纳米Cu固体材料的X射线衍射与正电子湮没研究

 采用自悬浮-冷压法，在不同压力下制得纳米Cu固体材料并对其在不同温度和保温时间下进行退火，利用X射线衍射(XRD)和正电子湮没寿命谱(PAS)分析对材料的结构和微观缺陷进行了表征。XRD分析表明，压制而得的样品晶粒度为20 nm，低于300 ℃退火3 h后并未发现晶粒显著长大；PAS分析表明，压制后的样品缺陷主要为单空位和空位团，大空隙很少，随着退火温度的升高和退火时间的延长，单空位通过扩散结合成空位团，大空隙也在温度较高时分解为空位团，导致空位团的含量增加，而单空位和大空隙的含量降低。     

纳米Fe3 O4 颗粒的正电子湮没谱学研究

测量了磁性纳米Fe₃O₄颗粒的X射线衍射谱(XRD)、正电子湮没寿命谱(PALS)和符合多普勒展宽谱(CDBS),研究了不同压力和退火温度对磁性纳米Fe₃O₄颗粒物相、电子结构、缺陷及电子动量分布等的影响. XRD,PALS,CDBS测量结果表明:纳米Fe₃O₄颗粒的缺陷浓度随压力的增加而增大,但物相和缺陷类型并未发生变化;磁性纳米Fe₃O_{4< 关键词： 正电子 3}O₄')" href="#">Fe₃O₄ 寿命谱 多普勒展宽谱     

Co掺杂纳米ZnO微结构的正电子湮没研究

利用正电子湮没技术研究了10 at.% Co掺杂的Co₃O₄/ZnO纳米复合物中退火对缺陷的影响. 利用X射线衍射(XRD)测量了Co₃O₄/ZnO纳米复合物的结构和晶粒尺寸. 随着退火温度升高,Co₃O₄相逐步消失,ZnO晶粒尺寸也有显著增加. 经过1000 ℃以上退火后,Co₃O₄相完全消失,并出现了CoO的岩盐结构. 正电子湮没寿命测量显示出Co₃O₄ /ZnO纳米复合物中存在大量的Zn空位和空位团. 这些空位缺陷可能存在于纳米复合物的界面区域. 当退火温度达到700 ℃后Zn空位开始恢复,空位团也开始收缩. 900 ℃以上退火后,所有空位缺陷基本消失,正电子寿命接近ZnO完整晶格中的体态寿命值. 符合多普勒展宽谱测量也显示Co₃O₄ /ZnO纳米复合物经过900 ℃以上退火后电子动量分布与单晶ZnO基本一致,表明界面缺陷经过退火后得到消除. 关键词： ZnO 界面缺陷 正电子湮没     

中子嬗变掺杂前后Ge纳米晶的结构和性质

采用第一性原理计算模拟Ge纳米晶在中子嬗变掺杂(NTD)后受空位、O和As杂质的影响.结果表明,退火方法引入的O并不能消除纳米晶中的辐照致空位缺陷的影响,而NTD 产生的As掺杂能补偿这些空位缺陷并消除禁带中产生的杂质能级,从而改善半导体掺杂性能.计算还发现,由于较高的电负性,纳米晶中O对Ge原子较强的吸附作用阻止了空位的形成,导致与缺陷相关的非辐射发光中心的浓度减小,发光效率提高,因此中子辐照掺杂前的高温退火处理是非常有必要的.计算较好地解释了已报道的实验结果. 关键词： Ge纳米晶 中子嬗变掺杂 第一性原理 空位缺陷     

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.     

中频磁脉冲处理Fe52Co34HfTB6Cu1非晶合金的正电子湮没研究

对熔体急冷法制备的非晶合金Fe52Co34HfTB6Cu1进行了不同频率的中频磁脉冲处理,用透射电子显微镜、穆斯堡尔谱、正电子湮没寿命谱等方法研究了处理前后试样的微观结构及结构缺陷变化．结果表明,经中频磁脉冲处理后,样品发生了部分纳米晶化,晶化量随磁脉冲频率增加而增加,当磁脉冲频率为2000Hz时,晶化量达33．1％：在淬态非晶样品中,正电子在类单空位中的湮没寿命t1为150．5ps,强度,1为77．7％,在微孔洞中的湮没寿命仡为349．7ps,强度I2为22．3％;随磁脉冲频率的增加,t1,t2值呈现减小的变化趋势,与淬态非晶相比,I1有所增加,如下降,t1,t2的平均值亍大幅降低．     

铝纳米晶的低温导电特性研究

采用真空热压技术将电磁感应加热-自悬浮定向流法制备的铝纳米粉末压制成块体样品.通过X射线衍射、透射电子显微镜、扫描电子显微镜及X射线能谱分析了铝纳米晶的微观结构,并用四探针法测量了不同温度下(8—300 K)样品的电阻率,研究了铝纳米晶的电阻率(ρ)随温度的变化规律.结果表明:由于晶界(非晶氧化铝)对电子的散射以及晶界声子对电子的散射效应,低温(40 K)下,铝纳米晶的本征电阻率随温度变化关系明显不同于粗晶铝,不仅呈现出T~4变化,还表现出显著的T3变化规律.因晶界等缺陷和非晶氧化铝杂质对电子的散射,铝纳米晶残余电阻率比粗晶铝电阻率大5—6个数量级.     

利用正电子湮没技术研究钾掺杂钨合金中的缺陷

钨合金中钾的掺杂会引入大量的缺陷,如尺寸几十纳米的钾泡、高密度的位错以及微米量级的晶粒带来的晶界等,这些缺陷的浓度和分布直接影响合金的服役性能.本文运用正电子湮没谱学方法研究钾掺杂钨合金中的缺陷信息,首先模拟计算了合金中各种缺陷的正电子湮没寿命,发现钾的嵌入对空位团、位错、晶界等缺陷的寿命影响很小;然后测量了不同钾含量掺杂钨合金样品的正电子湮没寿命谱,建立三态捕获模型,发现样品中有高的位错密度和低的空位团簇浓度,验证了钾对位错的钉扎作用,阐述了在钾泡形成初期是钾元素与空位团簇结合并逐渐长大的过程;最后使用慢正电子多普勒展宽谱技术表征了样品中缺陷随深度的均匀分布和大量存在,通过扩散长度的比较肯定了钾泡、晶界等缺陷的存在.     

中频磁脉冲处理Fe52Co34Hf7B6Cu1非晶合金的正电子湮没研究

对熔体急冷法制备的非晶合金 Fe₅₂Co₃₄Hf₇B₆Cu₁ 进行了不同频率的中频磁脉冲处理, 用透射电子显微镜、穆斯堡尔谱、正电子湮没寿命谱等方法研究了处 理前后试样的微观结构及结构缺陷变化. 结果表明,经中频磁脉冲处理后,样品发生了部分纳米晶化, 晶化量随磁脉冲频率增加而增加, 当磁脉冲频率为2000 Hz时, 晶化量达33.1%; 在淬态非晶样品中, 正电子在类单空位中的湮没寿命τ₁为150.5 ps, 强度 I₁为77.7%, 在微孔洞中的湮没寿命τ₂为349.7 ps,强度I₂为22.3%; 随磁脉冲频率的增加, τ₁, τ₂值呈现减小的变化趋势, 与淬态非晶相比, I₁有所增加, I₂下降, τ₁, τ₂的平均值τ大幅降低.     

正电子湮没谱和光致发光谱研究掺锌GaSb质子辐照缺陷

用正电子湮没谱和光致发光谱研究了质子辐照后掺锌GaSb中的缺陷.通过分析正电子的缺陷寿命τ₂及强度I₂的变化发现,在高能质子的辐照下产生了双空位缺陷V_GaV_Sb,可能同时产生了小的空位团.正电子平均寿命τ_av和S参数随着质子辐照剂量的变化也证明了这一结论.通过分析不同质子辐照剂量下掺锌GaS     

JRQ and JPA irradiated and annealed reactor pressure vessel steels studied by positron annihilation

The paper is focused on a comprehensive study of JRQ and JPA reactor pressure vessel steels from the positron annihilation lifetime spectroscopy (PALS) point of view. Based on our more than 20 years’ experience with characterization of irradiated reactor steels, we confirmed that defects after irradiation start to grow and/or merge into bigger clusters. Experimental results shown that JPA steel is more sensitive to the creation of irradiation-induced defects than JRQ steel. It is most probably due to high copper content (0.29?wt.% in JPA) and copper precipitation has a major impact on neutron-induced defect creation at the beginning of the irradiation. Based on current PALS results, no large vacancy clusters were formed during irradiation, which could cause dangerous embrittlement concerning operation safety of nuclear power plant. The combined PALS, small angle neutron scattering and atomic probe tomography studies support the model for JRQ and JPA steels describing the structure of irradiation-induced clusters as agglomerations of vacancy clusters (consisting of 2–6 vacancies each) and are separated from each other by a distribution of atoms.     

Reply to ‘On substructure in titanium alloy martensite’

Thermal stability of nanocrystalline Cu prepared by compacting nanoparticles (mean grain size about 50?nm) under high pressure has been studied by means of positron annihilation lifetime spectroscopy and X-ray diffraction. A gradual increase of mean grain size in the sample is observed with an increase in ageing time at 180°C, indicating an increase of volume fraction of the ordered regions. Furthermore, during the ageing, the increase in average size of the vacancy clusters in grain boundaries is confirmed by the positron lifetime results. The recrystallization is observed at the temperature of about 180°C, and becomes significant above 650°C. Three annealing stages, which are at the intervals 180–400°C, 400–650°C and 650–900°C have been characterized by positron average lifetime. The average volume of the defects almost remains constant in the interval 400–650°C but becomes considerably smaller in the interval 650–900°C.     

Computational studies of the effect of hydrogen on the thermalized positron state in amorphous silicon

The two-component density functional theory is applied to the study of the thermalized positron state in simulated structures of hydrogenated amorphous silicon. Results show that positron properties in bulk and ad hoc defect structures are sensitive to the defect free-volume. Using the normalized positron density, it is determined that the thermalized positron state is weakly localized at hydrogen-decorated vacancy-like complexes, and not at microscopic open volume defects. These defect complexes form as clusters of hydrogen-passivated dangling bonds. It is also found that hydrogen enhances the delocalization of positron density in the simulated structures. The relevance of the present results to the interpretation of actual positron lifetime spectroscopy in real materials is discussed.     

Detection of hydrogen in neutron-irradiated nickel using positron lifetime spectroscopy

Hydrogen in nano-voids in neutron-irradiated nickel has been detected using positron annihilation lifetime spectroscopy (PALS). As positron lifetime is greatly affected by nano-voids bound with hydrogen, special attention was paid to the analysis. The positron lifetime of neutron-irradiated nickel at higher irradiation doses increased with the dose, which is an indicator for vacancy cluster (nano-void) formation in the lattice. The introduction of hydrogen in well-annealed nickel by electrical charging also resulted in an increase in positron lifetime due to vacancy formation. In neutron-irradiated nickel specimens, hydrogen charging shortened the positron lifetime from 456 to 334 ps (irradiation dose: 3 × 10^?3 dpa). Isochronal annealing behaviour of hydrogen-charged nickel and neutron-irradiated nickel was also studied. Positron trapping rate was calculated using a simple trapping model. Thermal desorption spectroscopy was used for the investigation of hydrogen behaviour in non-irradiated hydrogen-charged nickel.     

Application of positron annihilation spectroscopy on the ion implantation damaged Fe-Cr alloys

Four different Fe-Cr binary alloys with Cr content 2.5-11 wt% were studied in details using various methods. Transmission electron microscopy (TEM) and X-ray diffraction (XRD) were applied to obtain basic information, required for standard positron annihilation lifetime spectroscopy (PALS) spectra analysis. Additionally, PALS measurements were performed on as-received state as well as on helium implanted specimens. The He implantation was proposed for simulation of radiation damage and obtain high doses even in near surface areas (up to 1 μm). The implantation was based on the SRIM code simulation and next DPA calculations. Final concentration of vacancy type defects were calculated for 250 keV He²⁺ beam and the maximum was determined in 600 μm depth. Such specimens are very suitable for positron beam study of vacancy type defect mobility as a result of thermal treatment, which will be performed simultaneously in the future.     

Investigation of microstructure thermal evolution in nanocrystalline Cu

The microstructure of nanocrystalline Cu prepared by compacting nanoparticles (50-60 nm in diameter) under high pressures has been studied by means of positron lifetime spectroscopy and X-ray diffraction. These nanoparticles were produced by two different methods. We found that there are order regions interior to the grains and disorder regions at the grain boundaries with a wide distribution of interatomic distances. The mean grain sizes of the nanocrystalline Cu samples decrease after being annealed at 900 °C and increase during aging at 180 °C, which are observed by X-ray diffraction, revealing that the atoms exchange between the two regions. The positron lifetime results clearly indicate that the vacancy clusters formed in the annealing process are unstable and decomposed at the aging time below 6 hours. In addition, the partially oxidized surfaces of the nanoparticles hinder grain growth when the samples age at 180 °C, and the vacancy clusters inside the disorder regions, which are related to Cu₂O, need longer aging time to decompose. The disorder regions remain after the heat treatment in this work, in spite of the grain growth, which will be good for the samples keeping the properties of nanocrystalline material.     

The role of quenched‐in vacancies for the decomposition of aluminium alloys

The very early stages of decomposition during room temperature storage, i.e. just a few minutes after quenching, are investigated by positron annihilation lifetime spectroscopy for both an AlMgSi alloy and an AlCuMg alloy. It turns out that by freezing the decomposition kinetics during measurements we can detect vacancy–solute atom pairs. The formation of larger solute clusters with structural vacancies is seen by an increase of the mean positron lifetime in the course of storage at room temperature (RT). Earlier findings concerning aging at RT were unable to discover this effect. The detected changes are interpreted in terms of cluster formation. Thus we show that positron annihilation spectroscopy (PAS) is one of the very few methods to access early stages of decomposition in metallic alloys. Moreover, the lower limit of the concentration of quenched‐in vacancy‐like defects is calculated to be at least 2 × 10^–5 per atom. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Divacancy complexes induced by Cu diffusion in Zn-doped GaAs

Positron annihilation spectroscopy was applied to investigate the nature and thermal behavior of defects induced by Cu diffusion in Zn-doped p-type GaAs crystals. Cu atoms were intentionally introduced in the GaAs lattice through thermally activated diffusion from a thin Cu capping layer at 1100 °C under defined arsenic vapor pressure. During isochronal annealing of the obtained Cu-diffused GaAs in the temperature range of 450?850 K, vacancy clusters were found to form, grow and finally disappear. We found that annealing at 650 K triggers the formation of divacancies, whereas further increasing in the annealing temperature up to 750 K leads to the formation of divacancy-copper complexes. The observations suggest that the formation of these vacancy-like defects in GaAs is related to the out-diffusion of Cu. Two kinds of acceptors are detected with a concentration of about 10¹⁶ ? 10¹⁷ cm^?3, negative ions and arsenic vacancy copper complexes. Transmission electron microscopy showed the presence of voids and Cu precipitates which are not observed by positron measurements. The positron binding energy to shallow traps is estimated using the positron trapping model. Coincidence Doppler broadening spectroscopy showed the presence of Cu in the immediate vicinity of the detected vacancies. Theoretical calculations suggested that the detected defect is V _Ga V _As-2Cu_Ga.     

A study of defects in deformed FeSi alloys using positron annihilation techniques

Steels with high amounts of silicon are used in electrical applications due to their low magnetostriction, high electrical resistivity and reduced energy losses, but they exhibit poor formability. The slow positron beam of Gent is used to investigate defects in different deformed FeSi alloys. It was found that the concentration of defects for the alloys deformed at high temperatures are different from the ones related to the alloys deformed at room temperature. These results are correlated to the results of positron annihilation lifetime spectroscopy (PALS).     

Computed positron lifetimes in vacancies and vacancy-iron clusters in gold

Annihilation characteristics are calculated for positrons trapped in clean and impurity decorated vacancy clusters in Au. The positron lifetime depends strongly on the structure of the clusters. In a strongly relaxed vacancy cluster, the lifetime can become smaller than the lifetime in a single vacancy. The substitution of some neighbour atoms of a vacancy cluster by Fe atoms has only a minor effect on the positron lifetimes.