US3444365A - Continuously evacuated corpuscularray apparatus,such as electron microscope,having a cryogenically cooled specimen cartridge - Google Patents
Continuously evacuated corpuscularray apparatus,such as electron microscope,having a cryogenically cooled specimen cartridge Download PDFInfo
- Publication number
- US3444365A US3444365A US497894A US3444365DA US3444365A US 3444365 A US3444365 A US 3444365A US 497894 A US497894 A US 497894A US 3444365D A US3444365D A US 3444365DA US 3444365 A US3444365 A US 3444365A
- Authority
- US
- United States
- Prior art keywords
- cartridge
- specimen
- heat
- conducting
- springs
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 238000001816 cooling Methods 0.000 description 15
- 239000007789 gas Substances 0.000 description 6
- 210000002105 tongue Anatomy 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000004804 winding Methods 0.000 description 3
- 239000004020 conductor Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 201000009310 astigmatism Diseases 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/02—Details
- H01J37/20—Means for supporting or positioning the object or the material; Means for adjusting diaphragms or lenses associated with the support
Definitions
- CONTINUOUSLY EVACUATED PUSCULAFPRAY APPARATUS SUCH AS ELECTRON MICROSCOPE, HAVING A CRYOGENICALLY COOLED SPECIMEN CARTRIDGE Filed Oct. 19, 1965
- CONTINUOUSLY EVACUATED CORPUSCULAR- RAY APPARATUS SUCH AS ELECTRON MICRO- SCOPE, HAVING A CRYOGENICALLY COOLED SPECIMEN CARTRIDGE Wolfram Loebe, Berlin, Germany, assignor to Siemens Aktiengesellschaft, Kunststoff, Germany, a corporation of Germany Filed Oct. 19, 1965, Ser. No. 497,894 Claims priority, applicgtion Gigi-many, Nov.
- My invention relates to corpuscular ray apparatus, particularly electron microscopes which, during operation, are continuously exhausted by a vacuum pump and have a specimen-accommodating cartridge connected with a cryogenic cooling device.
- corpuscular-ray apparatus are described in the copending application of K. H. Herrmann and W. Loebe, Ser. No. 392,088, filed Aug. 26, 1964, and assigned to the assignee of the present invention.
- the above-mentioned copending application proposes to provide a specimen cartridge composed of two coaxial portions.
- the first portion accommodates the specimen carrier, usually a centrally apertured diaphragm.
- the first portion is surrounded by the second portion of the cartridge which is in good heat-conducting connection with a cryogenic device.
- My invention relating to corpuscular-ray apparatus, preferably but not exclusively to electron microscopes, generally of the above-mentioned type in which a two-part specimen cartridge is cryogenically cooled, has for its purpose to permit retaining the desired protection against soiling of the specimen, while also permitting low-temperature cooling of the specimen, without any deficiency as regards heat transfer conditions or positioning of the specimen.
- I provide a corpuscular-ray apparatus of the type continuously evacuated when in operation, with an object cartridge composed of two coaxial portions substantially in the above-mentioned manner, but provide as heat conducting components a number of metal springs and distribute them within the cartridge and about the ray axis of the cartridge in a rotationally symmetrical arrangement.
- the rotationally symmetrical heat-conducting components can also consist of at least one wire, tape or braid.
- the heatconductances of these springs are so chosen that, during cryogenic cooling of the cartridge in the above-described manner, the resulting steady-state temperature at the specimen carrier and at the specimen is higher than the temperature of the cartridge portion that coductively connects it with the cryogenic cooling means.
- the necessary heat conductance of the rotationally symmetrical spring arrangement is obtained by giving the heat-conducting springs consisting, for example, of copper or copper alloys, a proper cross section and an effective length.
- an apparatus affords the assurance that, for any cooling of the specimen carrier with the specimen, there will always occur a temperature gradient between the cooled second cartridge portion on one hand, and the specimen on the other hand, so that the temperature of the specimen, even if the latter is also being cooled, is always at least slightly higher than the temperature of the surrounding second cartridge portion.
- the specimen therefore, is never the coldest spot in the vacuum space of the apparatus so that the atoms and molecules of residual gases and vapors cannot precipitate upon the specimen.
- the heat-conducting structures further afford the assurance that in any event a good heat-conducting contact exists between these structures, on the one hand, and the two cartridge portions, on the other hand, and that any forces or moments exerted between the two cartridge portions by the heat-conducting structures are rotaitonally symmetrical with respect'to the axis of the corpuscular-ray so that there is no tendency of affecting the positioning of the specimen.
- the springs are prefer-ably formed by tongues extending from an annular marginal member in the radially inward direction.
- the tongues may be produced by cutting radial slits into the annular spring and are preferably given an individually arcua-te shape curving away from the plane of the marginal annular member.
- the springs may also be curved alternately in opposed axial directions. Such ring-type springs need not be fastened to either cartridge portion but may simply be placed between them before the removable first portion is seated in proper position against the second portion.
- Such openings are produced in a particularly simple manner by supporting the specimen carrier on heat-conducting struts into which the adjacent end of the first portion is subdivided, the spaces between the struts then forming the exhaust openings.
- FIG. 1 is an axial section through the objective-lens portion of the electron microscope comprising a specimenaccommodating cartridge device according to the invention.
- FIG. 2 shows in schematical perspective a portion of a ring-shaped multi-tongue spring which forms part of the device illustrated in FIG. 1.
- the illustrated portion of the electron microscope comprises an objective lens assembly 3 with two coaxial and axially spaced pole shoes 1 and 2. Coaxially mounted above the pole shoes is an object cartridge 4 composed of two portions 5 and 6. The first portion 5 is seated in a partly illustrated specimen table or stage 7. The second portion 6 of the cartridge is in good heat-conducting connection with a cooling rod 8 whose other end is immersed into a cryogenic vessel (not illustrated). The second cartridge portion 6 is rigidly and firmly attached to the lens system 3 but is thermally insulated therefrom by insulating inserts 9 consisting, for example, of sleeves made of synthetic plastic.
- the first cartridge portion 5 has a conical top member 10 which serves for removably inserting the portion 5 into a hollow conical seat or neck of the specimen stage 7.
- Two tubular members 12 and 13 are separately join-ted with the conical top member 10 by being screwed together therewith.
- Memember 12 constitutes the holder for the object carrier 14, and part 13 is an elongated tubular insert which forms a holder for a centrally aper-tured diaphragm 15.
- the two cartridge portions 5 and 6 have respective front faces of annular shape which lie opposite each other and extend perpendicularly to the ray axis and hence to the direction of seating motion of the first cartridge portion 5.
- the two annular faces serve as abutments for a good conducting connecting structure constituted by a multitongue annular spring member 16 separately shown in FIG. 2.
- the individual springs 16a form curved tongues which extend radially inwardly from a ring-shaped marginal portion of the spring member 16. These spring tongues have the effect that when the cryogenic cooling device of which the cooling rod 8 forms part, is in operation, the specimen carrier 14 and the specimen mounted thereupon are cooled to a temperature which is always slightly higher than the temperature of the second cartridge portion 6 surrounding the specimen.
- the conical top member 10 of the first cartridge portion possesses a zone 17 formed of heat-insulating material.
- the entire top member 10 may be made of insulating or poorly heat-conducting material, in which case the inner surface of the top member facing the electron ray must be metallized and be electrically connected with metal parts of the equipment in order to prevent the accumulation of static electric charges.
- the lower end of the first cartridge portion 5 which holds the specimen carrier 14 is subdivided into a number of struts of which only two are visible in FIG. 1 at 12a and 12b.
- the interspaces between these struts form openings through which the space within the first cartridge portion is continuously exhausted during operation of the electron microscope, so that any atoms or molecules of residual gases or vapors are exhausted from within the first cartridge portion.
- a diaphragm 18 is mounted on the second cartridge portion 6, preferably in heat-insulated relation thereto. Such heat insulation is secured by interposition of an insulating insert 19 and serves to prevent excessive cooling of the diaphragm 18 which might result in icing of this diaphragm and consequently, since the diaphragm is located in the electron-optical gap of the objective lens 3, may cause disturbing astigmatism of the lens.
- the 'apertured diaphragm 20 of the lens assembly is at least approximately at normal room temperature.
- This diaphragm is mounted on a slider 21 by means of which the diaphragm is displaceable transversely of the ray axis.
- the space surrounding the lens diaphragm 20 may also be cooled, or a further diaphragm mounted at a somewhat lower location on an extension of a second cartridge portion may be cooled, so that the space enclosed within the second cartridge portion approaches as best as feasible the properties of a chamber enclosed within cooled walls.
- the first cartridge portion 5 with a heater in the region where this portion is in contact with the specimen carrier and the heatconducting spring structures.
- the heater then permits regulating the temperature of the specimen.
- the temperature may be measured, for exmaple, by thermocouples arranged in the number required for proper temperature measurement.
- the illustrated embodiment has a heater winding 22 coaxially mounted on the tubular member 12.
- the terminals of winding 22 are to be connected to a controllable source of electric current outside of the microscope structure, so that the temperature of the specimen can be controlled or regulated.
- a thermocouple or other heat sensor may be mounted at a suitable locality for response to the temperature of the specimen.
- the second portion 6 of the cartridge it is preferable to attach the second portion 6 of the cartridge to the objective lens structure of the corpuscularray apparatus, whereas the first cartridge portion 5 with the specimen carrier 14 is made removable from the vacuum vessel for such purposes as exchanging the specimen.
- the second cartridge portion therefore, can be introduced through a vacuum lock or sluice to be removably seated in the specimen stage 7.
- the heat-conducting springs 16a are bindingly stressed between the two cartridge portions when the first portion 5 is properly seated in the specimen stage.
- This facilitates designing the two cartridge portions as mechanically independent structural units so that an exchange of the specimen or the removal of diaphragms for cleaning purposes or the like becomes possible simply by sluicing only the first cartridge portion out of the vacuum vessel.
- This is a relatively simple matter because the first cartridge 5 portion is not directly in connection with the cryogenic cooling device. Consequently no additional manipulations or expedients are necessary in order to re-establish the necessary heat-conducting connection etween the two cartridge portions after inserting a new specimen or diaphragm into the apparatus.
- the springs of heat-conducting material in the preferred embodiment of the invention, may also be arranged on surface areas of the respective cartridge portions that extend parallel to the direction of motion of the first cartridge portion 5 when the latter is being inserted into the specimen stage 7, so that this cartridge portion during seating is virtually guided by the springs.
- care must be taken that during such seating of the cartridge portion no excessive forces are imposed upon the springs as this may impair the proper centering of the specimen with respect to the corpuscularray.
- the invention is not limited to the particular example of the embodiment illustrated.
- the two portions of the specimen cartridge need not be designed as separable units in the illustrated manner.
- the second cooled cartridge portion may be given a shape which upwardly surrounds the upper cartridge portion where the diaphragm 15 is supported by means of a cooled tube.
- a specimen-accommodating device within said vessel structure comprising a specimen cartridge having first and second coaxial component portions, said first cartridge portion being removably seated in said specimen stage, a specimen carrier held by said first cartridge portion, said second cartridge portion surrounding said first cartridge portion in the region of said carrier and being attached to said lens system, and heat-conducting structure interconnecting said cartridge portions which are otherwise thermally insulated from each other, said heat-conducting structure comprising springs symmetrically disposed about the axis of said cartridge, said springs being under stress when said first portion has been inserted into said specimen stage, and a cryogenic device in cooling contact with only the second one of the cartridge portions, said heat-conducting structure having a heat conductance whereat the steady state temperature of said first cartridge portion and said specimen carrier held thereby is higher than that of said second cartridge portion cooled by contact with said cry
- said two cartridge portions having respective faces extending transverse to the axis and being located opposite and in axially spaced relation to each other, said two faces forming respective abutments engaged by said springs.
- said springs forming respective legs of an annular member having a marginal ring portion from which said springs extend radially inwardly, said individual springs having arcuate shape curving out of the plane of said marginal ring portion.
- said first cartridge portion having exhaust openings at 10- calities surrounded by said second portion so that gas residues may be exhausted through said openings.
- said first cartridge portion having its end adjacent to said specimen carrier subdivided so as to form mutually spaced struts, said exhaust openings being formed by the spaces intermediate said struts, and said specimen carrier being held by and between said struts.
- said first cartridge portion having a heater winding mounted in the region of said specimen carrier and said heatconducting structure.
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Sampling And Sample Adjustment (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DES94316A DE1254779B (de) | 1964-11-25 | 1964-11-25 | An der Pumpe arbeitender Korpuskularstrahlapparat, insbesondere Elektronenmikroskop,mit einer einen Objekttraeger aufnehmenden und mit einer Tiefkuehlvorrichtung in Verbindung stehenden Objektpatrone |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3444365A true US3444365A (en) | 1969-05-13 |
Family
ID=7518613
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US497894A Expired - Lifetime US3444365A (en) | 1964-11-25 | 1965-10-19 | Continuously evacuated corpuscularray apparatus,such as electron microscope,having a cryogenically cooled specimen cartridge |
Country Status (3)
| Country | Link |
|---|---|
| US (1) | US3444365A (de) |
| DE (1) | DE1254779B (de) |
| GB (1) | GB1127440A (de) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4427891A (en) | 1979-09-20 | 1984-01-24 | Georges Adrien J P | Variable temperature stage device for electron microscope |
| US4663944A (en) * | 1985-07-12 | 1987-05-12 | Cornell Research Foundation, Inc. | Cryogenic sample stage for an ion microscope |
| US5811122A (en) * | 1995-05-26 | 1998-09-22 | Kansas State University Research Foundation | Hide/polymer and leather/polymer composite materials formed by in situ polymerization of polymer precursors impregnated into hide and leather |
| US20080013195A1 (en) * | 2005-01-08 | 2008-01-17 | Carl Zeiss Microlmaging Gmbh | Temperable Lens, Especially For Microscopes |
| CN105789004A (zh) * | 2016-04-20 | 2016-07-20 | 兰州大学 | 一种全温区热电两场扫描电镜原位物性测量台 |
| US10775285B1 (en) * | 2016-03-11 | 2020-09-15 | Montana Intruments Corporation | Instrumental analysis systems and methods |
| US11125663B1 (en) | 2016-03-11 | 2021-09-21 | Montana Instruments Corporation | Cryogenic systems and methods |
| US11956924B1 (en) | 2020-08-10 | 2024-04-09 | Montana Instruments Corporation | Quantum processing circuitry cooling systems and methods |
| US12071998B2 (en) | 2018-10-09 | 2024-08-27 | Montana Instruments Corporation | Cryocooler assemblies and methods |
| US12253205B1 (en) | 2018-09-28 | 2025-03-18 | Montana Instruments Corporation | Thermal transfer line assemblies, methods of manufacturing thermal transfer line assemblies, and thermal transfer methods |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2543825A (en) * | 1948-04-26 | 1951-03-06 | Phillips Petroleum Co | X-ray diffraction apparatus |
| US3171955A (en) * | 1962-03-30 | 1965-03-02 | Rca Corp | Temperature controlled and adjustable specimen stage for scientific instruments |
| US3226542A (en) * | 1961-12-07 | 1965-12-28 | Ass Elect Ind | Mass spectrometer arc-type ion source having electrode cooling means |
-
1964
- 1964-11-25 DE DES94316A patent/DE1254779B/de active Pending
-
1965
- 1965-10-19 US US497894A patent/US3444365A/en not_active Expired - Lifetime
- 1965-11-24 GB GB49976/65A patent/GB1127440A/en not_active Expired
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2543825A (en) * | 1948-04-26 | 1951-03-06 | Phillips Petroleum Co | X-ray diffraction apparatus |
| US3226542A (en) * | 1961-12-07 | 1965-12-28 | Ass Elect Ind | Mass spectrometer arc-type ion source having electrode cooling means |
| US3171955A (en) * | 1962-03-30 | 1965-03-02 | Rca Corp | Temperature controlled and adjustable specimen stage for scientific instruments |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4427891A (en) | 1979-09-20 | 1984-01-24 | Georges Adrien J P | Variable temperature stage device for electron microscope |
| US4663944A (en) * | 1985-07-12 | 1987-05-12 | Cornell Research Foundation, Inc. | Cryogenic sample stage for an ion microscope |
| US5811122A (en) * | 1995-05-26 | 1998-09-22 | Kansas State University Research Foundation | Hide/polymer and leather/polymer composite materials formed by in situ polymerization of polymer precursors impregnated into hide and leather |
| DE102005001102B4 (de) * | 2005-01-08 | 2021-04-29 | Carl Zeiss Microscopy Gmbh | Temperierbares Objektiv für Mikroskope |
| US20080013195A1 (en) * | 2005-01-08 | 2008-01-17 | Carl Zeiss Microlmaging Gmbh | Temperable Lens, Especially For Microscopes |
| US7800848B2 (en) * | 2005-01-08 | 2010-09-21 | Carl Zeiss Microimaging Gmbh | Temperable lens, especially for microscopes |
| US11125663B1 (en) | 2016-03-11 | 2021-09-21 | Montana Instruments Corporation | Cryogenic systems and methods |
| US10775285B1 (en) * | 2016-03-11 | 2020-09-15 | Montana Intruments Corporation | Instrumental analysis systems and methods |
| US11378499B2 (en) | 2016-03-11 | 2022-07-05 | Montana Instruments Corporation | Instrumental analysis systems and methods |
| CN105789004B (zh) * | 2016-04-20 | 2018-01-23 | 兰州大学 | 一种全温区热电两场扫描电镜原位物性测量台及测量方法 |
| CN105789004A (zh) * | 2016-04-20 | 2016-07-20 | 兰州大学 | 一种全温区热电两场扫描电镜原位物性测量台 |
| US12253205B1 (en) | 2018-09-28 | 2025-03-18 | Montana Instruments Corporation | Thermal transfer line assemblies, methods of manufacturing thermal transfer line assemblies, and thermal transfer methods |
| US12071998B2 (en) | 2018-10-09 | 2024-08-27 | Montana Instruments Corporation | Cryocooler assemblies and methods |
| US11956924B1 (en) | 2020-08-10 | 2024-04-09 | Montana Instruments Corporation | Quantum processing circuitry cooling systems and methods |
| US12262510B2 (en) | 2020-08-10 | 2025-03-25 | Montana Instruments Corporation | Quantum processing circuitry cooling systems and methods |
Also Published As
| Publication number | Publication date |
|---|---|
| DE1254779B (de) | 1967-11-23 |
| GB1127440A (en) | 1968-09-18 |
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