材料物理实验方法-电子顺磁共振-2010-4.pptVIP

材料物理实验方法 ——电子顺磁共振波谱EPR/ESR概论 陈 家 富 合肥微尺度物质科学国家实验室 理化中心顺磁室 jfchen@ustc.edu.cn 2010年5月 调制幅度对ESR波谱强度和线形的影响：5 × 10-4 mol/L 哌啶酮氮氧自由基水溶液。 EPR—共振波谱仪 EPR—共振波谱仪 Signal distortion and shift due to excessive time constants Time constants filter out noise by slowing down the response time of the spectrometer. If we choose a time constant which is too long for the rate at which we scan the magnetic field, we can distort or even filter out the very signal which we are trying to extract from the noise. 时间常数选择实例: EPR—共振波谱仪 3、磁铁系统 EPR谱仪中，采用电磁铁作为磁场源，对其要求是均匀、稳定。当需要较高磁场时，通常采用超导磁体作磁场源。 电磁铁系统要包括稳压、稳流装置。 JES-FA200型(JEOL)谱仪，磁场强度最高1.3 T（13000 Gs）。 EPR—共振波谱仪 The magnetic field controller allows us to sweep the magnetic field in a controlled and precise manner for our ESR experiment. It consists of two parts: One part which sets the field values and the timing of the field sweep and another part which regulates the current in the windings of the magnet to attain the requested magnetic field value. EPR—共振波谱仪 The magnetic field controller The magnetic field regulation is accomplished by comparing the voltage from the Hall probe with the reference voltage given by the other part of the controller. When there is a difference between the two voltages, a correction voltage is sent to the magnet power supply which changes the amount of current flowing through the magnet windings. Eventually the error voltage drops to zero and the field is stable or locked. This occurs at each discrete step of a magnetic field scan. 磁场校正：可通过霍尔元件在磁场中取样，并反馈回去再控制磁场。 EPR—共振波谱仪 磁场扫宽的选择: EPR—共振波谱仪 EPR—共振波谱仪 Block diagram of an ESR Spectrometer 4、EPR谱仪主要性能指标 1）灵敏度 Sensitivity 能够检测出自旋共振信号所需要的最少量。 （仪器能够检测的最小顺磁中心数N） 对DPPH而言：10-13 mol 2）分辨率 Resolution 能够分开两条谱线的最小距离。 2.35?T or better (for JES-FA200) 3）磁场稳定性 Magnet Stability Short term: 0.3 ?T Long term: 1.5 ?T EPR—共振波谱仪 EPR—应用实例 五、电子顺磁共振波谱应用实例 1、自旋捕获(集) Spin Trapping R ? + 自旋捕集剂 自旋加合物 自旋捕获（集）— Spin trapping技术是60年代末发展起来的一种短寿