Investigation of the growing surfaces of crystal by X-ray scattering at small glancing angle incidence

A compact ultrahigh-vacuum X-ray diffractometer was designed and constructed using a small rotating-anode X-ray source of 18 kW。Its UHV specimen chamber is 200 mm high and 140 mm in diameter and can be evacuated up to 3*10^\-8> Pa。X射线穿过一个薄薄的窗户进入了房间，直径为0.2毫米厚和30毫米。发散和散射的X射线通过另一个窗口取出，0.4毫米厚，60毫米直径。所有设备、一个旋转阳极X射线源、一个单位单色仪和一个双圈差计都安装了超高压规格室和一个传统的闪烁计数器，只布置在一个光学表上，宽70厘米，长90厘米。腔室内特殊持有者的配置，是为目前的表面眩光角度分布设计的，可以从真空室外进行控制。超高压室有两个蒸发细胞，用于制剂准备和一个加热器，使制剂关闭。这一安排允许我们在不断增长的晶体表面的原位观测中进行，根据沉积角度X射线散射方法的含义，对机械抛光的银多晶体表面的亮度进行了初步实验，给出了一个顺序为10^3计数·秒^<-1>的散射X射线强度在其特定反射角度，足以产生表面结构的显著解释，下一个实验是估计PbSe的增长表面（111）是由X射线散射方法的度量。我们成功地在PbSe的分层对分层生长的原位观测中（111）通过表面X射线散射，使用18千瓦的小旋转阳极X射线源的X射线。

A compact ultrahigh-vacuum X-ray diffractometer was designed and constructed using a small rotating-anode X-ray source of 18kW.Its UHV specimen chamber is 200mm high and 140mm in diameter and can be evacuated up to 3*10^<-8> Pa. The X-ray is incident into the chamber through a thin Be window, 0.2mm thick and 30mm in diameter. Diffracted and scattered X-rays are taken out through another Be window, 0.4mm thick and 60mm in diameter. All the equipments, a rotating-anode X-ray source, an incident monochromator, and a two-circle diffractometer onto which a UHV specimen chamber and a conventional scintillation counter are mounted, are arranged on only one optical table, 70cm wide and 90cm in length. Configuration of the specimen holder in the chamber, which is designed for the surface glancing angle scatterings at present, can be controlled from outside of the vacuum. The UHV chamber has two evaporation cells for specimen preparation and a heater to anneal the specimen. This arrangement allows us to perform in situ observations of the growing crystal surfaces during the deposition by means of glancing angle X-ray scattering method.A preliminary experiment of the glancing angle scattering of mechanically polished silver polycrystal surfaces gave an order of 10^3 count・sec^<-1> of scattered X-rays intensity at its specular reflection angle, which is enough to derive a significant interpretation of the surface structure.The next experiment was estimation of the growing surface of PbSe (111) by means of glancing angle X-ray scattering method. We success to perform in situ observation of layr-by-layr growth of PbSe (111) by surface X-ray scattering with the use of X-ray from the small rotating-anode X-ray source of 18kW.