Development of 3-D DX-ray Analytical Microscope and micro-nano analysis under actual environment

利用多毛细管X射线透镜，研制了微型X射线荧光检测仪。这种多毛细管X射线透镜使我们能够产生几十微米的微束X射线，从而对微区进行元素分析。利用该仪器进行了以下几个方面的研究：1)可变面积的元素x射线测绘多毛细管透镜得到的光斑大小与距透镜输出端的距离密切相关。因此，可以通过改变与镜头的距离来改变光斑大小。因此，我们提出了大面积可以用大光斑来测量，而小面积可以用小光斑来测量。2)藜麦种子X射线荧光元素图谱具有独特的优势：在常压条件下(即不需要高真空条件)进行无损元素分析。这一优点对活体样品的分析非常有帮助，因为活体样品不能在真空条件下安装。因此，我们拍摄了藜麦种子在生长过程中在环境空气压力下的X射线元素图。将种子放在样品架上的棉花上，样品架的一端放入水箱中，这样种子就可以在X射线测量过程中生长。结果发现，K从种子向茎中迁移，而Ca在种子生长过程中仍留在种子中。3)显微XRF和原子力显微镜的结合使我们能够获得原子水平的表面形态，但很难提取化学信息，即元素的区分。因此，将原子力显微镜和X射线荧光技术结合起来是非常有吸引力的。实际上，我们证明了组合仪器工作良好。4)三维XRF仪器我们制备了两个多毛细管透镜用于激发和检测。通过将两个透镜的焦点精确地调整在一个位置，就可以在三维空间中分析一个小区域。我们已经对这种技术进行了研究。

By using a polycapillary x-ray lens, micro-XRF instrument was developed. This polycapillary x-ray lens enables us make a micro x-ray beam of about several tens micro meters, leading to elemental analysis of micro region. Using this instrument, following research subjects were studied :1) Elemental x-ray mapping with changeable areaThe spot size obtained by polycapillary lens critically depends on distance from the output end of the lens. Therefore, it is possible to change the spot size by changing the distance from the lens. Thus, we proposed that a large area could be measured a large spot size, while a small area could be measured by a small spot size. BY using this technique, a total measuring time could be reduce,2) Elemental mapping of quinoa seedXRF has unique advantages : non-destructive elemental analysis at ambient air pressure (that is, high vacuum conditions are not required). This advantages are very helpful for analysis of living sample, because the living sample cannot be installed in vacuum condition. Thus, we took the x-ray elemental maps for quinoa seed at ambient air pressure during growth. The seed was put on the cotton on the sample holder, whose end was put into the water tank ; therefore, the seed could grow up during the x-ray measurement. As a result, it was found that K moved from the seed to stem, while Ca still remained in the seed during the growth.3) Combination of micro XRF with AFMAFM (atomic force microscope) enables us take surface morphology with atomic level ; however, it is difficult to take chemical information, that is, distinguish of elements. Therefore, it is very attractive to combine AFM and XRF. Actually, we demonstrated that the combined instrument worked well.4) 3-D XRF instrumentWe prepared two polycapillalry lens for excitation and detection. By adjusting the focusing points of two lens exactly at one position, it is possible to analyze a small region in 3 dimensional space. We have investigated this technique.