US2858444A - Object-holding device for electron microscopes - Google Patents

Object-holding device for electron microscopes Download PDF

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Publication number
US2858444A
US2858444A US521852A US52185255A US2858444A US 2858444 A US2858444 A US 2858444A US 521852 A US521852 A US 521852A US 52185255 A US52185255 A US 52185255A US 2858444 A US2858444 A US 2858444A
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United States
Prior art keywords
heat conductive
chamber
cooling
electron
temperature
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Expired - Lifetime
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US521852A
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English (en)
Inventor
Leisegang Siegfried
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Siemens and Halske AG
Siemens Corp
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Siemens Corp
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B33/00—Disazo and polyazo dyes of the types A->K<-B, A->B->K<-C, or the like, prepared by diazotising and coupling
    • C09B33/02—Disazo dyes
    • C09B33/08—Disazo dyes in which the coupling component is a hydroxy-amino compound
    • C09B33/10—Disazo dyes in which the coupling component is a hydroxy-amino compound in which the coupling component is an amino naphthol
    • 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

  • My invention relates to electron microscopes and has for its object to provide for such microscopes an objectholding device that prevents or greatly minimizes contamination of the object and/or affords subjecting an object of organic substance to controlled decomposition by electron irradiation.
  • the above-described objects are achieved by subjecting at least a major portion of the chamber walls that limit the half-spaces on both sides respectively of the object, as well as the object itself, to cooling by heat conductance.
  • the cooling of the object does not result in increased contamination as long as a sufficiently large portion of the surrounding walls is simultaneously cooled.
  • the object and the Walls surrounding it are cooled down to a temperature of minus 80 centigrade and below. It has been found that this particular temperature represents a critical point for the effect of the cooling provided according to the present invention. If one approaches this temperature from higher values, then the velocity of contamination decreases down to zero. If the temperature drops below minus 80 centigrade, then the substance of the object begins to decompose, and this decomposition occurs more rapidly with a further reduction in temperature.
  • the chamber is preferably heat-insulated from other parts. of the microscope, and the heat from the chamber is dissipated through a good heat-conducting rod which extends to the outside of the microscope and has its exterior end immersed in a coolant, for instance liquid air.
  • a coolant for instance liquid air
  • thermo-element For measuring the temperature, a thermo-element can be mounted on the object cartridge. The thermo-electrically generated voltage is conducted through the cooling rod to the outside of the microscope so movements of the specimen-supporting table as well as the exchange of the object are not obstructed or impeded.
  • the thermoelement may be used to control a regulating member for maintaining the cooling temperature at a desired constant value.
  • Fig. 1 shows a sectional view of the object cartridge according to the invention
  • Fig. 2 shows a cross-section of a magnetic objective lens of an electron microscope equipped with the new object cartridge,.and
  • Fig. 3 shows a corresponding cross-section through the microscope tube.
  • the object cartridge embodying this invention comprises a generally cylindrical object cartridge member 1 into which is inserted a chamber structure 3, 4 consisting of copper.
  • This structure is heat-insulated from the body of the cartridge 1 by an annular intermediate member 2 of poor heat conductivity, which consists for instance of resinous plastic such as the plastic known under the trademark Trolitul.
  • the interior of the structure 3, 4 forms a cooling chamber 71.
  • the copper bushing 3 is capped at the bottom by screw cap 4.
  • Cap 4 comprises the specimen or object holder. It has a central cavity 40 in which are located the objectholding diaphragm 5 and the closure diaphragm 6. The diaphragms shade off a portion of the electron ray.
  • the object or specimen is indicated at 11 in Fig. l.
  • Bushing 3 is provided with apertures 7 and 70, which are axially aligned with aperture 40 of the cap. These openings form a passage for the electron ray.
  • the cooling chamber 3, 4 is in good heat-conducting connection with a cooling rod 8 of copper whose outer end is immersed in a coolant, as will be apparent from Fig. 2.
  • a block 9 of a different metal which forms a thermo-element together with the metal of which the bushing 3 is made.
  • the block 9 consists of a copper-nickel alloy known under the trade-mark Ni.
  • the voltage of the thermoelement formed by the parts 3 and 9 is etfective between the cooling rod 8 and a centrally located conductive pin 10.
  • the pin has point contact With the block 9 in order to dissipate a minimum amount of heat from the vicinity of the measuring location. Thus it does not disturb the temperature conditions in the vicinity of the thermoelement. This voltage is available at the outside of the microscope for the above-mentioned measuring or automatic regulating purposes as is herein below described.
  • the excitation winding of the objective lens is denoted by 110 and the magnetizable enclosure of the lens is denoted by 12.
  • the lens field proper is formed between the two pole shoes 13 and 14, which form the objective lens.
  • the object cartridge is introduced from above into the supporting table 15.
  • the heat conducting rod 8 passes through a bore 16 in the table 15 and is axially displaceably mounted in the outer rim portion 17 of the objective-lens body or casing.
  • a vacuum tight seal is secured by means of a rubber gasket 18.
  • a flange 19 attached to the rod 8 is engaged by a helical pressure spring 20. This spring, together with the flange 19, is held within a heat-insulating sleeve 21.
  • the rod 8 carries a downwardly-extending copper piece 22 which is immersed in a vessel 23 containing liquefied air for cooling of the rod 8.
  • the vessel 23 is vertically displaceable and can be raised or lowered by means of a motor 24 through a rack and gear mechanism 25.
  • a contactor 26 controls the motor to operate in one or the other direction. Contactor 26 connects the motor 24 with a current supply line 27. The contactor is in turn controlled by an amplifier 28 connected in the circuit of the thermo-element 3, 9 and which also contains a reference thermo-element 29.
  • Fig. 3 the object cartridge or specimen-supporting table 15 and the inserted object cartridge 1 are seen in top view.
  • the devices for displacing the table 15 in coordinate directions and to any desired extent comprise two control rods 30, 31 which form an angle of 90 with each other. These control rods pass through the body 17 of the objective lens in the conventional, vacuum-tight manner.
  • Two counter bias members 34 and 35 are located opposite the respective control rods 31 and 30 and are guided in the lens body 17 and urged inwardly by respective springs 32 and 34.
  • the cooling rod 8 is located between the counter bias members 34, 35 and is displaced relative to each of them by an angle of 45.
  • the cooling rod 8, as described above, is biased by the spring 20. It will be recognized that it is possible to conduct the.
  • thermo-voltage of the thermo-element 3, 9 through the rod 8 and the central pin to the outside of the microscope housing, without causing the object cartridge to be impeded or obstructed by the crosswise movement of table 15.
  • the rod 8 and pin 10 operate within the range of the object cartridge in cooperation with the sliding surfaces apparent from Fig. 1, so that the table and the cartridge 1 inserted therein can perform their displacing movements without hindrance.
  • an object holding device comprising a support, a structure carried by said support and thermally insulated therefrom, said structure forming a chamber having two coaxial apertures which are located on opposite sides respectively of said chamber and are in the electron optical axis of the microscope, said structure having at one axial end thereof an object mounting device comprising a member having a central opening in spaced coaxial disposition with respect to the apertures of said structure, the outer periphery of said member being in heat conductive contact with said structure, and a cooling device having a heat conductive body in heat conductive connection with said structure and extending away from the outer side of said structure to conductively dissipate heat from said chamber and object.
  • an object holding device comprising a support, a structure centrally carried by said support and thermally insulated therefrom, said structure forming a central chamber and having two coaxial apertures which are located on opposite sides respectively of said chamber and are in the electron optical axis of the microscope, said structure having at one axial end thereof a mounting device, a pair of spaced disc members in said mounting device having central openings in spaced coaxial disposition with respect to the apertures of said structure, one of said discs being an object mounting device, the outer periphery of said disc members being in heat conductive contact with said structure, and cooling means in heat conductive contact with said structure for cooling said structure down to at least minus centigrade.
  • an object holding device comprising an annular support, a structure centrally mounted in said support and thermally insulated therefrom, said structure forming a central chamber and having two coaxial apertures which are located on opposite sides respectively of said chamber and are in the electron optical axis of the microscope, a centrally apertured object holding member mounted in said structure, the aperture of said holding member being coaxial with respect to said coaxial apertures, and cooling means for reducing the temperature of said structure and said object holding member down to minus 80 centigrade or lower.
  • an object holding device comprising an annular support, a structure centrally mounted in said support and thermally insulated therefrom, said structure forming a central chamber and having two coaxial apertures which are located on opposite sides respectively of said chamber and are in the electron optical axis of the microscope, a centrally apertured object holding member mounted on said structure, the aperture of said holding member being coaxial with respect to said coaxial apertures, cooling means for reducing the temperature of said structure and said object holding member down to minus 80 centigrade or lower, said cooling means comprising a heat conductive rod having one end in contact with said structure and a heat conductive member immersed at one end in a low temperature coolant, the other end of said heat conductive rod being heat conductively connected with said heat conductive member.
  • the combination comprising an annular support member, a structure centrally mounted in said support member and thermally insulated therefrom, said structure forming a central chamber having opposite coaxially spaced end apertures which are in the electron optical axis of the microscope, a centrally apertured object holding member mounted on said structure, the aperture of said holding member being coaxial with respect to said end apertures, an ancured in said table, and cooling means for reducing the temperature of said structure and said object holding member down to minus 80 centigrade' or lower, said cooling means comprising a heat conductive rod having one end'in contact with said structure, a container filled with a low temperature coolant, a heat conductive member partially immersed in said coolant, the other end of said heat conductive rod being joined with said heat conductor rod, and resilient means for constraining said one end of said rod in heat conducting contact with said structure.
  • the combination comprising an annular support member, a structure centrally mounted in said support member and thermally insulated therefrom, said structure forming a central chamber having opposite coaxially spaced end apertures which are in the electron optical axis of the microscope, a centrally apertured object holding member mounted on said structure, the aperture of said holding member being coaxial with respect to said end apertures, an annular objective coil member, a displaceable table on said objective coil member, said support member being secured in said table, and cooling means for reducing the temperature of said structure and said object holding member down to minus 80 centigrade or lower, said cooling means comprising a heat conductive rod having one end in contact with said structure, a container filled with a low temperature coolant, a heat conductive member partially immersed at one end in said coolant, the other end of said heat conductive rod being joined with said heat conductor rod, and thermo-electric means associated with said structure for measuring the temperature thereof.
  • the combination comprising an annular support member, a structure centrally mounted in said support member and thermally insulated therefrom, said structure forming a central chamber. having opposite coaxially spaced end apertures which are in the electron optical axis of the microscope, a centrally apertured object holding member mounted on saidstructure, the aperture of said holding member being coaxial with respect to said end apertures, an annular objective coil member, a displaceable table on said objective coil member, said support member being secured in said table, and cooling means for reducing the temperature of said structure and said object holding member down to minus 80 centigrade or lower, said cooling means comprising a heat conductive rod having one end in contact with said structure, a container filled with a low temperature coolant, and a heat conductive member partially immersed in said coolant, the other end of said heat conductive rod being joined with said heat conductor rod, thermo-electric means associated with said structure for providing a control voltage proportional to the temperature of said structure, drive mechanism for varying the amount of immersion of said heat conductive member
  • thermo-element device producing a regulatory reference voltage
  • an object holding device comprising a support means, a heat conductive structure carried by said support means, the support means and structure being thermally insulated from each other, said structure forming a chamber having two coaxial apertures serving for the passage of electron rays and located on opposite sides respectively of said chamber, an apertured object holding means mounted in said chamber the aperture of which is on the axis defined by said coaxial apertures, and means for chilling the said heat conductive structure comprising an external cooling means located outside the microscope and a heat conductive body in heat conductive connection with thesaid structure and the said cooling means.
  • an object holding device comprising a support means, a heat conductive structure carried by said support means, the support means and structure being thermally insulated from each other, said structure forming a chamber having two coaxial apertures serving for the passage of electron rays and located on opposite sides respectively of said chamber, an apertured object holding means mounted in said chamber the aperture of which is on the axis defined by said coaxial apertures, and means for chilling the said heat conductive structure comprising an external cooling means located outside the microscope and a heat conductive body in heat conductive connection with the said structure and the said cooling means, the object holding means being in heat conducting relation to the structure, whereby it also is chilled.
  • an object holding device comprising a support means, a heat conductive structure carried by said support means, the support means and structure being thermally insulated from each other, said structure forming a chamber having two coaxial apertures serving for the passage of electron rays and located on opposite sides respectively of said chamber, an apertured object holding means mounted in said chamber the aperture of which is on the axis defined by said coaxial apertures, and means for chilling the said heat conductive structure comprising an external cooling means located outside the microscope and a heat conductive body in heat conductive connection with the said structure and the said cooling means, the object holding means being in heat conducting relation to the structure, whereby it also is chilled, the cooling means comprising means capable of cooling the inner walls of the heat conductive structure and the apertured object holding means down to at least below 0 C.
  • an object holding device comprising a support means, a heat conductive structure carried by said support means, the support means and structure being thermally insulated from each other, said structure forming a chamber having two coaxial apertures serving for the passage of electron rays and located on opposite sides respectively of said chamber, an apertured object holding means mounted in said chamber the aperture of which is on the axis defined by said coaxial apertures, and means for chilling the said heat conductive structure comprising an external cooling means located outside the microscope and a heat conductive body in heat conductive connection with the said structure and the said cooling means, and means responsive to the temperature of said heat conductive structure to control the chilling means to control the temperature of said heat conductive structure.
  • an object holding device comprising a support means, a heat conductive structure carried by said support means, the support means and structure being thermally insulated from each other, said structure forming a chamber having two coaxial apertures serving for the passage of electron rays and located on opposite sides respectively of said chamber, an apertured object holding means mounted in said chamber the aperture of which is on the axis defined by said coaxial apertures, and means for chilling the said heat conductive structure comprising an external cooling means located outside the microscope and a heat conductive body in heat conductive connection with the said structure and the said cooling means, the said heat conductive body comprising a hollow rod, an electro-conductive element passing through the hollow rod, a thermo-couple element carried by said heat con- References Cited in the file Of this patent ductive structure in position for contact with said electro- UNITED STATES A S conductive element, the thermo-couple element and the electro-conductive element comprising means responsive 2220973 Manon 1940 5 2,264,210 Krause Nov. 25, 1941 to the

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Electron Sources, Ion Sources (AREA)
US521852A 1954-07-14 1955-07-13 Object-holding device for electron microscopes Expired - Lifetime US2858444A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DES40018A DE1106439B (de) 1954-07-14 1954-07-14 Mit einer Kuehlvorrichtung ausgeruesteter Objekthalter fuer Elektronenmikroskope

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US (1) US2858444A (enrdf_load_stackoverflow)
CH (1) CH332309A (enrdf_load_stackoverflow)
DE (1) DE1106439B (enrdf_load_stackoverflow)
GB (1) GB794356A (enrdf_load_stackoverflow)
NL (2) NL198831A (enrdf_load_stackoverflow)

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2927209A (en) * 1957-07-05 1960-03-01 Jones Richard Norman Spectrometric cell structure and charging method therefor
US3008044A (en) * 1960-02-25 1961-11-07 Gen Electric Application of superconductivity in guiding charged particles
US3112398A (en) * 1960-02-15 1963-11-26 Shimula Yoshihiro Device for cooling the specimen in X-ray diffraction apparatus
US3124680A (en) * 1958-09-13 1964-03-10 Agent
US3151241A (en) * 1961-02-07 1964-09-29 Siemens Ag Heatable specimen carrier for electron radiation apparatus
US3171956A (en) * 1962-03-30 1965-03-02 Rca Corp Variant temperature environment for specimen stage of scientific instrument
US3171957A (en) * 1962-03-30 1965-03-02 Rca Corp Specimen holder for an electron microscope with means to support a specimen across a thermocouple junction
US3244877A (en) * 1961-02-28 1966-04-05 Siemens Ag Adjustable specimen holder for an electron microscope with heat conducting feathered leaf springs
US3373277A (en) * 1963-04-19 1968-03-12 Max Planck Gesellschaft Object cartridge wherein the specimen carrier is surrounded by a cooling chamber
US3387132A (en) * 1963-09-09 1968-06-04 Siemens Ag Particle beam apparatus with a cryogenically cooled specimen cartridge that is below the specimen holder temperature
US3521056A (en) * 1967-02-03 1970-07-21 Nippon Electron Optics Lab Adjustable specimen stage for electron beam apparatus employing adjusting levers arranged to minimize beam defocussing resulting from thermal expansion of stage components
US3525228A (en) * 1969-02-04 1970-08-25 Atomic Energy Commission Nonboiling liquid target for a high-energy particle beam
US3548189A (en) * 1965-06-16 1970-12-15 Aden B Meinel Method employing ion beams for polishing and figuring refractory dielectrics
US3973125A (en) * 1965-09-16 1976-08-03 Siemens Aktiengesellschaft Corpuscular-ray apparatus with a cryogenically cooled specimen space
US4071766A (en) * 1974-03-28 1978-01-31 Mta Kozponti Kemiai Kutato Intezet Micro-chamber for electron optical examinations particularly for the electron microscopic examination of biological objects
US4262194A (en) * 1979-12-18 1981-04-14 The United States Of America As Represented By The Department Of Health, Education & Welfare High resolution electron microscope cold stage
US4427891A (en) 1979-09-20 1984-01-24 Georges Adrien J P Variable temperature stage device for electron microscope
US5168004A (en) * 1988-08-25 1992-12-01 Basf Aktiengesellschaft Melt-spun acrylic fibers possessing a highly uniform internal structure which are particularly suited for thermal conversion to quality carbon fibers
CN119024903A (zh) * 2024-08-21 2024-11-26 崂山国家实验室 一种亚毫秒时间分辨率冷冻电镜样品温度控制系统

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT227797B (de) * 1961-04-13 1963-06-10 Hans Dipl Ing Dr Techn List Einrichtung zum Einstellen und Verändern der Raumlage von in einer Behandlungskammer zu behandelnden Gegenständen

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2220973A (en) * 1939-03-31 1940-11-12 Rca Corp Electron microscope
US2264210A (en) * 1937-11-20 1941-11-25 Krause Karl Means for mounting objects in electron microscopes
CH236120A (de) * 1942-04-29 1945-01-15 Fides Gmbh Verfahren zur Untersuchung eines Objektes in einem Korpuskularstrahlapparat.

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE659092C (de) * 1934-12-12 1938-04-25 Ernst Ruska Dr Ing Einschleusvorrichtung fuer an der Pumpe betriebene Korpuskularstrahlapparate
DE902535C (de) * 1941-12-11 1954-01-25 Manfred Von Ardenne Objekthalter fuer Elektronenstrahlgeraete

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2264210A (en) * 1937-11-20 1941-11-25 Krause Karl Means for mounting objects in electron microscopes
US2220973A (en) * 1939-03-31 1940-11-12 Rca Corp Electron microscope
CH236120A (de) * 1942-04-29 1945-01-15 Fides Gmbh Verfahren zur Untersuchung eines Objektes in einem Korpuskularstrahlapparat.

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2927209A (en) * 1957-07-05 1960-03-01 Jones Richard Norman Spectrometric cell structure and charging method therefor
US3124680A (en) * 1958-09-13 1964-03-10 Agent
US3112398A (en) * 1960-02-15 1963-11-26 Shimula Yoshihiro Device for cooling the specimen in X-ray diffraction apparatus
US3008044A (en) * 1960-02-25 1961-11-07 Gen Electric Application of superconductivity in guiding charged particles
US3151241A (en) * 1961-02-07 1964-09-29 Siemens Ag Heatable specimen carrier for electron radiation apparatus
US3244877A (en) * 1961-02-28 1966-04-05 Siemens Ag Adjustable specimen holder for an electron microscope with heat conducting feathered leaf springs
US3171956A (en) * 1962-03-30 1965-03-02 Rca Corp Variant temperature environment for specimen stage of scientific instrument
US3171957A (en) * 1962-03-30 1965-03-02 Rca Corp Specimen holder for an electron microscope with means to support a specimen across a thermocouple junction
US3373277A (en) * 1963-04-19 1968-03-12 Max Planck Gesellschaft Object cartridge wherein the specimen carrier is surrounded by a cooling chamber
US3387132A (en) * 1963-09-09 1968-06-04 Siemens Ag Particle beam apparatus with a cryogenically cooled specimen cartridge that is below the specimen holder temperature
US3548189A (en) * 1965-06-16 1970-12-15 Aden B Meinel Method employing ion beams for polishing and figuring refractory dielectrics
US3973125A (en) * 1965-09-16 1976-08-03 Siemens Aktiengesellschaft Corpuscular-ray apparatus with a cryogenically cooled specimen space
US3521056A (en) * 1967-02-03 1970-07-21 Nippon Electron Optics Lab Adjustable specimen stage for electron beam apparatus employing adjusting levers arranged to minimize beam defocussing resulting from thermal expansion of stage components
US3525228A (en) * 1969-02-04 1970-08-25 Atomic Energy Commission Nonboiling liquid target for a high-energy particle beam
US4071766A (en) * 1974-03-28 1978-01-31 Mta Kozponti Kemiai Kutato Intezet Micro-chamber for electron optical examinations particularly for the electron microscopic examination of biological objects
US4427891A (en) 1979-09-20 1984-01-24 Georges Adrien J P Variable temperature stage device for electron microscope
US4262194A (en) * 1979-12-18 1981-04-14 The United States Of America As Represented By The Department Of Health, Education & Welfare High resolution electron microscope cold stage
US5168004A (en) * 1988-08-25 1992-12-01 Basf Aktiengesellschaft Melt-spun acrylic fibers possessing a highly uniform internal structure which are particularly suited for thermal conversion to quality carbon fibers
CN119024903A (zh) * 2024-08-21 2024-11-26 崂山国家实验室 一种亚毫秒时间分辨率冷冻电镜样品温度控制系统

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Publication number Publication date
NL198831A (enrdf_load_stackoverflow)
NL101213C (enrdf_load_stackoverflow)
CH332309A (de) 1958-08-31
GB794356A (en) 1958-04-30
DE1106439B (de) 1961-05-10

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