NMR measuring assembly with cold bore of the cryostat

Patent metadata

Field	Value
Publication number	US-11953570-B2
Application number	US-202217882192-A
Country	US
Kind code	B2
Filing date	Aug 5, 2022
Priority date	Feb 7, 2020
Publication date	Apr 9, 2024
Grant date	Apr 9, 2024

Abstract

An NMR measuring arrangement (20) includes a cryostat (1), a superconducting magnet coil system (2) and an NMR probe (3). The cryostat has an evacuated vacuum container (5) and forms a bore (10). A wall (12) of the bore delimits the vacuum container. The cryostat forms only one evacuated gap (13) in a space (18) between the magnet coil system and the wall of the bore. At least a segment of the wall of the bore is thermally coupled to a heat sink of the cryostat. As a result, the NMR measurement arrangement provides more precise NMR measurements (in particular with a higher spectral resolution and/or a higher signal-to-noise ratio) on measurement samples.

First claim

What is claimed is:

1. Nuclear magnetic resonance (NMR) measuring arrangement, comprising
a cryostat having an evacuated vacuum container, wherein the cryostat forms a bore having a bore wall that delimits the vacuum container,
a superconducting magnet coil system having a magnet bore, wherein the magnet coil system is arranged directly inside or indirectly inside the vacuum container, wherein the cryostat, for thermally insulating the magnet coil system, forms one or more evacuated gaps between the superconducting magnetic coil system and the vacuum container in a sequence from the inside out, and wherein the bore extends through the magnet bore, and
an NMR probe having a radio frequency (RF) coil system, wherein the NMR probe is arranged outside the vacuum container, and wherein the NMR probe is arranged at least partially in the bore,
wherein the cryostat forms only one evacuated gap in a space extending between the magnet coil system and the bore wall,
wherein at least a length of a segment of the bore wall is thermally coupled to a heat sink of the cryostat, and
wherein the bore wall also delimits a hermetically sealed space outside the vacuum container,
wherein the sealed space extends in the bore in a longitudinal direction of the cryostat at least over the length of the segment.

2. NMR measuring arrangement according to claim 1 , wherein the bore wall and a housing wall of the NMR probe are sealed against one another with one or more seals.

3. NMR measuring arrangement according to claim 1 , further comprising a lock chamber formed at an opening of the bore and configured to introduce and to discharge the NMR probe for an at least partial arrangement in the bore.

4. NMR measuring arrangement according to claim 1 , further comprising a pump device configured to evacuate the sealed space.

5. NMR measuring arrangement according to claim 1 , further comprising a dry gas filling device configured to fill the sealed space with a dry gas.

6. NMR measuring arrangement according to claim 1 , wherein the cryostat comprises a dry gas flushing device configured to flush the bore with a dry gas at least in the region of the segment.

7. NMR measuring arrangement according to claim 1 , further comprising a heating device.

8. NMR measuring arrangement according to claim 1 , wherein at least the segment of the bore wall is substantially thermally decoupled from a remainder of the vacuum container which remainder corresponds to a room temperature jacket of the vacuum container, whereby a remaining thermal coupling is less than 0.1 W/K.

9. NMR measuring arrangement according to claim 8 , wherein the bore wall consists of, with respect to the longitudinal direction, a central portion and two outer portions, and wherein the central portion is made from a material with a higher specific thermal conductivity and/or with a greater wall thickness than materials of the two outer portions.

10. NMR measuring arrangement according to claim 1 , wherein the bore wall, in a central portion with respect to the longitudinal direction, is provided on a radially outer side of the bore wall with a coating which has a higher specific thermal conductivity than does a basic structure of the bore wall without the coating.

11. NMR measuring arrangement according to claim 10 , wherein the coating is formed at least in a region around a magnetic center of the magnet coil system with interruptions running in a longitudinal direction of the bore.

12. NMR measuring arrangement according to claim 1 , wherein the heat sink, to which at least the length of the segment of the bore wall is thermally coupled,
is a nitrogen container of the cryostat or a radiation shield of the cryostat connected to the nitrogen container, or
is a warmer cooling stage of a cryocooler or a radiation shield connected to the warmer cooling stage of the cryocooler, or
is a radiation shield which is cooled by evaporating helium from a cryogenic container, wherein the cryogenic container is arranged in the vacuum container and contains the magnet coil system.

13. NMR measuring arrangement according to claim 1 , wherein at least the length of the segment of the bore wall is thermally coupled to
at least part of the NMR probe, and/or
a gradient coil system which is arranged separately from the probe or as part of the probe in the bore, and/or
a shim coil system which is arranged separately from the probe or as part of the probe in the bore.

14. NMR measuring arrangement according to claim 1 , wherein the length of the segment of the bore wall extends in a longitudinal direction of the bore at least over a length of an active region of the RF coil system.

15. NMR measuring arrangement according to claim 1 , wherein the length of the segment of the bore wall extends in a longitudinal direction of the bore at least over a length of the magnet coil system.

16. Method for operating the NMR measuring arrangement according to claim 1 , comprising: carrying out an NMR measurement on a measurement sample arranged in the NMR probe, during the NMR measurement, cooling at least the segment of the bore wall to a temperature T wall <250K, and, at least in the region of the segment, either evacuating the bore or filling the bore with a dry gas or flushing the bore with the dry gas.

17. Method according to claim 16 , further comprising cooling at least part of the NMR probe during the NMR measurement by thermally coupling the NMR probe to at least the segment of the bore wall.

18. Method according to claim 16 , wherein at least part of the NMR probe is cooled by a cooling device incorporated into the NMR probe, wherein at least the segment of the bore wall limits an input of thermal radiation into the NMR probe.

19. Method for operating the NMR measuring arrangement according to claim 3 , comprising replacing a spent NMR probe with a replacement NMR probe in the NMR measuring arrangement, said replacing comprises removing the spent NMR probe from the bore, discharging the spent NMR probe through the lock chamber, introducing the replacement NMR probe through the lock chamber, and at least partially inserting the replacement NMR probe into the bore, while maintaining a vacuum or a dry gas filling in the bore at least in the region of the segment of the wall of the bore.

20. Method for operating the NMR measuring arrangement according to claim 6 , comprising replacing a spent NMR probe with a replacement NMR probe in the NMR measuring arrangement, said replacing comprises removing the spent NMR probe from the bore and at least partially inserting the replacement NMR probe into the bore, while flushing the bore at least in the region of the segment with a dry gas, with the dry gas flushing device.

21. Method for operating the NMR measuring arrangement according to claim 7 , comprising replacing a spent NMR probe with a replacement NMR probe in the NMR measuring arrangement, wherein said replacing comprises removing the spent NMR probe from the bore and at least partially inserting the replacement NMR probe into the bore, while heating the bore with the heating device at least in a region of the segment, whereby a formation of condensation is avoided on the bore wall.

Assignees

• Bruker Switzerland Ag

Inventors

• Wikus Patrick

Classifications

• G01R33/3804 Primary

  Additional hardware for cooling or heating of the magnet assembly, for housing a cooled or heated part of the magnet assembly or for temperature control of the magnet assembly · CPC title

• G01R33/3815 Primary

  with superconducting coils, e.g. power supply therefor · CPC title

• G01R33/3875

  using correction coil assemblies, e.g. active shimming · CPC title

• H01F6/04

  Cooling · CPC title