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WO1996037905A1 - Procede d'ionisation par decharge lumineuse de magnetron haute frequence et source d'ions - Google Patents

Procede d'ionisation par decharge lumineuse de magnetron haute frequence et source d'ions Download PDF

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Publication number
WO1996037905A1
WO1996037905A1 PCT/DE1996/000938 DE9600938W WO9637905A1 WO 1996037905 A1 WO1996037905 A1 WO 1996037905A1 DE 9600938 W DE9600938 W DE 9600938W WO 9637905 A1 WO9637905 A1 WO 9637905A1
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WO
WIPO (PCT)
Prior art keywords
target
ion source
glow discharge
frequency
magnetic field
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/DE1996/000938
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German (de)
English (en)
Inventor
Anatolij Saprykin
Sabine Becker
Hans-Joachim Dietze
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.)
Forschungszentrum Juelich GmbH
Original Assignee
Forschungszentrum Juelich GmbH
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 Forschungszentrum Juelich GmbH filed Critical Forschungszentrum Juelich GmbH
Publication of WO1996037905A1 publication Critical patent/WO1996037905A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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]

Definitions

  • the invention relates to methods according to the preamble of claim 1 for high-frequency operated magnetron glow discharge ionization, in particular in a low-pressure argon plasma for mass spectrometry, in particular non-conductive solid samples. Furthermore, the invention relates to an ion source according to the preamble of claim 3.
  • ionization methods are used as prior art in mass spectrometry for direct evaporation (atomization) and ionization of the sample material to be examined, and ion sources are used which allow simultaneous evaporation (atomization) of the solid samples and ionization of the vaporized sample atoms.
  • the object is achieved by a method according to the entirety of the features according to claim 1.
  • a further expedient variant is found in the dependent sub-claim 2.
  • the object is achieved by an ion source according to claim 3.
  • the invention according to claim 1 provides a method for highly sensitive evaporation (atomization) and ionization in a high frequency operated magnetron Glow discharge ion source at low argon pressure.
  • this method can be used for mass spectrometric analysis of conductive, semiconducting and non-conductive solids, liquids and gases.
  • the method according to the invention is used both for the determination of the main, minor or trace element concentrations and for isotope or depth profile analysis.
  • the method can be used universally for solving analytical problems in solid state physics such as in surface physics, materials research, geology, nuclear physics and solid state chemistry. On the one hand it is for the quantitative determination of trace element concentrations, on the other hand it is also. suitable for deep profile analysis of bulk materials and thick layers.
  • the method is used in the isotope analysis of all chemical elements, especially in solid samples with different conductivity, such as metals, alloys, semiconductors or insulators.
  • the invention further relates to a system with an ion source for sample evaporation and ionization (ion source), for example in combination with one high-resolution double-focusing mass spectrometer for ultra-sensitive trace element analysis and depth profile analysis of various sample materials - especially non-conductive ceramics and thick insulating layers.
  • ion source for sample evaporation and ionization
  • the glow discharge ion source which contains a chamber in which a target as cathode, a sputtering gas for removing particles from the target, and an opening to a mass spectrometer unit, has a magnet on the back of the target, which is arranged so that the magnetic field lines in the plasma area are oriented towards the target surface.
  • the ion source can thus be operated with a lower sputtering gas pressure, in particular argon pressure, and the ion source as a result has a higher sensitivity.
  • the method according to the invention allows sample material to be effectively vaporized (atomized) and ionized in a high-frequency magnetron glow discharge of a low-pressure argon plasma.
  • the invention is explained in more detail with reference to figures and embodiment. Show it:
  • Figure 1 Planar magnetron glow discharge ion source
  • Figure 2 Schematic diagram of the interface between the high-frequency generator and the high-frequency glow discharge ion source
  • VB VE - magnetic and electrical field gradient vector
  • V electron drift vector
  • Figure 4 Coupling of a high-frequency magnetron glow discharge ion source with a mass spectrometer
  • Table 1 Influence of the magnetic field on the ion intensities of the gas discharge species and the matrix components using a planar high-frequency GDMS for a glass sample.
  • FIG. 1 The experimental arrangement of a planar magnetron glow discharge ion source for flat sample geometries is shown in FIG. 1.
  • the ion source consists of a magnet and sample holder 1 made of copper for flat and pin-shaped sample geometries, the ion source housing 6, preferably made of VA steel anode with a back 2 made of copper and a flat sample 3, basically supplied big size [cathode (3)].
  • the arrangement also has an argon inlet system 4, an interface 5 to the mass spectrometer MS, a magnetic ring 7, and a Viton O-ring 8 and an insulating intermediate piece 9 [Macor (9)].
  • the glow discharge ion source (GD ion source) is directly coupled to a mass spectrometer (e.g. double-focusing system).
  • the GD ion source is located in an ion source chamber which is used for evacuation, e.g. with a turbomolecular pump is provided.
  • Highly pure argon (for example with a purity of 99.9995%) is preferably introduced as the discharge gas into the GD ion source via the gas inlet system 4.
  • the argon pressure in the GD ion source (PGD) is - depending on the selected sample material - 0.1 to 10 Pa, for example.
  • Optimal discharge conditions with maximum ion current intensities are measured in such a system with an output of 20-30 W and a plasma gas pressure of 1-3 Pa.
  • the back cover made of solid copper of the GD ion source is connected to a cooling system (vapor of liquid nitrogen). In this way, a temperature of the ion source of up to 50 ° C can be maintained during the sputtering process.
  • a power meter 2 in which the electrical circuit diagram for the voltage supply on the sample is shown, A power meter 2, a high-frequency filter 4, a low-frequency filter 5, a DC voltmeter and a high-voltage power supply HS can be removed.
  • the sputtering rate, in particular of compact, non-conductive sample materials, and thus the sensitivity of the analysis method (high-frequency-operated magneton GDMS) can be increased by at least one order of magnitude. Due to the lower working pressure compared to the high-frequency GDMS (PQD 0.1 -lhPa), the molecular ion or cluster ion formation rate (e.g. the argide) drops significantly. As a result, the detection limits for element trace analysis are significantly reduced down to the ppb concentration range.
  • the dimensions of the magnet must be selected so that a smooth crater floor is created during the sputtering process.
  • FIG. 1 The technical implementation of the coupling of a high-frequency glow discharge ion source with a commercial mass spectrometer is shown in FIG.
  • a coupling e.g. be provided with an HR-ICP-MS (high resolution inductively coupled plasma mass spectrometer), the inductively coupled plasma ion source being substituted by the high-frequency magnetron glow discharge ion source.
  • An advantage of such a device configuration is that the ion source is at ground potential and 05
  • Table 1 shows the analytical results from mass spectra of the high-frequency GDMS without and with the influence of a magnetic field on the sample surface in comparison to one another.
  • the experimental results show an increase in the total ion current by more than an order of magnitude. Furthermore, an increase in the intensity of the sample ions which are relevant for the analysis and on the other hand a reduction in the plasma ions which disrupt the analysis were achieved in this way.

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

Abstract

L'invention concerne un procédé d'ionisation de matériau d'échantillonnage, selon lequel un plasma est produit sur une cible contenant le matériau d'échantillonnage, par décharge lumineuse de magnétron haute fréquence, et le matériau d'échantillonnage est extrait de la cible au moyen d'un gaz de pulvérisation pour être transmis à une spectromètre de masse, puis est ionisé. Un champ magnétique est produit à la surface de la cible, de manière à ce que dans la zone du plasma, les lignes de champ magnétique soient orientées en direction de la surface de la cible. Il est avantageux de prévoir un aimant sur la face de la cible opposée au plasma, disposé de manière à ce que dans la zone du plasma, les lignes de champ magnétique soient orientées en direction de la surface de la cible.
PCT/DE1996/000938 1995-05-23 1996-05-21 Procede d'ionisation par decharge lumineuse de magnetron haute frequence et source d'ions Ceased WO1996037905A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19518374.6 1995-05-23
DE1995118374 DE19518374A1 (de) 1995-05-23 1995-05-23 Verfahren zur hochfrequenzbetriebenen Magnetron-Glimmentladungsionisation, sowie Ionenquelle

Publications (1)

Publication Number Publication Date
WO1996037905A1 true WO1996037905A1 (fr) 1996-11-28

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Application Number Title Priority Date Filing Date
PCT/DE1996/000938 Ceased WO1996037905A1 (fr) 1995-05-23 1996-05-21 Procede d'ionisation par decharge lumineuse de magnetron haute frequence et source d'ions

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DE (1) DE19518374A1 (fr)
WO (1) WO1996037905A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108615668A (zh) * 2018-04-04 2018-10-02 中国科学院上海硅酸盐研究所 运用环形磁场增强射频辉光放电质谱离子信号强度的装置及方法
CN108896648A (zh) * 2018-04-04 2018-11-27 中国科学院上海硅酸盐研究所 运用阵列磁铁增强射频辉光放电质谱信号强度的装置及方法
WO2019192494A1 (fr) * 2018-04-04 2019-10-10 中国科学院上海硅酸盐研究所 Appareil et procédé pour améliorer l'intensité de signal d'une spectrométrie de masse à décharge luminescente à radiofréquence
US10468240B2 (en) 2018-04-03 2019-11-05 Glow Technology KK Glow discharge system and glow discharge mass spectroscope using the same

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102014226039A1 (de) * 2014-12-16 2016-06-16 Carl Zeiss Smt Gmbh Ionisierungseinrichtung und Massenspektrometer damit

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DD146366A1 (de) * 1979-09-26 1981-02-04 Frieder Bigl Vorrichtung zur erzeugung von ionen-oder neutralteilchenstrahlen
DD251436A1 (de) * 1986-07-28 1987-11-11 Akad Wissenschaften Ddr Ionenquelle
DE4235064A1 (de) * 1992-10-17 1994-04-21 Leybold Ag Vorrichtung zum Erzeugen eines Plasmas mittels Kathodenzerstäubung

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
L. MC CIAG ET AL: "Pressure sensitivity of emission intensities and plasma voltage for a planar magnetron glow discharge", APPLIED SPECTROSCOPY, vol. 44, no. 7, 1990, BALTIMORE US, pages 1176 - 1182, XP002012588 *
MYERS D P ET AL: "CHARACTERIZATION OF A RADIO-FREQUENCY GLOW DISCHARGE/TIME-OF-FLIGHT MASS SPECTROMETER", APPLIED SPECTROSCOPY, vol. 48, no. 11, 1 November 1994 (1994-11-01), pages 1337 - 1346, XP000484193 *
SHI Z ET AL: "APPLICATION OF A MAGNETRON GLOW DISCHARGE TO DIRECT SOLID SAMPLING FOR MASS SPECTROMETRY", APPLIED SPECTROSCOPY, vol. 49, no. 9, 1 September 1995 (1995-09-01), pages 1232 - 1238, XP000524518 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10468240B2 (en) 2018-04-03 2019-11-05 Glow Technology KK Glow discharge system and glow discharge mass spectroscope using the same
CN108615668A (zh) * 2018-04-04 2018-10-02 中国科学院上海硅酸盐研究所 运用环形磁场增强射频辉光放电质谱离子信号强度的装置及方法
CN108896648A (zh) * 2018-04-04 2018-11-27 中国科学院上海硅酸盐研究所 运用阵列磁铁增强射频辉光放电质谱信号强度的装置及方法
WO2019192494A1 (fr) * 2018-04-04 2019-10-10 中国科学院上海硅酸盐研究所 Appareil et procédé pour améliorer l'intensité de signal d'une spectrométrie de masse à décharge luminescente à radiofréquence

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Publication number Publication date
DE19518374A1 (de) 1996-11-28

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