Cooled NMR probe head with thermal insulation of the sample

• US 6,441,617 B2
• Filed: 01/22/2001
• Issued: 08/27/2002
• Est. Priority Date: 02/12/2000
• Status: Active Grant

• Current Assignee: Bruker Switzerland AG (Bruker Corporation)
• Original Assignee: Bruker Biospin AG (Bruker Corporation)
• Inventors: Marek, Daniel
• Primary Examiner(s): Lefkowitz, Edward
• Assistant Examiner(s): Shrivastav, Brij B.
• Application Number:
  US09/765,279
• Publication Number:
  US 20010013779A1
• Time in Patent Office: 582 Days
• Field of Search: 324/321, 324/315, 324/314, 324/309, 324/307, 324/322, 324/300, 324/318, 324/248, 505/845
• US Class Current: 324/318
• CPC Class Codes: G01R 33/30 Sample handling arrangements, e.g. sample cells, spinning mechanisms
• CPC Class Codes: G01R 33/34023 Superconducting RF coils
• CPC Class Codes: G01R 33/34092 RF coils specially adapted for NMR spectrometers

Abstract

An NMR (=nuclear magnetic resonance) probe head comprising an RF (=radio frequency) receiver coil system, which can be cooled down to cryogenic temperatures, and a room temperature pipe (4), extending in a z direction, for receiving a sample tube (6) containing sample substance (7) to be examined by NMR measurements is characterized in that at least one, preferably several radiation shields (9) extending in the z direction and surrounding the room temperature pipe (4) in a radial direction are disposed between the RF receiver coil system (1) and the room temperature pipe (4) which are formed of one or several materials oriented in the z direction and are almost completely transparent to RF fields, at least have an absorption of <5%, preferably <1% for RF fields to thereby provide simple and substantial reduction in the temperature gradient in the z direction during operation without thereby impairing the NMR measurement.

Claims

1. An NMR (nuclear magnetic resonance) probe head for examining a sample substance in a sample tube, the probe head comprising:

an RF receiver coil system;

means for cooling said receiver coil system to cryogenic temperatures;

a room temperature pipe extending along a z-direction, said room temperature pipe for receiving the sample tube; and

at least one radiation shield disposed between said receiver coil system and said room temperature pipe, said at least one shield extending in the z-direction and surrounding said room temperature pipe in a radial direction, said radiation shield comprising at least one material oriented in the z-direction, wherein said at least one material is substantially transparent to RF fields.

2. The NMR probe head of claim 1 wherein N radiation shields are disposed in radial sequence between said receiver coil system and said room temperature pipe, wherein N≧

2.

3. The NMR probe head of claim 2, wherein said N radiation shields are spaced apart from one another in a radial direction, said N radiation shields being one of out of contact, in point contact, and in linear contact with another.

4. The NMR probe head of claim 1, wherein said radiation shield has a radial thickness which is <

0.1mm.

5. The NMR probe head of claim 1, wherein said radiation shield comprises a material which absorbs or reflects radiation in a wavelength range of 10 μ

m≦

λ

≦

100 μ

m and which is substantially transparent to radiation in a wavelength range of λ

>

100 mm.

6. The NMR probe head of claim 5, wherein said radiation shield comprises glass or quartz.

7. The NMR probe head of claim 1, wherein said radiation shield comprises a unidirectional foil.

8. The NMR probe head of claim 1, wherein said radiation shield comprises a unidirectional fabric.

9. The NMR probe head of claim 8, wherein said fabric comprises at least one of fiber mats and fiber glass mats.

10. The NMR probe head of claim 1, wherein said radiation shield comprises at least one of rods, fibers, glass fibers, and quartz fibers, oriented in the z-direction and disposed radially about an axis of said room temperature pipe.

11. The NMR probe head of claim 10, wherein said radiation shield comprises fiber bundles.

12. The NMR probe head of claim 10, wherein said rods or fibers are freely disposed in space and are attached only at ends thereof.

13. The NMR probe head of claim 10, further comprising a support pipe disposed coaxially with respect to said room temperature pipe to which said rods or fibers are mounted.

14. The NMR probe head of claim 10, wherein said rods or fibers are mounted to a side of said room temperature pipe facing said receiver coil system.

15. The NMR probe head of claim 10, wherein said rods or fibers are mounted to one of a support pipe and said room temperature pipe using a glue transparent to RF radiation.

16. The NMR probe head of claim 10, wherein said rods or fibers are densely packed in a peripheral direction about an axis of said room temperature pipe.

17. The NMR probe head of claim 1, further comprising a centering device for centering the sample tube in its measuring position about an axis of said room temperature pipe.

18. The NMR probe head of claim 17, wherein said centering device comprises at least one spacer which is disposed between said room temperature pipe and the sample tube and distributed symmetrically about a z-axis of said room temperature pipe.

19. The NMR probe head of claim 18, wherein said at least one spacer is disposed in one of an area of a bottom of the sample tube in its measuring position and in a region of a feed opening of said room temperature pipe at a side of said room temperature pipe facing the sample tube.

20. The NMR probe head of claim 18, wherein said spacer is disposed along an entire axial length of said receiver coil system at a side of said room temperature pipe facing the sample tube.

21. The NMR probe head of claim 18, wherein said spacer comprises strips of flexible material extending in a direction of the z-axis, whose ends, facing away from the sample tube in its measuring position, are rigidly connected to said room temperature pipe, and whose ends, facing the sample tube in its measuring position, have a bead that bulges towards the sample tube, said bead having a free leg seating on said room temperature pipe.

22. The NMR probe head of claim 18, wherein said spacer comprises at least one of a material which is transparent to RF radiation and a magnetically compensated material.

23. The NMR probe head of claim 18, wherein said spacer comprises sheet metal strips having a thickness of approximately 100μ

m and a width transverse to a z axis of approximately 0.5 mm to 2mm.

24. The NMR probe head of claim 1, further comprising a tempering means disposed between said receiver coil system and the sample, said tempering means extending in a direction and surrounding the sample tube in a radial direction, said tempering means comprising material which is substantially transparent to RF fields.

25. The NMR probe head of claim 24, wherein said tempering means comprises a layer radially surrounding the sample tube in an axial region of said receiver coil system, said layer having a radial thickness which is <

1 mm and which is made from a material which at least partially absorbs radiation in a wavelength range of 100nm≦

λ

≦

100μ

m and which is transparent to radiation in a wavelength range of λ

>

100mm.

26. The NMR probe head of claim 25, further comprising a heating means for uniform heating of said layer.

27. The NMR probe head of claim 26, wherein said heating means comprises a device for irradiating said layer with one of radiation in a wavelength range of 100 nm≦

λ

≦

100 μ

m and heat radiation.

28. The NMR probe head of claim 27, wherein said irradiating device is disposed on a side of said room temperature pipe facing said receiver coil system.

29. The NMR probe head of claim 25, wherein said layer surrounds a surface of said room temperature pipe.

30. The NMR probe head of claim 25, wherein said layer is disposed about said room temperature pipe in axially extending strips which are separated from one another in a peripheral direction.

31. NMR probe head of claim 25, wherein said layer can be electrically heated.

32. The NMR probe head of claim 24, wherein said tempering means comprises at least one heating coil of thin material having good electric conductance, wherein each of said at least one heating coil comprises an outgoing and return conductor, wherein said outgoing and return conductors are electrically connected to one another at one end and can be supplied with heating current from a current source at an other end.

33. The NMR probe head of claim 32, wherein said outgoing and return conductors are disposed bifilarly in close mutual adjacency.

34. The NMR probe head of claim 33, wherein said outgoing and return conductors comprise two longitudinal strips disposed one on top of an other, which are electrically insulated from one another via an insulation layer or insulation strip.

35. The NMR probe head of claim 32, wherein said outgoing and return conductors comprise materials having different magnetic susceptibilities which are selected such that said heating coil is magnetically compensated towards an outside.

36. The NMR probe head of claim 32, wherein said at least one heating coil is disposed in a spiral fashion about said room temperature pipe.

37. The NMR probe head of claim 32, wherein one of several and at least 8 heating coils are disposed at a separation from one another in a peripheral direction about a z axis of said room temperature pipe and extending parallel to the z-direction.

38. The NMR probe head of claim 32, wherein said heating coil is spatially oriented for minimal coupling to said receiver coil system.

39. The NMR probe head of claim 32, wherein said heating coil comprise a thin material exhibiting good electrical conductance and having a cross-section between 1 μ

m² and 100 μ

m².

40. The NMR probe head of claim 32, further comprising a low-pass filter circuited between said current source and said heating coil.

41. The NMR probe head of claim 32, further comprising a parallel resonant circuit disposed between said current source and said heating coil, said resonant circuit resonating at a frequency most sensitive for NMR measurements.

42. The NMR probe head of claim 32, wherein said current source generates alternating current.

43. The NMR probe head of claim 1, wherein said at least one material is absorbing of RF fields by <

5 %.

44. The NMR probe head of claim 43, wherein said at least one material is absorbing of RF fields by <

1 %.

45. The NMR probe head of claim 2, wherein 5 ≦

N <

25.

46. The NMR probe head of claim 4, wherein said radiation shield has a radial thickness which is <

50 μ

m.

47. The NMR probe head of claim 23, wherein said sheet metal strips have said width transverse to said z axis of approximately 1 mm.

48. The NMR probe head of claim 24, wherein said material of said tempering means is high in thermal conductivity.

49. The NMR probe head of claim 24, wherein said material of said tempering means is absorbing of RF fields by <

5 %.

50. The NMR probe head of claim 49, wherein said material of said tempering means is absorbing of RF fields by <

1 %.

51. The NMR probe head of claim 25, wherein said layer has a radial thickness <

50 μ

m.