Paul Scherrer Institute, CH-5232 Villigen PSI, Switzerland.
J Magn Reson. 2013 Sep;234:58-66. doi: 10.1016/j.jmr.2013.06.009. Epub 2013 Jun 22.
In standard Dynamic Nuclear Polarization (DNP) electron spins are polarized at low temperatures in a strong magnetic field and this polarization is transferred to the nuclear spins by means of a microwave field. To obtain high nuclear polarizations cryogenic equipment reaching temperatures of 1 K or below and superconducting magnets delivering several Tesla are required. This equipment strongly limits applications in nuclear and particle physics where beams of particles interact with the polarized nuclei, as well as in neutron scattering science. The problem can be solved using short-lived optically excited triplet states delivering the electron spin. The spin is polarized in the optical excitation process and both the cryogenic equipment and magnet can be simplified significantly. A versatile apparatus is described that allows to perform pulsed dynamic nuclear polarization experiments at X-band using short-lived optically excited triplet sates. The efficient (4)He flow cryostat that cools the sample to temperatures between 4 K and 300 K has an optical access with a coupling stage for a fiber transporting the light from a dedicated laser system. It is further designed to be operated on a neutron beam. A combined pulse ESR/DNP spectrometer has been developed to observe and characterize the triplet states and to perform pulse DNP experiments. The ESR probe is based on a dielectric ring resonator of 7 mm inner diameter that can accommodate cubic samples of 5mm length needed for neutron experiments. NMR measurements can be performed during DNP with a coil integrated in the cavity. With the presented apparatus a proton polarization of 0.5 has been achieved at 0.3 T.
在标准动态核极化 (DNP) 中,电子自旋在低温强磁场中被极化,这种极化通过微波场传递到核自旋。为了获得高核极化,需要达到 1 K 或以下的低温设备和提供数特斯拉的超导磁铁。这种设备强烈限制了在核物理和粒子物理中的应用,在这些应用中,粒子束与极化核相互作用,以及在中子散射科学中。这个问题可以通过使用短寿命的光学激发三重态来解决,从而传递电子自旋。在光学激发过程中,自旋被极化,并且可以显著简化低温设备和磁铁。描述了一种多功能设备,该设备允许在 X 波段使用短寿命光学激发三重态进行脉冲动态核极化实验。高效(4)氦流致冷机将样品冷却到 4 K 至 300 K 之间的温度,具有光学通道,带有耦合级,用于光纤将光从专用激光系统传输。它还设计用于在中子束上运行。已经开发了组合脉冲 ESR/DNP 光谱仪来观察和表征三重态,并进行脉冲 DNP 实验。ESR 探头基于 7 毫米内径的介电环形谐振器,可容纳用于中子实验的 5 毫米长的立方样品。在 DNP 期间,可以通过集成在腔中的线圈进行 NMR 测量。使用所提出的设备,在 0.3 T 时实现了 0.5 的质子极化。