乙酰二茂铁缩4—苯氨基硫脲与UO^2＋2,Hg^2＋,Ni^2＋,Zn^2＋,的…

乙酰二茂铁缩４－苯氨基硫脲（Ｃ１９Ｈ１９Ｎ３ＳＦｅ）与某些金属离子在无水乙醇中反应得到了希夫碱配合物Ｍ．Ｌ．Ｘ２．ｎＨ２Ｏ（Ｍ为ＵＯ＾２＋２，Ｈｇ＾２＋，Ｎｉ＾２＋，Ｚｎ＾２＋，Ｌ为Ｃ１９Ｈ１９Ｎ３ＳＦｅ；ＮＯ＾－３，Ｃｌ＾－，１／２ＳＯ＾２－４；ｎ＝０－６）并对配合物的组成及某些物理化学质进行了测试和表征。     

纳米材料Fe2O3的X射线衍射与正电子湮没研究

给出了纳材料Ｆｅ２Ｏ３的Ｘ射线衍射与正电子湮没辐射多普勒展宽的实验结果。发现样品分别经４００℃４ｈ和８００℃４ｈ退火后，原来的γ－Ｆｅ２Ｏ３均转变成αＦｅ２Ｏ３，而且颗粒尺寸分别增加到３８．７ｎｍ与９２．９ｎｍ；样品的线形参数均随退火温度高而减小。     

乙酰二茂铁缩4－苯氨基硫脲与UO_2~（2＋）、Hg~（2＋）、Ni~（2＋）、Zn~（2＋）的希夫碱配合物的合成与表征

乙酰二茂铁缩４－苯氨基硫脲（Ｃ_（１９）Ｈ_（１９）Ｎ_３ＳＦｅ）与某些金属离子在无水乙醇中反应得到了希夫碱配合物Ｍ·Ｌ·Ｘ_２·ｎＨ_２Ｏ（Ｍ为ＵＯ_２~（２＋）、Ｈｇ~（２＋）、Ｎｉ~（２＋）、Ｚｎ~（２＋）；Ｌ为Ｃ_（１９）Ｈ_（１９）Ｎ_３ＳＦｅ；Ｘ为ＮＯ３－、Ｃｌ－、ＳＯ_４~（２－）；ｎ＝０—６），并对配合物的组成及某些物理化学性质进行了测试和表征。     

MOSSBAUER SPECTROSCOPY OF HIGH T_c YBa_2 (Cu_(3-x)Fe_x )O_y

ＭＯＳＳＢＡＵＥＲＳＰＥＣＴＲＯＳＣＯＰＹＯＦＨＩＧＨＴ＿ｃＹＢａ＿２（Ｃｕ＿（３－ｘ）Ｆｅ＿ｘ）Ｏ＿ｙ￥ＬｉＳｈｉ（李士）ａｎｄＬｉＹｉｎｈｕａ（李印华）（ＩｎｓｔｉｔｕｔｅｏｆＨｉｇｈＥｎｅｒｇｙＰｈｙｓｉｃｓ，Ｂｅｉｊｉｎｇ１０００８０，Ｃｈｉ...     

亚铁法测定HNO3-H2C2O4混合液中的NO3-

对测定ＴＲＰＯ流程Ｈ２Ｃ２Ｏ４反萃液中的ＮＯ３＾－的分析条件进行了研究。在Ｈ２ＳＯ４介质中,Ｆｅ＾２＋、与ＮＯ３＾－作用,定量释放出ＮＯ,并立即同过量Ｆｅ＾２＋反应生成有色的亚硝酰配合物,利用这种性质用分光光度法或容量法测定ＮＯ＾－３浓度。实验结果表明,在氨磺酸存在下,质量比Ｒ（ＮＯ２＾－／ＮＯ＾－３）和Ｒ（Ｃ２Ｏ４＾－２／ＮＯ＾－３）＝１９０时,对ＮＯ＾－３的测定无影响,分光光度法测定ＮＯ＾－３     

非晶合金Fe73.1Cu1.2Nb3.2Si12.5B10.0晶化的Mossbauer研究

采用Ｍｏｓｓｂａｕｅｒ效应和ＸＲＤ分析方法研究了非晶合金Ｆｅ７３．１Ｃｕ１．２Ｎｂ３．２Ｓｉ１２．５Ｂ１０．０的晶化。实验表明，该非晶合金有两个晶化阶段。在第一阶段晶化后，样品主要由ＤＯ３型的α－ＦｅＳｉ合金的超细颗粒和作为晶界的非晶相两部分组成。随着退火温度的上升，晶化相的含量增加，非晶相含量减少。在第二阶段晶化后，残余的非晶相就晶化为Ｆｅ２Ｂ和Ｆｅ２３Ｂ６化合物以及可能为Ｆｅ－Ｎｂ－Ｂ之类的顺     

EDXRF法直接测定铁氧体中MnO,ZnO和Fe2O3的含量

用ＥＤＸＲＦ法直接测定锰锌铁氧体中ＭｎＯ、ＺｎＯ和Ｆｅ２Ｏ３含量是采用软、硬件相结合的办法，成功地分解ＭｉｌＫ和ＦｅＫ重迭峰，并对特定基体效应提出具体对策。由２３８Ｐｕ同位素源和正比计数管组成的探测系统，对ＭｎＯ、ＺｎＯ和Ｆｅ２Ｏ３的测量准确度分别为０．１４％、０．１０％和０．１７％。     

分光光度法测定dl—HMPAO冻干药盒中微量Sn（II）

采用分光光度法及Ｓｎ（Ⅱ）－Ｆｅ（Ⅲ）－邻二氮菲（Ｐｈｅｎ）体系测定ｄｌ－ＨＭＰＡＯ冻干药盒中微量Ｓｎ（Ⅱ）。在ｐＨ≈５的酸度下，Ｓｎ（Ⅱ）还原Ｆｅ（Ⅲ）生成红色的Ｆｅ（Ⅱ）－Ｐｈｅｎ配合物。该配合物的最大吸收波长λｍａｘ＝５１０ｎｍ，计算得到表观摩尔吸光系数为２．０×１０＾４ｌ·ｍｏｌ＾－１·ｃｍ＾－１。Ｓｎ（Ⅱ）浓度基０－２．５μｇ／ｍｌ内符合比尔定律。     

核纯U3Si2粉末中铀的测定

试样用ＨＮＯ３－ＨＦ分解，加入Ｈ２ＳＯ４后加热至Ｈ２ＳＯ４冒烟以除去Ｓｉ，ＨＮＯ３和ＨＦ。在含有氨基磺酸的浓磷酸溶液中，用过量ＦｅＳＯ４将铀（Ⅳ）。剩余的Ｆｅ＾２＾＋以钼（Ⅳ）作催化剂，用ＨＮＯ３氧化。加入ＶＳＯ４溶液后，用标准Ｋ２Ｃｒ２Ｏ７溶液滴定铀（Ⅳ）至铀（Ⅵ），以电位法确定滴定终点。方法的精密度优于±０．１％，误差≤±∩．１％。     

高注量快中子辐照在α—Al2O3中产生空洞的正电子湮没研究

采用正电子湮没技术研究３×１０＾２０／ｃｍ＾２中子注量，Ｅｎ≥１ＭｅＶ快中子辐照在α－Ａｌ２Ｏ３中产生的辐照效应，实验发现α－Ａｌ２Ｏ３在辐照后的８５０℃退火形成尺寸约为０．７ｎｍ的空洞。     

Fabrication and characterization of He-charged ODS-FeCrNi films deposited by a radio-frequency plasma magnetron sputtering technique

He-charged oxide dispersion strengthened(ODS)FeCrNi films were prepared by a radiofrequency(RF)plasma magnetron sputtering method in a He and Ar mixed atmosphere at150℃.As a comparison,He-charged FeCrNi films were also fabricated at the same conditions through direct current(DC)plasma magnetron sputtering.The doping of He atoms and Y_2O_3 in the FeCrNi films was realized by the high backscattered rate of He ions and Y_2O_3/FeCrNi composite target sputtering method,respectively.Inductive coupled plasma(ICP)and x-ray photoelectron spectroscopy(XPS)analysis confirmed the existence of Y_2O_3 in FeCrNi films,and Y_2O_3 content hardly changed with sputtering He/Ar ratio.Cross-sectional scanning electron microscopy(SEM)shows that the FeCrNi films were composed of dense columnar nanocrystallines and the thickness of the films was obviously dependent on He/Ar ratio.Nanoindentation measurements revealed that the FeCrNi films fabricated through DC/RF plasma magnetron sputtering methods exhibited similar hardness values at each He/Ar ratio,while the dispersion of Y_2O_3 apparently increased the hardness of the films.Elastic recoil detection(ERD)showed that DC/RF magnetron sputtered FeCrNi films contained similar He amounts(~17 at.%).Compared with the minimal change of He level with depth in DC-sputtered films,the He amount decreases gradually in depth in the RF-sputtered films.The Y_2O_3-doped FeCrNi films were shown to exhibit much smaller amounts of He owing to the lower backscattering possibility of Y_2O_3 and the inhibition effect of nano-sized Y_2O_3 particles on the He element.     

铁氮化合物FexN(x≈2)的穆斯堡尔研究

在不同组成比的高纯Ａｒ和Ｎ２气氛下,用ＲＦ溅射纯铁制备成不同含氮量的ＦｅｘＮ（１．６＜ｘ＜２．２）。用质子深度弹性散射对样品中的Ｆｅ、Ｎ、Ｏ、Ｃ进行分析,Ｘ光电子谱仪用于鉴定铁的氧化程度。采用穆斯堡尔效应测量室温时和经２００、２５０、３００℃退火的样品。对照Ｘ衍射实验结果表明,在铁的化学计量接近２时,随氮气氛的增加,或者经退处理后,其相结构会从正交结构的ζ－Ｆｅ２Ｎ向密堆六方结构的ε－Ｆｅ２Ｎ或准     

双束强辐照对氧化物弥散强化铁素体型合金强化相稳定性影响

采用双束复合辐照装置,研究了He存在条件下,强辐照对长期时效后的ODS合金中强化相(Y2O3)的稳定性和辐照损伤特征的影响。实验结果表明:双束强辐照下,ODS合金中强化相不稳定,发生聚集长大并造成附近基体中Ti、Y浓度增高,导致空洞尺寸和空洞肿胀增加,并对这一结果从理论上进行解释。     

Y2O3压致结构相变的研究

本文采用金刚石对顶砧高压装置（DAC），利用同步辐射X－ray衍射，对Y2O3粉末样品进行了原位高压X－ray衍射实验，最高压力达到23GPa。在研究的压力范围内观察到两个相变。在12.8GPa压力点，Y2O3由稀土倍半氧化物的立方结构转变为单斜结构。在21.8GPa压力点，样品由单斜结构转变为另一个新相，但由于样品峰的消失，无法判断其结构。卸压后样品为单斜结构，说明Y2O3第一个压致结构相变为不可逆相变。     

放射性废有机溶剂（TBP／OK）稳定化技术研究

磷酸三丁酯／煤油废有机溶剂是核设施产生的中低放废物之一。本文研究了废溶剂在Ｈ２Ｏ２－Ｆｅ＾２＋／ＴｉＯ２－Ｈ２ＳＯ４体系中的氧化分解行为，分析了Ｈ２Ｏ２用量，催化剂，温度，ｐＨ值等主控因素对反应进程及结果的影响。     

Stabilization and volume reduction of radioactive spent ionexchange resins

Stabilization and volume reduction of spent radioactive ion-exchangeresins(IERs) were studied.Stabilization technology includes volume reduction with wet chemical oxidation process and immobilization of the residue into cement.Under suitable conditions,the exhausted radioactive ion-exchange resins were dissolved successfully in a H2O-Fe^2 /Cu^2 catalytic oxidation system(Fenton reagent).The analytical results indicated that the radioactive nuclides loaded in the resins were concentrated in decomposed solution and solid residues.The process parameters of wet chemical oxidation and solidification were also obtained.The decomposition ratios were 100% and more than 90% for cation and amion IERs respectively.The waste volume was decerased by 40% compared with that of original spent resins.     

Dy3+激活的几种硼酸盐在VUV-VIS范围的光谱性质

本文报道了SrAl2B2o7:Dy^3 、BaAl2B2O7:Dy^3 、SrAl3BO7:Dy^3 、La2CaB10O19:Dy^3 的紫外－真空紫外（UV－VUV）激发光谱和UV激发下的发射光谱。根据发射光谱讨论了Dy^3 离子在这几种基质中发光的黄蓝比（Y／B）。在VUV激发光谱中推测了Dy^3 的f-d跃迁及电荷迁移态（CTS）和基质吸收的位置。     

Nanoscale characterisation of ODS-Eurofer 97 steel: An atom-probe tomography study

Laser-pulsed atom-probe tomography has been used to study the nanoscale features present in an ODS-Eurofer 97 alloy. A core/shell structure was found for particles 5-10 nm in diameter. The particle cores were primarily Y and O, enriched with Mn and Si resulting in a metal (Y, Mn and Si) to oxygen ratio of M:O ∼2:3. The ∼2 nm thick outer-shell region of the particles exhibited partitioning of V, Cr, Ta, C and N together with the core elements in many cases. Detailed compositional measurements have also been made on the smallest of the yttria-based oxide clusters down to 2 nm in diameter. The 2 nm clusters were found to have a non-stoichiometric oxide composition, enriched in oxygen compared to Y₂O₃, and evidence for the existence of a shell around these smaller particles was found.     

Ab initio simulation of yttrium oxide nanocluster formation on fcc Fe lattice

Using results of density functional theory (DFT) calculations the first attempt towards the understanding of Y₂O₃ particles formation in oxide dispersed strengthened (ODS) ferritic-martensitic steels was performed. The present work includes modeling of single defects (O impurity atom, Fe vacancy and Y substitute atom), interaction between substituted Y atoms, Y-Fe vacancy pairs and oxygen impurity atoms in the iron matrix. The calculations have showed the repulsive interaction between the two Y substitute atoms at any separation distances that might mean that the oxygen atoms or O atoms with vacancies are required to form binding between atoms in the yttrium oxide nanoclusters.     

Stoichiometric characterization of YBaCuO superconductors with nuclear probes

Nuclear probes using energetic (MeV range) charged particle irradiation and prompt detection of atomic and nuclear signals are powerful tools to determine quickly and accurately the chemical constituants of YBaCuO superconductors. PIXE in milliprobe geometry is used to determine the actual concentration ratios of Y/Ba and Cu/Ba, with an accuracy of 3% or better. Calculated matrix effects in the detection of characteristic K X-rays allow accurate determinations even when the composition of samples are very different from reference materials. RBS of 2 MeV α-particles is used to certify the homogeneity of the Y-Ba-Cu composition without reference material to a thickness of 250 μg/cm² under the surface. Deuteron microbeam irradiation leads to simultaneous composition maps of all the elements (YBaCuO) in volume of 5 × 5 × 5 μm using X-rays and protons as identification signals.