Kikuma Jun, Tsunashima Masamichi, Ishikawa Tetsuji, Matsuno Shin-ya, Ogawa Akihiro, Matsui Kunio, Sato Masugu
Analysis and Simulation Center, Asahi-KASEI Corporation, Japan.
J Synchrotron Radiat. 2009 Sep;16(Pt 5):683-6. doi: 10.1107/S0909049509022080. Epub 2009 Jul 2.
Hydrothermal formation of tobermorite from a pre-cured cake has been investigated by transmission X-ray diffraction (XRD) using high-energy X-rays from a synchrotron radiation source in combination with a newly designed autoclave cell. The autoclave cell has a large and thin beryllium window for wide-angle X-ray diffraction; nevertheless, it withstands a steam pressure of more than 1.2 MPa, which enables in situ XRD measurements in a temperature range of 373 to 463 K under a saturated steam pressure. Formation and/or decomposition of several components has been successfully observed during 7.5 h of reaction time. From the intensity changes of the intermediate materials, namely non-crystalline C-S-H and hydroxylellestadite, two pathways for tobermorite formation have been confirmed. Thus, the newly developed autoclave cell can be used for the analyses of reaction mechanisms under specific atmospheres and temperatures.
利用同步辐射源产生的高能X射线，结合新设计的高压釜单元，通过透射X射线衍射（XRD）研究了由预固化饼状材料水热生成雪硅钙石的过程。该高压釜单元有一个用于广角X射线衍射的大而薄的铍窗；尽管如此，它能承受超过1.2 MPa的蒸汽压力，这使得在饱和蒸汽压力下，能在373至463 K的温度范围内进行原位XRD测量。在7.5小时的反应时间内，已成功观察到几种组分的形成和/或分解。根据中间材料即非晶态C-S-H和羟硅钙石的强度变化，已确认了雪硅钙石形成的两条途径。因此，新开发的高压釜单元可用于分析特定气氛和温度下的反应机理。
