EP2707896A1 - Traitement thermique par injection d'un gaz caloporteur. - Google Patents

Traitement thermique par injection d'un gaz caloporteur.

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Publication number
EP2707896A1
EP2707896A1 EP12725101.5A EP12725101A EP2707896A1 EP 2707896 A1 EP2707896 A1 EP 2707896A1 EP 12725101 A EP12725101 A EP 12725101A EP 2707896 A1 EP2707896 A1 EP 2707896A1
Authority
EP
European Patent Office
Prior art keywords
gas
precursor
temperature
injection
cooling
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Withdrawn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
EP12725101.5A
Other languages
German (de)
English (en)
French (fr)
Inventor
Grégory SAVIDAND
Daniel Lincot
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.)
Electricite de France SA
Centre National de la Recherche Scientifique CNRS
Original Assignee
Electricite de France SA
Centre National de la Recherche Scientifique CNRS
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 Electricite de France SA, Centre National de la Recherche Scientifique CNRS filed Critical Electricite de France SA
Publication of EP2707896A1 publication Critical patent/EP2707896A1/fr
Withdrawn legal-status Critical Current

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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/324Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/18Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
    • H01L31/186Particular post-treatment for the devices, e.g. annealing, impurity gettering, short-circuit elimination, recrystallisation
    • H01L31/1864Annealing
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02518Deposited layers
    • H01L21/02521Materials
    • H01L21/02568Chalcogenide semiconducting materials not being oxides, e.g. ternary compounds
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02612Formation types
    • H01L21/02614Transformation of metal, e.g. oxidation, nitridation
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02656Special treatments
    • H01L21/02664Aftertreatments
    • H01L21/02667Crystallisation or recrystallisation of non-monocrystalline semiconductor materials, e.g. regrowth
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/34Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies not provided for in groups H01L21/0405, H01L21/0445, H01L21/06, H01L21/16 and H01L21/18 with or without impurities, e.g. doping materials
    • H01L21/42Bombardment with radiation
    • H01L21/423Bombardment with radiation with high-energy radiation
    • H01L21/428Bombardment with radiation with high-energy radiation using electromagnetic radiation, e.g. laser radiation
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005Apparatus not specifically provided for elsewhere
    • H01L21/67011Apparatus for manufacture or treatment
    • H01L21/67098Apparatus for thermal treatment
    • H01L21/67109Apparatus for thermal treatment mainly by convection
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005Apparatus not specifically provided for elsewhere
    • H01L21/67242Apparatus for monitoring, sorting or marking
    • H01L21/67248Temperature monitoring
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/677Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for conveying, e.g. between different workstations
    • H01L21/67739Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for conveying, e.g. between different workstations into and out of processing chamber
    • H01L21/6776Continuous loading and unloading into and out of a processing chamber, e.g. transporting belts within processing chambers
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/0248Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
    • H01L31/0256Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
    • H01L31/0264Inorganic materials
    • H01L31/032Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/0248Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
    • H01L31/0256Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
    • H01L31/0264Inorganic materials
    • H01L31/032Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
    • H01L31/0322Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312 comprising only AIBIIICVI chalcopyrite compounds, e.g. Cu In Se2, Cu Ga Se2, Cu In Ga Se2
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/0001Technical content checked by a classifier
    • H01L2924/0002Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy
    • Y02E10/541CuInSe2 material PV cells

Definitions

  • the invention relates to the field of heat treatment of materials including thin layers, and more particularly so-called “rapid thermal treatments” (translation of the term “Rapid Thermal Process”). These are typically processes capable of applying increases of at least 700 ° C in a time of the order of a minute.
  • This technique is particularly advantageous for annealing semiconductors in thin layers deposited on substrates.
  • the inertia of the furnace in which the heat treatment is applied is a permanent problem in this type of technique. It is indeed difficult to control the rise in temperature (and also the cooling, in particular but not exclusively for quenching effects).
  • temperature sensors are usually positioned near the heating elements and near the substrate to know the temperature, as accurately as possible. Industrial adaptation of this type of process for large substrates then requires significant costs.
  • the wavelengths used are short (0.76 to 2 ⁇ ) or medium (2 to 4 ⁇ ) infrared; the temperature of the substrate (and of the layer (s) that the substrate carries) is controlled by the power emitted by the infrared emitters and can follow very fast climbs such as reaching 700 ° C. in less than one hour. minute;
  • the substrate passes from a cold chamber to a hot chamber possibly via a buffer enclosure at intermediate temperature; the speed of travel of the substrate allows the control of the temperature ramps;
  • the substrate is deposited on a magnetic substrate holder and a magnetic field is applied by creating an induced current in the substrate holder, which heated by the Joule effect by heating the substrate.
  • the thermal behavior of the reaction chambers is dependent on the optical characteristics of the substrate
  • the second type of process has the disadvantage of using a hot chamber remaining at a fixed temperature.
  • the enclosure must then have a dimension adapted to the surface of the substrate, which increases the energy consumption and hence the industrial application costs.
  • the substrate is often made of glass and then heats much more rapidly on its lower face (in contact with the substrate holder) than on its upper face, which causes thermal gradients in the glass thickness. The thermal stresses caused often lead to glass breakage.
  • the temperature measurement is always indirect (on the substrate holder, on a wall of the oven, or other).
  • the present invention improves the situation.
  • the thermal treatment by projection of a hot gas makes it possible to set the temperature of the substrate and the thin layer that it carries.
  • a gas with a high heat capacity is preferably chosen.
  • argon is a good candidate, already as a neutral gas (thus not likely to react undesirably with the thin layer), but also for its heat capacities.
  • the gas thus rises very quickly in temperature and then brings the heat directly to the surface of the substrate. It is no longer necessary to position a temperature sensor near the substrate.
  • the gas projection can be continuous. Control of the temperature in heating (and also in cooling) is advantageously achieved by techniques with very low cost of implementation.
  • a tool for managing the temperature ramps in rise and cooling then makes it possible to couple the controls of both the heating and the cooling of the substrate.
  • the projection of the gas on the surface of the substrate makes it possible to control the actual temperature applied.
  • this parameter In addition to the temperature of the heat transfer gas, it also controls the flow of the gas injection on the precursor. As will be seen with reference to FIGS. 4 (a) and 4 (b), this parameter has an influence on the surface temperature of the precursor receiving the gas injection.
  • the heat transfer gas may comprise at least one of hydrogen, argon and nitrogen, these gases being advantageous because of their thermal capacities for the transport of heat.
  • the gas preheating comprises, in a concrete embodiment described below, a rise in temperature of the gas of the order of 1000 ° C.
  • the injection of gas produces a rise in temperature at the surface of the precursor receiving the gas, of the order of a few tens of degrees per second, for an injected gas flow rate of the order of a few liters per minute. (for example between 3 and 6 liters per minute).
  • the temperature rise of the precursor can reach at least 400 ° C on the surface in a few tens of seconds, with a distance between the precursor and a gas injection outlet on the precursor less than five centimeters.
  • the method may further comprise an injection of cold gas, for example after annealing to produce a quenching effect.
  • the surface of the precursor receiving the cold gas can be cooled to a speed of the order of 100 ° C in a few seconds.
  • Such an embodiment described above is advantageous, in particular but not exclusively, for a precursor comprising atomic species of columns I and III, and optionally VI, of the periodic table of the elements, for obtaining, after heat treatment, the a thin layer on a substrate of an I-III-VI 2 alloy with photovoltaic properties. It can also be considered for elements of columns I, II, IV, VI (preferably Cu, Zn, Sn, S or Se) for the formation of an alloy I 2 -II-IV-VL- Elements of the column V, as phosphorus can also be considered, especially for the formation of II-IV-V alloys (eg ZnSnP).
  • the present invention also aims at a heat treatment installation for the implementation of the method above, and comprising:
  • a gas routing circuit comprising heating means and / or gas cooling means
  • the injector may simply be in the form of a tubing (bearing the reference 5 in FIG. 8 (a) or FIG. 8 (b)) of a conduit (3) gas injection on the precursor.
  • the heating means comprise a thermal resistance capable of releasing heat by applying a current flowing in the resistor.
  • the heating means may further comprise a control circuit of the intensity of this current to adjust the heating temperature of the resistor and hence the temperature of the gas to be injected.
  • the cooling means may comprise a Pelletier effect module and / or a refrigerant circuit, and also a control circuit for adjusting the cooling temperature of the gas.
  • At least one stop valve / gas flow (for a binary operation of the injection as will be seen in the detailed description below). This valve can also be used to adjust the flow of injected gas.
  • the installation advantageously comprises relative displacement means of the injector relative to the precursor, at least in height (in vertical configuration or not) to adjust a distance between the injector and the precursor (and, from there, the temperature to the surface of the precursor as described hereinafter with reference to FIGS. 4 (a) and 4 (b)).
  • the installation may also include means for moving the precursor, relative to the injector, on a treadmill in a direction perpendicular to an injection axis of the gas from the injector.
  • An example of this type of installation for the implementation of a so-called "batch" type process will be described later with reference to FIG. 8 (a). This type of process is particularly advantageous for precursors deposited on non-flexible substrates, for example made of glass.
  • the installation can be designed to operate according to a so-called "roll-to-roll” method.
  • the installation comprises two motorized rollers on which the substrate is wound, and, by action of the rollers, the substrate is wound on a roll and unrolled from the other roll, creating a displacement of the precursor, relative to to the injector, in a direction perpendicular to an injection axis of the gas from the injector ( Figure 8 (b) on which the aforementioned rollers have references R1, R2).
  • FIG. 1 diagrammatically represents an installation for implementing the invention
  • FIG. 2 illustrates in particular the annealed zone on a precursor, by the implementation of the method of the invention
  • FIG. 3 schematically illustrates a device used for thermal characterization
  • FIG. 5 illustrates a parallel combination of heating elements for controlling the rise and fall rates in temperature of the gas;
  • Fig. 6 illustrates a series combination of heating elements for controlling the rise and fall rates in temperature of the gas
  • FIG. 7 shows an example of a possible heat treatment ramp from an installation shown in FIG. 5 or FIG. 6;
  • FIGS. 8 (a) and 8 (b) show schematically an example of integration of the installation on an industrial line, respectively of the "batch” (a) or “roll to roll” (b) type.
  • the precursor in the form of a thin layer
  • the notation "I” designates the elements of column I (respectively III and VI) of the periodic table of elements, such as copper (respectively indium and / or gallium and / or or aluminum, and selenium and / or sulfur).
  • the precursor comprises elements I and III, and it is obtained in the form of an alloy I-III following a first annealing ("reducing annealing" defined below).
  • the element VI may also be present initially in the precursor layer and the method of the invention provides for the injection of a hot gas to anneal the precursor and obtain its crystallization according to the stoichiometry I-III-VI 2 .
  • precursor a deposit composed of one or more of the elements: Cu, In, Ga, Al but also possibly Se, S, Zn, Sn, O, on a substrate;
  • annealing reducer an annealing of the precursor with a gas comprising at least one of the elements: alcohol, amines, hydrogen (H 2 );
  • reactive annealing a crystallization reaction which consists in reacting with a reactive element the precursor which has or has not undergone preliminary reduction annealing;
  • x a distance between the substrate and a pipe of a gas injection pipe on the precursor
  • Tr the annealing temperature at the surface of the precursor.
  • a gas inlet stream 1 undergoes a temperature change, for example a temperature rise, in a thermal enclosure comprising a duct 3 enclosing a heating element 4 to which a power supply 2 is applied.
  • outlet 5 of the duct 3 the gas has a temperature T (0, D, To) which is a function of its flow D in the duct 3 and the temperature To of the heating element 4.
  • the reference 6 in FIG. here a precursor based on Cu, In, Ga, Zn, Sn, Al, Se, and / or S, undergoing a heat treatment (or “annealing” hereinafter) at a temperature Tr (x, D, T 0 ) .
  • This annealing temperature Tr again depends on the flow D and the temperature To of the heating element, but also on the distance x separating the precursor 6 from the outlet pipe 5 of the pipe 3.
  • a circuit 7 for recovering gases More particularly, the injected gases can be recovered, to be then reheated and reinjected onto the precursor so as to have a closed circuit, advantageous for cost reasons.
  • the advantage of annealing by hot gas propulsion is that of annealing only the surface A of a precursor on substrate B.
  • the propulsion of the gas directly affects the surface of precursor and allows local annealing (zone A).
  • the other part (part B) is heated differently (heated to a lesser extent and especially more slowly).
  • a first advantage of such a localized annealing at the surface of the precursor is to avoid breakage of the glass substrate.
  • the gas used is, in this example embodiment, argon at a pressure P of 1 bar at the inlet 1 of the installation and at ambient temperature (around 20 ° C.).
  • FIG. 3 shows the elements of a device for measuring the temperature of the gas at the outlet 5.
  • the temperature Tr is sought here to measure the temperature Tr as a function, in particular, of the distance x at the outlet 5 of the enclosure (given for example in cm by a measurement rule MES).
  • the temporal evolution of the temperature Tr, for different measured distances x, is given in FIG. 4 (a), in particular for a gas flow D (argon) of 3 liters per minute.
  • the same evolution is shown in FIG. 4 (b) but with a flow rate D of 6 liters per minute.
  • the instant "0" on the x-axis corresponds to the opening of the gas injection valve in the chamber 1.
  • a second advantage of the invention is that it is possible to very finely control the temperature Tr of the gas injected on the precursor, by a control of the gas flow D and the position x of the substrate relative to the exit 5.
  • FIGS. 5 and 6 show an installation using a combination of heating / cooling elements with low thermal inertia.
  • Figure 5 shows a parallel combination of heating and cooling elements.
  • the inlet gas 1 is directed via a three-way valve VI to two circuits (a hot circuit at set temperature Te and a cold circuit at set temperature Tf). If the gas passes through the hot circuit (having a heating resistor 14 controlled by a variable power supply 12), its temperature is controlled by a control circuit comprising for example a potentiometer setting for example a supply voltage 12. Then, the The gas follows its path through a three-way valve V2 and exits conduit 5 to supply heat to the surface of the precursor.
  • a control circuit comprising for example a potentiometer setting for example a supply voltage 12.
  • the gas cools and in particular, its cooling temperature is controlled by a circuit of control (comprising for example a potentiometer) fixing for example a supply voltage 22.
  • a circuit of control comprising for example a potentiometer
  • the cooling temperature Tf of the cooling element 24 is controlled by the voltage of the power supply 22 and it is the same for the heating element 14 with the supply 12.
  • FIG. 7 illustrates by way of example an advantageous temperature ramp for selenization, applied by combining the variation of flow rate D with the heating of the elements of FIG. 6 for a position of the precursor at a fixed distance x.
  • the temperature of the gas is raised from room temperature (e.g. 25 ° C) to 600 ° C in one minute.
  • the temperature of the heating element increases. It stabilizes to apply a bearing at 600 ° C for one minute.
  • the cooling element is switched on so that the gas cools here in one minute up to 400 ° C.
  • the supply voltages of the two heating and cooling elements are stabilized and the flow rate of the gas is fixed to ensure a step of one minute at 400 ° C.
  • the gas is cooled from 400 ° C to -10 ° C in 2 minutes to produce a quenching effect for example.
  • the heating element is stopped and the cooling element is active during this period.
  • one or more hot gas injection steps for producing a rise in temperature on the surface of the precursor receiving the gas, of the order of a few tens of degrees per second,
  • steps of maintaining substantially constant temperature of the precursor and one or more cold gas injection steps for producing a temperature cooling at the surface of the precursor receiving the gas, of the order of a few tens of degrees per second.
  • steps may be, for some, inverted to define successive periods of heating, holding temperature or cooling, as shown in Figure 7.
  • these stages of heating, temperature maintenance, or cooling are connected in a predetermined sequence defining a temporal profile of temperature variation applied to the surface of the precursor receiving the gas, such as the profile represented by way of example on the FIG. 7, for a chosen sequence of heat treatment of the precursor.
  • a temporal profile of temperature variation applied to the surface of the precursor receiving the gas such as the profile represented by way of example on the FIG. 7, for a chosen sequence of heat treatment of the precursor.
  • heating resistors in the form of a strip or wire
  • an alloy of iron, chromium, nickel and aluminum, capable of rising to 1400 ° C. may for example be used. They are commercially available (eg distributed by the Swedish company Kanthal®).
  • Peltier effect modules or a cold gas circuit passing through a coil, can be used.
  • Peltier effect modules are thermoelectric systems operating as follows: a potential difference applied to a module allows cooling up to 18 ° C below ambient temperature. To go lower in temperature, vapor compressor systems are also known which make it possible to attain values below 0 ° C. There are commercially available gas coolers, several of which are presented in particular on the website www.directindustrv.fr. By the implementation of the invention, it is possible to apply "ultra-fast" temperature ramps, namely of the order of 500 ° C. in less than half a minute on the surface of a sample by propulsion of hot gas, and without thermal inertia.
  • samples to be annealed are scrolled on a line according to a so-called "batch" method.
  • the samples 52 are arranged one behind the other on a moving carpet 51, the carpet thus bringing each precursor to be heat treated under the gas injection pipe 3 (arrow 54).
  • the carpet stops the time necessary to treat the precursor. When the treatment time is exceeded.
  • the carpet brings the next sample, in the direction of scrolling 53, and repeats the sequence.
  • Such a type of method is particularly suitable when the substrate is non-flexible, for example glass.
  • the substrate 6 is flexible (for example a metal strip or polymer (s)) and unwound between two rollers R1, R2, according to a method of the type says "Roll to Roll".
  • the substrate 6 carrying the precursor is unwound and the treatment is carried out directly on its surface (arrow 54).
  • the precursor proceeds progressively by the action of rolls R1, R2.
  • the part to be treated is placed under the injection pipe 3.
  • the flow is then stopped.
  • another part of the untreated precursor replaces the previous one by actuating the rolls R1, R2 and the process is repeated.
  • the implementation of the invention can be fully automated since a single solenoid valve at the inlet of the duct 3 (and / or upstream of the duct 3) allows to pass or not a hot gas (or cold).
  • a binary design of the operation of such solenoid valve (s) makes it possible to determine the running time of the precursor in exact connection with the time of its processing.
  • Ultra-fast heat treatment can then be applied to the surface of a substrate in a very wide temperature range (from -50 ° C to 1000 ° C), with fine control of temperature rise rates and cooling rates. (through the gas flow rate, its temperature and the position of the substrate).
  • the injection of the gas on the precursor can be carried out under atmospheric pressure conditions and thus, it is not necessary to provide the injection in a closed chamber under vacuum or at low pressure.
  • the injection can be done in the open air.

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EP12725101.5A 2011-05-10 2012-05-03 Traitement thermique par injection d'un gaz caloporteur. Withdrawn EP2707896A1 (fr)

Applications Claiming Priority (2)

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FR1154015A FR2975223B1 (fr) 2011-05-10 2011-05-10 Traitement thermique par injection d'un gaz caloporteur.
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FR3004466B1 (fr) 2013-04-10 2015-05-15 Electricite De France Procede et dispositif d'electro-depot en geometrie cylindrique
JP2017216397A (ja) * 2016-06-01 2017-12-07 株式会社アルバック アニール処理装置およびアニール処理方法
CN107222165A (zh) * 2017-07-06 2017-09-29 北京铂阳顶荣光伏科技有限公司 具有加热装置的路面发电系统

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4923396A (en) * 1984-11-08 1990-05-08 Mitsubishi Jukogyo Kabushiki Kaisha Method and apparatus for heating a strip of metallic material in a continuous annealing furnace
WO2002044430A1 (en) * 2000-11-30 2002-06-06 The Boc Group Plc Quenching method and apparatus
JP2010001560A (ja) * 2008-11-04 2010-01-07 Philtech Inc 膜形成方法および膜形成装置

Family Cites Families (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4638148A (en) * 1983-09-21 1987-01-20 Robertshaw Controls Company Control system and control device for controlling a heating unit and method of making the same
KR930000784B1 (ko) * 1988-03-21 1993-02-04 유니온 카바이드 코포레이션 다영역공정에서 흐름바이어스를 조절하는 방법 및 장치
US5361587A (en) * 1993-05-25 1994-11-08 Paul Georgeades Vapor-compression-cycle refrigeration system having a thermoelectric condenser
US5985691A (en) * 1997-05-16 1999-11-16 International Solar Electric Technology, Inc. Method of making compound semiconductor films and making related electronic devices
SE521206C2 (sv) * 2002-02-20 2003-10-14 Flow Holdings Sagl Förfarande för kylning av en ugnskammare för varmisostatisk pressning och en anordning härför
WO2004056461A2 (en) * 2002-12-17 2004-07-08 E.I. Du Pont De Nemours And Company Method of producing nanoparticles using a evaporation-condensation process with a reaction chamber plasma reactor system
US20070169810A1 (en) * 2004-02-19 2007-07-26 Nanosolar, Inc. High-throughput printing of semiconductor precursor layer by use of chalcogen-containing vapor
JP4652120B2 (ja) * 2004-05-21 2011-03-16 株式会社半導体エネルギー研究所 半導体装置の製造装置、およびパターン形成方法
US20070111367A1 (en) * 2005-10-19 2007-05-17 Basol Bulent M Method and apparatus for converting precursor layers into photovoltaic absorbers
JP2007269589A (ja) * 2006-03-31 2007-10-18 Nagaoka Univ Of Technology 硫化物薄膜の作製方法
US8066863B2 (en) * 2006-12-07 2011-11-29 Solopower, Inc. Electrodeposition technique and apparatus to form selenium containing layers
US8093493B2 (en) * 2007-04-30 2012-01-10 Solyndra Llc Volume compensation within a photovoltaic device
EP2232576A2 (en) * 2007-12-06 2010-09-29 Craig Leidholm Methods and devices for processing a precursor layer in a group via environment
US20090260670A1 (en) * 2008-04-18 2009-10-22 Xiao-Chang Charles Li Precursor ink for producing IB-IIIA-VIA semiconductors
DE102009011695A1 (de) * 2009-03-09 2010-09-16 Centrotherm Photovoltaics Ag Verfahren und Vorrichtung zur thermischen Umsetzung metallischer Precursorschichten in halbleitende Schichten
DE102009037299A1 (de) * 2009-08-14 2011-08-04 Leybold Optics GmbH, 63755 Vorrichtung und Behandlungskammer zur thermischen Behandlung von Substraten
JP2013512311A (ja) * 2009-11-25 2013-04-11 イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー 結晶性銅カルコゲニドナノ粒子の水性製造方法、そのように製造されたナノ粒子、ならびにこれらのナノ粒子を組み込んだインクおよびコーテッド基板

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4923396A (en) * 1984-11-08 1990-05-08 Mitsubishi Jukogyo Kabushiki Kaisha Method and apparatus for heating a strip of metallic material in a continuous annealing furnace
WO2002044430A1 (en) * 2000-11-30 2002-06-06 The Boc Group Plc Quenching method and apparatus
JP2010001560A (ja) * 2008-11-04 2010-01-07 Philtech Inc 膜形成方法および膜形成装置

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of WO2012153046A1 *

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CN103703550A (zh) 2014-04-02
US20140080249A1 (en) 2014-03-20
AU2012252173B2 (en) 2014-12-18
KR20140035929A (ko) 2014-03-24
AU2012252173A1 (en) 2013-11-14
CA2834209A1 (fr) 2012-11-15
JP2014519701A (ja) 2014-08-14
WO2012153046A1 (fr) 2012-11-15
FR2975223B1 (fr) 2016-12-23
FR2975223A1 (fr) 2012-11-16
JP5795430B2 (ja) 2015-10-14
AU2012252173A2 (en) 2014-06-05

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