US3729629A - Method for producing preparations for electromicroscopic examination - Google Patents

Method for producing preparations for electromicroscopic examination Download PDF

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Publication number
US3729629A
US3729629A US00095725A US3729629DA US3729629A US 3729629 A US3729629 A US 3729629A US 00095725 A US00095725 A US 00095725A US 3729629D A US3729629D A US 3729629DA US 3729629 A US3729629 A US 3729629A
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United States
Prior art keywords
organic polymer
specimen
chamber
electrons
preparation
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Expired - Lifetime
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US00095725A
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English (en)
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E Jakopic
F Grasenick
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Individual
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/081—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing particle radiation or gamma-radiation
    • B01J19/085—Electron beams only
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32—Polishing; Etching
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21H—OBTAINING ENERGY FROM RADIOACTIVE SOURCES; APPLICATIONS OF RADIATION FROM RADIOACTIVE SOURCES, NOT OTHERWISE PROVIDED FOR; UTILISING COSMIC RADIATION
    • G21H5/00—Applications of radiation from radioactive sources or arrangements therefor, not otherwise provided for 
    • 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
    • H01J37/30—Electron-beam or ion-beam tubes for localised treatment of objects
    • H01J37/305—Electron-beam or ion-beam tubes for localised treatment of objects for casting, melting, evaporating, or etching
    • H01J37/3053—Electron-beam or ion-beam tubes for localised treatment of objects for casting, melting, evaporating, or etching for evaporating or etching

Definitions

  • the basis of the process according to the present invention is therefore the irradiation with electrons of a relatively low energy of the material that is to be investigated and to be sure under conditions which will largely prevent an impermissible heating of the preparation and a growth of disturbing layers of polymerize (contamination). Because of their low energy the depth of penetration by the electrons is slight.
  • the thickness of this layer can be estimated according to known formulas, whereby one will obtain numerical values, for example, for polyethylene:
  • FIG. 1 is a diagram showing the increase with the dose of the insoluble share of branched polyethylene
  • FIG. 2 is a diagrammatic view of a ray producer system with a cooling means and circuit.
  • an electron ray producing system will be required in which the beam current and the beam voltage can be regulated as much as possible independently of one another and in which an even density of the beam current on the preparation will be produced.
  • the ray producing system of a TV picture tube were carried out, whose oxide cathode was replaced by a large surface cathode coated with lanthanum boride.
  • Lanthanum boride is suitable as an emission layer in the case of good emission characteristics, above all, whenever the recipient is being frequently ventilated because an action by the air will not harm this cathode in its cold state.
  • FIG. 2 shows the diagram of the ray producer system with a cooling chamber and also the circuit for operation of the ray producing system.
  • the numeral 1 on the drawing designates the electron gun, 2 the electron lens, 3 the cooling chamber, 4 a thermoelement, 5 the Faraday cage, 6 an insulating ring, 7 a plate for the preparation and 8 the preparation itself. Further letters A, B and C designate sources for the voltage and D a recorder.
  • FIG. 2 shows on the left-hand bottom, in section, the diagram of the cooling chamber.
  • a Faraday cage mounted on the inside is inserted into the cooling chamber.
  • foils made of polyvinyl alcohol, polyethylene terephthalate (Mylar), acetobutyrate (Triafol), also millipore filters and nucleopore filters were irradiated. Investigations were made with Mylar foils, millipore filters and nucleopore filters.
  • the foil Prior to the irradiation of the Mylar foils, the foil was cauterized or etched with activated oxygen in a high frequency gas discharge for the purpose of developing the structure.
  • activated oxygen in a high frequency gas discharge for the purpose of developing the structure.
  • nucleopore filters In pictures of nucleopore filters, one can recognize the homogeneousness of the pores which continue to the inside of the filter as approximately cylindrical channels, and these filters are built up differently than the foam-like diaphragm filters and they are particularly interesting in the cases of analytical work.
  • the irradiated material shows that the channels follow some holes as hose-like structures, but in most cases however these formations are lacking since they are torn away during the separation process. It is probable that by a high accelerating voltage and because of the greater depth of penetration brought forth thereby, a better mechanical stability of the hose-like formations will be achieved.
  • the separation process according to the invention is particularly suited also for the investigation of biological objects as well as complex colloidal systems, preferably in connection with freeze drying or low temperature sublimation (for example, in the case of swol len plastics or plastic emulsions), since a presentation of a third dimension becomes possible therewith. Furthermore, in contrast to the imprint technique, the differences in the thickness of the mass (enclosures, pores, etc.) can be made directly visible.
  • organic polymer being selected from the group consisting of polyvinyl alcohol, polyethylene terephthalate, and acetobutyrate; reducing the pressure within said chamber to at least 10' torr.;
  • a process as in claim 1 further comprising a step of etching said organic polymer with activated oxygen in a high frequency gas discharge prior to irradiating with said electron beam.

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Toxicology (AREA)
  • Biochemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Treatments Of Macromolecular Shaped Articles (AREA)
US00095725A 1969-09-24 1970-12-07 Method for producing preparations for electromicroscopic examination Expired - Lifetime US3729629A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
AT902069A AT294937B (de) 1969-09-24 1969-09-24 Verfahren zur Herstellung von Präparaten für die elektronenmikroskopische Untersuchung

Publications (1)

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US3729629A true US3729629A (en) 1973-04-24

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US00095725A Expired - Lifetime US3729629A (en) 1969-09-24 1970-12-07 Method for producing preparations for electromicroscopic examination

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US (1) US3729629A (de)
JP (1) JPS4824659B1 (de)
AT (1) AT294937B (de)
DE (1) DE2046720A1 (de)
GB (1) GB1286883A (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030020024A1 (en) * 1999-12-29 2003-01-30 Etienne Ferain Method for creating pores and microporous film

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0544077U (ja) * 1991-10-09 1993-06-15 シンガー日鋼株式会社 ボビン

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3612871A (en) * 1969-04-01 1971-10-12 Gen Electric Method for making visible radiation damage tracks in track registration materials

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3612871A (en) * 1969-04-01 1971-10-12 Gen Electric Method for making visible radiation damage tracks in track registration materials

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030020024A1 (en) * 1999-12-29 2003-01-30 Etienne Ferain Method for creating pores and microporous film

Also Published As

Publication number Publication date
AT294937B (de) 1971-12-10
GB1286883A (en) 1972-08-23
DE2046720A1 (de) 1971-04-15
JPS4824659B1 (de) 1973-07-23

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