Cryogenic sample stage for an ion microscope

• US 4,663,944 A
• Filed: 07/12/1985
• Issued: 05/12/1987
• Est. Priority Date: 07/12/1985
• Status: Expired due to Fees

• Current Assignee: Cornell Research Foundation Incorporated (Cornell University)
• Original Assignee: Cornell Research Foundation Incorporated (Cornell University)
• Inventors: Bernius, Mark T., Morrison, George H.
• Primary Examiner(s): Capossela, Ronald C.
• Application Number:
  US06/754,111
• Time in Patent Office: 669 Days
• Field of Search: 62/62, 62/78, 62/320, 62/514 R, 250/309, 250/443.1, 250/442.1
• US Class Current: 62/51.1
• CPC Class Codes: F25D 3/10 using liquefied gases, e.g. liquid air for cooling semiconductor devices H01L23/445
• CPC Class Codes: H01J 37/20 Means for supporting or positioning the objects or the material; Means for adjusting diaphragms or lenses associated with the support introducing the objects H01J37/18
• CPC Class Codes: H01J 49/0409 Sample holders or containers containers for retaining a material to be analyzed, B01L3/50, for DNA, C12Q1/6834, for biological materials, G01N33/543
• CPC Class Codes: H01J 49/0468 with means for heating or cooling the sample

Abstract

A cryogenic sample stage for an ion mass spectrometry system. A mounting is adjustable relative to the ion microscope lens system to maintain alignment with the immersion lens. Sample temperatures below -150° C. are maintained by circulating cooling fluid to the mounting section thereby allowing a direct analysis of frozen-hydrated biological samples.

Claims

1. A cryogenic sample stage for an ion microscope having a lens system with an ion emission-immersion lens to form an image of a sample under study comprising:

a mounting section for a sample under study, means coupled to and providing a cooling fluid to said mounting section; and

means to adjust the position of said mounting section relative to said ion emission-immersion lens of said microscope lens system.

2. The apparatus of claim 1 wherein said mounting system comprises a sample holder mount coupled to said means to provide a cooling fluid, a sample holder mounted to said sample holder mount, and a temperature sensor attached to said sample holder.

3. The apparatus of claim 2 wherein said sample holder comprises a stainless steel frame, a copper body mounted in said frame serving as a thermal reservoir and a semiconductor plate having surface receiving a sample.

4. The apparatus of claim 3 wherein said semiconductor plate is mounted on a metallic cylinder, said metallic cylinder having means to removably mount to said copper body.

5. The apparatus of claim 2 wherein said means to provide a cooling fluid comprises a thermally conductive mass and means to fix said sample holder mount to said thermally conductive mass.

6. The apparatus of claim 1, wherein said means to provide a cooling fluid comprises a source of cooling fluid, a feedtube coupled at one end to said source, and having a cooling chamber at the other end to circulate cooling fluid in a thermally conductive manner to said mounting section.

7. The apparatus of claim 6 wherein said means to supply a cooling fluid further comprising first outer sleeve concentric with said feedtube, said outer sleeve coupled to said means to adjust the position of said mounting section and an insulator coupling said outer sleeve to said mounting section, whereby cooling fluid passes from said feedtube with said cooling chamber and then into an annular space between said feedtube and said first outer sleeve for removal.

8. The apparatus of claim 7 wherein said means to supply a cooling fluid further comprises a second outer sleeve concentric with said feedtube and rotatable relative to it and, means coupled to said second outer sleeve to exhaust said cooling liquid from said annular space.

9. The apparatus of claim 7 wherein said means to adjust the position of said mounting section comprises a first flange coupled to said first outer sleeve, a bellows flange, a bellows coupled to both said first flange and said bellows flange, a mounting flange and adjustment means mounted on said bellows flange to move said first flange and said bellows flange relative to said mounting flange.

10. The apparatus of claim 9 wherein said adjustment means comprises an adjustment screw and a nut mounted on said bellows flange, said adjustment screw having one end adapted to abut against said mounting flange and fixed to said first flange at an opposite end.

11. The apparatus of claim 1 wherein said means to adjust the position of said mounting section comprises a first flange coupled to said means to provide a coupling fluid and second flange for mounting said sample stage to said microscope and means for carrying the distance between said first and second flanges.

12. The apparatus of claim 1 further comprises a thermistor coupled to said mounting section to measure the temperature thereof.

13. The apparatus of claim 1 wherein said means coupled to and providing a cooling fluid thermistor at one end with an expansion joint, and a ceramic insulator coupled to said expansion joint.

14. The apparatus of claim 13 wherein said mounting section comprises an expansion joint coupled to said ceramic insulator.