US3859535A - Apparatus for imparting contrast to a microscope object - Google Patents

Apparatus for imparting contrast to a microscope object Download PDF

Info

Publication number
US3859535A
US3859535A US262082A US26208272A US3859535A US 3859535 A US3859535 A US 3859535A US 262082 A US262082 A US 262082A US 26208272 A US26208272 A US 26208272A US 3859535 A US3859535 A US 3859535A
Authority
US
United States
Prior art keywords
electron
vacuum chamber
ion
source
gas
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
Application number
US262082A
Inventor
Gunter Bartz
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ernst Leitz Wetzlar GmbH
Original Assignee
Ernst Leitz Wetzlar GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Ernst Leitz Wetzlar GmbH filed Critical Ernst Leitz Wetzlar GmbH
Priority to US05/477,188 priority Critical patent/US3962057A/en
Application granted granted Critical
Publication of US3859535A publication Critical patent/US3859535A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

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
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/30—Electron or ion beam tubes for processing objects
    • H01J2237/31—Processing objects on a macro-scale
    • H01J2237/3151—Etching

Definitions

  • ABSTRACT The method of imparting contrast to the surface of an 30 Foreign Application priority Data object to be viewed microscopically comprises the June 21 1971 German 2130605 steps of 1ntroduc1ng the ob ect 1nto a vacuum chamy ber, connecting the object to the positive pole of a high voltage d.c. source, evacuating the chamber, [52] US.
  • the contrast is to be produced on a non-biological specimen.
  • a contrast may be generated on the surface of a non-biological specimen.
  • these methods have serious disadvantages.
  • wet etching and of anodic etching for generating colored layers on the specimen.
  • these methods are limited to a few particular applications.
  • By the so-called' annealing etching method thin colored oxide layers are produced on the object surface by heating the object in a special oven. But only few objects are suitable for this kind of operation.
  • an object of the present invention to provide a simple, effective method of producing contrast, especially color contrast, on the specimen to be examined. It is a further object to provide a method which consumes only little time. And it is a further object to provide a method which may be carried out under microscopic examination so that the user may establish the process and object conditions most favorable for the specific task.
  • a method of imparting contrast to a surface portion of an object to be investigated microscopically comprising the steps of introducing the object into a vacuum chamber, connecting the object to the positive pole of a regulatable high voltage direct current source, at least partially evacuating the chamber, bombarding a surface portion of the object with at least one gasconcentrated electron-ion beam, and feeding into the chamber gas which reacts chemically with the bombarded surface portion of the object.
  • the divergence of the impinging ion beam may be varied during the process and different gases may be introduced into the chamber successively.
  • the gases may also be introduced simultaneously as a mixture.
  • a relative movement between the object and the impinging beam may be generated.
  • a vacuum chamber I which is provided with an object carrier 2, which is connected electrically to the positive pole of a high voltage direct current source 3 and to earth.
  • the object 4 is mounted on the carrier 2.
  • the vacuum chamber 1 is provided with an ion gun 5 of the gas discharge type, which is connected on the one hand with the negative pole of the source 3, on the other hand with a regulatable gas source 6.
  • the vacuum chamber has an inlet 7 through which reagent gas is supplied, and an outlet 8 connected to a vacuum pump 9.
  • the ion gun 5 is operated by switching on the high tension and the gas supply from the source 6. There forms a gasconcentrated beam, the boundaries of which light up. The focussing of this beam is controlled in each case according to magnitude of the surface portion of the object, which is to be irradiated by the fine regulation of the gas supply from the source 6, for example by means of a needle valve. Simultaneously a gas reacting with the. object in a chemical way is supplied via the inlet 7. Under the effect of the electron beam and negative or neutralized ions, a reaction layer characteristic of the component parts of the object material then formsfwhich after conclusion of the contrasting process can be observed under a microscope and evaluated.
  • an indiyidual inlet 7 for the reaction gas it is possible to feed the gas directly via the ion gun 5. Also, a mixture of different gases may be fed into the chamber during the bombardment of the object.
  • the object carrier may be equipped with a suitable cooling device of known kind. Conversely, it may be desirable to increase the reaction speed and this can be achieved, for example, by heating the object.
  • the object carrier may be provided with a corresponding heating device.
  • reaction layers display, in direction towards the object parts not irradiated, a contrast falling off towards the edge.
  • means may be provided to effect relative movement between object and beam, which secure an uniform bombardment of all desired object surface portions.
  • the object may be bombarded simultaneously by beams derived from a plurality of electron-ion-beam sources.
  • the respective beams may then be directed towards the object from different directions and can be arranged to impinge on different surface portions of the object.
  • An apparatus for imparting contrast to the surface portion of an object to be investigated microscopically comprising: i
  • a combined electron-ion gun ('5) of the gas discharging type mounted in the wall of the vacuum chamber opposite from the object carrier, the cathode of said combined electron-ion gun being connected to the negative pole of the DC. source and means for supplying a reagent gas into the vacuum chamber;

Abstract

The method of imparting contrast to the surface of an object to be viewed microscopically comprises the steps of introducing the object into a vacuum chamber, connecting the object to the positive pole of a high voltage d.c. source, evacuating the chamber, bombarding the surface of the object with a gasconcentrated electron-ion beam, and feeding into the chamber a gas which reacts chemically with the bombarded object surface. Under the effect of the electron beam and negative or neutralized ions then forms a reaction layer characteristic of the component parts of the object material which layer, after the conclusion of the contrasting process can be observed and evaluated under a microscope.

Description

Unite States Patent 1191 Bartz Jan. 7, 1975 [54] APPARATUS FOR IMPARTING CONTRAST 3,477,936 11/1969 Gillery et al, 204/192 o A MICROSCOPE OBJECT 3,604,970 9/1971 Culbertson et a1. 204/298 X 3,650,930 3/1972 Jones et a]. 204/177 Inventor: Gunter Bartl, Wetzlar, G y 3,704,216 11/1972 Kinstley et a1 204/164 [73] Assignee: Ernst Leitz GmbH, Wetzlar,
Germany Primary Examiner-F. C. Edmundson [22] F] d J 12 1972 Attorney, Agent, or FirmKrafft & Wells 1e une [21] Appl. No.: 262,082 [57] ABSTRACT The method of imparting contrast to the surface of an 30 Foreign Application priority Data object to be viewed microscopically comprises the June 21 1971 German 2130605 steps of 1ntroduc1ng the ob ect 1nto a vacuum chamy ber, connecting the object to the positive pole of a high voltage d.c. source, evacuating the chamber, [52] US. Cl 250/542, 220045126948, 22054/l59321, bombarding the surface of the Object with a g [51] Int Cl Bolk A61 concentrated electron-ion beam, and feeding into the [58] Field 56 chamber a gas which reacts chemically with the b0m "556 barded object surface Under the effect of the electron beam and negative or neutralized ions then forms a tion layer characteristic of the component parts of [56] References Cited mac the ob ect mater1al whlch layer, after the conclus1on UNITED STATES PATENTS of the contrasting process can be observed and evalu- 2,200,909 5/1940 Berghaus 6! al. 204/298 X ated under a microscope 3,308,049 3/1967 Jones et al. 250/531 3,418,229 12/1968 Lakshmanon et a1. 204/164 1 Claim, 1 Drawlng Figure 5/ f7 L a Patented Jan, 7, 1975 3,859,535
if the contrast is to be produced on a non-biological specimen. There are, of course, several methods known by which a contrast may be generated on the surface of a non-biological specimen, however, all these methods have serious disadvantages. There are, for example, the methods of wet etching and of anodic etching for generating colored layers on the specimen. However, these methods are limited to a few particular applications. By the so-called' annealing etching method thin colored oxide layers are produced on the object surface by heating the object in a special oven. But only few objects are suitable for this kind of operation.
Further, a method of producing thin, highly refracting and light-transmissive layers on the object is known, which layers amplify considerably the natural object contrast. The layer is produced by evaporation in a high vacuum. This method, however, is only applicable in scientific research and not in routine investigations,
on account of the great expenditures both of apparaferent erosion of the component parts of the object.
Subsequent oxydization by positive air or oxygen ions will highly amplify the contrast. However, the exact relation between the grey shades or the color and the chemical material is greatly lost by the ion-etching.
It is, therefore, an object of the present invention to provide a simple, effective method of producing contrast, especially color contrast, on the specimen to be examined. It is a further object to provide a method which consumes only little time. And it is a further object to provide a method which may be carried out under microscopic examination so that the user may establish the process and object conditions most favorable for the specific task.
SUMMARY OF THE INVENTION According to the invention, there is provided a method of imparting contrast to a surface portion of an object to be investigated microscopically, comprising the steps of introducing the object into a vacuum chamber, connecting the object to the positive pole of a regulatable high voltage direct current source, at least partially evacuating the chamber, bombarding a surface portion of the object with at least one gasconcentrated electron-ion beam, and feeding into the chamber gas which reacts chemically with the bombarded surface portion of the object.
In addition to the above steps the divergence of the impinging ion beam may be varied during the process and different gases may be introduced into the chamber successively. However, the gases may also be introduced simultaneously as a mixture. Further, it is possible to bombard the object simultaneously with the beams of several ion sources. And finally, a relative movement between the object and the impinging beam may be generated.
BRIEFDESCRIPTION OF THE DRAWING 'The invention will be more readily comprehended from the following description when taken in conjunction with the appending drawing which shows an appa ratus for performing the invented method.
DESCRIPTION OF THE PREFERRED EMBODIMENT For carrying out the method, a vacuum chamber I is used, which is provided with an object carrier 2, which is connected electrically to the positive pole of a high voltage direct current source 3 and to earth. The object 4 is mounted on the carrier 2. The vacuum chamber 1 is provided with an ion gun 5 of the gas discharge type, which is connected on the one hand with the negative pole of the source 3, on the other hand with a regulatable gas source 6. The vacuum chamber has an inlet 7 through which reagent gas is supplied, and an outlet 8 connected to a vacuum pump 9. After the object 4 is mounted on the object carrier 2 and the vacuum chamber 1 is closed, an underpressure of for example 10 Torr is generated in the vacuum chamber by means of the vacuum pump 9 and maintained. Now the ion gun 5 is operated by switching on the high tension and the gas supply from the source 6. There forms a gasconcentrated beam, the boundaries of which light up. The focussing of this beam is controlled in each case according to magnitude of the surface portion of the object, which is to be irradiated by the fine regulation of the gas supply from the source 6, for example by means of a needle valve. Simultaneously a gas reacting with the. object in a chemical way is supplied via the inlet 7. Under the effect of the electron beam and negative or neutralized ions, a reaction layer characteristic of the component parts of the object material then formsfwhich after conclusion of the contrasting process can be observed under a microscope and evaluated.
Instead of using, as shown, an indiyidual inlet 7 for the reaction gas, it is possible to feed the gas directly via the ion gun 5. Also, a mixture of different gases may be fed into the chamber during the bombardment of the object.
In order to protect objects against impermissible heating during the reaction, the object carrier may be equipped with a suitable cooling device of known kind. Conversely, it may be desirable to increase the reaction speed and this can be achieved, for example, by heating the object. For this purpose, the object carrier may be provided with a corresponding heating device.
The reaction layers display, in direction towards the object parts not irradiated, a contrast falling off towards the edge. In order to counteract this, means may be provided to effect relative movement between object and beam, which secure an uniform bombardment of all desired object surface portions.
The object may be bombarded simultaneously by beams derived from a plurality of electron-ion-beam sources. The respective beams may then be directed towards the object from different directions and can be arranged to impinge on different surface portions of the object.
[t is possible to provide one or more stops or masks in the path of the or each bombarding beam, which cause an exact limiting of the bombarded region.
What is claimed is:
1. An apparatus for imparting contrast to the surface portion of an object to be investigated microscopically, the apparatus comprising: i
a. a non-grounded vacuum chamber (1);
b. an object carrier (2) inside the vacuum chamber for disposing an object thereon, the carrier being connected to one wall of the chamber;
0. a high voltage D.C. source (3) outside the vacuum chamber, the positive pole of the DC. source being connected to the object carrier and to the ground;
d. a combined electron-ion gun ('5) of the gas discharging type mounted in the wall of the vacuum chamber opposite from the object carrier, the cathode of said combined electron-ion gun being connected to the negative pole of the DC. source and means for supplying a reagent gas into the vacuum chamber;
f. means for evacuating the vacuum chamber; and g. switching means located between said negative pole and said electron-ion upon closing of which the voltage between the object an d the electron-ion gun causes an electron-ion beam to impinge on the object where a layer characteristic of the component parts of the object material is formed.

Claims (1)

1. An apparatus for imparting contrast to the surface portion of an object to be investigated microscopically, the apparatus comprising: a. a non-grounded vacuum chamber (1); b. an object carrier (2) inside the vacuum chamber for disposing an object thereon, the carrier being connected to one wall of the chamber; c. a high voltage D.C. source (3) outside the vacuum chamber, the positive pole of the D.C. source being connected to the object carrier and to the ground; d. a combined electron-ion gun (5) of the gas discharging type mounted in the wall of the vacuum chamber opposite from the object carrier, the cathode of said combined electron-ion gun being connected to the negative pole of the D.C. source and being so adjusted that an electron-ion-beam derived from the gun impinges on an object, which is electrically conductive, positioned on the object carrier, and wherein the ion gun of the said combined electron-ion gun has a regulatable gas source connected thereto for bombarding said surface portion of an object with a gas concentrated electron ion-beam; e. means for supplying a reagent gas into the vacuum chamber; f. means for evacuating the vacuum chamber; and g. switching means located between said negative pole and said electron-ion upon closing of which the voltage between the object and the electron-ion gun causes an electron-ion beam to impinge on the object where a layer characteristic of the component parts of the object material is formed.
US262082A 1971-06-21 1972-06-12 Apparatus for imparting contrast to a microscope object Expired - Lifetime US3859535A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US05/477,188 US3962057A (en) 1971-06-21 1974-06-07 Method of imparting contrast to a microscope object

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE2130605A DE2130605C3 (en) 1971-06-21 1971-06-21 Contrasting method for objects to be examined microscopically

Related Child Applications (1)

Application Number Title Priority Date Filing Date
US05/477,188 Division US3962057A (en) 1971-06-21 1974-06-07 Method of imparting contrast to a microscope object

Publications (1)

Publication Number Publication Date
US3859535A true US3859535A (en) 1975-01-07

Family

ID=5811289

Family Applications (1)

Application Number Title Priority Date Filing Date
US262082A Expired - Lifetime US3859535A (en) 1971-06-21 1972-06-12 Apparatus for imparting contrast to a microscope object

Country Status (8)

Country Link
US (1) US3859535A (en)
JP (1) JPS5616367B1 (en)
AT (1) AT336306B (en)
CH (1) CH541137A (en)
DE (1) DE2130605C3 (en)
FR (1) FR2142998B1 (en)
GB (1) GB1353424A (en)
SE (1) SE375381B (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4307283A (en) * 1979-09-27 1981-12-22 Eaton Corporation Plasma etching apparatus II-conical-shaped projection
US4614639A (en) * 1985-04-26 1986-09-30 Tegal Corporation Compound flow plasma reactor
US4915917A (en) * 1987-02-19 1990-04-10 The Johns Hopkins University Glow discharge unit
US5148714A (en) * 1990-10-24 1992-09-22 Ag Processing Technology, Inc. Rotary/linear actuator for closed chamber, and reaction chamber utilizing same

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2433690C2 (en) * 1974-07-12 1984-04-26 Kernforschungszentrum Karlsruhe Gmbh, 7500 Karlsruhe Device for the surface treatment of a metallographic sample

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2200909A (en) * 1937-11-30 1940-05-14 Berghaus Metallization of metal articles by cathode disintegration
US3308049A (en) * 1963-03-06 1967-03-07 Gen Electric Glow discharge apparatus for treating workpieces
US3418229A (en) * 1965-06-30 1968-12-24 Weston Instruments Inc Method of forming films of compounds having at least two anions by cathode sputtering
US3477936A (en) * 1967-06-29 1969-11-11 Ppg Industries Inc Sputtering of metals in an atmosphere of fluorine and oxygen
US3604970A (en) * 1968-10-14 1971-09-14 Varian Associates Nonelectron emissive electrode structure utilizing ion-plated nonemissive coatings
US3650930A (en) * 1969-10-27 1972-03-21 Gen Electric Glow discharge masking process
US3704216A (en) * 1969-09-11 1972-11-28 Texas Instruments Inc Method of depositing a metal oxide film by electron bombardment

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2200909A (en) * 1937-11-30 1940-05-14 Berghaus Metallization of metal articles by cathode disintegration
US3308049A (en) * 1963-03-06 1967-03-07 Gen Electric Glow discharge apparatus for treating workpieces
US3418229A (en) * 1965-06-30 1968-12-24 Weston Instruments Inc Method of forming films of compounds having at least two anions by cathode sputtering
US3477936A (en) * 1967-06-29 1969-11-11 Ppg Industries Inc Sputtering of metals in an atmosphere of fluorine and oxygen
US3604970A (en) * 1968-10-14 1971-09-14 Varian Associates Nonelectron emissive electrode structure utilizing ion-plated nonemissive coatings
US3704216A (en) * 1969-09-11 1972-11-28 Texas Instruments Inc Method of depositing a metal oxide film by electron bombardment
US3650930A (en) * 1969-10-27 1972-03-21 Gen Electric Glow discharge masking process

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4307283A (en) * 1979-09-27 1981-12-22 Eaton Corporation Plasma etching apparatus II-conical-shaped projection
US4614639A (en) * 1985-04-26 1986-09-30 Tegal Corporation Compound flow plasma reactor
US4915917A (en) * 1987-02-19 1990-04-10 The Johns Hopkins University Glow discharge unit
US5148714A (en) * 1990-10-24 1992-09-22 Ag Processing Technology, Inc. Rotary/linear actuator for closed chamber, and reaction chamber utilizing same

Also Published As

Publication number Publication date
CH541137A (en) 1973-08-31
FR2142998A1 (en) 1973-02-02
SE375381B (en) 1975-04-14
GB1353424A (en) 1974-05-15
DE2130605C3 (en) 1974-02-07
FR2142998B1 (en) 1973-07-13
JPS5616367B1 (en) 1981-04-16
DE2130605A1 (en) 1973-01-11
AT336306B (en) 1977-04-25
ATA491772A (en) 1976-08-15
DE2130605B2 (en) 1973-07-19

Similar Documents

Publication Publication Date Title
EP1238406B1 (en) Gas cluster ion beam smoother apparatus
JP4926067B2 (en) Ionizer and method for gas cluster ion beam formation
US4740267A (en) Energy intensive surface reactions using a cluster beam
US4775789A (en) Method and apparatus for producing neutral atomic and molecular beams
JPS6254078A (en) Apparatus for depositing membrane to substrate by cathodic sputtering treatment
US4541890A (en) Hall ion generator for working surfaces with a low energy high intensity ion beam
JPH0543785B2 (en)
US4496449A (en) Electron beam etching of integrated circuit structures
US3859535A (en) Apparatus for imparting contrast to a microscope object
GB881458A (en) Method for heating materials by electron bombardment in a vacuum
JPH1125894A (en) Plasma ion shower sample treating device and its method
EP0094473B1 (en) Apparatus and method for producing a stream of ions
EP0658917A2 (en) Fine-processing apparatus using low-energy neutral particle beam
US3962057A (en) Method of imparting contrast to a microscope object
US5089289A (en) Method of forming thin films
US20090020415A1 (en) "Iontron" ion beam deposition source and a method for sputter deposition of different layers using this source
JP2849771B2 (en) Sputter type ion source
JPH08104980A (en) Cluster ion beam sputtering device
KR900008155B1 (en) Method and apparatus for forming a thin fim
JPH0214426B2 (en)
US3138736A (en) Electron beam generator system
JPH10106798A (en) High-speed atomic beam source
JPH03111558A (en) Sputtering device
JPS60262964A (en) Device for vapor-depositing compound thin film
CN116259518A (en) Method for analyzing ionization condition of powder in offline mode