US3328146A - Method of producing an analyzer electrode system for mass spectrometers - Google Patents

Method of producing an analyzer electrode system for mass spectrometers Download PDF

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Publication number
US3328146A
US3328146A US295631A US29563163A US3328146A US 3328146 A US3328146 A US 3328146A US 295631 A US295631 A US 295631A US 29563163 A US29563163 A US 29563163A US 3328146 A US3328146 A US 3328146A
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United States
Prior art keywords
tube
rods
grooves
mold
portions
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Expired - Lifetime
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US295631A
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English (en)
Inventor
Hanlein Walter
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.)
Siemens Schuckertwerke AG
Siemens Corp
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Siemens Corp
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Priority claimed from DES80532A external-priority patent/DE1297360B/de
Application filed by Siemens Corp filed Critical Siemens Corp
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Publication of US3328146A publication Critical patent/US3328146A/en
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/26—Mass spectrometers or separator tubes
    • H01J49/34—Dynamic spectrometers
    • H01J49/42—Stability-of-path spectrometers, e.g. monopole, quadrupole, multipole, farvitrons
    • H01J49/4205—Device types
    • H01J49/421—Mass filters, i.e. deviating unwanted ions without trapping
    • H01J49/4215—Quadrupole mass filters
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/49002—Electrical device making
    • Y10T29/49117—Conductor or circuit manufacturing
    • Y10T29/49204—Contact or terminal manufacturing
    • Y10T29/49208—Contact or terminal manufacturing by assembling plural parts
    • Y10T29/49218—Contact or terminal manufacturing by assembling plural parts with deforming

Definitions

  • FIG. 1 W. HANLEIN METHOD OF PRODUCING AN ANALYZER ELECTRODE SYSTEM FOR MASS SPECTROMETERS June 27, 1967 2 Sheets-5heet 1 Filed July 17, 1963 FIG. 1
  • FIGA A first figure.
  • Patents 2,939,952 and 2,950,389 in which ions of different specific charges .are shot, from an ion source, between a number of elongated field electrodes that extend substantially parallel to the trajectory direc tion and are kept at an electric potential, generally composed of a high-frequency alternating component and a direct component, so that certain ions, depending upon their mass, are deflected onto the analyzer electrodes whereas others pass through the electrode field and ultimately impinge upon a collector electrode.
  • An object of my invention is also to devise a relatively simple manufacturing process that results in a mass-spectrometer analyzer system of improved stability so as to assure accurate dimensions and absence of internal twist after prolonged periods of operation.
  • a twist-free assembly of elongated and symmetrically parallel electrode rods for a mass-spectrometer analyzer system is produced by placing or pulling a tube of electrically poorly conducting, softenable material coaxially over a core mold whose perimetric surface is provided with grooves that extend parallel to the core axis. Thereafter, the material of the tube, then jacketing the core, is softened so that it enters into the grooves and fits snugly into them. After hardening of the material, the tube portions then protruding inwardly into the grooves form properly correlated surfaces corresponding in contour and extent to the electrode surfaces to be ultimately obtained.
  • these protruding inner surfaces are metallized so that they are available as analyzer electrodes which are rigidly spaced relative to each other at the proper mutual and diagonal distances.
  • Suitable as electrically poorly conducting material for the tube is glass or synthetic plastic, preferably tetrafluoroethylene as available in the trade under the name Teflon.
  • the core mold instead of being provided with four grooves, may be given any other desired even number of grooves uniformly distributed about the periphery.
  • the cross section of the grooves is inwardly convex such as approximately semicircular or parabolic.
  • a metallic body preferably of stainless steel is suitable as a core mold. This core body is preferably ground and polished.
  • the grooves can be produced in any suitable manner, for example by grinding them into the body.
  • the material of the core mold should have a greater coefiicient of thermal expansion than the material of the softenable tube material,
  • the heating and resulting softening of the tube material preferably is accomplished by inductive heating of the metallic core mold.
  • electric current-supply leads may also be attached to the inwardly protruding rod-shaped portions of the tube.
  • the tube Prior to softening and during softening, the tube can 'be closed and evacuated.
  • FIG. 1 is explanatory and shows schematically a complete mass-spectrometer apparatus of the above-mentioned type.
  • FIG. 2 shows schematically a mutual arrangement of four analyzer electrodes in such a mass filter.
  • FIG. 3 is a cross section along line A-B in FIG. 4 through a core mold covered by a glass tube during a stage of the process according to the invention.
  • FIG. 4 is a lateral view of a core mold fused into a glass tube.
  • FIG. 5 shows the same fused-off glass tube with an enclosed core mold but surrounded by an induction heater winding as used during the softening stage in the process according to the invention.
  • FIG. 6 shows schematically and in perspective a glass tube, cut to proper length and provided with four grooves, this tube having metallized inner surfaces and thus constituting the product of the method.
  • FIG. 7 shows separately a portion of the glass tube with an electric conductor wire attached to one of the analyzer electrodes.
  • FIG. 8 is a plan view of the portion shown in FIG. 7.
  • a spectrometer tube 1 has an envelope 5 containing an ion source 2, and a group of rod-shaped deflector electrodes 3 each having a circular cross section, L0- catcd at the end of the ion-beam path is a cup-shaped collector electrode 4.
  • the ion source 2 and the collector electrode 4 are coaxially spaced from each other and thus define a center axis for the ion beam issuing from the source 2 toward the electrode 4.
  • the electrode rods 3 are uniformly distributed about the ion-beam axis and extend parallel thereto. A total number of four such electrodes rnav be used.
  • the above-mentioned envelope 5 of the cell 1 is vacuumtightly sealed and has a nipple or neck 6 connected with a tank 7 containing the gaseous mixture to be investigated.
  • the rod electrodes 3 are electrically connected in pairs to a high-frequency generator 8 which supplies electric energy of suitable voltage and frequency.
  • the current due to the ions impinging upon the collector 4 is amplified by an amplifier 9 and supplied to a recorder 10 or other indicating or measuring device.
  • Another measuring instrument 10' is provided for supervising the electron emission of the cathode in the ion source 2.
  • the requirements to be met by the analyzer system will be understood from the diagram shown in FIG. 2.
  • the four analyzer rods 3- are identified as rods 11, 12, 13 and 14 in FIG. 2.
  • the four rods, as seen in FIG. 2, are arranged at the corners of a square.
  • the mutual spacing a between each two rods must be accurately equal to the spacing between any other two rods, and the length of the diagonal spacings b must also be accurately identical. These dimensions must also be the same over the entire axial length of the analyzer system.
  • the accuracy heretofore attainable by mechanical adjustment amounts to a few multiples of 10 microns; however, the system may become skewed or twisted during heating-up of the spectrometer.
  • FIG. 3 a glass tube 21 of originally cylindrical shape is used.
  • a metal core mold 23 accurately machined, ground and polished is axially inserted into the glass tube.
  • the mold is provided with grooves of semicircular cross section.
  • the mold is preferably made of Cr-Ni steel or other stainless alloy steel. According to another embodiment of the invention the grooves are parabolic in cross section.
  • the glass tube is given a constriction above and below the mold 23 and then fused off.
  • the interior of the tube may be connected to a vacuum pump, so that the heated glass tube is pulled tightly about the core mold.
  • one end of the glass tube may also remain open and may then be connected with a vacuum pump for the duration of the entire molding process.
  • the glass tube 21 with the enclosed mold 23 is then placed in a furnace, and the entire assembly is heated to a temperature slightly above the transformation point of the glass. After some time, the glass enters into the grooves 22 of the mold 23 (FIG. 3). During subsequent cooling, the mold 23 contracts more strongly than the glass tube, so that when the ends of the glass tube are severed off, the mold can be pulled out of the remaining glass tube.
  • the tube then has four hollow-cylindrical portions that protrude inwardly along the entire length of the cut-off tube as is apparent from FIG. 6.
  • the inner surfaces of these protruding portions are then metallized or mirrored, for example by vaporizing gold onto these surfaces or depositing gold by cathode spattering. In FIG. 6 the metallized inner surfaces on the projections are identified by shading and denoted by 25. In this manner, a twist-free analyzer system of accurate dimensions is produced, which retains the original dimensions virtually during the lifetime of the mass spectrometer.
  • the above-described heating operations required for softening the glass tube can also be effected, in part or entirely, by means of induction heating.
  • the tube 21 is shown in FIG. surrounded over substantially its entire length by an induction heater coil 24 which during operation is energized by high-frequency current.
  • the attachment of the electric conductors to the rodshaped protruding portions of the tubular structure is effected by fusing them in during the softened condition of the structure in the manner described with reference to FIGS. 7 and 8.
  • the conductors attached to the metallized portions should protrude as little as possible from the active, convex surfaces of the electrodes.
  • the ends should be pressed or otherwise embedded into this surface so that they lie flush therewith or stay beneath the convex surface, this being not shown in FIGS. 7 and 8.
  • the conductor wire 26 has a circular cross section.
  • the wire consisting of platinum or any other material used for lead-ins passing through glass, has its outer end bent in the reverse direction and also fused together with a glass, plastic or other moldable material being used for the tubular structure.
  • the metallization is preferably placed upon the protruding portions of the tubular structure after the conductor wires are attached. As a result, the metallization also takes care of providing for a good metallic contact between the fused-in wires and the vapor-deposited metal layer that is ultimately effective as the electrode surface proper.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
US295631A 1962-07-21 1963-07-17 Method of producing an analyzer electrode system for mass spectrometers Expired - Lifetime US3328146A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DES80532A DE1297360B (de) 1962-07-21 1962-07-21 Verfahren zum Herstellen eines verwindungsfreien Analysatorsystems fuer ein Multipolmassenfilter

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CH (1) CH409463A (de)
GB (1) GB1003240A (de)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4052181A (en) * 1976-02-13 1977-10-04 Nasa Acoustic energy shaping
US4079254A (en) * 1975-09-11 1978-03-14 Analog Technology Corporation Mass spectrometer filter
US4117321A (en) * 1974-06-18 1978-09-26 Varian Mat Gesellschaft Mit Beschrankter Haftung Electrode system for multipoles and especially for multipole or monopole mass spectrometers
US4213557A (en) * 1977-08-23 1980-07-22 Dr. Franzen Analysentechnik Gmbh & Co. Kommanditgesellschaft Method for producing a mass filter analyzer system and analyzer system produced according to the method
JPS63152846A (ja) * 1986-11-19 1988-06-25 Yokogawa Hewlett Packard Ltd マスフィルター
US5298745A (en) * 1992-12-02 1994-03-29 Hewlett-Packard Company Multilayer multipole
DE19511248A1 (de) * 1994-03-25 1995-09-28 Hewlett Packard Co Universalvierpol und Verfahren zur Herstellung desselben
US5644131A (en) * 1996-05-22 1997-07-01 Hewlett-Packard Co. Hyperbolic ion trap and associated methods of manufacture
US5852270A (en) * 1996-07-16 1998-12-22 Leybold Inficon Inc. Method of manufacturing a miniature quadrupole using electrode-discharge machining
US20070138389A1 (en) * 2005-12-19 2007-06-21 Korea Research Institute Of Standards And Science Hyperbolic quadrupole mass filter made of platinum group metal coated quartz tube

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2138201B (en) * 1983-03-28 1986-07-16 Prutec Ltd Mass spectrometer

Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1301714A (en) * 1913-09-09 1919-04-22 Karl Kueppers Method of and apparatus for forming glass tubes.
US1406542A (en) * 1922-02-14 Electjeiode
US1583464A (en) * 1924-09-13 1926-05-04 Western Electric Co Method of forming glassware
US1953625A (en) * 1930-04-04 1934-04-03 Gen Scientific Corp Electrode for luminous positive column gaseous conducting devices
US2219107A (en) * 1939-08-29 1940-10-22 Rca Corp Electron discharge device
US2359501A (en) * 1937-11-27 1944-10-03 Gen Electric Sealing-in apparatus
US2556864A (en) * 1950-09-27 1951-06-12 Gen Electric Coated grid for electron discharge tubes
US2822501A (en) * 1955-01-10 1958-02-04 Research Corp Slow-wave guide for traveling wave tubes
US2874325A (en) * 1952-02-05 1959-02-17 Ets Claude Paz & Silva Electrode for electric discharge apparatus
US2933634A (en) * 1956-06-22 1960-04-19 Westinghouse Electric Corp Electron discharge device
US2945327A (en) * 1955-11-28 1960-07-19 Gen Electric Method of manufacturing electric lamps or similar devices
US3025426A (en) * 1960-02-18 1962-03-13 Westinghouse Electric Corp Press seal

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1406542A (en) * 1922-02-14 Electjeiode
US1301714A (en) * 1913-09-09 1919-04-22 Karl Kueppers Method of and apparatus for forming glass tubes.
US1583464A (en) * 1924-09-13 1926-05-04 Western Electric Co Method of forming glassware
US1953625A (en) * 1930-04-04 1934-04-03 Gen Scientific Corp Electrode for luminous positive column gaseous conducting devices
US2359501A (en) * 1937-11-27 1944-10-03 Gen Electric Sealing-in apparatus
US2219107A (en) * 1939-08-29 1940-10-22 Rca Corp Electron discharge device
US2556864A (en) * 1950-09-27 1951-06-12 Gen Electric Coated grid for electron discharge tubes
US2874325A (en) * 1952-02-05 1959-02-17 Ets Claude Paz & Silva Electrode for electric discharge apparatus
US2822501A (en) * 1955-01-10 1958-02-04 Research Corp Slow-wave guide for traveling wave tubes
US2945327A (en) * 1955-11-28 1960-07-19 Gen Electric Method of manufacturing electric lamps or similar devices
US2933634A (en) * 1956-06-22 1960-04-19 Westinghouse Electric Corp Electron discharge device
US3025426A (en) * 1960-02-18 1962-03-13 Westinghouse Electric Corp Press seal

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4117321A (en) * 1974-06-18 1978-09-26 Varian Mat Gesellschaft Mit Beschrankter Haftung Electrode system for multipoles and especially for multipole or monopole mass spectrometers
US4079254A (en) * 1975-09-11 1978-03-14 Analog Technology Corporation Mass spectrometer filter
US4052181A (en) * 1976-02-13 1977-10-04 Nasa Acoustic energy shaping
US4213557A (en) * 1977-08-23 1980-07-22 Dr. Franzen Analysentechnik Gmbh & Co. Kommanditgesellschaft Method for producing a mass filter analyzer system and analyzer system produced according to the method
JPS63152846A (ja) * 1986-11-19 1988-06-25 Yokogawa Hewlett Packard Ltd マスフィルター
EP0268048A3 (en) * 1986-11-19 1989-07-26 Hewlett-Packard Company Quartz quadrupole for mass filter
JP2585030B2 (ja) 1986-11-19 1997-02-26 ヒューレット・パッカード・カンパニー マスフィルター
DE4341149C2 (de) * 1992-12-02 2001-05-17 Agilent Technologies Inc Multipolvorrichtung und Verfahren zum Herstellen einer Multipolvorrichtung
US5298745A (en) * 1992-12-02 1994-03-29 Hewlett-Packard Company Multilayer multipole
DE4341149A1 (de) * 1992-12-02 1994-06-09 Hewlett Packard Co Vielschicht-Multipol
DE19511248A1 (de) * 1994-03-25 1995-09-28 Hewlett Packard Co Universalvierpol und Verfahren zur Herstellung desselben
US5616919A (en) * 1994-03-25 1997-04-01 Hewlett-Packard Company Universal quadrupole and method of manufacture
US5644131A (en) * 1996-05-22 1997-07-01 Hewlett-Packard Co. Hyperbolic ion trap and associated methods of manufacture
US5852270A (en) * 1996-07-16 1998-12-22 Leybold Inficon Inc. Method of manufacturing a miniature quadrupole using electrode-discharge machining
US20070138389A1 (en) * 2005-12-19 2007-06-21 Korea Research Institute Of Standards And Science Hyperbolic quadrupole mass filter made of platinum group metal coated quartz tube
US7453061B2 (en) 2005-12-19 2008-11-18 Korea Research Institute Of Standards And Science Hyperbolic quadrupole mass filter made of platinum group metal coated quartz tube

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CH409463A (de) 1966-03-15
GB1003240A (en) 1965-09-02

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