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WO2007008191A1 - Nebuliseur a source de plasma - Google Patents

Nebuliseur a source de plasma Download PDF

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Publication number
WO2007008191A1
WO2007008191A1 PCT/US2005/024001 US2005024001W WO2007008191A1 WO 2007008191 A1 WO2007008191 A1 WO 2007008191A1 US 2005024001 W US2005024001 W US 2005024001W WO 2007008191 A1 WO2007008191 A1 WO 2007008191A1
Authority
WO
WIPO (PCT)
Prior art keywords
source
plasma
capillary
electrospray
plasma source
Prior art date
Application number
PCT/US2005/024001
Other languages
English (en)
Inventor
Michael Ahern
Howard M. Kingston
Original Assignee
Metara, Inc.
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 Metara, Inc. filed Critical Metara, Inc.
Priority to PCT/US2005/024001 priority Critical patent/WO2007008191A1/fr
Priority to TW094123459A priority patent/TW200703412A/zh
Publication of WO2007008191A1 publication Critical patent/WO2007008191A1/fr

Links

Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/10—Ion sources; Ion guns
    • H01J49/105—Ion sources; Ion guns using high-frequency excitation, e.g. microwave excitation, Inductively Coupled Plasma [ICP]
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/10—Ion sources; Ion guns
    • H01J49/107—Arrangements for using several ion sources
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/10—Ion sources; Ion guns
    • H01J49/16—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission
    • H01J49/165—Electrospray ionisation

Definitions

  • the present invention relates to chemical analysis using mass spectrometers, and in particular to mass spectrometers using a plasma and an electrospray ionization source.
  • Mass spectrometers and other systems are used for measurement of the concentration of analytes or the detection and measurement of contaminants and trace additives in solutions and gase's .
  • process solutions for wafer cleaning, etching and other forms of surface preparation are routinely analyzed using mass spectrometers with plasma ionization sources, one type is an inductively coupled plasma mass spectrometer (ICP-MS) .
  • ICP-MS inductively coupled plasma mass spectrometer
  • the measurements made by ICP-MS are used to determine and manage the quality of process solutions.
  • ⁇ ltrapure water (UPW) dilute hydrofluoric acid
  • HF HF
  • SCl Standard Clean 1, ammonium hydroxide and hydrogen peroxide in water
  • SC2 hydroochloric acid and hydrogen peroxide in water
  • mass spectrometry is often used to achieve sensitivity of parts per billion (ppb) or parts per trillion
  • ppt It is commonly used to quantitatively measure the amount of contamination present or the concentration of a constituent in the solution.
  • U.S. Pat. Appl. Serial No. 10/004,627 which is incorporated by reference in its entirety, discloses an automated analytical apparatus measuring contaminants or constituents present in trace concentrations using a form of Isotope Dilution Mass Spectrometry (IDMS) and an electrospray ionization source.
  • IDMS Isotope Dilution Mass Spectrometry
  • a sample of interest is spiked with a known amount of an appropriate isotopic species. This spike is to be used as an internal standard during the mass spectrometry measurement.
  • the relative ratios of peak areas present in the mass spectra of the sample species of interest and the isotopically enriched calibrated spike are used to determine the concentration of the chemical constituents of interest in the sample.
  • speciation mode Two modes for analyzing samples are used in the analysis method of this patent application: speciation mode and elemental mode. These modes are enabled by an electrospray ionization source.
  • an electrospray ionization source is often used, such as disclosed in U.S. Pat. No. 6,060,705 entitled “Electrospray and Atmospheric Pressure Chemical Ionization Sources", which is incorporated by reference in its entirety.
  • This type of source provides a "soft" ionization (i.e., occurring at lower energy) in which molecular information is retained. This information is required for the successful identification of organics and molecular complexes that may be present in a process solution or gas.
  • speciation mode collisions between the ions and other molecules are relatively soft, leaving the majority or major fractions of the structure of the original molecule intact.
  • the collisions are much more energetic ("harder") through the creation of more highly accelerated ions (with higher energy) that break the molecular species into their elemental or individual atomic components.
  • the energetics present in the electrospray ionization source are not sufficient to break all components of the molecular species that may be present into their elemental components even in the hard ionization mode.
  • the elemental sensitivity when using this type of source is limited by the fact that elemental species are distributed in a number of molecular fragments even after ionization. In this case, all peaks containing the element must be identified and analyzed after background subtraction if the optimum sensitivity is to be obtained.
  • an elemental ion of a given type will be concentrated into one peak that is relatively easy to identify and analyze without the errors associated with multiple peak fittings and background subtractions that must occur for the former case.
  • Another shortcoming of the electrospray source is its degraded ionization efficiency for some species including metals in the presence of strongly acidic or basic solutions. This degradation significantly reduces the sensitivity for trace contamination and other constituents that are important for successful measurement of the analyte.
  • an inductively coupled plasma (ICP) ionization source is often preferred due to its ability to completely break molecules into their elemental components. Strong acids and bases are also effectively neutralized in the plasma, another important feature.
  • An ICP source works in general by coupling radio frequency (RF) energy into a gas stream containing the nebulized liquid or gas sample with the result that the sample is immediately heated to several thousand degrees. Molecules break apart at these temperatures and collision energies leaving only elemental ions. Since this technique breaks all of the molecular bonds, this ionization technique can provide very high elemental sensitivity; however, all molecular information is lost. ICP sources that are currently available for sample ionization are too large and intrusive for successful integration into current electrospray mass spectrometry systems.
  • microwave energy a higher frequency radiation than that used in ICP-MS instruments, is capable of inducing plasma that can successfully ionize analytes into elemental components for mass spectrometry analysis.
  • ⁇ microwave source due to its shorter wavelength, can be made significantly smaller than commercially available ICP sources normally used in mass spectrometry.
  • the smaller size makes its integration into an electrospray ionization source mass spectrometer instrument possible while keeping the electrospray source operational as an alternative ionization source, i.e., the mass spectrometer can then be operated with an electrospray ion source or a microwave induced plasma ion source or a combination of the two.
  • Metals incorporated into semiconductor devices can affect device parameters, reliability, and yield. Knowing the oxidation state or molecular binding provides root cause source information. ' Organics deposited on wafer surfaces can affect transistor gate oxide thickness control and gate oxide reliability. It is desirable to have as low a detection limit as possible for metal contaminants while still having the ability to analyze molecular species present in process solutions .
  • One aspect of the present invention provides the integration of a plasma ionization source and an electrospray , ionization capability in a mass spectrometer such that the different ionization sources can be operated independently or together to achieve sample ionization in the way that is optimal for the analytical need at hand.
  • One embodiment makes use of a microwave-induced plasma (MIP) source for this purpose due to its relatively small size, successful ionization characteristics, and a lower power dissipation.
  • MIP microwave-induced plasma
  • the present invention enables operation without compromise to either method of ionization and provides the ability to switch from one ionization source to another under electrical and software control without any hardware changes.
  • MIP source on electrospray off.
  • a liquid or gas is delivered to a nebulizer which forms an uncharged spray when mixed with a carrier gas, which could be Ar, He or N 2 .
  • the MIP source is energized and provides the ionization necessary for MS analysis.
  • MIP source off MIP source off, electrospray on.
  • the MIP source is not energized, and invisible with respect to the normal operation of the electrospray source for ionization.
  • the electrospray provides the ionization required for MS analysis .
  • a mass spectrometer contains a plasma source coupled to an electrospray ionization source via a capillary or tube.
  • the plasma source in one embodiment is an inductively coupled plasma (ICP) source and in another embodiment is a microwave induced plasma (MIP) source.
  • ICP inductively coupled plasma
  • MIP microwave induced plasma
  • a microwave plasma source is placed in series between the sample introduction or spray chamber and the mass spectrometer.
  • a quartz capillary or tube of other usable material runs from the sample introduction or spray chamber that is normally at atmospheric pressure, through the center of the microwave cavity and into the entrance of the mass spectrometer that is at a pressure reduced from atmospheric-
  • the liquid or gas sample is injected through either the electrospray needle or through a nebulizer into the sample introduction chamber.
  • the quartz tube has a smaller inside diameter at its opening into the sample introduction chamber and then opens up into a larger diameter inside the microwave cavity and may or may not close back down to a smaller diameter at the other end or entrance to the mass spectrometer.
  • the dimensions of the quartz tube are as follows: an outside diameter (OD) of 6.5 mm and a length of 10 cm, with the end at the sample introduction end portion having an inside diameter (ID) of 0.5 mm and a length of 4 cm, and the second portion having an ID of 4 mm and a length of 6 cm (initiating just before the plasma generation region and ending at the entrance to the mass spectrometer region) .
  • the larger inside diameter of the middle portion acts as a pressure reducer in the region where the plasma is generated and the ionization takes place.
  • the small entrance portion of the capillary is large enough to allow an aerosol to pass through without coating the inside of the tube, but small enough to result in a significant pressure differential between the sample introduction chamber and the plasma region.
  • the addition of the MIP source requires a relatively simple mechanical interface.
  • the addition to the length of the overall tool i'S a fraction of the length of the original sample introduction chamber, keeping the size of the combined sources manageable.
  • the electrospray can be adjusted to create either positive or negative ions that will be preferentially attracted to the entrance of the capillary due to the positive or negative voltage applied between the electrospray and the electrode surrounding the end of the capillary during normal operation.
  • this mode it may be possible to introduce certain species preferentially for analysis while reducing the introduction of others. This has the potential for minimizing spectral background and interferences for selected species.
  • the ions and the neutrals that enter the capillary will be driven into the reduced pressure region where the microwave-induced plasma is formed. Normal MIP ionization will then occur as in the first and second modes.
  • the present invention enables detection of atomic species to parts per trillion (ppt) , and potentially beyond, by the use of a relatively low power, small plasma ionization source that can be compatibly inserted between an electrospray source and the entrance to a mass spectrometer.
  • the electrospray mode that enables complementary molecular analysis capability remains fully operational. It also enables the use of plasma ionization for the breakdown of strong acidic or basic solutions for trace metals analysis that is difficult and sometimes impossible with electrospray ionization sources.
  • the present invention provides molecular specie detection, identification and quantitative analysis as well as ultimate analytical sensitivity for trace metals.
  • the benefits of both high sensitivity elemental analysis (ICP ionization, for example) with the ability to perform molecular analysis at the same time or nearly the same time (electrospray ionization source, for example) is combined into one system.
  • An advantage of having both modes present is that with the plasma source turned on, there is a high elemental sensitivity, allowing for the detection and measurement of trace metal concentration. With the electrospray sourced turned on and the plasma source turned off, molecular species will remain largely intact for analysis in the mass spectrometer allowing for the detection and identification of molecular and organic species and contaminants and their quantitative analysis in the analyte.
  • the ability to analyze full molecular species in the electrospray ionization mode provides information that enables the identification of the origin of trace metal or any other contaminants present in the analyte.
  • Figure 1 shows a portion of a system for analyzing gases and chemical solutions according to one embodiment of the present invention
  • Figure 2 shows a 2 sample calibration curve for cobalt using the present invention
  • Figures 3, 4, and 5 are examples of cobalt mass spectra for different solutions using the present invention.
  • Figure 6 shows a portion of the system of Figure 1 according to another embodiment .
  • FIG. 1 is a diagram showing a portion of an apparatus 100 for analyzing gases and chemical solutions according to one embodiment of the present invention.
  • Apparatus 100 includes an electrospray needle or nebulizer 102 that directs nebulized liquid into a sample introduction or spray chamber 104 at atmospheric pressures.
  • spray chamber 104 may be filled with helium and an aerosol that could be highly acidic.
  • Electrospray needle 102 may be one built by Analytica of Branford or may alternatively be a Burgener nebulizer (e.g., an Ari Mist model), in which the electrospray is used as an atomizer and is not energized electrically.
  • the nebulized liquid is drawn from a sample of solution to be analyzed, such as a SC2 or UPW bath.
  • the nebulized aerosol is formed by combining a carrier gas, such as argon, helium, or nitrogen, with the analyte to form a spray.
  • a carrier gas such as argon, helium, or nitrogen
  • the pressure of the carrier gas as it is introduced into electrospray needle 102 is approximately 60 to 120 psi. This results in a gas flow rate of approximately 200 standard ml/rain through the output of the nebulizer needle.
  • the incoming liquid flow rate ⁇ of the analyte) is approximately 5 to 75 microliters /min.
  • the ions are then drawn toward the entrance of a capillary or quartz tube 106 by an electric field (for example from a charge of - 5 kV to -6 kV at the entrance of the quartz tube) . Further, in one embodiment, heated N 2 or He gas is introduced around the entrance of quartz tube 106 to drive off residual solvent molecules.
  • an additional nebulizer or nebulizers are located in the sample introduction or spray chamber 104. These nebulizers (not shown) may be used to produce an aspirated spray of the analyte for introduction into tube 106 as an alternative to using the electrospray source.
  • quartz tube 106 has a first end portion 108 and a second end portion 110.
  • First end portion 108 is inserted into sample introduction or spray chamber 104 for receiving the samples to be analyzed, and second end portion 110 is adjacent to a first skimmer 112.
  • quartz tube 106 has an outside diameter of approximately 6.5 mm and a length of approximately 10 cm.
  • the first portion 108 of tube 106 starting from sample introduction chamber 104 has an inside diameter of approximately 0.5 mm and a length of approximately 4 cm, while second portion 110 has an inside diameter of approximately 4 mm and a length of approximately 6 cm.
  • first end portion 108 reduces the pressure of the ion stream as it passes through first end portion 108 and into second end portion 110, where a plasma 114 is generated.
  • first end portion 108 is heated to minimize water content in the plasma. Any suitable heater can be used, such as a heater 116 positioned adjacent a portion of first end portion 108 capable of temperatures up to approximately 100 0 C. The heater or heaters can help in reducing or eliminating water droplets within the tube that can diminish the effectiveness of the plasma.
  • Another method of desolvating the aerosol before it reaches the plasma generation area is to direct a heated drying gas into the spray inside the sample introduction chamber.
  • the gas used is typically nitrogen or helium.
  • the second portion 110 of the capillary is positioned in the plasma generation region 114 of a plasma generation source 118, which in one embodiment is an MIP source microwave cavity, such as a Beenakker Microwave Cavity from Opthos Instruments, Inc. of Maryland.
  • a conventional microwave power supply (not shown) is coupled to the plasma generation source 118.
  • This source is able to deliver up to 300 W at a freguency of 2.45 GHz to the cavity to a generate plasma at 50 Torr. Higher powers may also be suitable with some analytes and different hardware construction materials.
  • the plasma is generated between two skimmer plates or cones.
  • An inductively coupled plasma (ICP) source can be used as an alternative, once the technology has advanced to the point where small suitable sources as in the MIP case, are available.
  • the end of second end portion 110 is secured or sealed the first skimmer plate 112 (Skimmerl) by an 0-ring 120.
  • the 0-ring is made from a material called Kalrez 4079, which is used in industry for plasma applications and has been reported to be useable in temperatures up to 600 0 F. With this type of 0-ring, the power supplied is to be no more than 200 W, since higher energy levels are likely to degrade the 0-ring, resulting in seal leakage.
  • first skimmer plate 112 the distance between first skimmer plate 112 and the center of the plasma is approximately 12 mm. Further, first skimmer plate 112 has an opening that lets ions pass from quartz tube 106 to a skimmer cone 122 (Skimmer2). In one embodiment, the opening is approximately 0.5 to 1 mm in diameter.
  • molecules and/or ions from the nebulized or ionized analyte will travel through the capillary from the spray chamber into the capillary and on into the plasma zone 114 where all species will in general be fully ionized if the plasma is on.
  • the pressure difference between sample introduction chamber 104 and the vacuum present in a hexapole ion guide 123 portion of the mass spectrometer provides the driving force for movement of the analyte, whether it is in ionized form or not, and some carrier and heating gas, through the capillary, into the plasma generation region and into the entrance of the mass spectrometer at the end 110 of the capillary tube 106.
  • Ions generated in the plasma or earlier in the electrospray will exit the quartz tube and enter skimmer cone 122.
  • a large voltage difference between the capillary exit and the skimmer cone entry causes collisions between the ions and collision gas molecules, with ions then entering hexapole ion guide or trap 123.
  • This provides an additional mode of ionization as an assist to electrospray ionization for electrospray only operation (standard electrospray ionization mass spectrometry procedure) .
  • Ions then enter the hexapole ion guide where ions in the mass range of interest are retained, while allowing other ions and neutrals to escape.
  • Ions enter the mass spectrometer such as a time-of- flight mass spectrometer from Analytica of Branford, Connecticut.
  • the charge-to-mass ratio of all captured ions is then measured per normal mass spectrometry procedures. Constituents and contaminants present in the analyte are identified.
  • a pulser imparts each packet of ions with the same kinetic energy.
  • the ions drift through the analyzer, the ions separate based on their masses, with lighter ions traveling faster than heavier ions.
  • ions are reflected by an ion mirror back to towards a detector plate at the top of the drift tube. Lighter ' ions hit the detector first, and by determining the time of ion arrival, the mass of different ions is determined.
  • Figure 6 shows another embodiment of the present invention, wherein the capillary or tube 106 includes a third portion 600 extending from second portion 110 into a mass spectrometer 602.
  • Third portion 600 has a narrower inside diameter than second portion 110.
  • tube 106 is approximately 28 cm in length, with first portion 108 having an inner diameter of 0.6 mm and a length of 4 cm, second portion 110 having an inner diameter of 4 mm and a length of 4 cm, and third portion 600 having an inner diameter of 0.6 mm and a length of 20 cm.
  • a "soft" ionization source such as electrospray
  • a "hard” ionization source such as plasma ionization
  • plasma or MIP source 118 is on, while the electrospray source is off with apparatus 100 for generating atomic species.
  • apparatus 100 operates like a standard plasma source mass spectrometer.
  • the liquid or gas is delivered to nebulizer 102 which forms an uncharged spray when mixed with a carrier gas, such as, but not limited to Ar, He or N 2 .
  • MIP source 118 is energized and provides the ionization necessary for mass spectrum analysis.
  • MIP source 118 is off, while the electrospray source on for generating molecular species.
  • apparatus 100 operates like a standard electrospray mass spectrometer.
  • the electrospray provides the ionization required for mass spectrum analysis.
  • both MIP source 118 and the electrospray source are on.
  • the electrospray ionization source will act as a selectivity mode for desired analytes.
  • the electrospray will select either positive or negative ions and the MIP source will fragment them completely to their elemental components.
  • the nebulizer needle is used for aspiration of the incoming solution into the sample introduction chamber
  • the electrospray needle is used to aspirate fluid into the chamber. Gas injection can potentially be through either source .

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Electron Tubes For Measurement (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

L'invention concerne une source d'ionisation MIP par plasma induite par électro-pulvérisateur/micro-ondes et utilisée comme source d'ionisation pour un spectromètre de masse (118). L'électro-pulvérisateur peut être mis en oeuvre en mode positif ou négatif ou peut être éteint (104). L'instrument peut être mis en oeuvre dans plusieurs modes. L'instrument possède sa sensibilité élémentaire maximale quand l'électro-pulvérisateur est éteint et la MIP allumée. Le fonctionnement en mode mixte permet potentiellement de déterminer des informations supplémentaires relatives aux constituants chimiques présents dans les analytes. Les informations moléculaires peuvent être obtenues dans un mode d'électo-pulvérisateur pur et sont utilisées pour analyser des composés organiques.
PCT/US2005/024001 2004-02-05 2005-07-06 Nebuliseur a source de plasma WO2007008191A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PCT/US2005/024001 WO2007008191A1 (fr) 2005-07-06 2005-07-06 Nebuliseur a source de plasma
TW094123459A TW200703412A (en) 2004-02-05 2005-07-11 Nebulizer with plasma source

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/US2005/024001 WO2007008191A1 (fr) 2005-07-06 2005-07-06 Nebuliseur a source de plasma

Publications (1)

Publication Number Publication Date
WO2007008191A1 true WO2007008191A1 (fr) 2007-01-18

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PCT/US2005/024001 WO2007008191A1 (fr) 2004-02-05 2005-07-06 Nebuliseur a source de plasma

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2456131A (en) * 2007-12-27 2009-07-08 Thermo Fisher Scient Sample Excitation apparatus and method for spectroscopic analysis
CN109545648A (zh) * 2018-12-27 2019-03-29 昆山禾信质谱技术有限公司 一种复合电离装置
CN116840010A (zh) * 2023-07-03 2023-10-03 暨南大学 一种雾化室进气装置

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5051557A (en) * 1989-06-07 1991-09-24 The United States Of America As Represented By The Secretary Of The Department Of Health And Human Services Microwave induced plasma torch with tantalum injector probe
US6060705A (en) * 1997-12-10 2000-05-09 Analytica Of Branford, Inc. Electrospray and atmospheric pressure chemical ionization sources

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5051557A (en) * 1989-06-07 1991-09-24 The United States Of America As Represented By The Secretary Of The Department Of Health And Human Services Microwave induced plasma torch with tantalum injector probe
US6060705A (en) * 1997-12-10 2000-05-09 Analytica Of Branford, Inc. Electrospray and atmospheric pressure chemical ionization sources

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2456131A (en) * 2007-12-27 2009-07-08 Thermo Fisher Scient Sample Excitation apparatus and method for spectroscopic analysis
WO2009083242A1 (fr) * 2007-12-27 2009-07-09 Thermo Fisher Scientific (Bremen) Gmbh Appareil à exciter les échantillons et procédé d'analyse spectroscopique
GB2456131B (en) * 2007-12-27 2010-04-28 Thermo Fisher Scient Sample excitation apparatus and method for spectroscopic analysis
US8637812B2 (en) 2007-12-27 2014-01-28 Thermo Fisher Scientific (Bremen) Gmbh Sample excitation apparatus and method for spectroscopic analysis
CN109545648A (zh) * 2018-12-27 2019-03-29 昆山禾信质谱技术有限公司 一种复合电离装置
CN109545648B (zh) * 2018-12-27 2024-04-30 昆山禾信质谱技术有限公司 一种复合电离装置
CN116840010A (zh) * 2023-07-03 2023-10-03 暨南大学 一种雾化室进气装置
CN116840010B (zh) * 2023-07-03 2024-05-03 暨南大学 一种雾化室进气装置

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