用于原位小角X射线测量的可变温液体样品槽的研制  

A variable temperature tank for solution SAXS in-situ measurement at BSRF

作　　者：王成龙[1,2] 刘光华[1] 韩海姣 吴忠华[2] 默广[2] 

机构地区：[1]天津工业大学,天津300387 [2]中国科学院高能物理研究所,北京100049

出　　处：《核技术》2016年第10期12-16,共5页Nuclear Techniques

基　　金：国家自然科学基金(No.11305198;No.U1332107;No.U1532105);煤炭资源与安全开采国家重点实验室开放课题(No.SKLCRSM14KFA02);绿色催化与分离北京市重点实验室资助~~

摘　　要：根据小角X射线散射(Small angle X-ray scattering,SAXS)技术特点和北京同步辐射装置1W2A小角站光源参数,设计了一款用于液体样品原位变温测试的样品槽。该样品槽采用双面变温方式使样品温度整体均匀,涵盖5-95oC较宽温度范围;待测溶液厚度不仅可根据溶液组分进行调节,且在变温过程中保持恒定,利于提高数据质量。通过设计,实现了待测溶液和背底溶液同时变温和交替测量,节省了宝贵的同步辐射机时。ANSYS热分析表明,设备结构设计合理,样品处温度精度通过校正能得到进一步提高。通过检测聚酰胺-胺(Polyamidoamine,PAMAM)树形大分子结构随温度的变化,表明该样品槽满足液体原位变温SAXS测试要求。Background： Nano-scale structure in solutions can be studied by small angle X-ray scattering （SAXS） techniques at synchrotron radiation facilities. For solution samples, no suitablein-situ variable temperature tank is available to meet the Beijing Synchrotron Radiation Facility （BSRF） 1W2A station’s requirements.Purpose： This study aims to develop anin-situ variable temperature tank for solution samples according to the special requirements of SAXS and light parameters of 1W2A station at BSRF.Methods： The liquid samples are heated from both sides to reach a uniform status from 5 oC to 95 oC. The solution thicknesses can be adjusted according to their compositions and can maintain a constant during the heating process, which is helpful to increase the data quality. The sample and corresponding background diluent are heated or cooled simultaneously and can be measured alternately. ANSYS was employed to verify the proper structure of the tank.Results： Thermoanalysis results show the rational design of this liquid sample tank, and the temperature was further calibrated for high precision. The structural changes of polyamideamine with temperature were measured using this tank.Conclusion： The proposed variable temperature tank meets the requirements of SAXSin-situ measurements for solution samples at BSRF. All expected functionalities have been satisfied.

关 键 词：小角X射线散射 样品槽 温度校正 

分 类 号：TL99[核科学技术—核技术及应用]