The effect of aluminium coating on elemental standards in X-ray microanalysis

The standardisation of frozen hydrated bulk biological specimens using gelatin standards is described. The relationship between corrected elemental X-ray counts and ionic concentration was found to be linear, and minimum detectable limits for each element are stated. Variations in uncorrected standard curves were found to be due to changes in aluminium coating thickness. There was an inverse relationship between coating thickness and elemental X-ray counts. The factors causing this are discussed. To avoid errors arising from inconsistent aluminium thickness, experimental material should only be compared with standards of similar aluminium net counts. This can be achieved most easily by mounting and analysing specimen and standard together.     

Synthesis of selenium nanoparticles in the presence of silk fibroin

This paper describes a solution-phase approach to the synthesis of selenium nanoparticles by reducing selenious acid solution with ascorbic acid in the presence of silk fibroin. The monodispersed spherical selenium colloid particles obtained were very stable in silk fibroin solution and characterized by Atomic force microscopy and X-ray techniques. The influences of temperature and ultrasonication on the morphology of selenium nanoparticles were also discussed. The experiments showed that the selenium nanoparticles with various morphologies could be obtained under different temperatures and the appropriate ultrasonication time was 60 min. This result indicated that the silk fibroin molecules intimately associated with the surface of the selenium particles and controlled the growth particles.     

铀表面初始氧化行为的电子能量损失谱研究

利用俄歇电子能谱仪获取了表面清洁的铀及其在氧化过程中的电子能量损失谱(EELS)，研究这些电子能量损失谱线显示：清洁表面铀的等离子损失的实验值与理论值较为符合；随着氧化程度的加剧，体等离子体(BP)、表面等离子体(SP)以及价带间跃迁所造成的电子能量损失峰发生了明显的连续偏移和强度的变化，表明室温下清洁表面铀暴露微量纯氧后，在铀表面上发生了U→UO→UO2初始氧化过程。同时，又采用了俄歇电子能谱(AES)和X射线光电子谱(XPS)对照分析了铀的初始氧化过程。     

A novel method for determination of polyester end-groups by NMR spectroscopy

An efficient, convenient and quantitative method for characterising polyester end-groups is described. We have found that trichloroacetyl isocyanate (TAI) reacts rapidly and quantitatively with both carboxyl [C(O)OH] and hydroxyl (OH) chain ends to form derivatives that can be readily determined by ¹H NMR spectroscopy. The TAI capped end-groups give rise to characteristic imidic NH resonances in a normally clear region of the ¹H NMR spectrum [δ∼10-11.5 for C(O)-O-C(O)-NH-C(O)CCl₃ from C(O)OH, δ∼8-9 for O-C(O)-NH-C(O)CCl₃ from OH]. The method has been successfully applied to quantitative determination of the end-groups of a wide variety of oligomeric polyesters. It has also been applied to higher molecular weight polyesters including commercial, bottle grade, poly(ethylene terephthalate) (PET) and PET based copolyesters (e.g. PETG).     

新型超微晶软磁合金FePCCuMoSi微观结构缺陷的正电子湮没研究

用正电子湮没方法研究了新型超微晶软磁合金的微观结构缺陷，样品选用的是在不同温度下退火的Ｆｅ８１Ｐ１２Ｃ３Ｃｕ１Ｍｏ０．５Ｓｉ２．５合金，结果表明，合金的微观结构构陷大小，密度随退火温度有规律地变化，这种现象可能与非晶的晶化过程有关。     

Determination of the width of the transition layer between the crystalline and amorphous zones in nylon 1010 by SAXS

The width of the transition layer between the crystalline and amorphous zones in nylon 1010 was determined by SAXS with point collimation and long-slit collimation, respectively. The width of the transition layer, E, was found to be 1.7 nm. The results show that the width of the transition layer is independent of crystallinity.     

电子束、离子束与蓝宝石相互作用的研究

研究了电子束、离子束作用于Al2O3表面时成分的变化，表明无论电子束或离子束都能使Al2O3发生分解，产生导电的元素Al。实验在PHI610·SAM上进行，电子束轰击下（3keV，O．5μA，入射角60°）10s就有元素Al分解出来，2min以后就达到饱和，分解析出量随时间成a（1－e－bt）的关系。离子束轰击下同样发生元素Al的分解，但当Ei＞3keV时，由于剥离速率加大，溅射5min时表面Al峰反而比1min时要弱。这时表面Al含量处于分解析出与溅射剥离的动态平衡中。实验还发现了Al2O3的解析与表面成分有关（如碳的含量）。最后讨论电子束与离子束的解析机理。     

四种别藻蓝蛋白三聚体的时间分辨荧光光谱研究

研究了从Ａｎａｂａｎａｖａｒｉｂｉｌｉｓ中提取的４种别藻蓝蛋白ＡＰＣＩ，ＡＰＣＩＩ，ＡＰＣＩＩ及ＡＰＣＢ三聚体的稳态光谱和皮秒荧光光谱。采用Ｍｏｎｔｅ－Ｃａｒｌｏ方法对瞬态荧光光谱进行拟合，实验结果表明：ＡＰＣＩ荧光有两个带，其中第一个带位于６６２ｎｍ，有两个时间组分：３５．８ｐｓ和１．６７ｎｓ；第二个带位于６８０ｎｍ，有两个时间组分：３４．２ｐｓ和１．６４ｎｓ；ＡＰＣＩＩ瞬态荧光位于６６０ｎｍ，有两个时间组分：２０．４ｐｓ和１．６４ｎｓ；ＡＰＣＩＩ瞬态荧光位于６６０ｎｍ，有两个时间组分：２３．８ｐｓ和１．７６ｎｓ；ＡＰＣＢ瞬态荧光有两个带，其中第一个带位于６６２ｎｍ，有两个时间组分：３６．６ｐｓ和１．４５ｎｓ；第二个带位于６８０ｎｍ，有两个时间组分：２５．８ｐｓ和１．６２ｎｓ。实验结果一方面说明了藻胆体核内４种别藻蓝蛋白形成能量传递的两条途径；另一方面瞬态荧光解叠结果揭示了ＡＰＣＩ和ＡＰＣＢ三聚体内能量传递的超快过程。     

氮化钛薄膜的高分辨AES谱和XPS谱研究

着重讨论了TiNx薄膜俄歇电子谱的定量分析方法和X射线光电子谱中线形的变化。利用已知组元强度定量分析技术和Ti的LMV俄歇电子峰，探讨TiNx薄膜中N含量的定量方法。由该方法给出的定量结果与X射线光电子谱定量结果相一致。同时，利用X射线光电子谱测定了TiN和Ti2N2p轨道的结合能。并针对Ti2p峰形随N含量的变化，给出新的解释。     

材料研究中系列试样的单标样法 X 射线定量分析

本文提出了用一个标样进行系列试样 X 射线定量相分析的方法.它克服了一般 X 射线定量方法需要混合研磨和手续烦复的缺点以及无标样 X 射线定量方法存在病态方程不易解决的问题.该方法对常规 X 射线定量分析具有普遍的实用性.