铝含量对LaNi5-xAlx合金氘化与去氘化热力学函数的影响

测定了LaNi5-xAlx(x=0.0、0.1、0.2、0.3)的氘化与去 氘化热力学参数,评价了LaNi5-xAlx中铝含量对氘化与去氘化热力学函 数的影响。研究结果表明,合金的坪台压力和吸氘容量随x的增加而降低;坪率随x 的增加而增加;热力学焓变与熵变随x的增加而减少;滞后系数Hf随x的增加而减少 。     

氚老化对LaNi_(4.9)Al_(0.1)的动力学性能的影响

测定了不同材龄的LaNi4 .9Al0 .1氘化与去氘化动力学参数 ,评价了氚老化对LaNi4 .9Al0 .1动力学性能的影响。研究结果表明 ,氚老化不改变合金的氘化与去氘化的反应级数 ;反应速率随老化时间的增加而降低 ;活化能随老化时间的增加而增加     

LaNi5氚老化效应的实验研究

测定了老化LaNi5料的解吸等温线及去氘化热力学参数.评价了氚老化对LaNi5贮氢性能的影响.结果表明,氚老化使LaNi5解吸等温线形貌发生重大改变.与新鲜材料相比,老化2140天后,在373 K下,坪台压力降低了约50%,坪斜由0.033到0.130,可逆吸氢容量减少了约1.3 mmol.g-1.老化LaNi5料去氘化反应热力学焓变ΔH和熵变ΔS分别由30.1 kJ.mol-1和105 J.mol-1.K-1增加到44.5 kJ.mol-1和128 J.mol-1.K-1.     

氚老化对LaNi4.9Al0.1的动力学性能的影响

测定了不同材龄的LaNi4.9Al0.1氘化与去氘化动力学参数,评价了氚老化对LaNi4.9Al0.1动力学性能的影响.研究结果表明,氚老化不改变合金的氘化与去氘化的反应级数;反应速率随老化时间的增加而降低;活化能随老化时间的增加而增加.     

氘化对KH2PO4晶体微观缺陷影响的正电子湮没研究

采用传统降温法从不同程度氘化(x=0, 0.51, 0.85)的生长溶液中生长氘化KH₂PO₄(KDP) 晶体, 利用正电子湮没技术(正电子寿命谱和多普勒展宽谱)、结合X射线衍射谱(XRD) 结构分析, 对KDP晶体氘化生长的微观缺陷进行了研究, 讨论了氘化程度对晶体内部微观结构特性、缺陷类型和浓度的影响. XRD结果显示晶胞参数a, b值随氘含量的增加而增加, c值无明显变化; 正电子寿命谱结果发现随着氘化浓度的提高, KDP晶体内部中性填隙缺陷以及氧缺陷不断增加, 引起晶体晶格畸变; 氢空位、K空位、杂质替位缺陷不断发生缔合反应形成复合缺陷, 缺陷浓度不断减少; 团簇、微空洞等大尺寸缺陷也在不断发生聚合反应, 缺陷浓度表现为不断减少. 多普勒实验结果表明随着氘化程度的提升, 晶体内部各类缺陷表现为同步变化. 实验结果表明, KDP晶体在低浓度氘化生长(50%以内)下缺陷反应较弱, 而在高浓度氘化(50%以上)下的缺陷反应显著增强.     

氘化锆的XRD与TG-DSC分析

利用钨杆发热的电阻镀膜机对锆进行蒸发成膜，衬底选择金属钼。蒸镀之前，衬底经950℃的高温氢气还原后置于10^-5Pa的真空中1000℃脱气1h。氘化时，样品先在10^-4Pa真空中升温至550℃脱气，而后根据对样品的吸氘浓度要求，向氘化反应系统中充入理论计算的氘量，样品在降温过程中与充入的氘气进行反应。用于TG-DSC分析的体材氘化锆氘化时的初始氘气压强为2000Pa，其余的工艺参数与锆膜的氘化过程相同。实验所用金属材料的纯度均大于99．9％，气体纯度大于99％。     

聚苯乙烯的氘化及其性能研究

采用聚苯乙烯(PS)催化氘化技术,在使苯环被氘化饱和的基础上,成功地制备出了部分氘化的聚环己基乙烯（D-PVCH,C8H8D6）。用傅里叶红外光谱仪、核磁共振仪对D-PVCH的结构进行了表征,结果表明与目标产物吻合,即苯环被氘饱和转化为环己基,氘代率为41.5%。采用差式扫描量热仪和热重分析仪分析了D-PVCH的热性能,结果表明D-PVCH的玻璃化转变温度为125 ℃,5%失重温度为403 ℃。另外,D-PVCH可溶于常见溶剂,如石油醚、环己烷和甲苯等。与PS相比,D-PVCH具有较好的热稳定性和良好的溶解性能。     

氘化及氦离子注入对钪膜的表面形貌和相结构的影响

采用XRD, SEM, AFM等详细研究了氘化及氦离子注入对钪膜的表面形貌和相结构的影响. 结果表明,在单晶硅及抛光Mo基片上制备的钪膜均具有(002)晶面择优取向;钪膜氘化后表面会出现大量孔洞, 氘化后氘化钪(ScD₂)晶粒长大,但内部会残留少量未完全氘化反应的晶粒尺寸较小的 ScD_0.33/Sc晶粒;氦离子注入对钪及氘化钪的表面形貌没有明显影响, 离子注入的氦将在钪及氘化钪晶格中聚集成泡,导致氦离子注入层中的钪及氘化钪衍射峰向低角度偏移, 并且氦泡的聚集具有择优取向性.     

Tb0.3Dy0.7(Fe1-xAlx)1.95合金的自旋重取向和穆斯堡尔

系统研究了室温和77K温度时Tb0.3Dy0.7(Fe1-xAlx)1.95(x=0,0.05,0.1,0.15,0.2,0.25,0.3,0.35)合金中金属Al替代Fe对自旋重取向和穆斯堡尔谱的影响. 结果发现,Tb0.3Dy0.7(Fe1-xAlx)1.95合金的易磁化方向随成分和温度在{110}面逐渐偏离了立方晶体的主对称轴,即自旋重取向. 室温下,当x=0.15时,Tb0.3Dy0.7(Fe1-xAlx)1.95合金中出现了少量非磁性相;x>0.15时,合金完全呈顺磁性;而77K温度下,x=0.2时合金仍然呈磁性相. 在室温和77K温度时,超精细场Hhf均随Al元素的增加而减小,而同质异能移IS随Al元素的增加而增加,四极劈裂QS随Al含量呈无规律的变化.     

Tb0.3Dy0.7(Fe1-xAlx)1.95合金的磁致伸缩、自旋重取向和穆斯堡尔谱研究

系统研究了室温下Tb0.3Dy0.7(Fe1-xAlx)1.95(x=0,0.05,0.1,0.15,0.2,0.25,0.3,0.35)合金中金属Al替代Fe对晶体结构、磁致伸缩、各向异性和自旋重取向的影响.结果发现,x<0.4时,Tb0.3Dy0.7(Fe1-xAlx)1.95完全保持MgCl2立方Laves相结构,晶格常量a随Al含量x的增加而增大.磁致伸缩测量发现,随着替代量x的增多磁致伸缩减小,x>0.15时超磁致伸缩效应消失;x<0.15时磁致伸缩在低场下(H≤4kA/m)有小幅增加,高场下迅速减小,而且易趋于饱和,说明添加少量Al有助于减小磁晶各向异性.内禀磁致伸缩λ111随Al替代量x的增加大幅度降低.对于0≤x<0.15,穆斯堡尔效应表明,随Al含量的增加Tb0.3Dy0.7(Fe1-xAlx)1.95合金中发生了自旋重取向,易磁化方向经历了[111]→[u v 0]→[u v w]的转变.由相对磁化率随温度的变化关系可以看出,Al替代Fe使自旋重取向温度降低.当x=0.15时,Tb0.3Dy0.7(Fe1-xAlx)1.95合金中出现了少量非磁性相;x>0.15时,合金在室温下呈现顺磁性.     

De-Pake-ing transform analysis of fully deuterated malonic acid

The analysis of deuterium wideline NMR spectra has been an essential step in characterizing the dynamics of molecules in the solid-state. Although clearly important, the identification of quadrupolar coupling constants (QCCs) from the powder patterns is often complicated by poor sensitivity and/or spectral overlap. Previously, others have demonstrated the utility of “de-Pake-ing”, a mathematical transform that yields the QCCs in a straightforward manner for symmetric (η = 0) sites. In this short paper, we describe our analysis of a powder sample of perdeutero-malonic acid, a molecule with two distinct deuteron environments and asymmetries. The methylene sites are immediately amenable to the standard de-Pake-ing transform analysis due to their low asymmetry. However, the de-Pake-ing methodology for the acid deuterons, for which the asymmetry deviates significantly from zero, requires more analysis to extract their QCCs. The impact of this work on the future application of de-Pake-ing to a wider range of samples is also discussed.     

Structure of the ground states in the isotope substituted H3 molecular ions

The bound state properties and general structure of some H⁺₃-like molecular ions are determined from the results of direct numerical computations. All our calculations are performed with the use of non-adiabatic variational expansion written in the basis of five-body (= ten-dimensional) gaussoids. A large number of geometrical properties and expectation values of many inter-particle delta-functions are presented for the H₂D⁺, H₂T⁺, D₂H⁺, D₂T⁺, T₂H⁺, T₂D⁺ and HDT⁺ two-electron five-body ions. The problem of inter-particle correlations in five-body systems and related problem of adiabatic divergence in the H⁺₃-like ions are also briefly discussed.     

NMR of residual protons in partly deuterated anisotropic materials with phase-alternated decoupling of deuterium spins

A new method is presented for decoupling spins with S = 1 like deuterium in anisotropic media while observing other spins such as residual protons in partly deuterated samples. The carrier frequency of a weak radiofrequency (RF) field is applied near the center of the doublet arising from the quadrupolar interaction of the S = 1 spins. The phase of the RF field is periodically reversed with intervals matching the reciprocal of the magnitude of the quadrupolar splitting. It is shown by theory and experiment that, even when the irradiating field is quite weak, the efficiency of this phase-alternated decoupling scheme is much better than for simple continuous-wave irradiation at the center of the doublet, an established technique which is usually referred to as double quantum decoupling. The phase-alternated experiment makes it possible to decouple large quadrupolar interactions with a weak RF field. A theoretical analysis and numerical simulations are presented to demonstrate the decoupling performance. Proton spectra of partly deuterated dibromobutane in a liquid crystalline solvent have been recorded to illustrate the efficiency of phase-alternated deuterium decoupling.     

重氢原子进入钛晶体中引起的晶体结构转变与电解重水过程中“过热”现象的关系

对重氢原子进入钯或钛晶体中可能引起常温核聚变的机理探讨与实验研究结果，已在文献［１］中作了报导。后来又对钛阴极材料，在使用前后进行了Ｘ射线结构分析。发现在电解过程中发生过“过热”现象的钛阴极材料的晶体结构由原来的密排六方结构转变为立方结构，而没有发生“过热”现象的钛阴极材料的晶体仍然保持电解前的密排六方结构     

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利用一套四极质谱气体分析与测试系统,开展MicroVision Plus四极质谱计的氦(He)、氘(D2)分辨性能实验。分别向分析室送入He和D2,记录质谱图,得到质量刻度和分辨率等信息。He+峰位为(4.0022±0.0006)amu;D2+峰位为(4.0246±0.0006)amu。在10-6～10-4Pa的分压范围,观察到He和D2的分辨率随其分压强的增大而减小。在10-7Pa-m3-s-1的He漏孔条件下,调节D2送气量,He+/D2+分压峰值比在10-1量级可以分辨出He。     

氘束轰击石墨化学腐蚀的实验研究

石墨的化学腐蚀实验是在ＬＡＳ－２０００二次离子质谱仪的分析室中进行的，用高能氘离子束或与电子束联合辐照石墨，石墨温度从３００－１０００ＫＷ可调。辐照下释放的产物用四极质谱探头进行了质谱分析，得到了１．３μＡ、３ｋｅＶ氘束轰击下ＤＳＭＦ－８００石墨释放氘甲烷的温度特性，在７８０Ｋ处有一释放高峰。     

Effect of surface oxidation on the surface condition and deuterium permeability of a palladium membrane

Oxidation and deoxidation of a Pd membrane was conducted in a quartz tube oven in a temperature range of 23-500 °C. The micromorphology and chemical composition of the Pd membrane surface was characterized using scanning electronic microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). Micropores and PdO began to form on the Pd membrane surface after oxidation at 240 °C for 1 h and their quantity increased gradually with increasing temperature. A rough Pd membrane surface was obtained when the temperature rose to 500 °C. The PdO on the Pd membrane surface was completely deoxidized once more using H₂ at room temperature, but the rough surface morphology caused by oxidation remained. The deuterium permeability of the Pd membrane was tested using special equipment in the China National Key Laboratory and the results indicated that the rough Pd membrane surface had higher deuterium permeability than the original membrane. The improved deuterium permeability could be attributed to the higher Pd membrane surface area, which provided deuterium atoms with more adsorption sites and dissociation sites.     

DEUTERIUM INFLUX PROFILE ALONG THE APEX OF THE UPPER X-POINT TILES IN JET

ＤＥＵＴＥＲＩＵＭＩＮＦＬＵＸＰＲＯＦＩＬＥＡＬＯＮＧＴＨＥＡＰＥＸＯＦＴＨＥＵＰＰＥＲＸ－ＰＯＩＮＴＴＩＬＥＳＩＮＪＥＴ￥Ｙ．Ｋ．Ｚｈｕ（ＳｏｕｔｈｗｅｓｔｅｒｎＩｎｓｔｉｔｕｔｅｏｆＰｈｙｓｉｃｓ，Ｐ．Ｏ．Ｂｏｘ４３２，Ｃｈｅｎｇｄｕ６１００４１...     

Ga1—xAlxAs外延片有源区Al组份的测定方法

由于ＧａＡｓ与ＡｌＡｓ晶格常数相近，ＧａＡｓ晶格常数为０．５６５３５ｎｍ，ＡｌＡｓ的晶格常数为０．５６６０５ｎｍ，当固熔体中Ａｌ组份ｘ值从０变到１时，晶格常数变化约为０．１５％．因此，在ＧａＡｓ衬底上生长Ｇａ１－ｘＡｌｘＡｓ时，在界面处的失配位错少，...     

Labelling Studies for Structure Elucidation of a New Hydroxymetabolite of Tramadol

Abstract

Tramadol, racemic 1-(3-methoxyphenyl)-2-(dimethylaminomethyl)cyclohexane-1-ol, is an effective analgesic drug. Metabolites of tramadol described so far originate from O- and N-demethylation and are excreted in urine directly or after conjugation. A further metabolite was found in human liver microsome incubations and in the urine of volunteers after ingestion of tramadol. To elucidate the structure of the new metabolite, seven deuterated isotopomers of tramadol have been synthesized and ingested by volunteers. The mass spectra of the metabolites derived showed (i) that it was a hydroxy metabolite, (ii) that the hydroxy group was not located on the aromatic ring, the side chain, or the positions 2 and 6 of the cyclohexane ring, (iii) that the hydroxy-group was introduced to one of the the positions 3, 4 or 5 of the cyclohexane ring. The hydroxy metabolite was formed preferentially from the (-)-enantiomer, (1S,2S)-tramadol.