Oxidative cleaning method and apparatus for electron microscopes using an air plasma as an oxygen radical source

• US 6,105,589 A
• Filed: 01/11/1999
• Issued: 08/22/2000
• Est. Priority Date: 01/11/1999
• Status: Expired due to Term

• Current Assignee: Ronald A. Vane
• Original Assignee: Ronald A. Vane
• Inventors: Vane, Ronald A.
• Primary Examiner(s): EL ARINI, ZEINAB
• Application Number:
  US09/228,318
• Time in Patent Office: 589 Days
• Field of Search: 134/1.1, 134/1.2, 134/18, 204/192.34, 204/298.36
• US Class Current: 134/1.1
• CPC Class Codes: B08B 7/0035 by radiant energy, e.g. UV, laser, light beam or the like
• CPC Class Codes: B82Y 15/00 Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
• CPC Class Codes: H01J 2237/022 Avoiding or removing foreign or contaminating particles, debris or deposits on sample or tube
• CPC Class Codes: H01J 2237/28 Scanning microscopes
• CPC Class Codes: H01J 37/02 Details
• CPC Class Codes: H01J 37/32055 Arc discharge
• CPC Class Codes: H01J 37/32862 In situ cleaning of vessels and/or internal parts

Abstract

An improved method and apparatus are provided for cleaning the specimen and interior specimen chamber of Electron Microscopes, and similar electron beam instruments. The apparatus consists of a glow-discharge, oxygen-radical generator placed on a specimen chamber port with an excitation source to create a low-power glow-discharge plasma inside the generator. Air or other oxygen and nitrogen mixture is admitted to the generator at a pressure between 0.3 Torr and 5 Torr. The low power glow discharge is used to disassociate oxygen preferentially over nitrogen to create the oxygen radicals. The oxygen radicals then disperse by convection throughout the chamber to clean hydrocarbons from the surfaces of the chamber, stage and specimen by oxidation to CO and H₂ O gases. The excitation power of the plasma is limited to limit the nitrogen ion production that destroys the oxygen radicals and to limit the projection of the electrically active plasma into the specimen chamber. The optical emission or color of the plasma is observed for the selection of the correct power level for maximum oxygen radical production.

Claims

1. A method for simultaneous cleaning of specimen chamber, specimen and stage for Scanning Electron Microscope, Transmission Electron Microscope, Scanning Electron Microprobe or other charged particle beam instruments to remove hydrocarbon contaminants by oxidation by generating oxygen radicals from air or other nitrogen/oxygen gas mixtures under vacuum conditions produced within said specimen chamber of said instruments, said method comprising the steps of:

a) providing means for producing said oxygen radicals by a glow-discharge plasma;

b) providing means for temperature or power control of said glow-discharge plasma; and

c) using said temperature and power control to minimize ionization of nitrogen and maximize oxygen radical production in said plasma.

2. A method for simultaneous cleaning of specimen chamber, specimen, and stage as described in claim 1, further including the step of providing a plasma chamber connected to or inside said specimen chamber of said instruments to contain said glow discharge plasma.

3. A method for simultaneous cleaning of specimen chamber, specimen, and stage as described in claim 1, further including the step of providing a means of introducing air or other nitrogen/oxygen gas mixtures directly into said glow discharge plasma.

4. A method for simultaneous cleaning of specimen chamber, specimen, and stage as described in claim 1, further including the step of providing a vacuum gauge means and a gas regulating system means to regulate introduction of a gas into said instruments'"'"' specimen chamber.

5. A method for simultaneous cleaning of specimen chamber, specimen, and stage as described in claim 1, further including the step of controlling pressure within said specimen chamber to between 5 Torr and 0.3 Torr whereby said oxidation of hydrocarbons within said specimen chamber by said oxygen radicals is maximized.

6. A method for simultaneous cleaning of specimen chamber, specimen, and stage as described in claim 5 further including the step of employing a controller apparatus means to monitor chamber vacuum and to control venting and evacuation of said chamber, said gas mixture, said pressure, and glow-discharge power according to a planned sequence.

7. A method for simultaneous cleaning of specimen chamber, specimen, and stage as described in claim 1, further including the step of using means of venting and evacuation of said chamber provided by said instruments to partially backfill said specimen chamber with gas and then to re-evacuate said chamber.

8. A method for simultaneous cleaning of specimen chamber, specimen, and stage as described in claim 1 further including the step of using a means of observing optical emission or color from said plasma whereby said vacuum conditions and plasma temperature may be adjusted for maximum production of said oxygen radicals.

9. Apparatus for simultaneous cleaning of specimen chamber, specimen and stage for Scanning Electron Microscope, Analytical Electron Microscope, Scanning Electron Microprobe or other charged particle beam instruments to remove hydrocarbon contaminants by oxidation by generating oxygen radicals from air or other nitrogen/oxygen gas mixtures under vacuum conditions within said specimen chamber of said instruments, said apparatus comprising:

a means for producing oxygen radicals by a glow-discharge plasma; and

a means for temperature or power control of said glow-discharge plasma whereby within said plasma ionization of nitrogen can be minimized and the production of said oxygen radicals can be maximized.

10. Apparatus for simultaneous cleaning of specimen chamber, specimen, and stage as described in claim 9 with a plasma chamber connected to or inside the specimen chamber of said instruments to contain said glow discharge plasma.

11. Apparatus for simultaneous cleaning of specimen chamber, specimen, and stage as described in claim 10 further including a means of introducing air or other nitrogen/oxygen gas mixtures directly into said glow discharge plasma.

12. Apparatus for simultaneous cleaning of specimen chamber, specimen, and stage as described in claim 9 further including a vacuum gauge means and a gas regulating system means to regulate introduction of said gas mixtures into said glow discharge plasma.

13. Apparatus for simultaneous cleaning of specimen chamber, specimen, and stage as described in claim 12 further including a controller apparatus means that monitors said chamber vacuum and controls at least one of venting, evacuation, gas flow, gas mixture, pressure, and glow-discharge power according to a planned sequence.

14. Apparatus for simultaneous cleaning of specimen chamber, specimen, and stage as described in claim 13 wherein said apparatus is connected to means of venting and evacuation said specimen chamber of said instruments to partially backfill said specimen chamber with a gas and then to re-evacuate said chamber.