Radio-frequency powered glow discharge device and method with high voltage interface

• US 5,325,021 A
• Filed: 09/11/1992
• Issued: 06/28/1994
• Est. Priority Date: 04/09/1992
• Status: Expired due to Fees

• Current Assignee: Clemson University, United States Department of Energy
• Original Assignee: Clemson University
• Inventors: Duckworth, Douglas C., Lewis, Trousdale A., Donohue, David L., Marcus, R. Kenneth
• Primary Examiner(s): Pascal, Robert J.
• Assistant Examiner(s): KINKEAD, ARNOLD M
• Application Number:
  US07/944,216
• Time in Patent Office: 655 Days
• Field of Search: 250/288, 250/281, 315/221 R, 315/244, 315/163, 315/176, 315/111.21, 315/111.41, 315/111.81, 315/111.51
• US Class Current: 315/111.51
• CPC Class Codes: H01J 49/105 using high-frequency excitation, e.g. microwave excitation, Inductively Coupled Plasma [ICP]

Abstract

A high voltage accelerating potential, which is supplied by a high voltage direct current power supply, is applied to the electrically conducting interior wall of an RF powered glow discharge cell. The RF power supply desirably is electrically grounded, and the conductor carrying the RF power to the sample held by the probe is desirably shielded completely excepting only the conductor'"'"'s terminal point of contact with the sample. The high voltage DC accelerating potential is not supplied to the sample. A high voltage capacitance is electrically connected in series between the sample on the one hand and the RF power supply and an impedance matching network on the other hand. The high voltage capacitance isolates the high DC voltage from the RF electronics, while the RF potential is passed across the high voltage capacitance to the plasma. An inductor protects at least the RF power supply, and desirably the impedance matching network as well, from a short that might occur across the high voltage capacitance. The discharge cell and the probe which holds the sample are configured and disposed to prevent the probe'"'"'s components, which are maintained at ground potential, from bridging between the relatively low vacuum region in communication with the glow discharge maintained within the cell on the one hand, and the relatively high vacuum region surrounding the probe and cell on the other hand. The probe and cell also are configured and disposed to prevent the probe'"'"'s components from electrically shorting the cell'"'"'s components.

Claims

1. An apparatus for using radio frequency electromagnetic energy to form a glow discharge from a solid sample for use in a mass spectrometer, whether the sample is electrically conducting or nonconducting, and whether the sample is machineable or nonmachineable, the apparatus comprising:

(a) an enclosure,

i) said enclosure defining a vacuum chamber,

ii) said enclosure defining an electrically conducting counterelectrode having a surface exposed to the interior of said vacuum chamber;

(b) means for disposing the sample relative to said counterelectrode such that application of a predetermined radio frequency electrical potential between the sample and said counterelectrode in the presence of an inert gas inside said vacuum chamber forms a sustainable glow discharge;

(c) means for generating a radio frequency electromagnetic potential;

(d) means for electrically connecting to the sample the radio frequency electromagnetic potential generated by said generating means;

(e) means for applying a preselected high direct current voltage to said counterelectrode to aid in providing ions from the glow discharge for subsequent analysis;

(f) means for matching the impedance of said generating means and a combination of said connecting means, said counterelectrode, the sample disposed by said disposing means, said disposing means, and the glow discharge, said impedance matching means being electrically connected in series between said electrically connecting means and said generating means; and

(g) means for blocking direct current flow between said electrically connecting means and said impedance matching means due to said preselected high direct current voltage.

2. An apparatus as in claim 1, wherein said sample disposing means includes:

i) an annular insulating member configured and disposed with one end connected to said enclosure and defining an elongated opening therethrough; and

ii) a vacuum sealing O-ring configured and disposed about said elongated opening in the vicinity of the end of said annular insulating member opposite said one end connected to said enclosure.

5. An apparatus as in claim 1, wherein said electrically connecting means comprises:

i) a radio frequency coaxial cable,

ii) a first coaxial connector electrically connected to one end of said radio frequency coaxial cable,

iii) an elongated conductor having a first end and a second end disposed opposite said first end, said first end of said conductor being electrically connected to said first coaxial connector,

iv) a second coaxial connector disposed so that upon engaging said first coaxial connector said second end of said conductor electrically engages the sample during operation of the apparatus,

v) an electrically insulating sheath surrounding said conductor between said first and second ends of said conductor, and

an electrically conducting shield surrounding said conductor upstream of where said terminal contacts the sample.

6. An apparatus as in claim 1, wherein said sample disposing means includes an external mounting plate and a flexible gasket for sealing the sample against said mounting plate.

7. An apparatus as in claim 1, further comprising:

(h) an inductive impedance electrically connected as a choke coil to protect said impedance matching means and said radio frequency electromagnetic potential generating means against electronic shorting of said direct current flow blocking means.

8. An apparatus as in claim 1, further comprising:

(h) an inductive impedance electrically connected in series between said counterelectrode and said means for applying a preselected high direct current voltage to said counterelectrode.

9. An apparatus as in claim 8, further comprising:

(i) a capacitive impedance electrically connected in parallel between said inductive impedance and said means for applying a preselected high direct current voltage to said counterelectrode.

10. An apparatus as in claim 1, wherein said high direct current voltage applying means includes a direct current transformer.

11. An apparatus as in claim 1, wherein said radio frequency electromagnetic potential generating means includes a radio frequency generator capable of generating at least 300 volts at a frequency of at least one megahertz.

12. An apparatus as in claim 1, wherein said direct current blocking means includes an isolating high voltage capacitance electrically connected in series between said electrically connecting means and said impedance matching means.

13. An apparatus as in claim 1, wherein said impedance matching means includes a high voltage capacitor electrically connected in series with said radio frequency electromagnetic electric potential generating means.

14. An apparatus as in claim 1, wherein said means for generating a radio frequency electromagnetic potential includes means for electrically shielding the generated radio frequency electromagnetic potential.

15. An apparatus as in claim 14, wherein said means for electrically shielding the generated radio frequency electromagnetic potential, comprises:

i) a cylindrically configured electrically conducting shield surrounding said electrically connecting means upstream of where said electrically connecting means electrically connects the radio frequency electromagnetic potential to the sample.

16. An apparatus as in claim 1, further comprising:

i) a mass spectrometer configured and disposed for receiving matter removed from the glow discharge for subsequent analysis.

3. An apparatus for using radio frequency electromagnetic energy to form a glow discharge from a solid sample for use in a mass spectrometer, whether the sample is electrically conducting or nonconducting, and whether the sample is machineable or nonmachineable, the apparatus comprising:

(a) an enclosure,

i) said enclosure defining a vacuum chamber,

ii) said enclosure defining an electrically conducting counterelectrode having a surface exposed to the interior of said vacuum chamber;

(b) means for disposing the sample relative to said counterelectrode such that application of a predetermined radio frequency electrical potential between the sample and said counterelectrode in the presence of an inert gas inside said vacuum chamber forms a sustainable glow discharge;

(c) means for generating a radio frequency electromagnetic potential;

(d) means for electrically connecting to the sample the radio frequency electromagnetic potential generated by said generating means;

(e) means for applying a preselected high direct current voltage to said counterelectrode to aid in providing ions from the glow discharge for subsequent analysis;

(f) means for matching the impedance of said generating means and said combination of said connecting means, said counterelectrode, the sample disposed by said disposing means, said disposing means, and the glow discharge, said impedance matching means being electrically connected in series between said electrically connecting means and said generating means; and

(g) mean for blocking direct current flow between said electrically connecting means and said impedance matching means, wherein said connecting means comprises;

i) a first coaxial connector configured to be electrically connected to one end of a radio frequency coaxial cable,

ii) an elongated conductor having a first end and a second end disposed opposite said first end, said first end of said conductor being electrically connected to said first coaxial connector,

iii) an electrically conducting sample holder member having one end configured to receive a sample therein and having an opposite end electrically connected to said second end of said conductor,

iv) an annular insulator member configured and disposed to surround a predetermined length of said conductor extending from said sample holder member toward said first end of said conductor,

v) an adapter member configured and disposed to form a vacuum-tight seal with the exterior surface of an intermediate circumferential portion of said insulator member,

vi) an electrically conducing probe body configured and disposed to surround said conductor and extending between and electrically connecting said first coaxial connector and said adapter member,

vii) an electrically insulating sleeve configured and disposed to surround said conductor and said insulator member and extending between said first coaxial connecter and said adapter member and disposed between said probe body and said annular insulator member, and

viii) an annular cap member configured and disposed with one end forming a vacuum-tight seal with the end of said insulator member disposed farther away from said sample holder member, said annular cap member having a second end configured and disposed to form a vacuum-tight seal with said conductor.

4. An apparatus as in claim 3, wherein said sample disposing means includes:

an annular insulating member configured and disposed with one end connected to said enclosure and defining an elongated opening therethrough; and

ii) a vacuum sealing O-ring configured and disposed about said elongated opening in the vicinity of the end of said annular insulating member opposite said one end connected to said enclosure and further configured to form a vacuum-tight seal against said insulator member when said insulator member is inserted into said elongated opening; and

iii) wherein said elongated opening is configured so that when the sample is disposed inside said enclosure to sustain a glow discharge on the surface of the sample exposed to said counterelectrode, said O-ring is disposed between said adapter and said sample holder member.

17. A method for using radio frequency electromagnetic energy to transform a solid sample, whether the sample is electrically conducting or nonconducting, into a glow discharge source and analyzing the sample with a mass spectrometer, the method comprising the steps of:

(a) enclosing an inert gas within a vacuum chamber defining a counterelectrode having a surface exposed to the interior of said vacuum chamber;

(b) disposing the sample relative to said counterelectrode such that application of a predetermined radio frequency electrical potential between said sample and said counterelectrode in the presence of said inert gas inside said vacuum chamber forms a sustainable glow discharge;

(c) electrically connecting the sample in series to an isolating high voltage capacitance;

(d) electrically connecting in series said isolating high voltage capacitance to a capacitive impedance matching network;

(e) electrically connecting in series to said capacitive impedance matching network, means for generating a radio frequency electromagnetic potential;

(f) applying a radio frequency electromagnetic potential between said counterelectrode and said sample via said isolating high voltage capacitance; and

(g) applying a preselected high direct current voltage to said counterelectrode to accelerate ions from said vacuum chamber to a mass spectrometer for analysis.

18. A method as in claim 17, further comprising the step of:

(a) electrically connecting an inductance between said capacitive impedance matching network and said isolating high voltage capacitance and between said means for generating a radio frequency electromagnetic potential and said counterelectrode.

19. A method as in claim 17, further comprising the steps of:

(a) enclosing said vacuum chamber inside a higher vacuum enclosure;

(b) maintaining at electrical ground potential, said impedance matching network and said means for generating a radio frequency electromagnetic potential; and

(c) preventing components maintained at ground electrical potential from bridging between said vacuum chamber and said higher vacuum enclosure.