US3699331A - Double pass coaxial cylinder analyzer with retarding spherical grids - Google Patents

Double pass coaxial cylinder analyzer with retarding spherical grids Download PDF

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US3699331A
US3699331A US175575A US3699331DA US3699331A US 3699331 A US3699331 A US 3699331A US 175575 A US175575 A US 175575A US 3699331D A US3699331D A US 3699331DA US 3699331 A US3699331 A US 3699331A
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cylinder
analyzer
cylinders
screens
axis
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Paul W Palmberg
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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
    • H01J49/28—Static spectrometers
    • H01J49/282—Static spectrometers using electrostatic analysers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/44—Energy spectrometers, e.g. alpha-, beta-spectrometers
    • H01J49/46—Static spectrometers
    • H01J49/48—Static spectrometers using electrostatic analysers, e.g. cylindrical sector, Wien filter
    • H01J49/482—Static spectrometers using electrostatic analysers, e.g. cylindrical sector, Wien filter with cylindrical mirrors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/44—Energy spectrometers, e.g. alpha-, beta-spectrometers
    • H01J49/46—Static spectrometers
    • H01J49/48—Static spectrometers using electrostatic analysers, e.g. cylindrical sector, Wien filter
    • H01J49/484—Static spectrometers using electrostatic analysers, e.g. cylindrical sector, Wien filter with spherical mirrors

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  • ABSTRACT A charged particle analyzer is provided wherein a retarding grid consisting of two spaced screen members formed of spherical sections having a concentric center located at the surface of the sample being analyzed is utilized to control the entering velocity of the charged particles into a double pass, coaxial cylinder analyzer.
  • the invention is utilized in an electron spectroscopy for chemical analysis (ESCA) apparatus.
  • a sample to be analyzed is irradiated with generally monochromatic soft X-rays.
  • Al Ka X-rays which have an energy of about 1486 eV.
  • Other sources of activation may be used, such as an electron gun or high energy photons.
  • the sample gives off emitted electrons which have an energy range determined by the elements that the sample is made of.
  • the energy distribution is determined with sufficiently high resolution, one can also establish the chemical environment which a particular atom has based upon the energy distribution of the emitted electrons.
  • the objects of the invention are accomplished through a combination of a specially constructed retarding grid and a double pass cylindrical mirror analyzer.
  • FIG. 1 is a side elevational view, mostly in cross-section, of an analyzer and certain peripheral equipment in accordance with the invention
  • FIG. 2 is a front elevational view of an aperture disc for use in the apparatus of FIG. 1;
  • FIG. 3 is a front elevational view of a second aperture for use in the apparatus of FIG. 1;
  • FIG. 4 is a front elevational view of a field termination plate utilized in the apparatus of FIG. 1;
  • FIG. 5 is a side elevational view of a grid forming mold
  • FIG. 6 is a side cross-sectional view of the cylinder analyzer of FIG. 1 with a schematic illustration of circuitry for use therewith.
  • the resolution of a cylinder analyzer is determined by the geometry of the instrument. This means that (AE)/E is equal to a constant determined by the geometry of the instrument. If one reduces the energy of electrons entering the cylinder analyzer, one can in crease the resolution of the instrument. For example, if the instrument has a designed resolution of 0.3 percent, this means that for electrons having an initial energy of 1000 eV, the resolution will be 3 eV. By decreasing the energy of electrons from an initialenergy of 1000 eV to 100 eV, with a retarding grid in accordance with the invention, one can increase the resolution of the measurement from 3 eV to 0.3 eV. This resolution proves adequate for ESCA measurements.
  • the retarding grid assembly in accordance with my invention is constructed of two concentric spherical sections, as will be described hereinbelow.
  • an analysis should be performed on electrons being emitted from a point source on the sample being analyzed. If this ideal was actually the case, the cylinder analyzer would perform in an optimum manner, as focusing of the electrons analyzed would be lessof a problem. However, in virtually every form of analysis utilizing a cylinder analyzer, this ideal condition is not met. In particular, when one utilized X-rays as the irradiating source, it is extremely difficult to concentrate the X-rays into a region that could be considered a point source. Imaging of the source of the electrons in the sample then becomes a problem, and the resolution of the instrument is decreased.
  • my invention accomplishes its purposes of providing high resolution even though it uses a relatively large source.
  • my invention Through use of my invention, one can irradiate a large region of the sample without adversely affecting the analysis, as only those X-ray excited electrons within a well-defined re gion are able to pass through both regions of the analyzer.
  • the double grid increases the virtual source size by deflecting electrons which do not originate from the ideal point source. Those electrons which are deflected during passage through the grids will not have proper trajectories to pass through both analyzers.
  • FIG. 1 there is illustrated in primarily cross-sectional view an analyzer in accordance with the present invention.
  • the apparatus in accordance with FIG. 1 includes an inner cylinder 11 and an outer cylinder 12, which are held in concentric alignment with one another by end ceramic plates 13 and a center ceramic plate 14.
  • Cylinders 11 and 12 are constructed of a non-magnetic metal like copper, as are other metallic portions unless noted otherwise.
  • a magnetic shielding member 15 Surrounding substantially the entire construction is a magnetic shielding member 15 which may be mu metal.
  • Inner cylinder 11 is provided with a series of annular openings l6, l7, l8 and 19 around the periphery thereof. Small regions 20 of the original cylinder wall are retained to support sections of the cylinder intermediate openings 16, 17, 18 and 19. Openings l6, l7, l8 and 19 are desirably covered by a fine mesh metallic screen which is desirably of about 100 lines per inch and has a transparency of about percent. This screen permits the majority of the electrons or other charged particles being analyzed to pass through the screen while substantially eliminating electric field fringing due to the discontinuity of the walls produced by these openings.
  • One end of the inner cylinder 11 is partially closed by grids 21 and 22, which will be described in greater detail below.
  • These grids are sphere segments having a common center of symmetry.
  • the sample 23 shown schematically
  • That portion of the sample to be analyzed is located at the center of symmetry of the grid members 21 and 22, and also on line with the axis of cylinders 11 and 12.
  • a source of irradiation energy such as an X-ray source, shown schematically as 24, is positioned to direct X-rays to strike as closely as possible to the symmetry point on the sample.
  • the irradiation gives rise to emission of electrons from the surface layers of the sample, whose energies are functions of the composition of the material and of the chemical environment in which the elements are as sociated. Some of the electrons emitted will follow the curved path illustrated by the dotted line 25 through the analyzer.
  • Grid members 21 and 22 are formed of fine wire screen of the same type utilized in covering the openings of holes 16, 17, 18 and 19.
  • the fine stainless steel screen is shaped over a block generally designated 26 of a material such as Teflon.
  • the block will have a radius of curvature corresponding to that desired for the individual grid. In the instance of grid.21, .the radius of curvature will, of course, be larger than that of grid 22.
  • grid 21 will have a radius of about 1 inch
  • grid 22 will have a radiusof about 0.9 inches.
  • a shoulder 27 is provided on the forming block so as to produce a flanged portion on the screen.
  • Suitable die means are provided for pressing the screen member onto block 26 and shoulder 27 to produce the final configuration.
  • grid 22 is fastened by means such as welding to a metal plate43 which is in electrical contact with outer magnetic shielding member 15.
  • Shielding member is electrically insulated from the balance of the assembly by ceramic 13.
  • the inner grid 21 is in electrical contact with and mounted to a flange 28 projecting into the center of cylinder ll.'Grid 21 and grid 22 are maintained in electrical isolation from one another by means of ceramic disc 13.
  • Spacing elements 13 and 14 are provided to maintain cylinders 1 1 and 12in fixed relationship to one another and to provide a special field termination means to prevent field fringing.
  • Each of these discs 13 and 14 is desirably formed of someelectrically insulating material, which is preferably ceramic. Alumina or quartz are particularly suitable for the purpose.
  • These discs are provided on the inner surface thereof with a conductive coating 29,. having a high resistivity of about 30 megohms. This high resistance coating aids in the reduction of field fringing, which adversely effects the paths of the electrons as they pass through the analyzer.
  • FIG. 4 there is generally illustrated a ceramic disc 13 in front elevationalview, which has been provided with a series of concentric conductors in annular form and identified 30 through 34,'respectively.-These rings are concentric with one another and with the axis of the ceramic plate. 13. Rings 30 through 34 are desirably formed by metallizing the surface of the ceramic discs 13 or 14 and then, by photolithographic masking and etching, removing the intermediate metal between the rings.
  • the rings will desirably be about 0.005 inch in width and a few microns in thickness.
  • Suitable metals include gold-chromiumalloys that have been vacuum sputtered onto the surface of the ceramic. The function of these rings is to provide equi-potential regions on the discs so as to minimize the effects caused by regions of resistivity that are not uniform within film 29.
  • the spacer 13 at the sample end may be in the form of a truncated cone rather than a flat washer shape as shown.
  • the forward edge of cylinder 12 would then be offset away from the sample, thus allowing a more simple positioning for the activation sources 24.
  • the intermediate ceramic disc 14 has been treated on opposite surfaces thereof in a manner analogous to that described with regard to FIG. 4. It should also be appreciated that the conductive coating 29 is in electrical contact with cylinders 1 1 and 12 at the inner and outer extremities thereof. This can be readily achieved by metallizing the inner and outer edges of the ceramic discs 13 and 14.
  • I provide an intermediate aperture disc 35.
  • the aperture disc 35 is secured in fixed relationship to cylinder 11 by a mounting means generally indicated as 36.
  • -Disc 35 is shown in front elevational view in FIG. 2
  • This narrow aperture 37 acts as a filter to provide essentially a near point source of electrons for the second stage of the analyzer.
  • Disc 40 is substantially identical to that of FIG. 2, both in thickness and dimension, while disc 39 is, as shown in FIG. 3, formed of a thin molybdenum disc of about 0.003 inches thickness, having a plurality of annular ring segment openings41 that are positioned concentric with, but off of, the central axis of the disc.
  • the function of such an off-axis aperture in disc 39 is described in the copending application of Bohn et al., Ser. No. 68,983, for AUGER ELECTRON. SPEC- TROSCOPY.
  • a tubular member 42 which functions in the invention as the first dynode of a photomultiplier.
  • the spherical grids 21 and 22 due to their configuration and posi' tioning, act to controllably decrease the energy of the electrons passing therethrough so as to provide a resolution of measurement down into a range necessary for determining the atomic number and chemical state of the atom from which the electron originated.
  • the source of electrons is redefined as the electrons pass through the intermediate aperture 37.
  • the second stage of the double pass analyzer has, by virtue of the aperture 37, a source at a precisely known distance from the detector 42.
  • the detector for the electrons is a electronmultiplier, of which element 42 forms the first dynode.
  • the double pass arrangement further provides a construction wherein magnetic effects are essentially eliminated by the interior position of the entire second stage of the double pass analyzer. The absence of magnetic interference further provides a higher degree of precision of the overall instrument.
  • FIG. 6 there is illustrated in cross section the analyzer in accordance with FIG. 1, with the principal portions thereof being shown in essentially schematic form. Electrical connections are made as shown to the various portions of the analyzer.
  • the outer mu metal shield 15 is connected by a lead 44 to ground and to one side of a voltage programmable power supply.
  • the outer cylinder 12 is electrically connected by lead 45 to a first floating power supply 47, while inner cylinder 11 is connected by means of lead 46 to the output of a second floating power supply 48.
  • grid 21 is at the same potential as inner cylinder 11, while grid 22 will be at the same potential as mu metal shield 15, which is at ground.
  • a digital ramp generator 49 supplies the timing logic both to the voltage programmable power supply 50 and to the pulse counting electronics and digital logic unit. It also supplies a signal to an X-Y recorder as schematically illustrated in the figure.
  • an electron multiplier As the receiving element for the charged particles (electrons) which pass through the detector, there is an electron multiplier, which is shown as having a power supply, with its output of the multiplier going to a pulse counting electronic and digital logic unit.
  • a digital to analog converter is utilized to convert the signal which then passes to the X-Y recorder as the Y axis signal.
  • the floating power supplies 47 and 48 may conveniently be Hewlett Packard Models 62098.
  • the voltage programmable power supply 50 may be Model OPS2000 of the Kepco Company of Flushing, New York.
  • a digital ramp generator 49 is conveniently a laboratory computer PDP8/E, and a D/A convertor available from Digital Equipment Corporation of Maynard, Massachusetts.
  • a conventional X-Y recorder can be utilized such as Model 70048 of the Hewlett Packard Company.
  • the system of FIG. 6 functions substantially as follows.
  • Sample 23 is irradiated by suitable means so as to emit electrons. These electrons then pass through screens 22 and 21, which aremaintained at ground and at some suitable elevated negative potential, respectively.
  • a scanning potential is applied to grid 21 to slow down the electrons passing between the two grids to a value such that the resolution of the instrument can detect the necessary differences in electron energy required for the' ESCA measurement.
  • the voltage V, applied between the inner cylinder 11 and outer cylinder 12, where 12 is negative with respect to 11, is
  • k is a constant and depends upon the diameters of the inner and outer cylinders of the analyzer.
  • the k is fixed for a particular analyzer geometry.
  • a constant differential between the two cylinders is maintained by means of a floating power supply 47.
  • Floating power supplies 47 and 48 are chosen so that their ratios of voltage are such that the energy of the electrons incident on grids 21 and 22 and passed by the analyzer is equal to V the voltage of the voltage programmable power supply. It should be appreciated that power supply 48 will be positive with respect to power supply 50 so that the scans can be made down to zero energy.
  • the electrons emitted from sample 23 pass through the grid arrangement 22-21 and enter the analyzer via opening 16, they are deflected by the more negative potential of outer cylinder 12 and follow the path generally marked 25.
  • the electrons are partially resolved and generally are focused on plate 35 containing the aperture 37'.
  • Aperture 37 functions to further resolve the electrons into a nearly point source of definite size and distance from the ultimate receiver 42.
  • the electrons which pass through opening 37 are further resolved and analyzed by passage through openings 18 and back through 19 and are ultimately focused by means of the double aperture system 39 and 40.
  • the resulting analysis has a high signal to noise ratio and permits far greater precision of measurements than has been known with instruments known heretofore.
  • An analyzer for determining the energy distribution of charged particles being emitted from a source comprisingi a. first and second metallic cylinders, the first of said cylinders having an outer diameter less than that of the inner diameter of the second cylinder and being positioned interior to the second cylinder, each of said cylinders having a common axis;
  • disc-shaped aperture means positioned interior to and intermediate the ends of said first cylinder in a plane generally perpendicular to said axis and dividing said analyzer into first and second stages, said disc having an opening therethrough at said axis, the opening defining the source of charged particles for said second stage;
  • said first cylinder defining a plurality of annularly spaced openings near each end of each stage of said first cylinder;
  • a retarding grid arrangement including first and second spherical section shaped screens positioned adjacent'a first end of said first cylinder, said screens being spaced from one another and having a common center of symmetry at the source of charged particles and along said axis, said screens being in electrical isolation from one another, they second of said screens being inelectrical contact with said first cylinder;
  • An electron spectroscopy chemical analysis system comprising:
  • first and second metallic cylinders a. first and second metallic cylinders, the first of said cylinders having an outer diameter less than that of Y the inner diameter of'the second cylinder and being positioned'interior to the second cylinder, each of said cylinders having a common axis;
  • disc-shaped aperture means positionedinterior to and intermediate the ends along the length of said first cylinder in a plane perpendicular to said axis and dividing said analyzer into first and second stages, said disc having an opening at said axis, the opening defining the source of charged particles for said second stage;
  • said first cylinder defining a plurality of annularly spaced openings near each end of each stage of said first cylinder;
  • a retarding grid arrangement including first and second spherical section shaped screens positioned adjacent the first end of said first cylinder, said screens being spaced from one another and having a common center of symmetry along said axis, said screens being in electrical isolation from one another, the second of said screens being in electrical contact with said first cylinder;
  • e. means for positioning a sample to be analyzed so.
  • X-ray source means arranged to direct a beam of X-rays onto said sample to be analyzed
  • Patent No. 3, 699, 33 Dated October 17, 1972 Inventor (3) Paul W. Palmberg It is certified that error appears in the above-identified patent and that said Letters Patent are hereby corrected as shown below:

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3783280A (en) * 1971-03-23 1974-01-01 Ass Elect Ind Method and apparatus for charged particle spectroscopy
US3870882A (en) * 1973-05-23 1975-03-11 Gca Corp Esca x-ray source
US4048498A (en) * 1976-09-01 1977-09-13 Physical Electronics Industries, Inc. Scanning auger microprobe with variable axial aperture
US4224518A (en) * 1978-12-21 1980-09-23 Varian Associates, Inc. Multistage cylindrical mirror analyzer incorporating a coaxial electron gun
US4309607A (en) * 1978-11-30 1982-01-05 Kernforschungsanlage Julich Gesellschaft Mit Beschrankter Haftung Electron-impact spectrometer
US4367406A (en) * 1981-01-13 1983-01-04 Trustees Of Boston University Cylindrical mirror electrostatic energy analyzer free of third-order angular aberrations
US5032724A (en) * 1990-08-09 1991-07-16 The Perkin-Elmer Corporation Multichannel charged-particle analyzer
WO2009053666A3 (en) * 2007-10-24 2009-07-30 Shimadzu Res Lab Europe Ltd Charged particle energy analysers
WO2010107861A1 (en) 2009-03-20 2010-09-23 Physical Electronics USA, Inc. Sample holder apparatus to reduce energy of electrons in an analyzer system and method
US20110168886A1 (en) * 2009-07-17 2011-07-14 Kla-Tencor Corporation Charged-particle energy analyzer
CN106568832A (zh) * 2016-10-31 2017-04-19 中国科学院国家空间科学中心 一种用于空间热等离子体能量和成分测量的传感器装置

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5831700B2 (ja) * 1975-06-06 1983-07-07 ニホンシンクウギジユツ カブシキガイシヤ イオンシツリヨウブンセキソウチ
JPS597736Y2 (ja) * 1977-02-25 1984-03-09 日本電子株式会社 電子分光装置
US6184523B1 (en) * 1998-07-14 2001-02-06 Board Of Regents Of The University Of Nebraska High resolution charged particle-energy detecting, multiple sequential stage, compact, small diameter, retractable cylindrical mirror analyzer system, and method of use
JPWO2008114684A1 (ja) * 2007-03-16 2010-07-01 国立大学法人 奈良先端科学技術大学院大学 エネルギー分析器、２次元表示型エネルギー分析器および光電子顕微鏡
CN110618443B (zh) * 2019-08-26 2021-04-13 北京控制工程研究所 一种等离子体推力器稳态离子流场测量装置及测量方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3582649A (en) * 1968-10-21 1971-06-01 Varian Associates Retarding field electron diffraction spectrometer having improved resolution
US3596091A (en) * 1969-05-19 1971-07-27 Varian Associates Induced electron emission spectrometer having a unipotential sample chamber
US3631238A (en) * 1969-11-17 1971-12-28 North American Rockwell Method of measuring electric potential on an object surface using auger electron spectroscopy

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3582649A (en) * 1968-10-21 1971-06-01 Varian Associates Retarding field electron diffraction spectrometer having improved resolution
US3596091A (en) * 1969-05-19 1971-07-27 Varian Associates Induced electron emission spectrometer having a unipotential sample chamber
US3631238A (en) * 1969-11-17 1971-12-28 North American Rockwell Method of measuring electric potential on an object surface using auger electron spectroscopy

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
High Sensitivity Auger Electron Spectrometer by Palmberg, Applied Physics Letter Oct. 15, 1969 Vol. 15 No. 8. *

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3783280A (en) * 1971-03-23 1974-01-01 Ass Elect Ind Method and apparatus for charged particle spectroscopy
US3870882A (en) * 1973-05-23 1975-03-11 Gca Corp Esca x-ray source
US4048498A (en) * 1976-09-01 1977-09-13 Physical Electronics Industries, Inc. Scanning auger microprobe with variable axial aperture
US4309607A (en) * 1978-11-30 1982-01-05 Kernforschungsanlage Julich Gesellschaft Mit Beschrankter Haftung Electron-impact spectrometer
US4224518A (en) * 1978-12-21 1980-09-23 Varian Associates, Inc. Multistage cylindrical mirror analyzer incorporating a coaxial electron gun
US4367406A (en) * 1981-01-13 1983-01-04 Trustees Of Boston University Cylindrical mirror electrostatic energy analyzer free of third-order angular aberrations
US5032724A (en) * 1990-08-09 1991-07-16 The Perkin-Elmer Corporation Multichannel charged-particle analyzer
US20110147585A1 (en) * 2007-10-24 2011-06-23 Nikolay Alekseevich Kholine Charged particle energy analysers
WO2009053666A3 (en) * 2007-10-24 2009-07-30 Shimadzu Res Lab Europe Ltd Charged particle energy analysers
US8373122B2 (en) * 2007-10-24 2013-02-12 Shimadzu Research Laboratory (Europe) Ltd Spheroidal charged particle energy analysers
WO2010107861A1 (en) 2009-03-20 2010-09-23 Physical Electronics USA, Inc. Sample holder apparatus to reduce energy of electrons in an analyzer system and method
US8071942B2 (en) 2009-03-20 2011-12-06 Physical Electronics USA, Inc. Sample holder apparatus to reduce energy of electrons in an analyzer system and method
US20100237240A1 (en) * 2009-03-20 2010-09-23 Physical Electronics USA, Inc. Sample holder apparatus to reduce energy of electrons in an analyzer system and method
US20110168886A1 (en) * 2009-07-17 2011-07-14 Kla-Tencor Corporation Charged-particle energy analyzer
US8421030B2 (en) * 2009-07-17 2013-04-16 Kla-Tencor Corporation Charged-particle energy analyzer
CN106568832A (zh) * 2016-10-31 2017-04-19 中国科学院国家空间科学中心 一种用于空间热等离子体能量和成分测量的传感器装置

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GB1338208A (en) 1973-11-21
DE2241612B2 (de) 1976-01-15
JPS5338948B2 (enrdf_load_stackoverflow) 1978-10-18
JPS4832589A (enrdf_load_stackoverflow) 1973-04-28
FR2150887B1 (enrdf_load_stackoverflow) 1976-08-13
FR2150887A1 (enrdf_load_stackoverflow) 1973-04-13
DE2241612A1 (de) 1973-03-08

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