EP0930810A1 - Plasmabrenner mit Verstellbarer Verteilung und Gasanalysenanlage die diesen Brenner gebraucht - Google Patents

Plasmabrenner mit Verstellbarer Verteilung und Gasanalysenanlage die diesen Brenner gebraucht Download PDF

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Publication number
EP0930810A1
EP0930810A1 EP98402992A EP98402992A EP0930810A1 EP 0930810 A1 EP0930810 A1 EP 0930810A1 EP 98402992 A EP98402992 A EP 98402992A EP 98402992 A EP98402992 A EP 98402992A EP 0930810 A1 EP0930810 A1 EP 0930810A1
Authority
EP
European Patent Office
Prior art keywords
gas
plasma
tube
injector
torch
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.)
Withdrawn
Application number
EP98402992A
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English (en)
French (fr)
Inventor
Martine Carre
Eric Coffre
Christian Trassy
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.)
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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
Priority claimed from FR9716619A external-priority patent/FR2773299B1/fr
Priority claimed from FR9716620A external-priority patent/FR2773300B1/fr
Application filed by Air Liquide SA, LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Publication of EP0930810A1 publication Critical patent/EP0930810A1/de
Withdrawn legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
    • H05H1/00—Generating plasma; Handling plasma
    • H05H1/24—Generating plasma
    • H05H1/26—Plasma torches
    • H05H1/30—Plasma torches using applied electromagnetic fields, e.g. high frequency or microwave energy

Definitions

  • the present invention relates to a torch with plasma, intended for the excitation of a gas with a view to its analysis.
  • the invention also relates to an installation analysis of a gas using such a plasma torch.
  • gas analysis techniques are indirect techniques, such as filtration, hydrolysis or bubbling, according to which the impurities with which it is to determine the concentration are extracted from the gas before analysis.
  • the technique of analysis by filtration uses a gas filtration membrane to analyze in order to retain the impurities it contains. These the latter are then dissolved in an acid solution, then analyzed, for example by spectrometry, with a view to determine the nature and concentration.
  • a gas sample to be analyzed is introduced into a thermal source, such as a plasma, capable of dissociating chemical species into free atoms present in the sample and then to excite and possibly to ionize the atoms obtained. These atoms excited are then detected from the measurement of different wavelengths they emit, or, if they are ionized, from the measurement of their mass.
  • a thermal source such as a plasma
  • the gas passing through this zone device experiences less excitation, which contributes to degrade the accuracy of the measurement.
  • the object of the invention is to overcome the drawbacks cited above.
  • a plasma torch for the excitation of a gas for analysis comprising an injector configured as a main tube intended to be connected to a gas supply source at analyze, and an external cylindrical double-walled sleeve, coaxial with the injector, and delimiting between its walls consecutive internal and external annular canal cylindrical supply of a plasma gas intended for be connected to a corresponding power source in view of the production of a plasma at the outlet of said sleeve, is characterized in that said injector is of diameter variable.
  • the invention also relates to an installation gas analysis, characterized in that it comprises a plasma torch as defined above, connected to a gas supply source to be analyzed, to a source supply of plasma gas and advantageously also to a source of gas to guide the gas to be analyzed in the plasma generated at the outlet of the torch in the gas plasma, and optical detection means capable of measure the light intensity emitted by impurities present in the plasma, connected to a processing unit comprising means for calculating the concentration of impurities from the light intensity value measured and at least one predetermined reference value, stored in a memory associated with said unit of treatment, and obtained by prior calibration.
  • a plasma torch is shown intended to dissociate the chemical species from a gas including impurities, to generate free atoms and excite the atoms thus obtained for the purpose of determining of the impurity concentration.
  • the gas to be analyzed consists of a gas used in the field of semiconductor manufacturing, such as halogen or fluorinated gas, and the impurities are formed by metallic elements such than nickel, iron, manganese ...
  • the plasma torch designated by the general numerical reference 10 includes: a central injector 12 configured in the form of a tube, a external cylindrical sleeve 14 with double wall (28/30) and a winding 16 connected to a high current source frequency 18.
  • the wall 20 of the injector internally defines a channel 26 intended to be connected to a power source torch 10 into a gas to be analyzed (not shown in this figure).
  • the sleeve 14 has an inner wall 28 and an outer wall 30 which extends beyond the free end of the inner wall 28.
  • These walls are made of a material suitable for the intended use, i.e. capable of withstanding high temperatures, for example silica glass.
  • the internal and external walls of the sleeve 14 delimit between them a cylindrical annular channel 32 connected, in operation, to a gas supply source plasmagen, e.g. Argon, for production of a plasma at the outlet of the sleeve.
  • a gas supply source plasmagen e.g. Argon
  • the consecutive external wall 30 of the sleeve forms the external wall of the torch 10 and is equipped, in the vicinity of its end edge, of the winding 16.
  • the latter is connected to the current source high frequency, conventional type, capable of delivering to the winding a current at a frequency between 5 MHz and 100 MHz.
  • the winding Under the action of the current source 18, the winding generates, as is conventional, an electromagnetic field radially decreasing towards the axis XX 'of the torch 10.
  • Plasma gas supplied through the channel annular 32, at a flow rate for example of 20 liters / minute, is delivered in an area where the value of the electromagnetic field is substantially maximum. The latter creates a plasma in the plasma gas by acceleration of its charged particles.
  • the plasma shows movements of recirculation under the effect of Lorentz forces applying to charged particles.
  • the gas velocity is negative in the axial zone, that is to say that the particles are animated by a movement directed upstream of the torch, considering the direction gas flow, which opposes the introduction of gas to analyze.
  • the gas to be analyzed is introduced into the internal supply channel 26 according to the direction represented by arrow F2 in the axial zone, at a rate commonly of the order of a few ml / minute at a few hundred ml / minute.
  • a detector photoelectric 34 is connected to a processing unit 36 calculating the concentration of impurities in gas from the wavelength value of the radiation emitted by particles of excited impurities, as will be described in detail later.
  • FIG. 2 shows an embodiment of the variable diameter injector according to the invention.
  • the injector 12 is here formed of two coaxial tubes external (20) and internal (90), the internal tube 90 being suitable to slide vertically inside the outer tube.
  • This sliding effect is, for the embodiment shown here, obtained by pneumatic control 91, acting on a micro-cylinder 92.
  • This internal tube driven by the micro-cylinder according to the mechanism which has just been described, can therefore slide vertically inside the outer tube 20.
  • Lowering the upper end of the inner tube relative to the upper end of the outer tube may typically be of the order of 1 to 2 cm.
  • the torch here comprises a central injector 12 a little particular which comprises, in accordance with one of the modes advantageous implementation of the invention previously mentioned, an additional external tube 22, coaxial with the tube main 20, and thus delimiting two coaxial channels internal and external respectively for one to the supply of gas to the torch to be analyzed and the other to supplying the torch with a guide gas for said gas at analyze in plasma.
  • the guide gas is delivered at a flow rate for example of the order of a few hundred ml / minute, and ensures therefore guiding the gas to be analyzed in the plasma P. This guidance thus opposes the action of Lorentz forces on the gas to be analyzed by helping to prevent the gas from analyze is deflected (i.e. ensuring that the whole of the sample reaches the plasma).
  • the gas guide whose composition is perfectly controlled, being driven towards the periphery of the torch instead of gas to be analyzed, deposits on the wall are thus avoided external 30, particles forming part of the gas to be analyzed, choosing the guide gas so appropriate.
  • the guide gas comprises helium or argon or a mixture of such gases.
  • the injection of a gas of guidance inside the injector is optional.
  • a simple tube 20 for injecting the gas to be analyzed without for example representing the presence an internal tube 90 coaxial with the external tube 20, and being able slide inside this outer tube 20 (mode of Figure 2).
  • the installation includes a plasma torch 54 according to the invention, for example similar to the torch described in the context of FIGS. 1 and 2, associated with a high frequency current generator 56, and at a photodetector 58 itself connected to a processing unit 60.
  • cylindrical sleeve torch 54 external is supplied with Argon (Ar) for create a plasma preferably at atmospheric pressure or slight depression.
  • the injector 62 intended to allow the introduction into the plasma of the gas to be analyzed is connected to a first mixer 64 comprising a first input 66 supplied with an inert gas, such as Argon, allowing to increase the gas drive speed to analyze, and a second input 68 connected to the output a second mixer 70.
  • a first mixer 64 comprising a first input 66 supplied with an inert gas, such as Argon, allowing to increase the gas drive speed to analyze, and a second input 68 connected to the output a second mixer 70.
  • Unit 76 has an entrance for admission aerosols from unit 78.
  • Unit 78 also has a gas inlet 86 allowing the admission of an inert gas such as argon.
  • the elements to be dosed at a known concentration and in a given form (liquid, solid or gaseous) closest to that of elements to be determined in the gas samples G.
  • the polluting elements can be in the form solid or gaseous, and more rarely liquid.
  • solid particles often present in chemical gases are less than one micron in size. For such a dimension, these small particles are rapidly volatilized and generate in an Argon plasma a light intensity identical to that generated by gaseous compounds.
  • gas 86 for example argon transports this aerosol to the desolvation unit.
  • the standard samples thus created are trained in plasma P by a gas similar to gas G, but lacking impurity, or by Argon.
  • the light intensity emitted by the impurities is detected by photodetector 58 (monochromator and / or polychromator) then stored in a memory 84 of the unit analysis 60.
  • the gas G is presented at the input of mixer 70 and is injected into the plasma P.
  • the light intensity emitted by the impurities of gas G is then presented at the input of the analysis unit 60.
  • the latter includes means of calculation of the type classic, ensuring the comparison between the intensity light detected impurities to be measured and the values of reference previously obtained and stored in the memory 84.
  • the exact concentration of particles in the gas G is thus for example obtained by identification of the sample whose corresponding signal has a wavelength and intensity identical to the values measured from gas G.
  • Figure 6 represents a schematic view in axial section of a torch plasma according to the invention, incorporating at the level of sleeve an intermediate tube.
  • the torch shown in Figure 6 indeed has a tube intermediate 40, coaxial with the sleeve 42, located between the outer and inner walls of the sleeve (42A and 42B), the tube intermediate 40 and the outer wall 42A of the sleeve delimiting a gas supply channel 45 protection of the external wall (42A) of the torch against solid deposits.
  • the torch shown in Figure 6 is provided with a winding 46 supplied by a current source at high frequency 48 and placed in the vicinity of the unit end of the torch, and a photodetector 50 connected to a processing unit 52.
  • the supply channel 45 is therefore connected to a shielding gas supply source (not shown) able to react with species likely to deposit on the internal surface of the external wall 42A of the torch to form a volatile compound.
  • the gas to be analyzed comprises silane (SiH 4 )
  • the shielding gas comprises chlorine, possibly mixed with argon, reacting with silicon to form SiCL 4 .
  • the latter compound is a volatile species, any deposit based on silicon is thus avoided.
  • the torch here comprises a central injector 38 a double-walled (38A, 38B) for injecting part of the gas to analyze and on the other hand a "guide" gas.

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Electromagnetism (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Plasma Technology (AREA)
EP98402992A 1997-12-29 1998-11-30 Plasmabrenner mit Verstellbarer Verteilung und Gasanalysenanlage die diesen Brenner gebraucht Withdrawn EP0930810A1 (de)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
FR9716619A FR2773299B1 (fr) 1997-12-29 1997-12-29 Torche a plasma a injecteur reglable et installation d'analyse d'un gaz utilisant une telle torche
FR9716619 1997-12-29
FR9716620 1997-12-29
FR9716620A FR2773300B1 (fr) 1997-12-29 1997-12-29 Torche a plasma et installation d'analyse de gaz utilisant une telle torche

Publications (1)

Publication Number Publication Date
EP0930810A1 true EP0930810A1 (de) 1999-07-21

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EP98402992A Withdrawn EP0930810A1 (de) 1997-12-29 1998-11-30 Plasmabrenner mit Verstellbarer Verteilung und Gasanalysenanlage die diesen Brenner gebraucht

Country Status (7)

Country Link
US (1) US6236012B1 (de)
EP (1) EP0930810A1 (de)
JP (1) JPH11248632A (de)
KR (1) KR19990063580A (de)
CN (1) CN1235274A (de)
SG (1) SG71892A1 (de)
TW (1) TW412636B (de)

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7511246B2 (en) * 2002-12-12 2009-03-31 Perkinelmer Las Inc. Induction device for generating a plasma
CN101495262B (zh) * 2005-03-11 2014-11-12 魄金莱默有限公司 等离子体及其使用方法
US7742167B2 (en) 2005-06-17 2010-06-22 Perkinelmer Health Sciences, Inc. Optical emission device with boost device
US8622735B2 (en) * 2005-06-17 2014-01-07 Perkinelmer Health Sciences, Inc. Boost devices and methods of using them
JP4489680B2 (ja) * 2005-10-03 2010-06-23 株式会社アドテック プラズマ テクノロジー マイクロ波プラズマ発生方法および装置
DE102006037995B4 (de) * 2006-08-14 2009-11-12 Bundesanstalt für Materialforschung und -Prüfung (BAM) Analyseverfahren für Festkörperproben und Vorrichtung zur Durchführung desselben
FR2928641B1 (fr) * 2008-03-14 2010-03-26 Centre Nat Rech Scient Procede de purification de silicium pour applications photovoltaiques
JP5965743B2 (ja) * 2012-06-27 2016-08-10 株式会社日立ハイテクサイエンス Ｉｃｐ装置及び分光分析装置並びに質量分析装置
AU2013290093B2 (en) 2012-07-13 2017-09-21 Peter Morrisroe Torches and methods of using them
CN104363689B (zh) * 2014-11-18 2017-02-08 聚光科技(杭州)股份有限公司 一种分析电源、矿粉分析装置及方法
CA2972418A1 (en) * 2014-12-29 2016-07-07 Fluidigm Canada Inc. Mass cytometry apparatus and methods

Citations (8)

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JPS60201239A (ja) * 1984-03-26 1985-10-11 Shimadzu Corp Ｉｃｐ発光分光分析用プラズマト−チ
EP0263031A2 (de) * 1986-10-03 1988-04-06 Commissariat A L'energie Atomique Induktiv gekoppelte Luft-Plasma-Vorrichtung für die spektrometrische Analyse von Elementen
US4766287A (en) * 1987-03-06 1988-08-23 The Perkin-Elmer Corporation Inductively coupled plasma torch with adjustable sample injector
JPS63210754A (ja) * 1987-02-27 1988-09-01 Shimadzu Corp Ｉｃｐ発光分析用試料導入装置
EP0296921A1 (de) * 1987-06-10 1988-12-28 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Mikrowellenplasmabrenner, einen solchen Brenner aufweisende Anlage und sie verwendendes Puderproduktionsverfahren
EP0358212A2 (de) * 1988-09-09 1990-03-14 Matheson Gas Products, Inc. Einführsystem für reaktive Gasproben in einen Plasmabrenner mit induktiv angekoppeltem Plasma
EP0397468A2 (de) * 1989-05-09 1990-11-14 Varian Associates, Inc. Spektroskopischer Plasmabrenner für Mikrowellenplasma
JPH05180772A (ja) * 1991-12-27 1993-07-23 Nkk Corp レーザー気化／誘導結合プラズマ分析方法及びプラズマ トーチ

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US4482246A (en) * 1982-09-20 1984-11-13 Meyer Gerhard A Inductively coupled plasma discharge in flowing non-argon gas at atmospheric pressure for spectrochemical analysis
JPS59182345A (ja) 1983-03-31 1984-10-17 Shimadzu Corp 液体クロマトグラフ発光分析装置
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
GB8917570D0 (en) * 1989-08-01 1989-09-13 Vg Instr Group Plasma source mass spectrometry
US5233156A (en) * 1991-08-28 1993-08-03 Cetac Technologies Inc. High solids content sample torches and method of use
US5908566A (en) * 1997-09-17 1999-06-01 The United States Of America As Represented By The Secretary Of The Navy Modified plasma torch design for introducing sample air into inductively coupled plasma

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60201239A (ja) * 1984-03-26 1985-10-11 Shimadzu Corp Ｉｃｐ発光分光分析用プラズマト−チ
EP0263031A2 (de) * 1986-10-03 1988-04-06 Commissariat A L'energie Atomique Induktiv gekoppelte Luft-Plasma-Vorrichtung für die spektrometrische Analyse von Elementen
JPS63210754A (ja) * 1987-02-27 1988-09-01 Shimadzu Corp Ｉｃｐ発光分析用試料導入装置
US4766287A (en) * 1987-03-06 1988-08-23 The Perkin-Elmer Corporation Inductively coupled plasma torch with adjustable sample injector
EP0296921A1 (de) * 1987-06-10 1988-12-28 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Mikrowellenplasmabrenner, einen solchen Brenner aufweisende Anlage und sie verwendendes Puderproduktionsverfahren
EP0358212A2 (de) * 1988-09-09 1990-03-14 Matheson Gas Products, Inc. Einführsystem für reaktive Gasproben in einen Plasmabrenner mit induktiv angekoppeltem Plasma
EP0397468A2 (de) * 1989-05-09 1990-11-14 Varian Associates, Inc. Spektroskopischer Plasmabrenner für Mikrowellenplasma
JPH05180772A (ja) * 1991-12-27 1993-07-23 Nkk Corp レーザー気化／誘導結合プラズマ分析方法及びプラズマ トーチ

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PATENT ABSTRACTS OF JAPAN vol. 013, no. 001 (P - 808) 6 January 1989 (1989-01-06) *
TRASSY ET AL.: "Dosage d'éléments métalliques dans le gaz. Etude d'une méthode directe.", JOURNAL OF HIGH TEMPERATURE CHEMICAL PROCESSES., no. 2, December 1993 (1993-12-01), pages 439 - 447, XP002076765 *

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Publication number Publication date
US6236012B1 (en) 2001-05-22
SG71892A1 (en) 2000-04-18
TW412636B (en) 2000-11-21
JPH11248632A (ja) 1999-09-17
CN1235274A (zh) 1999-11-17
KR19990063580A (ko) 1999-07-26

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