WO2012099547A1 - Procédé de commande dynamique de la densité d'atomes neutres dans une chambre à vide de plasma, et dispositif de traitement de matières solides par ledit procédé - Google Patents
Procédé de commande dynamique de la densité d'atomes neutres dans une chambre à vide de plasma, et dispositif de traitement de matières solides par ledit procédé Download PDFInfo
- Publication number
- WO2012099547A1 WO2012099547A1 PCT/SI2012/000001 SI2012000001W WO2012099547A1 WO 2012099547 A1 WO2012099547 A1 WO 2012099547A1 SI 2012000001 W SI2012000001 W SI 2012000001W WO 2012099547 A1 WO2012099547 A1 WO 2012099547A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- density
- oxygen
- nitrogen
- atoms
- hydrogen atoms
- Prior art date
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Classifications
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- 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
- C23C16/52—Controlling or regulating the coating process
-
- 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
- C23C16/50—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 using electric discharges
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- 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
- H01J37/32422—Arrangement for selecting ions or species in the plasma
-
- 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
- H01J37/32917—Plasma diagnostics
- H01J37/32935—Monitoring and controlling tubes by information coming from the object and/or discharge
- H01J37/32972—Spectral analysis
-
- 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
- H01J37/32917—Plasma diagnostics
- H01J37/32935—Monitoring and controlling tubes by information coming from the object and/or discharge
- H01J37/32981—Gas analysis
-
- 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
- H01J37/32917—Plasma diagnostics
- H01J37/3299—Feedback systems
Definitions
- the subject of the invention is a method for a dynamic control of neutral atom density with an active element in a plasma vacuum chamber and a device for the processing of solid materials by using said method.
- the control system Based on measurements and recordings of density of neutral oxygen, nitrogen or hydrogen atoms the control system receives input data, on the basis of which it generates control signals for the adjustment or control of the position of an active element, with a high coefficient for a heterogeneous surface recombination of oxygen, nitrogen or hydrogen atoms with a suitable motor.
- the system detects the density of neutral oxygen, nitrogen or hydrogen atoms by various methods, like catalytic probe, optical emission spectroscopy, optical absorption spectroscopy and titration.
- Such control provides for a dynamic regulation of neutral atom density in the environment of the processed sample (hereinafter: workpiece) regardless of discharge parameters and for an active change in the density of neutral atoms in the presence or absence of the workpiece regardless of discharge parameters.
- Plasma processing of materials is characterised by extreme quality, stability and environmental safety.
- oxygen, nitrogen or hydrogen plasma is very often used, especially as an alternative to environmentally unfriendly wet chemical methods. It is used especially for plasma purification, activation of organic materials, selective etching of polymeric composites, cold ashing of biological samples, in medicinal applications for the sterilisation of sensitive materials and for the synthesis of nanomaterials.
- Plasma is partly ionised gas. Fundamental plasma parameters are: electron temperature or electron energy distribution function, density of neutral atoms, density of neutral molecules in excited states with a stress on metastable states, and density of charged heavy particles or ions or positively and negatively charged molecules and atoms.
- Thermally stable plasmas are known, in which a sufficient level of ionisation is reached by the heating of gas.
- concentrations of electrons, ions, neutral atoms and molecules and the kinetic energy of the thermal movement of particles are uniformly dependent on temperature.
- a problem is the needed temperature, as the gas needs to be heated above 10 4 K. Therefore laboratory created thermally unstable plasmas are used, where ionisation of atoms or molecules is achieved inter alia by a discharge in the gas.
- Different types of discharge are known, like smouldering discharge, hot cathode direct current discharge, high-frequency discharge - radiofrequency or RF and microwave or MV or combined.
- a discharge with a strong external electric field causes an accelerated movement of free electrons in the gas, which are always present in the gas in small densities, up to the energy suitable for the ionisation of atoms or molecules.
- the external electric field can be direct or alternating. What is important is that the electrons are accelerated up to an energy sufficient enough to allow ionisation. Energy transfer of a high-frequency electric field is much more efficient for light electrons than heavy ions, therefore electron temperature or thermal energy of electrons is much higher than the ion temperature in the plasmas created by high-frequency discharge.
- the neutral atoms in poorly ionised plasma have the most important influence on physical and chemical reactions on the surface of a processed material. Ions have higher potential energy than neutral atoms and are therefore more chemically active. If we wanted to have a considerable share of ionised atoms, we would need thermally stable or "hot" plasma in order for the ionisation to reach a sufficient level. On the other hand, the "cold" or thermally unstable plasmas contain a considerably higher share of neutral atoms, which are normally more stable than ions.
- the density of oxygen atoms in a plasma system with a workpiece depends on the property of the sample, which is treated, i. e. of discharge parameters. These parameters are power, frequency and phase of a generator, vacuum level, gas flow pressure, reaction chamber shape, etc.
- the key problem is precise knowledge and maintenance of neutral atom density in the environment of the workpiece regardless of discharge parameters, as it often represents a changing drain of particles and active change in the density of neutral atoms in the presence or absence of a workpiece regardless of discharge parameters.
- Thermally unstable plasma is used in various ways both for academic and industrial purposes.
- a device for generating plasma with adequate density of neutral atoms is described in patent SI21903A.
- Laboratory plasma reactors are used in selective plasma etching of polymeric composite materials, especially of semi-conducting elements, for coating of materials with a CVD (Chemical Vapour Deposition) method, for the cleaning of surfaces and the purpose of plasma in medicinal applications is important in the sterilisation of sensitive materials.
- Plasma is also present in the most modern technologies, like the synthesis of nanomaterials.
- Some of the enumerated processing methods use neutral atoms, so knowledge and active control of the density of neutral atoms is of extreme importance, since it improves the yield and quality of processing methods.
- Two- or three- electrode systems are very often used, wherein at least one electrode is used for direct bias on a workpiece and the remaining ones are used for plasma excitation.
- Each of the electrodes is connected to its source via respective corresponding member and via feedback to the control system, which controls either the power or voltage supplied on electrodes or a frequency of an RF power source through control signals.
- Such methods are especially used to control electron temperature, density of ions or uniform plasma density.
- the invention comprises a method for a dynamic control of density of neutral atoms in a plasma vacuum chamber and a device for the processing of solid materials by using this method.
- Control of atoms is carried out by a special active element.
- the method is based on a control system with a feedback for a motorised control over the position of the active element, with a huge coefficient for heterogeneous surface recombination of atoms of oxygen, nitrogen or hydrogen, in a main plasma tube.
- Control over this active element provides for a dynamic regulation of density of neutral atoms in the environment of the workpiece regardless of discharge parameters and for a change in density of neutral atoms in the presence or absence of a workpiece regardless of discharge parameters.
- Fig. 1 schematic view of a vacuum part of the plasma system
- Fig. 2 schematic view of an electric or excitation part of the plasma system
- FIG. 3 schematic view of a control system with a feedback
- FIG. 4 schematic view of an embodiment in poorly ionised oxygen plasma with an active element with a huge coefficient for heterogeneous surface recombination of oxygen, nitrogen or hydrogen atoms
- Fig. 6 measurements of oxygen plasma dissociation at a pressure of 90 Pa, various excitation strengths and various positions of the active element with a huge coefficient for heterogeneous surface recombination of oxygen, nitrogen or hydrogen atoms.
- FIG. 1 A schematic view of a vacuum part of the plasma system is shown in Figure 1. It consists of a precise dosing valve 2 for gas flow from a gas bottle 1 , a discharge tube 4, a pressure gauge 3, an air flow valve 7, a vacuum pump 6 and its belonging valve 5.
- Figure 2 shows an electric or excitation part of the device, which consists of a high-frequency radio-frequency power generator 8 that is connected via coaxial cable 9 with a matching element 10.
- the matching element is connected with a radiofrequency coil 13 for exciting plasma via two rectifier elements 1 1 and 12, which measure input power into the discharge tube 4 and the power reflected from the antenna.
- the plasma excited by a transmission of electromagnetic waves via radiofrequency coil is called inductively coupled plasma.
- the matching element consists of two high-voltage, high-frequency, variable capacitors that serve to adjust the impedance of the system "antenna-plasma" to the impedance of the remaining circuit, which amounts to 50 ⁇ .
- FIG. 3 is a schematic view of a plasma system with an added control system.
- the entire system comprises the main discharge tube 4 and one or two side tubes 14 and 15.
- the electric part is represented by a radiofrequency coil 13, which is excited by a high-frequency RF power generator 8.
- the latter is connected with the matching element 10 via coaxial cable 9.
- a control system 16 gathers data at inputs and on the basis of input signals 17 and 18, through feedback, dynamically adapts an output control signal 19, with which it controls an active element 20 via motorised interface 21 with a huge coefficient for heterogeneous surface recombination of oxygen, nitrogen and hydrogen atoms.
- the data are gathered either by a catalytic probe 22 or an optical fibre 23 connected with a spectrometer 24. Any combination of said methods for data gathering is possible.
- the described control method is used to directly control the density of neutral atoms in the presence or absence of a workpiece, which represents a drain of particles, regardless of discharge parameters.
- an active element 20 with a huge coefficient for heterogeneous surface recombination of oxygen, nitrogen or hydrogen atoms was used and its position was changed manually.
- the active element may be any element with a huge coefficient for heterogeneous surface recombination of oxygen, nitrogen or hydrogen atoms, preferably a beam consisting of a multitude of arranged wires with a nanostructured surface.
- the wires are typically arranged longitudinally with respect to the orientation of the active element.
- the nanostructured surface typically consists of nanowires that are oriented perpendicularly to the geometrical surface of wires. Such configuration provides for high probability of heterogeneous surface recombination of oxygen, nitrogen or hydrogen atoms under simultaneous minimum resistance for gas flow in its environment.
- the length of the active element with a huge coefficient for heterogeneous surface recombination of oxygen, nitrogen or hydrogen atoms was 40 cm, of that not more than 13 cm of the surface were exposed to plasma.
- Oxygen plasma was used and the main discharge tube 4 of the plasma reactor was 80 cm long and had a diameter of 4 cm, whereas a side tube 14 was 10 cm long and had a diameter of 1.5 cm.
- Plasma was created with the radiofrequency coil 13 with six windings wound around the main tube along the length of 5.5 cm.
- the radiofrequency coil was connected with the high-frequency RF power generator 8 with a coaxial cable 9 via matching element 10.
- Measurements of density of neutral atoms and measurements of dissociations carried out by the described embodiment in oxygen plasma are shown in Figures 5 and 6.
- the measurements were performed at a pressure of 90 Pa with six different powers ranging between 0 and 600 W.
- the position of the active element with a huge coefficient for heterogeneous surface recombination of oxygen, nitrogen or hydrogen atoms was changed with respect to the position of the nickel optical catalytic probe and amounted between 4 cm right of the measuring probe tip and 7.5 cm left from the measuring probe tip.
- the method for a dynamic control of density of neutral atoms of oxygen, nitrogen or hydrogen in a plasma vacuum chamber of the invention is characterised in that the density of atoms in the vacuum chamber is controlled by the position of the movable active element with a huge coefficient for heterogeneous surface recombination of oxygen, nitrogen or hydrogen atoms.
- the movable element is connected with the control unit, which controls the position of the movable active element via density meter of oxygen, nitrogen or hydrogen atoms.
- the movable element may be motorised.
- the coefficient for heterogeneous surface recombination of the active element exceeds 0.001.
- the density meter of atoms is a catalytic probe or an optical spectrometer.
- the device for the processing of solid materials with neutral atoms of oxygen, nitrogen or hydrogen of the invention is characterised in that it comprises a vacuum chamber, a source of oxygen, nitrogen or hydrogen atoms, a density meter of oxygen, nitrogen or hydrogen atoms and a movable active element with a huge coefficient for heterogeneous surface recombination of oxygen, nitrogen or hydrogen atoms.
- the active element with a huge coefficient for heterogeneous surface recombination of oxygen, nitrogen or hydrogen atoms allows for a changing density of a flow of oxygen, nitrogen or hydrogen atoms between l x lO 18 and 1 x 10 25 m " V, preferably between l x l O 19 and S x lO ⁇ m ' 1 .
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Plasma Technology (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
L'invention a pour objet un procédé de commande dynamique de la densité d'atomes neutres ayant un élément actif dans une chambre à vide (4) de plasma, et un dispositif de traitement de matières solides par ledit procédé. Un système de commande reçoit des données d'entrée (17 et 18) résultant de mesures et d'enregistrements de la densité d'atomes neutres d'oxygène, d'azote ou d'hydrogène, sur la base desquelles il génère des signaux de commande pour ajuster ou commander la position de l'élément actif (20), à un coefficient de recombinaison de surface hétérogène élevé des atomes d'oxygène, d'azote ou d'hydrogène, avec un moteur approprié (21). Le système collecte les données de densité d'atomes neutres d'oxygène, d'azote ou d'hydrogène par différents procédés, par exemple sonde catalytique, spectroscopie d'émission optique (23 et 24) spectroscopie d'absorption optique et titration. Cette commande assure à la fois une commande dynamique de la densité d'atomes neutres dans l'environnement d'un échantillon à traiter, par exemple une pièce, indépendamment des paramètres de décharge, et une modification active de la densité d'atomes neutres en présence ou en absence de la pièce indépendamment des paramètres de décharge.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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SI201100023A SI23626A (sl) | 2011-01-19 | 2011-01-19 | Metoda za dinamično nadzorovanje gostote nevtralnih atomov v plazemski vakuumski komori in napravaza obdelavo trdih materialov s to metodo |
SIP-201100023 | 2011-01-19 |
Publications (1)
Publication Number | Publication Date |
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WO2012099547A1 true WO2012099547A1 (fr) | 2012-07-26 |
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PCT/SI2012/000001 WO2012099547A1 (fr) | 2011-01-19 | 2012-01-16 | Procédé de commande dynamique de la densité d'atomes neutres dans une chambre à vide de plasma, et dispositif de traitement de matières solides par ledit procédé |
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SI (1) | SI23626A (fr) |
WO (1) | WO2012099547A1 (fr) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20150332941A1 (en) * | 2012-10-09 | 2015-11-19 | Applied Materials, Inc. | Methods and apparatus for processing substrates using an ion shield |
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US20030155079A1 (en) | 1999-11-15 | 2003-08-21 | Andrew D. Bailey | Plasma processing system with dynamic gas distribution control |
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-
2011
- 2011-01-19 SI SI201100023A patent/SI23626A/sl not_active IP Right Cessation
-
2012
- 2012-01-16 WO PCT/SI2012/000001 patent/WO2012099547A1/fr active Application Filing
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US5266364A (en) | 1990-08-20 | 1993-11-30 | Hitachi, Ltd. | Method and apparatus for controlling plasma processing |
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CVELBAR U ET AL: "Behaviour of oxygen atoms near the surface of nanostructured Nb2O5", JOURNAL OF PHYSICS D: APPLIED PHYSICS, vol. 40, no. 8, 4 April 2007 (2007-04-04), IOP PUBLISHING, BRISTOL [GB], pages 2300 - 2303, XP020112359, ISSN: 0022-3727, DOI: 10.1088/0022-3727/40/8/S09 * |
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POBERAJ I ET AL: "Comparison of fiber optics and standard nickel catalytic probes for determination of neutral oxygen atoms concentration", JOURNAL OF VACUUM SCIENCE AND TECHNOLOGY: PART A, vol. 20, no. 1, 1 January 2002 (2002-01-01), AVS/AIP, MELVILLE, NY [US], pages 189 - 193, XP012005922, ISSN: 0734-2101, DOI: 10.1116/1.1427893 * |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20150332941A1 (en) * | 2012-10-09 | 2015-11-19 | Applied Materials, Inc. | Methods and apparatus for processing substrates using an ion shield |
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Publication number | Publication date |
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SI23626A (sl) | 2012-07-31 |
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