射线探测用碲锌镉晶体及其器件研究

采用改进的布里奇曼(B ridgm an)方法进行锌组分为0.15碲锌镉(Cd0.85Zn0.15Te)晶体的生长。通过严格控制晶体生长过程中Cd的蒸气分压,使得所生长的碲锌镉晶体在结晶质量方面达到了较好的水平。对其性能进行测试,红外透射比T>60%、沉积相密度<1×104/cm2、位错腐蚀坑密度DEPD<6×104/cm2、X射线衍射双晶回摆曲线半峰全宽FWHM<20 arcsec、电阻率ρ>1010Ω.cm。利用所生长的晶体初步制作了平面型单元碲锌镉射线探测器,所用晶体的尺寸为5 mm×5 mm×2.5 mm,制成的探测器在室温下对125I和241Am放射源进行了探测测量。对125I放射源,探测出了强度为74.5%的27.5 keV的γ射线特征峰,不能仔细分辨出强度为39.8%的27.2 keV的γ射线特征结构;对241Am放射源,探测出了59.5 keV的γ射线特征峰,分辨率优于6 keV,半峰全宽FWHM<10%,同时还能检测出Te、Cd的X射线逃逸的混合峰以及241Am低能Te-K系、Np-L系的两个X射线特征峰。     

一种基于热释电效应的X射线荧光分析谱仪

利用热释电晶体实现了一个X射线激发源,并以此激发源和高能量分辨率的硅漂移探测器构建了一个X射线荧光分析谱仪。首先通过分析计算热释电晶体厚度和靶厚度对产生X射线的影响选定了激发源的设计参数;然后测量了激发源发射的X射线本底,其能量范围在1～27 keV,包含有Cu和Ta的特征X射线,最大强度在每秒3 000个计数以上,对本底的测量同时显示出谱仪的探测器部分对Cu的8.05 keV特征峰的分辨率达到210 eV,具有很高的能量分辨率;最后使用该谱仪测试了Fe,Ti和Cr等三种单质样品和高钛玄武岩样品,测试结果表明该谱仪可以有效的分析出样品的元素成分。由于这种X射线荧光分析谱仪的各组成部分体积都很小,进一步便携化后非常适合于非破坏、现场和快速的元素分析场合。     

109Cd源激发的X射线荧光法无创伤测定人体骨铅含量

建立了用以体内测定骨铅含量的109Cd源作为激发源的X射线荧光测量系统. 该系统采用高纯锗探测器(10 mm×7 mm), 检测人体胫骨中铅被109Cd的88.0 keV的γ射线激发后产生的特征K层X射线. 采用铅的K层X射线对相干散射归一化的方法, 根据铅的K层X射线强度与相干散射强度的比值对胫骨模型铅含量之间的校正曲线, 便可得到人体骨铅的含量. 这种归一化的方法, 使测量结果的精确度不受骨外组织层厚度、骨的形状、大小、密度以及被测者位移的影响. 用含铅石膏制作的一组胫骨模型得到的校正曲线呈现良好的线性关系. 对急性铅中毒工人的试验性测量结果表明, 他们的骨铅含量明显高于对照组.     

微颗粒X射线荧光强度MCNPX模拟与WDXRF实验

为研究样品微颗粒在X射线荧光(XRF)分析中对测量结果的影响,运用蒙特卡罗模型MCNPX对X射线荧光仪进行建模,研究了样品颗粒粒径对X射线荧光特征峰强度、峰总比和源峰探测效率的影响,并设计波长色散X射线荧光光谱法(WDXRF)分析实验对模拟结果进行了检验。结果表明：对于样品微颗粒X射线荧光强度与粒径尺寸的关系,MCNPX模拟值与理论计算值保持一致;MCNPX模拟结果与WDXRF实验结果存在一定差异,这取决于MCNPX模型对待测样品状态的假设与实际情况存在一定的差异性;运用样品粉碎、研磨至小颗粒并进行压片处理的办法,可使WDXRF实测结果尽可能的减小与MCNPX理论模拟结果的差异性;在待测样品的颗粒粒径达到一定尺寸时,其峰总比、源峰探测效率、特征峰X射线荧光计数均趋于稳定值;颗粒粒径在某一特定尺寸范围之内,颗粒度效应的影响不容忽视;除此之外,颗粒度效应的影响基本可以忽略。论文充分考虑了待测样品颗粒粒径对XRF分析结果的影响,为减小因颗粒度效应引起分析结果的不确定性提供了一种可行的研究思路,该方法也可为X射线分析的生产实践提供一定的技术参考。     

硬X光弯晶谱仪的定量化标定方法

介绍了具有定量化测量能力的硬X光弯晶谱仪的结构, 利用Mo靶X光管的K特征线作为标定源, 使用绝对标定过的Si(Li)探测器对X光管出射的特征线谱进行强度和谱测量。结合X光管空间分布均匀的特点, 计算进入弯晶谱仪的光子数目, 采取了特征谱扣去轫致谱的计数处理方法, 得到了17 keV和19 keV处弯晶谱仪的绝对效率, 分别为4.3210-4和3.9410-4。     

Chemical Effect on K Shell X-ray Fluorescence Parameters and Radiative Auger Ratios of Co, Ni, Cu, and Zn Complexes

对钴、镍、铜、锌元素组成的不同配合物K壳层X射线的产生截面、谱线强度比、俄歇辐射强度比进行了测定,同时研究了化学效应对K壳荧光参数和俄歇辐射强度比的影响,并根据电荷转移过程解释了这些参数的变化. 采用59.5 keV的γ射线²⁴¹Am的环形放射源对样品进行激发. 用分辨率为150eV的Ultra-LEGe探测器在5.9 keV测定样品产生的K壳X射线.     

Influence of Chemical Effect on the Kβ/Kα Intensity Ratios and KβEnergy Shift of Co, Ni, Cu, and Zn Complexes

报导了钴、镍、铜、锌络合物中的化学效应对Kβ/Kα强度比和Kβ能量位移的影响. 实验样品用241Am环状放射源发出的能量为59.5 keV的γ射线激发. 对样品发射的K段X射线进行检测的检测器在5.9 keV处的分辨率为150 eV. 观察了不同配体对钴、镍、铜、锌络合物的Kβ/Kα强度比和Kβ能量转移的影响,并试图解释这些配体的性质对中心原子产生的化学效应. 对实验得到的Kβ/Kα强度比数据,理论计算获得的Kβ/Kα强度比数据及其它实验得到的纯钴、镍、铜、锌的Kβ/Kα强度比数据进行了比较.     

PLXE、次级靶和放射性同位素源能量色散X射线光谱技术在微量元素分析方面的比较研究

能量色散X射线光谱分析技术广泛地应用于各种样品中微量元素的分析。但分析灵敏度在很大程度上取决于所采用的激发方法。本文试图对三种常用的激发方法在微量元素分析方面的潜力作一初步的评价。质子激发X射线发射(PIXE)分析和次级靶X射线能散分析系作者在美国加州大学劳伦斯实验室所作。放射性同位素源X射线能散分析数据部分引自文献,部分系从一台国内自己发展的系统上获得。用于比较分析的标准参考样品包括NBS的SRM157(果树叶)、SRM1577(牛肝藏)、SRM1633(煤飞尘)和USGS的标准岩石样品G-2、AGV-1、BCR-1和PCC-1。结果表明,在原子序数为30—40的范围内对一特定样品PIXE给出最佳的峰/背景比值。在该范围内PIXF可很容易获得0.5—1ppm的探测限,而其余二种方法通常能达到的探测极限为2—10ppm。但就较宽的范围来说PLXE并不见得明显地优于其它二种方法。事实上,在轻元素范围内PIXE的高X射线产额部分地被在该范围内较高的二次电子的轫致辐射背景所抵销,而在较高原子序数范围内PIXE的X射线产额急剧地下降。当在某些场合下能满足最佳激发条件时,次级靶的激发灵敏度常优于PIXE。放射性同位素源通常认为灵敏度较差,因为其光子发射通量较低,且可供选择的激发能量有限。但目前获得高强度的各种能量的放射性同位素已不是一件难事。当计数时间足够长时(1小时以上)75毫居的~(109)Cd源可激发出与Mo二次靶相当的峰/背景比值;150毫居的~(241)Am源可激发出明显可辨的～10ppm的BaK峰。~(238)Pu和~(55)Fe源在相应能量范围也可达到与二次级靶相当的效果。当然这是以牺牲测量时间为代价的。看来,对于能散X射线微量分析来说采用带Ti、Mo(或Ag)和Sm(或Ce)等次级靶的系统是最敏灵佳的选择。采用PIXE仅当样品量和大小为主要考虑时,或对中等原子序数的元素的分析度有较高要求时才有意义。放射性同位素源激发仍不失为一种有吸引力的方法,当时间和效率不作为一主要因素考虑时仍是值得采用的,这是因为其操作简单,结构紧凑,无须维护性能稳定而且价格低廉,     

样品厚度对薄膜法X射线荧光光谱测量的影响研究

分别以富集有Cr,Pb和Cd三种元素的尼龙薄膜样品及玻璃纤维滤膜为研究对象,采用滤膜叠加的方式,通过XRF光谱仪测量不同样品厚度下薄膜样品的XRF光谱,根据测得的尼龙薄膜样品中Cr,Pb,Cd元素及玻璃纤维滤膜中Ca,As和Sr元素特征XRF性质的变化,研究样品厚度对薄膜法XRF光谱测量的影响。结果表明：薄膜样品厚度对不同能量区间上元素特征谱线荧光性质的影响并不相同。元素特征谱线能量越大,元素特征X射线荧光穿透滤膜到达探测器的过程中损失越少;但由薄膜样品厚度增加引起的基体效应却越强,相应特征谱线位置处的背景荧光强度就越大,因此样品厚度增加所引起的基体效应对薄膜法XRF光谱测量的灵敏度影响就越大。对于特征谱线能量较低(能量小于7 keV)的元素,以增加薄膜样品厚度的方式来增加待测组分的质量厚度浓度,并不能有效地提高薄膜法XRF光谱测量的灵敏度;对于特征谱线能量较高的元素(能量＞7 keV),可以通过适当增加样品厚度以增加被测组分的质量厚度浓度的方式来提高XRF光谱测量的灵敏度,薄膜样品厚度在0.96～2.24 mm内,更有利于XRF光谱的测量与分析。该研究为大气及水体重金属薄膜法XRF光谱分析中薄样制备及富集技术提供了重要的理论依据。     

不同动能的~(129)Xe~(26+)与Au表面作用产生的X射线谱

测量了动能为350—600 keV和1.8—3.9 MeV的129Xe26+入射Au表面产生的X射线谱.结果表明,350—600 keV的Xe26+仅激发出了Au的Mα特征X射线,而1.8—3.9 MeV的Xe26+可激发出Au的Mζ,Mα,Mγ和Mδ特征X射线.分析了X射线强度和产额比与入射离子动能的关系,并估计了Xe26+激发Xe的L-X射线的动能阈值.     

钒钛磁铁矿样品主、次元素的快速分析方法研究

采用SI-PIN半导体探测器、241Am激发源和2048通道分析器及自行研制的SI-PIN 2000便携式X荧光分析仪,对钒钛磁铁矿直接粉末样品中Ti,V,Cr,Mn,Fe,Co,Ni,Cu等8个主、次元素进行了分析应用研究。文章叙述了所采用的直接粉末样品法的样品盒结构、基体校正的α系数计算方法、重叠干扰校正原则和漂移校正的方法,并且给出了所选择的分析条件和样品制备方法,分析过程简单、结果准确、分析速度快,特别适应矿山、冶金的生产原料分析需要,有良好的应用前景, 与封闭正比计数器X射线荧光分析仪相比,检出限降低了1个数量级。     

Si（Li）谱仪测定X射线荧光谱中CrKβ谱线化学位移的探索

采用放射源＾２４１Ａｍ５９．６ｋｅＶγ射线分别激发金属Ｃｒ、Ｃｒ２Ｏ３和Ｋ２ＣｒＯ４，用Ｓｉ（Ｌｉ）谱仪比较测量其Ｋｘ射线的能量。实验表明Ｋ２ＣｒＯ４和ＣｒＫβ能峰相对于金属Ｃｒ有２．１２±０．２７ｅＶ的位移。     

Determination of elements in some lichens growing in Giresun and Ordu province (Turkey) using energy dispersive X-ray fluorescence spectrometry

The concentration of five different elements in six lichens species of different regions in Giresun and Ordu (Turkey) was determined using the energy dispersive X-ray fluorescence method. A radioisotope excited X-ray fluorescence analysis using the method of multiple standard addition is applied to the elemental analysis of lichens. An annular 50 mCi ²⁴¹Am radioactive source and an annular 50 mCi ⁵⁵Fe radioactive source were used for excitation of characteristic K X-rays. An Si(Li)detector which has a 147 eV full-width at half-maximum for 5.9 keV photons was used for intensity measurements. A qualitative analysis of spectral peaks showed that the samples contained potassium, calcium, titanium, iron, and barium.     

Analytical performance of Compton/Rayleigh signal ratio by total reflection X-ray fluorescence (TXRF): A potential methodological tool for sample differentiation

The high sensitivity Compton and Rayleigh X-ray scattering signals can be used to gain valuable information on the chemical composition of various matrices, by exploiting the ratio of those signals as a function of the effective atomic number (Z_eff). Neither total reflection X-ray fluorescence (TXRF) nor the effect of the experimental setup, including sample preparation, X-ray excitation source selection, and band deconvolution procedure, has been assessed in this kind of approach. Here, a Compton/Rayleigh ratio and Z_eff-based TXRF method was set up and tested as an analytical tool for milk samples differentiation. The method was developed using a 90° scattering angle and assessed using different X-ray excitation sources: a molybdenum tube (Mo Kα 17.5 KeV) and a tungsten tube (W Lα 8.5 KeV and W-Brems 35 KeV). The evaluation of independent Compton and Rayleigh signals was performed by non-Gaussian and Gaussian curve resolution methods, and both height and area-based calculations were evaluated. Different sample preparation conditions were assessed. By using 11 standard materials, a calibration curve for Compton/Rayleigh ratio versus Z_eff was established. The method was tested to determine the Z_eff of milk samples, which enabled its use as a parameter to differentiate them. Good precisions were obtained with the Mo excitation source and the area-based calculations, which allowed to differentiate undiluted milk samples by species, treatment, and fat content according to their Compton/Rayleigh ratio. This simple and rapid method has the potential to be used for the differentiation of various types of samples, including liquids, solids, and aerosols.     

Measurement of the K shell X-ray production cross-sections and fluorescence yields for Nd,Eu, Gd,Dy and Ho using radioisotope X-ray fluorescence in the external magnetic field

The effect of external magnetic field on the K_α and K_β X-ray production cross-sections and K shell fluorescence yields for ferromagnetic elements Nd, Gd and Dy and paramagnetic elements Eu and Ho have been measured at the excitation energy of 59.5 keV γ -rays from ²⁴¹Am radioactive source of strength 100 mCi in the external magnetic field of intensities ±0.75 T. Furthermore, I_Kβ /I_Kα intensity ratios for these elements have been measured in the external magnetic field. The K X-rays from different targets were detected using a high resolution Si(Li) semiconductor detector. For B = 0, the measured K X-ray production cross-sections, K shell fluorescence yields and the I_Kβ /I_Kα intensity ratios were compared with the experimental and theoretical data in literature. The results have shown that the fluorescence parameters as photoionization cross section, fluorescence yield, radiation rates and spectral linewidth can change when the irradiation is conducted in a magnetic field.     

The Investigation of K Shell X-Ray Fluorescence Parameters for Sulphur Atom in Different 1 ,2,4-Triazoles

The measurement of K shell fluorescence parameters is an easy and practical way to investigate the electronic structures of elements in alloys,compounds or complexes.Since the number of valence electrons will change the screening effect,the measured parameters will be affected from the changes.In this study,the measured parameters were investigated for sulphur element according to the number of CH_2 groups.For the experimental measurements,the samples were excited by 59.5keVγrays from a 241 Am annular radioactive source.The emitted K X-rays from the samples were counted by ab Ultra-LEGe detector with a resolution of 150 eV at 5.9keV.     

Development of a K‐shell x‐ray fluorescence measurement of cadmium in bone

Cadmium is known to accumulate in the human body and chronic exposures have been clearly linked to adverse health effects, showing the kidney as the critical target organ. However, there is evidence of an association between extensive environmental exposure to cadmium and alterations in bone/calcium metabolism. Therefore, it is desirable to be able to measure bone cadmium non‐invasively in humans. Tibia was selected as a measurement site and source‐excited K‐shell x‐ray fluorescence was investigated both experimentally and computationally. Initially the 88 keV γ‐rays from ¹⁰⁹Cd were used to assess minimum detectable level (MDL) of cadmium in phantoms comprising plaster of Paris (bone) and wax (soft tissue). An MDL of 3–4µg g^?1 was achieved for overlying tissue thicknesses of up to 5 mm. Alternative sources were ¹²⁵I and ²⁴¹Am. Monte Carlo simulation showed that the spectral contrast for ¹²⁵I would be poor. The 60 keV γ‐rays from ²⁴¹Am were more promising, provided that the 26 keV γ‐rays were filtered out. Experiments with ²⁴¹Am confirmed that a lower MDL could be achieved. However, the product of MDL and square root of dose (a figure of merit) was not improved. Since effective doses for these source‐excited x‐ray fluorescence procedures are low (typically of the order of 0.1 µSv or less), it may be that lower MDL would be preferred over lower dose. Nevertheless, development continues as a further reduction in MDL is highly desirable. Copyright © 2005 John Wiley & Sons, Ltd.     

A comparative study on determination of uranium and thorium in their mixed oxides by EDXRF using tube and radioisotope X‐ray sources

Studies on the matrix effects of uranium and thorium on the determinations of each other in their mixed oxides using energy dispersive X‐ray fluorescence (EDXRF) spectrometry with tube and radioisotope excitations of U Lα and Th Lα are reported. An internal standard method for the determination of uranium and thorium in these mixed oxides is found suitable. Comparison of the analytical results of EDXRF determinations of uranium and thorium using tube and radioisotope excitation sources has been made. The analytical methodology involves preparation of mixed oxide calibration/sample mixtures of uranium and thorium oxides, mixing of internal standard yttrium in these mixtures, pelletizing the mixtures after thorough mixing and grinding using boric acid binder and measuring EDXRF spectra of the specimens thus prepared using Rh X‐ray tube as well as ¹⁰⁹Cd radioisotope source. The samples were analyzed for uranium and thorium on the basis of the calibration plots obtained by plotting the intensity ratios of the analyte and internal standard characteristic X‐ray lines and their corresponding amount ratios. An average precision of 1.2% (1 s RSD) was observed for the determination of U and Th and the results deviated from the corresponding expected values by 3% on average. Due to the refractory nature of thorium oxide, comparatively more grinding time was required for thorium determinations. Copyright © 2011 John Wiley & Sons, Ltd.     

基于虚拟刻度原理对放射性体源效率刻度方法的发展

采用蒙特卡罗模拟计算的方法,标定能够适用于不同HPGe探测器上的体源虚拟点源位置,需要对点源、体源的探测效率进行模拟计算。通过 241Am、137Cs、60Co点源和体源研究了HPGe晶体尺寸、类型对它们的虚拟点源位置的影响,模拟结果表明241Am虚拟点源位置随着探测器尺寸、类型的不同呈现明显的差异性,说明虚拟刻度原理对于探测器表面的小体积样品测量在低能区间是不可取的,最后采用 137Cs、60Co源得出体源高度与虚拟点源位置的半经验公式。通过实验室两台HPGe探测系统对尺寸Φ70 mm×65 mm标准土壤体源的探测效率进行计算,与模拟探测效率值、虚拟点源效率表征结果对比分析,验证了拟合一组表征虚拟点源位置的半经验公式是可行的。实验结果表明,对$\gamma $能量区间在300~2 000 keV进行体源的虚拟刻度时,选择可靠的定标源即可建立体源和虚拟点源位置的关系。这为解决监测工作中样品与探测器之间重复进行探测效率校准的问题提供了新的途径。