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Continuous Flow for Materials Synthesis, Assembly & Crystallisation at Diamond: Discovery & Delivery of High Value Materials

材料合成、组装的连续流程

基本信息

批准号：
1792175
负责人：
金额：
--
依托单位：
University of Bath
依托单位国家：
英国
项目类别：
Studentship
财政年份：
2016
资助国家：
英国
起止时间：
2016 至无数据
项目状态：
已结题

来源：
https://gtr.ukri.org/projects?ref=studentship-1792175
关键词：
Continuous Flow Materials Synthesis Assembly

项目摘要

The first stage of the Project will involve the development and installation of a descoped version of the Kinetically Regulated Automated Input Crystalliser device. The initial experimental work will target flow crystallisation of polymorphic molecular materials on Diamond's I11 beamline, while as part of the KRAIC devise development, immediate needs for adaptation to alternative beamlines will also be taken into account. Segmented flow, as implemented in the KRAIC devices, by nature operates at steady state ensuring all reactants experience the same conditions throughout the reactor. This means that for any point of the reactor length each passing slug is at the same stage of reaction/crystallisation enabling in-depth investigations into transient events such a polymorphic transitions. To develop the initial KRAIC device concept, the Parties have partnered with the Kapur and Meldrum groups at the University of Leeds who have pioneered in-situ power X-Ray Diffraction analysis using microfluidic devices with experience at both ESRF and Diamond. In a segmented flow environment each droplet of crystallisation solution is small and the flow rate means it is not possible to observe crystallisation in-situ with labsource diffractometers; this will be overcome by the use of the high flux available on Diamond beamlines. The KRAIC device mesoscale segmented flow crystalliser constructed at the University in collaboration with the University of Leeds, will be installed at Diamond's I11 beamline, incorporating viewing windows that can be accessed by vertical alignment of the mobile stage.A cooling crystallisation of the target polymorphic cocrystal system urea: barbituric acid will be performed using heated feed vessels and insulating coil holders. Segmentation of the methanol solution is achieved by addition of both inert carrier fluid (PFPE) and air with a crosspiece mixer ensuring plug flow and thus steady state operation. The slugs of solution then pass through coils of Fluorinated Ethylene Propylene tubing joined by a 3D printed viewing section with PTFE lined Kapton windows. The viewing section is placed in between two alternately ascending tubing coils such that the flow of solution passes it at regular intervals. This will enable us to direct the beam through various points of the crystalliser length remotely by vertical positioning of the large goniometer stage (+5 cm zaxis) in the second hutch of Diamond's I11 beamline (EH2). As the passing slurries are continually being replaced by new slurries, the X-ray Damage to each crystallite is minimised and long acquisition times can be possible if necessary.With the proposed acquisition time an amalgamated powder X-ray Diffraction pattern will be obtained for set points along the crystalliser length. Repeat experiments at set points will confirm steady state operation of segmented flow optimisation. A transition of UBA III to UBA I is expected over time/crysatalliser length especially at low flow rates. Online X-Ray monitoring of flow crystallisation processes is an exciting new area and use of mesoscale crystalliser in examining crystal structure evolution is hitherto unprecedented. The development of this technique could offer opportunities not just for the elucidation of crystallisation processes but also high throughput materials discovery. By using a flow crystalliser with multiple feeds a high range of permutations such as reactant ratio, pH and concentration can be very quickly evaluated using minimal material. There has been some work towards this goal but online X-Ray analysis of assays has yet to be realised.From this beginning the KRAIC device concept and its application across switchable function materials and target polymorphic systems will be explored. As the project evolves, the adaptation of alternative continuous crystallisation and materials assembly platforms will also be persued and assessed for deployment.

该项目的第一阶段将涉及开发和安装动力学调节自动输入结晶器设备的缩小版本。最初的实验工作将针对Diamond的I11光束线上多晶型分子材料的流动结晶，而作为KRAIC设计开发的一部分，也将考虑到适应替代光束线的迫切需要。在KRAIC装置中实施的分段流本质上在稳态下操作，确保所有反应物在整个反应器中经历相同的条件。这意味着，对于反应器长度的任何点，每个通过的段塞都处于相同的反应/结晶阶段，从而能够深入研究瞬态事件，例如多晶型转变。为了开发最初的KRAIC设备概念，缔约方与利兹大学的Kapur和Meldrum小组合作，他们率先使用ESRF和Diamond的微流体设备进行现场功率X射线衍射分析。在分段流动环境中，结晶溶液的每个液滴都很小，并且流速意味着不可能使用Labsource衍射仪原位观察结晶;这将通过使用Diamond光束线上可用的高通量来克服。KRAIC装置中尺度分段流动结晶器在大学与利兹大学合作建造，将安装在钻石的I11光束线，纳入观察窗口，可以通过垂直对齐的移动的阶段访问。目标多晶共晶系统尿素的冷却结晶：巴比妥酸将使用加热的进料容器和绝缘线圈架进行。甲醇溶液的分割是通过添加惰性载液（PFPE）和空气与十字混合器，确保活塞流，从而稳定状态操作。然后，溶液的小块通过氟化乙烯丙烯管的线圈，该线圈由带有PTFE内衬Kapton窗口的3D打印观察部分连接。观察部分被放置在两个交替上升的管道线圈之间，使得溶液流以规则的间隔通过它。这将使我们能够通过在Diamond的I11光束线（EH 2）的第二个箱中垂直定位大型测角仪台（z轴+5 cm），远程引导光束通过结晶器长度的各个点。由于通过的浆料不断被新浆料所取代，因此对每个微晶的X射线损伤最小化，必要时可以延长采集时间。在建议的采集时间内，将获得沿着结晶器长度的设定点的混合粉末X射线衍射图。在设定点重复实验将确认分段流量优化的稳态操作。预计随着时间/结晶器长度，特别是在低流速下，乌巴III转变为乌巴I。流动结晶过程的在线X射线监测是一个令人兴奋的新领域，使用中尺度结晶器检查晶体结构演变是前所未有的。这种技术的发展不仅可以为结晶过程的阐明，而且还可以为高通量材料的发现提供机会。通过使用具有多个进料的流动结晶器，可以使用最少的材料非常快速地评估大范围的排列，例如反应物比率、pH和浓度。已经有一些工作朝着这个目标，但在线X射线分析的化验尚未实现。从这个开始，KRAIC设备的概念和它在开关功能材料和目标多晶型系统的应用将被探索。随着项目的发展，还将说服和评估替代连续结晶和材料组装平台的适应性，以进行部署。