Solid-state NMR spectrometer, sample holder therefor, and method of solid-state NMR spectroscopy
A high-resolution solid-state NMR spectrometer which can measure a disklike sample. The spectrometer includes: a stator having an air bearing disposed within the static magnetic field, the rotor being disposed in the stator; and an engaging mechanism mounted in a one-end portion of the rotor and detachably holding a sample holder that holds the disklike sample.
1. A solid-state NMR spectrometer for obtaining a solid-state NMR spectrum by directing RE excitation pulses to a sample from a transmit coil while spinning a rotor at high speed about an axis tilted at a magic angle of about 54.7° to a static magnetic field, said spectrometer comprising:
a rotor having a concave bore;
a disklike sample-holding portion permitting a sample to be placed on its surface or received in an internal cavity formed in the sample-holding portion and a convex pillar portion mounted on a central portion of a rear surface of the disklike sample-holding portion, and wherein the sample-holding portion is mounted to an end portion of the rotor by the convex pillar portion inserted in the concave bore of the rotor;
a stator having an air bearing placed within the static magnetic field, the rotor being disposed in the stator; and
an engaging mechanism detachably holding said sample-holding portion.
2. The solid-state NMR spectrometer of claim 1 , wherein said transmit coil is held by a disk-shaped transmit coil holder which is designed to be capable of adjusting the distance between the transmit coil and a sample held on the disklike sample holding portion.
3. The solid-state NMR spectrometer of claim 2 , wherein said transmit coil holder is provided with an opening in a position corresponding to a central portion of the transmit coil to permit at least one type of light, microwaves, electric field, gas, and heating laser light which vary a physical property of the sample to act on the sample.
4. The solid-state NMR spectrometer of claim 1 , wherein said transmit coil is substantially identical in diameter to said disklike sample-holding portion.
5. The solid-state NMR spectrometer of claim 1 , wherein said disklike sample-holding portion is spun at high speed on a plane tilted at about 35.3° to the static magnetic field.
6. The solid-state NMR spectrometer of claim 1 , wherein said sample is a thin-film sample and placed on the surface of said disklike sample-holding portion.
7. The solid-state NMR spectrometer of claim 1 , wherein the sample is a powdered sample and loaded in the internal cavity of said disklike sample-holding portion.
8. A sample holder for use in the solid-state NMR spectrometer of claim 1 , said sample holder comprising:
a disklike sample-holding portion permitting the sample to be placed on its surface or received in an internal cavity formed in the sample holding portion; and
a pillar portion mounted in a central portion of a rear surface of the disklike sample-holding portion;
wherein the sample holder is mounted to the one-end portion of the rotor by said engaging mechanism via the pillar portion.
9. A method of solid-state NMR spectroscopy for obtaining a solid-state NMR spectrum by the use of the solid-state NMR spectrometer of claim 1 .
10. The method of solid-state NMR spectroscopy of claim 9 , wherein when the solid-state NMR spectrum is obtained, the sample held on or in the sample holder is acted on by at least one type of laser light, microwaves, heat rays, hot air, cold air, and electric power supplied via a wireless power feeding coil.