, 结晶质量变差, 甚至导致多晶产生.     

碱解聚对玉米秸秆的影响

以玉米秸秆为研究对象,氢氧化钠为解聚剂,研究了碱解聚前后玉米秸秆组份、表面形态、化学官能团和纤维结晶度的变化。结果表明:玉米秸秆中木质素的主要组成单体是H-木质素,解聚液中的酚类物质有4-羟基苯甲醛、香草醛、紫丁香醛、对香豆酸和阿魏酸。玉米秸秆经碱解聚,表面形态变得疏松而多孔,红外光谱下木质素的特征吸收峰消失,85%的木质素和52%的半纤维素被脱除,而纤维素的相对含量增加,结晶度增大。说明碱解聚有利于后续酶解和(或)其它生化方法的实施,以实现秸秆纤维的高值转化。     

姜黄素对人肝癌HepG2细胞毒性的分析

该文结合倒置显微镜、原子力显微镜(AFM)、CCK-8和流式细胞术定性定量研究了姜黄素对人肝癌细胞株HepG2细胞的毒性.AFM探测结果表明,姜黄素能够引起细胞发生不同程度的形变.细胞体积和高度均随细胞形变程度的加深而下降.细胞表面平均粗糙度(Ra)、均方根粗糙度(Rq)和粒径分布均随细胞形变程度的加深而增大.而AFM...     

速溶电纺载药PVP纳米纤维膜制备与表征

采用电纺工艺制备载豆腐果苷聚乙烯基吡咯烷酮纳米纤维膜.通过偏光显微镜确定电纺条件,利用扫描电镜对纤维膜表面形态进行观察;采用X-射线晶体衍射(XRD)和差示扫描量热分析(DSC)检测纤维膜中药物的存在状态,通过红外光谱分析药物与纤维基材之间的相互作用.结果表明载药纤维直径分布均匀(400~600 nm)、表面光滑无药物颗粒,药物与聚合物之间通过氢键作用、具有良好的相容性,XRD和DSC结果表明药物以无定形态高度分散于纳米纤维中,纤维膜中药物以"聚合物控释"机制在13.7 s左右完全溶解.     

邻苯二酚-四乙烯五胺改性超高分子量聚乙烯纤维

应用Cat-TEPA改性超高分子量聚乙烯(UHMWPE)纤维,在难黏附的纤维表面形成均匀涂层.采用透射电子显微镜(TEM)、红外光谱(FTIR)、X射线光电子能谱(XPS)、X射线衍射(XRD)、示差扫描量热(DSC)、热重分析(TGA)和静态接触角测试等手段对其结构和性能进行了表征,并通过单丝拔出实验研究改性前后纤维与环氧树脂之间的界面剪切强度(IFSS),探索了反应物配比、反应时间对表面性能的影响,并确定最佳改性条件.结果表明Cat-TEPA共沉积改性未影响纤维的结晶和热稳定性,改性后纤维表面浸润性得到改善,且适当增加反应时间和TEPA含量能够提高纤维和树脂之间的IFSS,当Cat-TEPA摩尔比为1:4,反应时间为24 h时效果最佳,与未改性纤维相比,界面剪切强度提升约44%.     

活性炭纤维对铂离子的还原吸附特征

利用不同的活化工艺,制备了水蒸汽活化和磷酸或氯化锌活化活性炭纤维,并借助扫描电镜(SEM)、X-射线衍射(XRD)和光电子能谱(XPS)等技术,研究了这些活性炭纤维对铂的还原吸附特征。结果表明,各活性炭纤维均能还原吸附铂离子,吸附容量为30mgPt/gC至90mgPt/gC之间。依据活性炭纤维种类的不同,还原吸附的铂呈粒状或放射性簇状存在于活性炭纤维表面,铂颗粒的粒径为几十nm至1μm之间。对纤维表面铂的XRD分析表明,还原吸附的铂呈无定型结构,但经过400℃高温处理后,颗粒转化为金属铂结晶形态。还原吸附铂后,活性炭纤维表面的含氧基团相应增加,显示其表面被氧化为羟基和羰基。     

丁苯、丁腈基聚氨酯的形态与性能

用示差扫描量热法 (DSC)、红外分光光度计 (FTIR)和原子力显微镜 (AFM)研究了端羟基聚丁二烯 苯乙烯共聚物 (HTBS)、端羟基聚丁二烯 丙烯腈共聚物 (HTBN)和端羟基聚丁二烯 (HTPB)与甲苯二异氰酸酯、1 ,4 丁二醇构成的溶液法聚二烯烃基聚氨酯 (PU)的形态结构 .结果表明HTPB和HTBS基PU的相分离程度很大 ,而HTBN基PU的相分离程度小 .这可能归因于HTBS软段的极性低 ,不能与硬段形成氢键 ,而HTBN软段中的腈基具有很强的极性 ,且可以与硬段形成氢键作用 ,增加了软硬段间的相容性 ,相分离程度明显降低 .AFM表明HTBN PU随着硬段含量提高 ,表面粗糙度增大 ,由软段为连续相逐渐过渡到双连续结构 .在硬段含量 6 3%时 ,HTBN和HTPB基PU均呈双连续结构 ,而HTBS PU中硬段为连续相 .HTBN PU软段的相区尺寸在1 2nm左右 ,表面粗糙度较大 ,HPBS PU软段的相区尺寸在 1 1nm左右 ,表面粗糙度最小 ,HTPB PU存在 1 4nm和 5 0nm大小不等的软段相区尺寸 .力学性能表明 ,在软段中引入苯乙烯和丙烯腈结构 ,可使聚氨酯抗张强度分别提高 1 5和 2倍 ,模量和断裂伸长率也明显提高     

原子力显微镜对中性粒细胞与K562细胞超微结构及机械性能的探测

采用原子力显微镜在纳米尺度下对正常中性粒细胞与白血病细胞株K562细胞的表面形貌及细胞的硬度、粘附力进行定性定量分析.结果表明,相比正常中性粒细胞的平均粗糙度(Ra=5.31±1.52 nm),K562细胞的超微结构更为复杂,细胞表面平均粗糙度显著升高(Ra=26.54±8.01 nm).此外,细胞的生物机械特性也有显著差别:中性粒细胞的硬度为9.5±1.3 kPa,AFM针尖与中性粒细胞的非特异性粘附力为135±23.4 pN;K562细胞的硬度为3.0±0.8 kPa,AFM针尖与K562细胞的非特异性粘附力为95±15.6 pN.AFM在单细胞水平上的探测表明,中性粒细胞和K562细胞的超微结构和机械特性均有明显差异.通过对细胞表面超微结构和力学特性的探测可以诊断慢性粒细胞白血病,原子力显微镜有望成为临床肿瘤诊断的工具.     

液相法制备具有双尺寸粗糙度的超疏水铜表面

基于简单的液相法,以硫代硫酸钠和氯化铜为原料在铜片表面上构筑了具有微/纳米双尺寸粗糙度的硫化铜膜.用X射线衍射(XRD)仪、扫描电镜(SEM)、能量色散X射线(EDX)光谱仪及光学视频接触角仪对处理前后的铜表面进行了表征和分析.处理后的超亲水铜表面经硬脂酸修饰后具有超疏水效应,静态接触角高达161°,5μL水滴滚动角低至2.5°左右.超疏水性能归因于表面具有双尺寸粗糙度和低表面能的硬脂酸.该方法简单,无需复杂制备过程和苛刻设备,所得超疏水铜表面具有优异的不粘附性、长时间储存的稳定性和一定的耐摩擦性能.     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。     

Synthesis of phenolic components of Grains of Paradise

Two vanilloids, (5E)-8-(4-hydroxy-3-methoxyphenyl)oct-5-en-4-one (1) and 4-[3-hydroxydecyl]-2-methoxyphenol (2), isolated from the dried seeds of Grains of Paradise (Aframomum melegueta), were synthesized; the latter compound was made as the S-enantiomer and the material derived from the seeds was found to be a 1:1.7 mixture of the R and S isomers. The synthetic route used should allow the preparation of analogs having extended alkyl chains and consequently different lipophilicity, and 3, a homolog of 2, was also prepared.     

Acid hydrolysis of carboxymethylcellulose of low degree of substitution

Cotton cellulose was swollen in a sodium hydroxide solution and carboxymethylated by a two-bath method for different periods of time for each process. The kinetics of acid hydrolysis and the crystallinity of the swollen and carboxymethylated samples were measured. The proportion of broken bonds, rate constants for hydrolysis, and permeability of cellulose to hydrolyzing agents were calculated. The susceptibility of glycosidic linkages to acid hydrolysis was improved by carboxymethylation more than by swelling in alkali. The increased accessibility of carboxymethylcellulose to acid was regarded as a consequence of increased intra-and intercrystalline swelling and of the glycosidic bonds' weakness caused by the electron-attracting carboxymethyl group on the C-6 position.     

Study of hydration of two cements of different strengths

Main hydration products of two cement pastes, i.e. CSH-gel, portlandite (P) (and specific surface S) were studied by static heating, and by SEM, TEM and XRD, as a function of cement strength (C-33 and C-43) hydration time (th) and subsequent hydration in water vapour.Total change in mass on hydration and air drying, M_o, increased with strength of cement paste and with hydration time. Content of water escaping at 110 to 220°C, defined as water bound with low energy, mainly interlayer and hydrate water, was independent on cement strength but its content increased with (th). Content of chemically bound (zeolitic) water in CSH-gel, escaping at 220-400°C, was slightly dependent on strength and increased with (th). It was possibly derived from the dehydroxylation of CSH-gel and AFm phase. Portlandite water, escaping at 400-500°C, was independent on cement strength and was higher on longer hydration. Large P crystals were formed in the weaker cement paste C-33. Smaller crystals were formed in C-43 but they increased with (th). Carbonate formated on contact with air (calcite, vaterite and aragonite), decomposed in cement at 600-700^oC. It was high in pastes C-33(1 month) and C-43(1 month), i.e. 5.7 and 3.3%, respectively; it was less than 1% after 6 hydration months (low sensitivity to carbonation) in agreement with the XRD study showing carbonates in the air dry paste (1month), and its absence on prolonged hydration (6 months) and on acetone treatment. Water vapour treatment of (6 months) pastes or wetting-drying increased this sensitivity.Nanosized P-crystals, detected by TEM, could contribute to the cement strength; carbonate was observed on the rims of gel clusters.This revised version was published online in November 2005 with corrections to the Cover Date.     

恶臭嗅辨实验室建设探讨

针对恶臭测试的环境影响问题,提出了解决的实例方案,并对方案的要点及优缺点进行讨论,此方案在实际操作中具有较好的效果。     

Estimation of Kinetic Parameters of Thermal Oxidation of Ilmenite

The aim of the presented work was the investigation of thermal oxidation of ilmenite in static air atmosphere. The investigations were carried out by use of a derivatograph (MOM, Hungary). The changes of crystallographic structure of investigated samples were identified by X-ray diffractometry on Philips PW-1710 diffractometer. In temperature above 500°C appears structure of hematite Fe₂O₃. On the basis of the thermogravimetric measurements, the contracting area and contracting volume models were found as the best fitting experimental data. This revised version was published online in August 2006 with corrections to the Cover Date.     

Mechanism of action of base-catalyzed oxygenation of phenol derivatives

Cyclopropyl derivative of 2,6-di-tert-butylphenol is synthesized as a probe to investigate the mechanism of base-catalyzed autooxidation of phenol derivatives. Our study indicates that one electron reduction of molecular oxygen from phenolate gives phenoxyl radical 3, a key intermediate of autooxidation. The coupling of phenoxyl radical and superoxide radical gives peroxylate anion 4 and produces the final epoxy alcohol adduct 6.     

氯氧化镁生成热的研究

用氧化镁氯化镁水溶液制备了8水合氯氧化镁[nMg(OH)2·MgCl2·8H2O], 并测定了其在盐酸中的溶解热, 实验结果表明, 氯氧化镁溶解热与n值呈线性关系, 根据溶解热求出5Mg(OH)2·MgCl2·8H2O和3Mg(OH)2·MgCl2·8H2O的生成热分别为-7727.1和5888.1kJ·mol^1^-。