US3729629A - Method for producing preparations for electromicroscopic examination - Google Patents
Method for producing preparations for electromicroscopic examination Download PDFInfo
- 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
- Authority
- US
- United States
- Prior art keywords
- organic polymer
- specimen
- chamber
- electrons
- preparation
- 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
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 20
- 230000001678 irradiating effect Effects 0.000 claims abstract description 6
- 229920000620 organic polymer Polymers 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 8
- -1 polyethylene terephthalate Polymers 0.000 claims description 8
- 229930195733 hydrocarbon Natural products 0.000 claims description 6
- 150000002430 hydrocarbons Chemical class 0.000 claims description 6
- 239000004698 Polyethylene Substances 0.000 claims description 5
- 229920000573 polyethylene Polymers 0.000 claims description 5
- 238000010894 electron beam technology Methods 0.000 claims description 4
- 238000005530 etching Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 150000002926 oxygen Chemical class 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 3
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 238000011835 investigation Methods 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 230000001105 regulatory effect Effects 0.000 abstract description 4
- 239000000126 substance Substances 0.000 description 11
- 230000035515 penetration Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 239000004215 Carbon black (E152) Substances 0.000 description 4
- 239000011888 foil Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 229920002799 BoPET Polymers 0.000 description 3
- 239000005041 Mylar™ Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005755 formation reaction Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- BAZVSMNPJJMILC-UHFFFAOYSA-N triadimenol Chemical compound C1=NC=NN1C(C(O)C(C)(C)C)OC1=CC=C(Cl)C=C1 BAZVSMNPJJMILC-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- 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.
Landscapes
- 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)
Abstract
A method for the production of preparation for electron microscopic investigation which includes irradiating the objects to be investigated in a high vacuum with electrons of a low energy and regulating an accelerating voltage to control the irradiation-chemical reaction.
Description
United States Patent 1 Grasenick et al.
METHOD FOR PRODUCING PREPARATIONS FOR ELEOTROMICROSCOPIC EXAMINATXON Inventors: Fritz Grasenick; Erich Jakopic, both of Steyrergasse 17, A 8010 Graz, Austria Filed: Dec. 7, 1970 App]. No.: 95,725
Foreign Application Priority Data Sept. 24, 1969 Austria ..9020/69 US. Cl. ..250 /49.5 TE, 250/83 CD, l56/2 Int. Cl ..H0lj 37/00. Field of Search 156/2; 250/83 CD Apr. 24. W73
[56] References Cited UNITED STATES PATENTS 3 6l2,87l lO/l97l Crawford et al. ..25()/83 CD Primary ExaminerJ. Steinberg Attorney-Watson, Cole, Grindle& Watson 57 ABSTRACT A method for the production of preparation for electron microscopic investigation which includes irradiating the objects to be investigated in a high vacuum with electrons of a low energy and regulating an accelerating voltage to control the irradiation-chemical reaction.
i 3 Claims, 2 Drawing Figures METHOD FOR PRODUCING PREPARATIONS FOR ELECTROMICROSCOPIC EXAMINATION This invention relates to a process for the production of preparations for electron microscopic investigation.
As is well known, the irradiation of organic high polymers with particles or quanta by radiation-chemical reaction frequently leads to a linking of the substances. This linking begins above a certain dose of irradiation (gel dose) and leads to the formation of an insoluble share which quickly increases with an increasing dose and which approaches a border value asymptotically. The development of an insoluble share in the irradiated substancemakes it appear possible to make use of this effect for the production of electron microscopic preparations of certain organic materials, such as for example polyethylene, rubber, and others. The question frequently arises indeed as to the structure of inhomogeneous organic materials which the expert working with the electron microscope tries to answer with the production and inventigation of thin slices, imprints and sheathings of the pertinent substance. However, the methods mentioned have various drawbacks such as for example, the development of deformations in the case of cutting thin slices or the effects which occur perhaps in the case of penetration of embedding agents into the substance. Impressions and sheathings mainly represent only the microgeometry of the surface and they will either permit no insight at all or only a very limited insight into the inside of the substance. Also the process of lifting thin layers from the organic substances by etching by means of activated oxygen and application of a layer of gelatin often does not lead to the goal, especially not when dealing with porous material. In these and other cases, the process according to the present invention will offer a remedy.
It is an object of the invention to create a process for the production of preparations for the electron microscopic investigation which no longer shows the previously explained defects of the known processes.
According to this invention, it will be solved in the case of a process for the production of preparations for the electron microscopic investigation by making use of radiation-chemical reactions by the fact that the objects to be investigated are irradiated in a high vacuum with electrons of low energy of maximum keV, so that within the area of a desirable penetration depth by the electrons which can be regulated by adjustment of accelerating voltage, a radiation-chemical reaction for example a linking of the material of the object will be brought about after which the irradiated layer having a different solubility is exposed by treatment of the nonirradiated object material and thus is ready for the known electron microscopic trans-irradiation.
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:
E(kev d(A) (E energy of the electrons in keV d depth of penetration in Angstrom units) Since thicknesses of layers of only a few hundred to a maximum of a few thousand A are needed for the electron microscopic investigation in the case of the customary irradiation voltages of 40 100 kV (depending on the density and a possibly existing porosity of the substance which is being irradiated), one must therefore use the irradiation, electron energy of a few tenths up to a few keV. The values given in the table however must be considered only as guide values and in the case of depth of penetration mentioned one is dealing with the so-called practical range, that is the distance from the surface of the preparation after passing through so that the kinetic energy of the electrons in the agent disappears. Nevertheless it becomes clear from the experiments made that the energy range used supplied fitting thicknesses of the layer.
For the linking of high polymer, a certain minimum irradiation dose is required.
Further object of the invention will be apparent from the following description when considered in connection with the accompanying drawings in which:
FIG. 1 is a diagram showing the increase with the dose of the insoluble share of branched polyethylene, and
FIG. 2 is a diagrammatic view of a ray producer system with a cooling means and circuit.
One can recognize from the curve of FIG. 1 that above a dose of approximately megarad it does not substantially increase any more.
For the production of natural or general layers according to the invention, 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. Experiments with 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. By regulation of the Wehneit voltage and of the focusing voltage, the density of the beam current on the preparation can be adjusted and the accelerating voltage of the electrodes can be varied dependent thereon. 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.
1f the irradiation of the preparation in the high vacuum (p 10 torr) is made without any special measures, then on the surface of the preparation a considerable or violent separation of layers of polymerizate (contamination) will occur. These layers originate as is known from hydrocarbon vapors which are present in standard installations even in the case of refined methods of operation. The vacuum pumps and gaskets, but also other components, which are located in the vacuum chamber and to which remnants of organic substances cling, are the main sources of these hydrocarbon vapors. These hydrocarbon vapors strike every surface inside the vacuum chamber with a finite dwell time and then are converted to a solid film by radiation-chemical reactions brought forth by the striking electrons. Now this disturbing phenomenon can be prevented for the most part by lowering the partial pressure of the hydrocarbon in the neighborhood of the preparation by the arrangement of a chamber cooled with liquid nitrogen. In that case the temperature of the cooling chamber should remain below l 30 C. At the same time, however, the object is to be at room temperature. FIG. 2 shows on the left-hand bottom, in section, the diagram of the cooling chamber. For the measurement of the preparation current, a Faraday cage mounted on the inside, is inserted into the cooling chamber.
For the production of the natural layers according to the invention, 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.
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. One can easily recognize the etching structure on the irradiated materials which shows itself in the natural layer. Besides the surface geometry, one can make visible here, inhomogeneous characteristics going beyond an imprint, remnants of catalysts, foreign substances, etc.
in the case of the investigation of millipore filters, a foam-like structure of the filter shows that the depth of penetration of the electrons is considerable since the thickness of the masses is light because of the porosity.
In this case the advantage of the natural layer process becomes particularly effective.
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. Probably, in this case too as in similar cases, the application of a reinforcing layer by evaporating quartz or gold prior to dissolving the organic substance and removing it will be advantageous for an increase in the stability and for the achievement of a cohesive pre aration.
he faithfulness in rendering pictures obtained with this process according to the invention is connected naturally with the type and magnitude of the effects of the induced rays which are caused by the electrons, and furthermore with the interference of the structure caused by the separation process. The linking of the frame of the organic substance brought about by the irradiation which frame consists mostly of carbon after a sufficiently high dose of rays (depending on the substance) is connected with a loss in mass. It is caused in the first place by the loss of hydrogen but depending on the compounding of the material, other gases too are liberated, such as for example C0, C0 CH N etc. The loss in mass may amount to 50 percent and more.
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.
We claim: 1. A process for the preparation of organic polymers for microscopic examination, comprising the steps of:
mounting an organic polymer specimen within a vacuum chamber, said 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.;
cooling the portions of said chamber remote from said specimen to at least l30 C. to reduce the partial pressures of hydrocarbons within said chamber and maintaining the specimen at substantially ambient temperature;
irradiating said specimen with a beam of electrons at an even beam density and the voltage of said electron beam is in the range of several tenths of a volt to several keV; and
removing at least a portion of the non-irradiated organic polymer.
2. A process as in claim 1 wherein the organic polymer is either branched or linear polyethylene and said irradiation dosage is in the range of 20 to Mrad.
3. 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.
Claims (3)
1. A process for the preparation of organic polymers for microscopic examination, comprising the steps of: mounting an organic polymer specimen within a vacuum chamber, said 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 5 torr.; cooling the portions of said chamber remote from said specimen to at least -130* C. to reduce the partial pressures of hydrocarbons within said chamber and maintaining the specimen at substantially ambient temperature; irradiating said specimen with a beam of electrons at an even beam density and the voltage of said electron beam is in the range of several tenths of a volt to several keV; and removing at least a portion of the non-irradiated organic polymer.
2. A process as in claim 1 wherein the organic polymer is either branched or linear polyethylene and said irradiation dosage is in the range of 20 to 80 Mrad.
3. 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.
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT902069A AT294937B (en) | 1969-09-24 | 1969-09-24 | Process for the production of preparations for examination by electron microscopy |
Publications (1)
Publication Number | Publication Date |
---|---|
US3729629A true US3729629A (en) | 1973-04-24 |
Family
ID=3610500
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US00095725A Expired - Lifetime US3729629A (en) | 1969-09-24 | 1970-12-07 | Method for producing preparations for electromicroscopic examination |
Country Status (5)
Country | Link |
---|---|
US (1) | US3729629A (en) |
JP (1) | JPS4824659B1 (en) |
AT (1) | AT294937B (en) |
DE (1) | DE2046720A1 (en) |
GB (1) | GB1286883A (en) |
Cited By (1)
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 (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH026931Y2 (en) * | 1984-12-27 | 1990-02-20 | ||
JPH0544077U (en) * | 1991-10-09 | 1993-06-15 | シンガー日鋼株式会社 | Bobbins |
Citations (1)
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 |
-
1969
- 1969-09-24 AT AT902069A patent/AT294937B/en not_active IP Right Cessation
-
1970
- 1970-09-22 DE DE19702046720 patent/DE2046720A1/en active Pending
- 1970-09-24 GB GB45610/70A patent/GB1286883A/en not_active Expired
- 1970-09-24 JP JP45083031A patent/JPS4824659B1/ja active Pending
- 1970-12-07 US US00095725A patent/US3729629A/en not_active Expired - Lifetime
Patent Citations (1)
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)
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 |
---|---|
GB1286883A (en) | 1972-08-23 |
DE2046720A1 (en) | 1971-04-15 |
AT294937B (en) | 1971-12-10 |
JPS4824659B1 (en) | 1973-07-23 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Danilatos et al. | Principles of scanning electron microscopy at high specimen chamber pressures | |
Bassim et al. | Recent advances in focused ion beam technology and applications | |
Brandes et al. | Submicron-resolution study of a thin Ni crystal using a brightness-enhanced positron reemission microscope | |
JP6143487B2 (en) | Method for making a vitrified sample for an electron microscope | |
Watt et al. | Charge contrast imaging of geological materials in the environmental scanning electron microscope | |
Cosslett | High-voltage electron microscopy | |
US3729629A (en) | Method for producing preparations for electromicroscopic examination | |
JP3428123B2 (en) | Method for producing surface-modified fluororesin | |
US4101772A (en) | Ion-beam etching method and an apparatus therefor | |
Ashworth | Field Eflasion Microscopy | |
Fullam | A closed wet cell for the electron microscope | |
CN109314031A (en) | Ion milling device | |
Orelovich et al. | Methods for preparing samples of track membranes for scanning electron microscopy | |
Jesser et al. | Adaptation of an ion accelerator to a high voltage electron microscope | |
US4340815A (en) | Preparation of material for examination by transmission electron microscopy techniques | |
Brandes et al. | Demonstration of positron re-emission microscopy using an immersion objective | |
Tuck | Surface studies of thermionic emitters by methods unique to them | |
Kawamata et al. | Direct Observation of Crystal Imperfections Introduced by Weak Electron Irradiation in Water-Etched KCl Single Crystal | |
Nikolaichik et al. | Electron beam writing in thin films of highly conducting solid electrolytes RbAg4I5 and CsAg4Br3− xI2+ x | |
Cosslett | Review Lecture-Perspectives in high voltage electron microscopy | |
Tagawa et al. | Application of the high resolution SEM to the fine structure study of polyethylene | |
JP2000266651A (en) | Preparation of analysis sample | |
Tacke et al. | High-resolution cryo-scanning electron microscopy of macromolecular complexes | |
Yang et al. | Stabilization and clarification of sections mounted on Formvar‐coated slot grids by deliberate irradiation in the electron beam | |
JPS5972040A (en) | Preparation of high polymer sample for electron- microscopic observation |