离子注入钇对Co-30Cr-6Al合金氧化动力学及氧化膜粘附性的影响

利用热天平与声发射同步测试技术研究了Co-30Cr-6Al合金中离子注入2×10~(17)Y~+/cm~2对合金氧化速率及氧化膜粘附性的影响。结果表明,1000℃氧化时,钇能降低合金的氧化速率,1100℃氧化时,由于未注钇合金形成了Al_2O_3内层膜,其氧化速率反而降低。两种氧化条件下钇都显著地改善了氧化膜的抗剥落性。尽管如此,1100℃/10h氧化后注钇合金的氧化膜于冷却过程中较未注钇合金氧化膜易于发生破裂。1100℃更长时间氧化,注钇和未注钇两种合金的氧化膜于恒温过程中即发生破裂。     

电活性铁氰化镍膜电极对稀土钇的电控离子分离

通过电沉积方法分别在镀铂石英晶片和铂基底上制备了电活性铁氰化镍膜,并考察了膜电极在含钇离子溶液中的电控离子交换性能. 在0.1 mol·L^-1的硝酸钇溶液中,使用循环伏安法及石英晶体微天平技术测试考察了铁氰化镍膜对钇离子的置入释放性能及对应的质量变化,同时比较了铁氰化镍膜电极在Y(NO₃)₃和Sr(NO₃)₂溶液中的电化学性能. 在0.1 mol·L^-1 [Y(NO₃)₃ + Sr(NO₃)₂]混合溶液中,通过循环伏安法分析了薄膜对Y³⁺/Sr²⁺离子的选择性. 用扫描电子显微镜观察了铁氰化镍膜的表面形貌,并通过X射线光电子能谱仪测定了膜在氧化和还原状态下的元素组成. 结果表明,铁氰化镍膜在含Y³⁺溶液中具有良好的离子交换行为,其中氧化过程薄膜质量减少,对应着钇离子的释放;还原过程薄膜质量增加,对应钇离子的置入;在0.0 V或0.9 V调控膜电极的氧化还原状态实现对钇离子的有效分离.     

钇离子注入的H13钢的抗氧化研究

研究了强束流钇注入的H13钢高温氧化特性,同时分析了氧化层的结构和钢中注入钇后抗氧化的原因。结果表明,钇的注入改变了钢表面的氧化模式,同未注入区相比,注入区的氧化膜致密,与基体结合好,氧化速率下降。     

硫和钇在含钇Ni3Al基IC6合金高温氧化过程中的界面行为

利用电子探针的元素线扫描技术,研究了添加钇后的ＩＣ６合金中钇和硫在１１００℃氧化时的界面行为,发现加钇后,由于在金属熔体中能脱硫同时形成的富钇相也能在高温氧化过程中作为硫的陷阱,减少了硫在氧化物基体界面上的扩散偏聚,提高了氧化物／基体之间的结合力,使得所形成的氧化物不易剥落,从而提高合金的高温氧化能力。钇提高ＩＣ６合金高温抗氧化能力的另一个原因是,钇能扩散到所形成的氧化物的晶界,提高氧化物的晶 界     

钛表面二氧化钛膜中氧空位点缺陷传输性能的电化学研究

"钛/TiO2氧化膜/溶液"界面电极体系的电化学性能主要决定于钛表面的TiO2氧化物膜.本文利用多种电化学技术,结合半导体物理的Mott-Schottky分析和Einstein方程,研究了金属钛在1.0mol·L-1HClO4溶液中表面半导体TiO2氧化膜的生长及氧化膜中氧空位点缺陷在外加电场作用下的传输性能,并根据离子性电荷传输与电子性电荷传输对电场变化响应时间之不同特点,确定氧化膜中点缺陷扩散系数.结果表明,电极电位或阳极析氧反应对稳态电流(iss)、氧化膜的阳极化常数(α)、膜中电场强度()、以及膜中氧空位点缺陷的扩散系数(D0)等重要物理化学参数,均有显著影响,并依据氧化膜中的结构变化进行分析.     

铁基体离子注入钯的腐蚀行为

研究了铁基体离子注入钯后的腐蚀行为。钯离子注入剂量为１×１０＾６～１×１０＾１８离子．ｃｍ＾－２注入能量４０ｄｅＶ．在ｐＨ＝５．０的０．５ｍｏｌ／Ｌ ＮａＡｃ／ＨＡｃ缓冲溶液中，用动电位扫描法测量了注钯后的铁的阳极溶解过程，用开腐蚀电位与浸泡时间的关系研究了修饰材料的耐蚀性。结果表明，钯离子的注入降低了铁的临界钝化电流，在ｐＨ＝５．０的醋酸盐缓冲溶液中保持较好的钝性。但当注入电极表面的氧化膜被还原     

注入Y离子对Ni3Al合金高温氧化行为的影响

以40 KeV的能量和3×1017 /cm2的剂量在Ni3Al合金中注入Y离子, 利用热重分析、 X射线衍射、扫描电镜、能谱分析和划痕分析等技术研究了离子注入对其900 ℃恒温氧化行为的影响. 结果表明 注入Y离子不仅改变了合金的氧化动力学, 而且改变了其氧化机理. 注入Y离子后合金氧化产物中的NiO含量大为增加, 从而降低了合金的抗氧化性能. 但Y离子的注入使NiO晶粒细化, 增强了氧化膜的塑性和粘附性.     

新型锂离子电池三维结构泡沫NiO电极的制备及电化学性能

通过固相氧化方法,以三维结构泡沫镍为基体和金属镍源,制备了三维结构泡沫氧化镍负极。XRD和SEM结果表明,经500℃氧化处理,泡沫镍基体上形成了NiO微米级的致密活性氧化层。通过充放电测试和循环伏安测试研究了电极的电化学性能,结果表明,三维结构泡沫氧化镍在放电电位区间0.05～3.2VvsLi/Li+,0.2C倍率下充放电,初始容量损失为20%,且经40次循环后,质量比容量为950mAh·g-1,三维泡沫氧化镍电极具有优异的循环容量保持性能。三维泡沫氧化镍具有的大的活性表面积,降低了界面反应的极化,从而提高了NiO电极的倍率放电性能。     

表面涂覆CeO_2对Co－40Cr合金氧化行为的影响

研究了表面涂覆ＣｅＯ２对Ｃｏ４０Ｃｒ合金在１０００℃、空气中恒温氧化和循环氧化的影响。并用扫描电镜／能谱（ＳＥＭ／ＥＤＸＳ）、电子探针（ＥＰＭＡ）、高分辨电子显微镜（ＨＲＥＭ）等测试手段对氧化膜的形貌和成分进行了观察分析。此外，还用声发射（ＡＥ）方法对氧化膜在热应力作用下发生的开裂和剥落进行了监测。结果表明，涂覆ＣｅＯ２后极大地提高了合金的抗恒温氧化和抗循环氧化性能。研究表明，涂覆的ＣｅＯ２主要以细小颗粒的形式高度弥散存在于氧化膜的外表面，并且主要分布于氧化物晶界上，其中部分ＣｅＯ２以更加细小（１０～２０ｎｍ）的形式存在于Ｃｒ２Ｏ３晶粒内部。这些弥散分布的ＣｅＯ２颗粒改变了Ｃｒ２Ｏ３氧化膜的生长机制，通过阻碍Ｃｒ３＋阳离子向外扩散，降低了氧化膜的生长速率，细化了氧化膜的晶粒并提高了膜的高温塑性，使氧化膜在基体上有较好的粘附性     

电活性质点Fe^2^+离子在六氰亚铁钒薄膜中的传输

电活性质点Fe^3^+可穿透六氰亚铁钒薄膜在玻璃碳基体电极表面于较负电位处直接氧化, 也可经VHF膜中氧化还原点位的媒介在较正电位处理膜-溶液界面及膜内部发生催化氧化. 两个过程分别在用VHF修饰过的旋转GC电极上的伏安曲线中产生, 可明确分辨的第一波和第二波. 第一波的极限电流受Fe^2^+离子在溶液中和膜中的扩散速率控制.VHF薄膜对Fe^2^+离子的透过能力, kDm/d, 为10^-^3-10^-^2cm.s^-^1数量级, 随膜厚度增大而减小, 不随溶液中Fe^2^+离子浓度改变.     

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。     

Determination of heats of detonation and influence of components of composite explosives on heats of detonation of high explosives

The heats of detonation of 20 simple high explosives and explosive mixtures were determined by means of an adiabatic detonation calorimeter designed by the authors. The results indicated that the performance of the instrument was reliable and the experimental data were very accurate. For explosive mixtures, there was a linear accumulative relationship between the heats of detonation of the explosive mixture and its components. Accordingly, the heats of detonation of explosive mixtures could be calculated directly from the heats of detonation of simple explosives and the characteristic heats of other components. The experiments showed that the gold or brass shell of the cylindrical charge could be substituted by a thick-walled porcelain shell, which had the advantage of cheapness.

     

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.     

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。     

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^-。     

Summary of development of the theory of stability of colloids and thin films

In this review, the research of the author in the field of colloidal systems is summarized. The factors influencing colloidal stability are systematized and analyzed. Examples are presented to illustrate the practical utilization of the theory of stability of colloids and thin films.This review was prepared on the basis of the works of the author, which were awarded the State Premium for 1991 in the field of science and technology, chemistry section.Institute of Physical Chemistry, Russian Academy of Sciences, 117915 Moscow. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 8, pp. 1708–1717, August, 1992.     

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.     

解决能源问题的新途径--光解水制氢的研究

面对日益枯竭的能源危机,氢能是一种洁净、最有前景的替代能源。目前在各种制氢的方法中光催化分解水制氢的研究最多,光解水过程中催化剂最关键,本文对利用太阳能光解水的途径、提高光催化反应效率以及光催化剂的开发研究进行了综述。