WO1991016723A1 - Appareil de production de radicaux gazeux - Google Patents

Appareil de production de radicaux gazeux Download PDF

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Publication number
WO1991016723A1
WO1991016723A1 PCT/GB1991/000556 GB9100556W WO9116723A1 WO 1991016723 A1 WO1991016723 A1 WO 1991016723A1 GB 9100556 W GB9100556 W GB 9100556W WO 9116723 A1 WO9116723 A1 WO 9116723A1
Authority
WO
WIPO (PCT)
Prior art keywords
discharge
discharge region
constriction
discharge tube
magnetic field
Prior art date
Application number
PCT/GB1991/000556
Other languages
English (en)
Inventor
Nigel Gordon Chew
Richard George Humphreys
Julian Simon Satchell
Original Assignee
The Secretary Of State For Defence In Her Britannic Majesty's Government Of The United Kingdom Of Great Britain And Northern Ireland
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 The Secretary Of State For Defence In Her Britannic Majesty's Government Of The United Kingdom Of Great Britain And Northern Ireland filed Critical The Secretary Of State For Defence In Her Britannic Majesty's Government Of The United Kingdom Of Great Britain And Northern Ireland
Priority to JP91506986A priority Critical patent/JPH05506328A/ja
Publication of WO1991016723A1 publication Critical patent/WO1991016723A1/fr
Priority to GB9221198A priority patent/GB2261986B/en

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
    • H01J37/32357—Generation remote from the workpiece, e.g. down-stream
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
    • C23C16/452—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by activating reactive gas streams before their introduction into the reaction chamber, e.g. by ionisation or addition of reactive species
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J27/00—Ion beam tubes
    • H01J27/02—Ion sources; Ion guns
    • H01J27/16—Ion sources; Ion guns using high-frequency excitation, e.g. microwave excitation
    • H01J27/18—Ion sources; Ion guns using high-frequency excitation, e.g. microwave excitation with an applied axial magnetic field
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/04—Arrangements of electrodes and associated parts for generating or controlling the discharge, e.g. electron-optical arrangement, ion-optical arrangement
    • H01J37/08—Ion sources; Ion guns
    • 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
    • H05H1/46—Generating plasma using applied electromagnetic fields, e.g. high frequency or microwave energy

Definitions

  • This invention relates to apparatus for the production of gaseous radicals.
  • Radicals are defined as atoms or molecules which possess an odd number of electrons. They are often short lived and are highly reactive, often combining with other radicals or molecules.
  • Gaseous radicals are often required for process such as etching, cleaning and layer growth of material in a chamber.
  • Gaseous radicals used in such processes include oxygen, nitrogen and hydrogen.
  • ECR electron cyclotron resonance
  • ECR ion source extremely expensive compared to a microwave cavity discharge radical source.
  • the kinetic energy of the ions produced has to be monitored and kept low, in order to avoid sputtering of the epitaxially grown material.
  • material growth using ions as a source of activated (ie not molecular) oxygen is not as effective as when radicals are used as a source of activated oxygen (Missert et al supra).
  • ECR ion sources do produce some radicals, the yield is small. More recently miniaturised ECR ion sources do produce some radicals, the yield is small.
  • ECR ion sources More recently miniaturised ECR ion sources have become available, (eg Wavemat Inc), 44780 Helm Street, Neighborhood, M148170, USA and Applied Science and Technology Inc, 35 Cabot Road, Woburn, MA 01801, USA). These sets of apparatus are easier to use than conventional ECR ion sources because the delivery of microwaves is by co-axial cable. The apparatus is much smaller due to the reduction in size of all the components, and thus the purchase and running costs are greatly reduced. However, these sets of apparatus still retain the disadvantages that the kinetic energy of the ions must be kept low and that, inevitably, it is mainly ions which are produced to the virtual exclusion of radicals.
  • US4683838 which generates a microwave induced plasma, which is confined by electromagnets
  • EP 0328076 The latter apparatus directs gas from a delivery tube into a large diameter microwave cavity having a microwave choke giving a high percentage of gas throughput.
  • apparatus for the production of gaseous radicals comprises:
  • a discharge tube having in serial order an inlet, a discharge region, a constriction which significantly restricts gaseous flow from the discharge region and an outlet.
  • the invention enables gas, suitable for producing radicals, to enter the discharge tube and flow through to the discharge region.
  • gas On flowing through the discharge region the gas encounters the co-operating effects of the coupled microwaves (as a discharge) and magnetic field, resulting in the production of gaseous radicals.
  • the constriction in the discharge tube inhibits free through flow of the gas to the outlet, thus increasing the likelihood of a given gaseous molecule in the discharge region breaking down to become radicals and increasing the yield of radicals flowing through the outlet.
  • the apparatus is normally operated with a gas pressure below atmospheric pressure providing radicals to low pressure systems.
  • the magnetic field must occur in the discharge region, although it may also occur elsewhere.
  • the strength of the magnetic field is preferably about sufficient to induce the ECR condition. This strength can be calculated from equation (1):
  • the constriction in the discharge tube is arranged to significantly restrict gaseous flow from the discharge region in order to lengthen residence time of through-flowing gas within the discharge region, and therefore presence of a constriction lowers gas conductance.
  • Gas conductance is defined as volume flow/pressure difference.
  • the constriction produces a ratio of gaseous pressure within the discharge region to gaseous pressure just downstream of the construction is 2:1 or greater. More preferably the ratio is 5:1 or greater. The ratio is greatly dependent upon such characteristics length of discharge tube downstream of the constriction and capacity of vacuum pumping facilities associated with any apparatus retrofitted to the apparatus for production of gaseous radicals. The closer the retrofitted apparatus occurs downstream of the constriction, then the higher the ratio becomes.
  • the preferred shape of the magnetic field within the discharge region is that of a magnetic-bottle, which may be seen in figure 4. This shape of magnetic field is preferred due to it producing a higher yield of radicals than other magnetic field shapes.
  • One other typical magnetic field shape is that such as produced by annular permanent magnets, and may be seen in figure 5.
  • a preferred embodiment of this invention contains a metal yoke. This yoke is used in such a way as to provide both a mechanical support for the apparatus and a convenient path for the completion of the magnetic field circuit between magnets.
  • This jacket can be used to help protect the discharge tube from breakage and to minimise or prevent microwave radiation leakage.
  • the discharge tube is made of a material with a low recombination coefficient for the radical to be produced.
  • Typical materials would be silica or pyrex for oxygen and hydrogen radicals, or pyrolitic boron nitride for nitrogen radicals.
  • the discharge tube has to be able to withstand relatively high temperature (typically up to about 500°C), and thus pyrex tubing may need to be cooled.
  • the discharge tube material is preferably transparent to microwaves. Thin coatings of passivating materials on the inner surface of the discharge tube, eg B 2 0 3 or P 0 5 can help to improve the radical yield. These coatings allow the discharge tube to be characterised by a lower recombination coefficient than would be achieved otherwise. Suitable passivating materials generally have low melting points, and thus can usually only be used as thin coatings.
  • the inner diameter of the discharge tube downstream of the constriction is of the order of tens of millimeters, with actual sizes very dependent upon retrofit conditions.
  • the region of the discharge tube upstream of the constriction and where radicals are produced has a typical maximum inner diameter of about 30 mm for microwave frequencies of about 2.54 GHz. Smaller diameters are, however, preferable in order to minimize the size of the discharge region, although there is a diameter below which a decrease in discharge tube diameter leads to higher recombination.
  • the preferred means of coupling microwaves to the discharge cavity is by the use of a microwave cavity, with the preferred geometry of microwave cavity being one which will accommodate the discharge tube in such a way that the electric field (E) is perpendicular to magnetic field (B).
  • this cable preferably has low loss at microwave frequencies.
  • the frequency of microwaves delivered to the coupling means is preferably one of the "spot" frequencies reserved for industrial use, eg. 2.45 GHz. although frequencies of between 900 MHz and 3 GHz are conveniently suitable. Where higher frequencies are used, then high magnetic fields are needed, and delivery of microwaves by coaxial cable becomes significantly less efficient.
  • the power of the microwaves is typically between 20 and 350 Watts. However, care must be taken when using high power levels not to induce excessive sputtering of the discharge tube walls.
  • the size of constriction in comparison with diameter of the discharge tube is a compromise between retaining the molecules within the discharge region for a sufficient length of time to dissociation, and removing the created radicals from the discharge region quickly enough to minimise recombination.
  • the dissociation and recombination characteristics of a gaseous molecule are a function of many circumstances eg. shape and size of coupling means, shape of the magnetic field and the power of the delivered microwaves.
  • the flow constriction is preferably a reduction of aperture to the equivalent of between 1 and 10mm diameter.
  • the aperture may be one, or many holes in the constriction.
  • Figure 1 is a cross-section view of apparatus for producing gaseous radicals.
  • Figure 2 is a cross-sectional view of figure 1 taken along the line x-x.
  • Figure 3 is a graph of oxygen radical yield against oxygen flow
  • Figure 4 is a schematic representation of a magnetic bottle - magnetic field shape.
  • Figure 5 is a schematic representation of magnetic field shape induced by the use of annular permanent magnets.
  • Gaseous radical producing source 1 may be seen in figure i.
  • a flow of oxygen passes through tube 2, in which there is a contriction 3.
  • Microwaves are coupled to a microwave cavity 4, formed within a casing 5, causing a discharge region 6.
  • Oxygen flows through the tube 2 into the discharge region 6, whereupon oxygen radicals are produced by the co- operating effects of the coupled microwaves and a magnetic field produced by annular magnets 7.
  • Free through-flow of the oxygen is inhibited by the constriction 3, and so there is an increase in the likelihood of an oxygen molecule within the discharge region 6 breaking down to produce oxygen radicals.
  • a metal yoke 8 provides mechanical support for the source 1, and also a convenient path for the completion of the magnetic field circuit between magnets.
  • Molecular oxygen (of purity 99.999Z) is provided by a gas delivery system 9, which has a flow control valve 10 and a monitoring pressure gauge 11.
  • the system 9 may optionally have a window 12, in order to provide a view down the length of the tube 2.
  • the gas delivery system 9 is attached to the source 1 by bolting a flange 13 and a clamping block 14 to cylinder 15. Where the source is used to produce a flow of radicals into a low pressure system 16, ten collett 17 and stops 18 prevent suction of the tube 2 downstream.
  • 0-rings 19 and 20 are used within cylinder 14 and against cylinder 21 respectively when low pressure sealing is required.
  • the yoke 8 provides support for a protective jacket 22.
  • the jacket has arms 23 which locate and support the annular magnets 7. Additionally the jacket 22 minimises or prevents leakage of microwave radiation.
  • a bolt 24 extends through the jacket 22 and the casing 5 and into the microwave cavity 4, and is used to adjust the microwave characteristics of the microwave cavity.
  • FIG. 2 gives a cross-section view through the axis marked x - x in figure 1.
  • Microwaves are generated and sent along coaxial cable 30.
  • the microwaves are delivered to a microwave coupling 31 via connecter 32.
  • Tuning of the microwaves in cavity 11 is achieved by use of screws 33 and 34.
  • Screw 33 can be secured by locking screw 34.
  • microwaves are generated at 2.54 GHz.
  • the power of the applied microwaves during operation can vary between 20 and 350 Watts, although typical running powers are about 100 Watts.
  • the tube 2 is made of silica, with the portion containing discharge region 6 of the tube having an inner diameter of 20mm.
  • the constriction 3 has an aperture diameter of 3mm, whilst downstream of the constriction the tube has an inner diameter of 22mm.
  • the stoppers 18 are bulges blown onto the tube at the time of manufacture.
  • the constriction 3 is made of silica. It may be an integral part of the tube or be an end to one part of the discharge tube which is then attached to the other part by a "push-fit" connection.
  • jacket 22 may also house cooling, such as possibly flushing water through carrier pipes, in the volume between its jacket 22 and casing 5.
  • Microwave cavities and associated microwave couplings 31 are commercially available, with Evanson type such as available from Electromedical Supplies (Greenham) Ltd, Wantage, Oxfordshire 0X12 7AD as catalogue number 216L being an example of a suitable means of coupling.
  • the magnets 7 are positioned by means of the arms of the jacket. These magnets are ferrite, and produce a field of 0.0875 Tesla within the discharge region 6.
  • the yoke 8 is made of iron.
  • Oxygen flows of up to about 100 seem can be used within the apparatus 20, although typical operating flows are 5 to 15 seem.
  • the yields of oxygen radicals increases with increasing flow.
  • the normalized percentage yield of oxygen radicals achieved with source 1 is between 5 " . and 1QZ . These yields are a measurement of yield occurring at a processing position within systems downstream of the source.
  • the preferred type of magnetic field shape within the discharge region is seen in figure 4.
  • the magnetic bottle shape 40 is outlined as a dotted line. This type of shape is difficult to achieve with permanent magnets such as the ferrite magnets 7, but can be achieved with the use of electromagnetic coils.
  • Magnets 7 induce a magnetic field shape of type 50, such a scan be seen in figure 5.
  • the exact field shape is dependent upon the positioning of magnets 7 with respect to the discharge region 6.
  • mass flow controller 10 is set to allow a constant flow of between 2 and 10 seem through the discharge tube 2 and into the system 16 operating at very low pressures.
  • Microwave power of about 100 Watts is turned on and delivered via coaxial cable 30 and microwave coupling 31 to microwave cavity 4. Initial runs of the source will require tuning of the microwave cavity by screws 24 and 33. Once this tuning has been carried out, then the cavity should need little, if any, adjustment for subsequent useage.
  • Window 12 can be used to view as to whether a discharge is present in the tube 2. Should there be no discharge, then a Tesla coil can be applied to window 12. This produces high AC Voltage, induces ions in the discharge tube and initiates the discharge.
  • the oxygen encounters the discharge of microwaves whilst flowing through the discharge region.
  • the co-operating effects of the discharge and the magnetic field at, or near, the ECR condition lead to the production of oxygen radicals at low oxygen flow rates.
  • the yield of radicals produced within the discharge region at low oxygen flow rates is enhanced by the constriction 3.
  • the yield of radicals reaching a processing position in the downstream low pressure system can be monitored using the method outlined by R G Humphreys et al (to be published in Superconductor Science and Technology). The percentage yield is obtained from the measured radical flux, the known mass flow and the estimated system conductances. Using source 1 the percentage yield is between 5Z and 10Z, with actual yield dependent upon oxygen flow as seen in figure 3.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Electromagnetism (AREA)
  • Combustion & Propulsion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Plasma Technology (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

On décrit un appareil de production de radicaux gazeux, muni d'un tube de décharge, un champ magnétique suffisant pour le confinement des électrons à l'intérieur de la région de décharge, et un rétrécissement en aval de la région de décharge. L'utilisation d'un rétrécissement en aval de la région de décharge prolonge le temps de séjour dans la région de décharge, et donc augmente la probabilité de production de radicaux gazeux. Une réalisation préférée de l'invention comporte un champ magnétique suffisant pour provoquer la résonance cylcotronique d'électrons (ECR) et un rétrécissement donnant un rapport de 5:1 ou plus entre la pression gazeuse dans la région de décharge et la pression gazeuse juste en aval du rétrécissement. D'autres caractéristiques préférées de l'invention comprennent l'utilisation d'une culasse métallique, d'une enveloppe métallique entrourant les parties exposées de l'appareil, d'un tube de décharge à faible coefficient de recombinaison et de fréquences micro-ondes industrielles standard.
PCT/GB1991/000556 1990-04-25 1991-04-23 Appareil de production de radicaux gazeux WO1991016723A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP91506986A JPH05506328A (ja) 1990-04-25 1991-04-23 ガス状ラジカルの製造装置
GB9221198A GB2261986B (en) 1990-04-25 1992-10-08 Gaseous radical producing apparatus

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB909009319A GB9009319D0 (en) 1990-04-25 1990-04-25 Gaseous radical source
GB9009319.6 1990-04-25

Publications (1)

Publication Number Publication Date
WO1991016723A1 true WO1991016723A1 (fr) 1991-10-31

Family

ID=10674987

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/GB1991/000556 WO1991016723A1 (fr) 1990-04-25 1991-04-23 Appareil de production de radicaux gazeux

Country Status (4)

Country Link
EP (1) EP0526491A1 (fr)
JP (1) JPH05506328A (fr)
GB (2) GB9009319D0 (fr)
WO (1) WO1991016723A1 (fr)

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0127523A1 (fr) * 1983-05-20 1984-12-05 Commissariat A L'energie Atomique Source d'ions à résonance cyclotronique des électrons
EP0164715A2 (fr) * 1984-06-11 1985-12-18 Nippon Telegraph And Telephone Corporation Source d'ions à micro-ondes
US4611121A (en) * 1983-04-19 1986-09-09 Nihon Shinku Gijutsu Kabushiki Kaisha Magnet apparatus
US4683838A (en) * 1984-06-29 1987-08-04 Hitachi, Ltd. Plasma treatment system
US4703180A (en) * 1984-10-30 1987-10-27 Hitachi, Ltd. Microwave discharge type ion source for ion injection devices
US4739169A (en) * 1985-10-04 1988-04-19 Hitachi, Ltd. Ion source
US4788473A (en) * 1986-06-20 1988-11-29 Fujitsu Limited Plasma generating device with stepped waveguide transition
JPH01225041A (ja) * 1988-03-03 1989-09-07 Mitsubishi Electric Corp イオン源装置
DE3915477A1 (de) * 1988-05-11 1989-11-23 Hitachi Ltd Mikrowellen-plasmaherstellungsvorrichtung
EP0344969A1 (fr) * 1988-06-03 1989-12-06 Eaton Corporation Source d'ions à résonance cyclotronique électronique

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10225041A (ja) * 1997-02-05 1998-08-21 Toshiba Corp モータ

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4611121A (en) * 1983-04-19 1986-09-09 Nihon Shinku Gijutsu Kabushiki Kaisha Magnet apparatus
EP0127523A1 (fr) * 1983-05-20 1984-12-05 Commissariat A L'energie Atomique Source d'ions à résonance cyclotronique des électrons
EP0164715A2 (fr) * 1984-06-11 1985-12-18 Nippon Telegraph And Telephone Corporation Source d'ions à micro-ondes
US4683838A (en) * 1984-06-29 1987-08-04 Hitachi, Ltd. Plasma treatment system
US4703180A (en) * 1984-10-30 1987-10-27 Hitachi, Ltd. Microwave discharge type ion source for ion injection devices
US4739169A (en) * 1985-10-04 1988-04-19 Hitachi, Ltd. Ion source
US4788473A (en) * 1986-06-20 1988-11-29 Fujitsu Limited Plasma generating device with stepped waveguide transition
JPH01225041A (ja) * 1988-03-03 1989-09-07 Mitsubishi Electric Corp イオン源装置
DE3915477A1 (de) * 1988-05-11 1989-11-23 Hitachi Ltd Mikrowellen-plasmaherstellungsvorrichtung
EP0344969A1 (fr) * 1988-06-03 1989-12-06 Eaton Corporation Source d'ions à résonance cyclotronique électronique

Also Published As

Publication number Publication date
GB9009319D0 (en) 1990-06-20
EP0526491A1 (fr) 1993-02-10
JPH05506328A (ja) 1993-09-16
GB2261986A (en) 1993-06-02
GB9221198D0 (en) 1993-01-06
GB2261986B (en) 1994-08-24

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