EP3510178A1 - Réacteur cvd et procédé de purge d'un réacteur cvd - Google Patents

Réacteur cvd et procédé de purge d'un réacteur cvd

Info

Publication number
EP3510178A1
EP3510178A1 EP17769005.4A EP17769005A EP3510178A1 EP 3510178 A1 EP3510178 A1 EP 3510178A1 EP 17769005 A EP17769005 A EP 17769005A EP 3510178 A1 EP3510178 A1 EP 3510178A1
Authority
EP
European Patent Office
Prior art keywords
metal
gas
process chamber
cleaning
passivation layer
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.)
Pending
Application number
EP17769005.4A
Other languages
German (de)
English (en)
Inventor
Marcel Kollberg
Wilhelm Josef Thomas KRÜCKEN
Francisco Ruda Y Witt
Markus Deufel
Mike PFISTERER
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.)
Aixtron SE
Original Assignee
Aixtron SE
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 Aixtron SE filed Critical Aixtron SE
Publication of EP3510178A1 publication Critical patent/EP3510178A1/fr
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
    • C23C16/4405—Cleaning of reactor or parts inside the reactor by using reactive gases
    • 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
    • C23C16/06—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 deposition of metallic material
    • C23C16/18—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 deposition of metallic material from metallo-organic compounds
    • 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
    • C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
    • C23C16/4404—Coatings or surface treatment on the inside of the reaction chamber or on parts thereof
    • 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
    • C23C16/455—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 introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45563—Gas nozzles
    • C23C16/45572—Cooled nozzles
    • 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
    • C23C16/22—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 deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/301—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • C23C16/303—Nitrides

Definitions

  • the invention relates to a CVD reactor with a susceptor which can be heated by a heating device, for receiving one or more substrates to be coated, with a gas inlet element for introducing a process gas into a process chamber arranged between a process chamber cover and the susceptor, the gas inlet element contains at least one metal, in particular stainless steel component, the at least one coming into contact with the process gas metal, especially stainless steel surface, at least one cooling channel for cooling the gas inlet member, at least one ne fed from a process gas inlet process gas inlet opening for introducing the one or more reactive Gas having process gas into the process chamber and a supplied from a cleaning gas supply line cleaning gas inlet opening for introducing a cleaning gas into the process chamber.
  • the invention further relates to a method for cleaning a process chamber of a CVD reactor, wherein in a cleaning step by introducing a cleaning gas into the process chamber at least a first deposition step by introducing at least one first reactive gas into the process chamber formed deposits on the surface of a susceptor by a chemical reaction with the cleaning gas at a first temperature, which is an elevated temperature, are converted into volatile components, which are transported out of the process chamber by means of a carrier gas, wherein the process chamber at least one stainless steel component, at least a metal, in particular stainless steel surface coming into contact with the process gas, has at least one cooling channel for cooling the gas inlet member, at least one of a process gas supply fed process gas inlet opening for introducing one or more reactive gases into the process chamber and a cleaning gas supplied from a cleaning gas inlet opening for introducing the cleaning gas into the process chamber.
  • a CVD reactor in which by means of a gas inlet member, an organometallic compound of the III main group and a hydride of the V main group are fed separately into a process chamber.
  • the process chamber has a bottom that is formed by a susceptor on which substrates rest, which are coated with reaction products of the two process gases, for example with GaN or other III-V semiconductor layers.
  • the process gases decompose thereby on hot surfaces within the process chamber, thus not only on the substrates, but also on the remaining spaces between the substrates.
  • the assignments there must be cleaned from time to time, in particular after each production cycle. For this purpose, a cleaning gas is fed into the process chamber through a separate gas inlet opening.
  • the cleaning gas is preferably chlorine, which is introduced into the process chamber together with nitrogen. There, with the aid of the etching gas at elevated temperatures, for example. At temperatures above 600 ° C, the deposits are converted into volatile chemical compounds, which are removed by means of the carrier gas from the process chamber.
  • a process is described, such as by applying stainless steel components within a process chamber to the surface thereof with an organometallic compound. Bonding and then provided with ambient air with a passivation layer.
  • This passivation layer has the property of preventing metal atoms from releasing from the stainless steel surface during a deposition step and being incorporated into the layer to be deposited.
  • the passivation layer is removed, so that it must be reapplied after the cleaning step. This is considered disadvantageous.
  • the prior art further includes a WO 2013/033428 A2, in which a cleaning method for cleaning the process chamber of an MOCVD
  • a cleaning plate is to be brought against a designed as a show-erhead gas inlet member.
  • an annular gap is to form, through which a gas flows, so that forms a diffusion barrier and prevents the cleaning gas comes into contact with the gas outlet surface of the showerhead.
  • US 6,060,397 describes a method for cleaning the process chamber of a CVD reactor using N 2 , C 2 F 6 and O 2 , wherein a plasma is generated from these cleaning gases with a plasma generator.
  • US 2011/0162674 AI describes a method to remove TiN residues from a process chamber of a CVD reactor. The cleaning gas used here is chlorine, which is activated with a plasma generator to form an etching plasma.
  • US 2012/0171797 A1 describes an apparatus and a method for depositing GaN or AlGaN layers for producing light-emitting diodes. As dopant Cyklopentadienylmagnesium is used.
  • US 2013/0005118 A1 describes a method for depositing III-V layers using a MOCVD reactor, which is cleaned after a deposition step by introducing chlorine, wherein the cleaning of the process chamber takes place at elevated temperatures.
  • an ALD method in which alternately different gases are introduced into a process chamber, wherein in each case only a monolayer deposits on a substrate. Two consecutively separated different monolayers should react with each other.
  • a metal surface of the process chamber is to be passivated, wherein initially an aluminum-containing organic starting material in the process chamber and then an oxygen donor is introduced into the process chamber, so that forms in a reaction alumina.
  • the invention has the object of developing the known cleaning method for cleaning a CVD reactor for use in MOCVD reactors in which the cleaning gas exposed metal surfaces have been provided in a conditioning step with a passivation layer and a usable for this purpose CVD Specify reactor.
  • a CVD reactor is used in which the metal surfaces coming into contact with the process gas are provided with a passivation layer.
  • a metal surface without a passivation layer has on its surface metal atoms which can come into reactive contact with one of the reactive gases, so that these metal atoms are peeled off. This is prevented with the passivation layer.
  • the metal component is, in particular, an alloy consisting of a plurality of metallic elements.
  • the alloy contains in particular iron. It is especially stainless steel.
  • a stainless steel surface not provided with a passivation layer has both iron and chromium atoms on its surface.
  • the metal-organic compounds used in the deposition of III-V layers and in particular doped III-V layers occurs on the metal, especially stainless steel surface to a chemical reaction of the organometallic compound with the local metal atoms, in which metal atoms of the Dissolve surface and enter as an organometallic compound in the gas phase within the process chamber.
  • the metal thus dissolved out of the surface of the alloy, in particular the stainless steel surface, in particular iron, can be installed in an undesired manner into the layer to be deposited on the substrate. Therefore, according to the invention, the metal or stainless steel components which come into contact with the process gas are provided with a passivation layer which at least impedes this detachment process.
  • the untreated, but cleaned stainless steel surface is exposed for a certain treatment time with an organometallic, gaseous compound.
  • an organometallic, gaseous compound which is preferably Cp 2 Mg.
  • the metal, in particular iron atoms of the organometallic compound which is preferably Cp 2 Mg.
  • the pretreated metal, in particular stainless steel surface is exposed to the ambient air, so that on the surface magnesium oxide, magnesium hydroxide or magnesium carbonate can form.
  • the gas inlet member is cooled in such a way that the surfaces of the metal, in particular stainless steel components exposed to the cleaning gas exceed a maximum temperature.
  • organometallic passivation layer or one consisting of oxides instead of such, in particular organometallic passivation layer or one consisting of oxides
  • Passivation layer it is also envisaged to coat the metal surface with a metal layer, in particular to nickel or chrome plating.
  • the metal coating can be applied by electroplating. It can also be vapor-deposited. It is preferably a coating of chromium or nickel. The coating can also consist of a precious metal.
  • the provided with a passivation layer metal, in particular stainless steel components preferably reach a maximum temperature of 100 ° C, more preferably a maximum temperature of 70 ° C.
  • the cleaning step takes place at temperatures of at least 600 ° C.
  • the process chamber is heated in the cleaning step to at least 700 ° C.
  • the gas inlet member has at least one metal component, in particular a stainless steel component.
  • the metal component in particular the stainless steel component, may have a surface which is electropolied. In electropolishing, the surface is substantially preferably smoothed so that the effective size of the surface is reduced.
  • the metal, in particular stainless steel component has a cooling channel for cooling the gas inlet member and a surface facing the process chamber. In the pointing to the process chamber surface of the metal, in particular stainless steel component are process gas inlet openings for introducing one or more reactive gases into the process chamber, which in depositing the The above-mentioned III-V layers serve as starting materials.
  • the metal, in particular stainless steel component also has a cleaning gas inlet opening for introducing a cleaning gas into the process chamber.
  • the cleaning gas may be chlorine. But it can also be a gas whose molecules have a halogen.
  • the one or more process gas inlet openings are connected to one or more process gas supply lines, so that separate process gases can be fed into the process chamber separately, which mix only within the process chamber.
  • the gas inlet member may be arranged in the center of a rotationally symmetrical about an axis designed process chamber, so that the process gases move in the radial direction through the process chamber.
  • the gas inlet member has in a vertical direction extending gas outlet openings for the exit of the process gas.
  • the process gas emerging from the gas inlet member flows through the process chamber between two walls, wherein a wall is formed by a susceptor lying substantially in a horizontal plane and a wall parallel thereto by a process chamber ceiling.
  • the feed of the cleaning gas is carried out by cleaning gas inlet openings, which are preferably associated with the process chamber ceiling.
  • the cleaning gas inlet openings may be arranged in a uniform circumferential distribution around the gas inlet member, wherein the annular zone in which the cleaning gas inlet openings are arranged, the gas inlet member may be immediately adjacent.
  • a directed cleaning gas stream preferably flows into the process chamber.
  • the cleaning gas inlet openings or an axis defining the flow direction have an angle through a cleaning gas inlet opening to a further axis directed transversely to the flow direction, the angle between the two axes being between 0 and 60 degrees.
  • the exiting from the cleaning gas inlet openings cleaning gas flow thus has a flow direction component, which is directed away from the gas inlet member.
  • the cleaning gas inlet opening is inclined relative to a vertical axis by 0 to 60 degrees, wherein preferably the angle of inclination is greater than 0 degrees and chosen so that as far as possible the cleaning gas in the direction of the gaatlassorgans back-carrying vortex form.
  • the gas inlet member may also have the shape of a showerhead.
  • the gas inlet member forms in this case, the process chamber ceiling and has a plurality of evenly arranged on the process chamber ceiling gas inlet openings through which one or more process gases can enter the process chamber.
  • the at least one cooling channel is arranged in such a way and flows through in such a way with a coolant, that the surface of the gas inlet member facing the process chamber does not become warmer than 100 ° C.
  • the passivation layer which is preferably at most 3 nm thick, is applied in at least one conditioning step, wherein each conditioning step comprises two substeps, namely a first step in which the organometallic compound is fed together with a carrier gas and a second substep in which air or an air-like gas mixture in the process chamber is introduced or the process chamber is only opened so that air or an air-like gas mixture can act on the metal, in particular stainless steel component. Between each of these sub-steps, a rinsing step may be provided.
  • the individual conditioning steps of the plurality of conditioning steps can likewise be separated in time by a rinsing step.
  • the surface can be heated to a temperature of more than 40 ° C.
  • metals for the metal component are not only alloys such as stainless steel, but also other, especially iron-containing alloys into consideration, but also those alloys that are suitable for use in a CVD reactor, for example.
  • the passivation layer can according to a development of the invention also simultaneously with the cleaning step, ie simultaneously with the introduction of chlorine generated. An already existing passivation layer can also be stabilized in the cleaning step.
  • the cleaning gas inlet openings are arranged such that the cleaning gas comes into contact with the metal surface or the passivation step in the cleaning step. However, there is no chemical reaction with the passivation layer.
  • the passivation layer is produced along with a chemical reaction of an organometallic component with the metal surface.
  • Fig. 2 also a partial section and a 180 ° drawn therein
  • a CVD reactor of the type described above is basically known from DE 10 2015 101 462 A1 and the literature cited therein and in particular cited.
  • the CVD reactor has a gas-tight housing to the outside, which is evacuated by means of a vacuum pump. Within the housing there is a process chamber 21.
  • the process chamber 21 has a process chamber bottom which is formed by a susceptor 2 made of coated graphite. On the susceptor 2, a multiplicity of substrates 4 are formed. which are coated in a CVD deposition process with a III-V layer, for example. GaN.
  • a heater 3 which heats the surface of the susceptor 2 facing the process chamber 21 to process temperatures which may be in the range between 700.degree. C. and 1200.degree.
  • the gas inlet element 1 is an essentially cylindrical body with gas inlet openings 8, 10, 12 arranged on the cylinder jacket wall for introducing various reactive gases, for example organometallic compounds and hydrides from the interior of the gas inlet element 1 into the process chamber surrounding the gas inlet element 1 21.
  • a directly above the susceptor 2 in the process chamber 21 opening gas inlet opening 8 is fed by a process gas supply line 7.
  • a directly below the process chamber ceiling 19 arranged inlet opening 12 is fed by a process gas supply line 11.
  • Intermediate gas inlet openings 10 are fed by a process gas supply line 9.
  • the outer surface of the portion of the gas inlet member 1, which has the process gas inlet openings 8, 10, 12, are stainless steel surfaces, which are provided with a passivation layer.
  • the passivation layer is applied before the first CVD deposition step.
  • a cooling chamber 17 in which by a coolant supply line 16, a coolant, for example. Water is fed, which flows out through a coolant discharge line 18 from the cooling channel 17. While the cooling channel 17 is arranged in the region of the susceptor 2, a further cooling channel 14 in the region of the process chamber ceiling 19 is arranged. This cooling channel 14 is fed with a coolant supply line 13. The coolant leaves the cooling channel 14 through a coolant outlet 15.
  • a device for feeding a cleaning gas is provided in the region of the process chamber ceiling 19.
  • An annular cleaning gas distribution chamber 22 is fed by a cleaning supply line 5.
  • the cleaning gas can flow into the process chamber 21 from the annular chamber.
  • the cleaning gas inlet openings 6 are arranged in the region of the process chamber ceiling 19.
  • the cleaning gas inlet openings 6 lie in a circular zone, which is directly adjacent to the gas inlet member 1.
  • the cleaning gas inlet openings 6 generate a directed gas stream into the process chamber 21, this gas stream having a flow direction component which is directed away from the gas inlet element 1.
  • the susceptor 2 and the process chamber ceiling 19 extend in a common plane, in particular a horizontal plane.
  • the surface normal to this plane can then be a vertical axis.
  • the cleaning gas inlet openings 6 have an axis which is directed at an acute angle to the surface normal, that is to say preferably to the vertical axis.
  • the angle of the axis of the cleaning gas inlet opening 6 to this transverse to the flow direction of the exiting the gas inlet member 1 process gas axis is 0 to 60 degrees. A preferred angle is 25 degrees.
  • the cleaning gas inlet openings 6, which are arranged in a uniform angular distribution about a center axis of the process chamber, preferably generate flows which emerge along an imaginary frustoconical surface from a gas outlet zone of the process chamber ceiling.
  • the stainless steel surfaces of the gas inlet member 1 are passivated. If other stainless steel surfaces are provided in the process chamber which can come into contact with one of the process gases, these stainless steel surfaces are also passivated. The passivation can be done by a coating.
  • the coating can be a metal coating, for example a chromium coating or a nickel coating.
  • the metal component 20 can therefore be chromed or nickel-plated.
  • the stainless steel surface may be electropolished to make it more resistant to chlorine attack. A preferred method for creating a passivation layer is described below:
  • a metal organic compound for example. Magnesocene is fed into the process chamber 21, so that magnesocene comes into contact with the stainless steel surface.
  • a second step after rinsing the process chamber 21, ambient air is introduced into the process chamber or the process chamber is opened so that ambient air can come into contact with the stainless steel surface. This sequence of steps is repeated several times with an intermediate rinsing step until a sufficiently thick or sufficiently closed passivation layer is formed. During conditioning, there are no substrates 4 in the process chamber 21.
  • the substrates 4 are introduced into the process chamber 21 after conditioning. Then, a III-V layer sequence is deposited on the substrates 4 in the known manner. After the completion of the deposition process and the removal of the substrates 4 from the process chamber 21, the process chamber is cleaned. For cleaning the process chamber 21, a mixture of chlorine and nitrogen through the cleaning gas inlet 5 and the cleaning gas inlet opening 6 is fed into the process chamber 21. By means of the heater 3, the susceptor 2 is brought to an elevated first temperature, which is at least 700 ° C.
  • the surface of the metal component 20 facing the process chamber 21, which is the lateral surface of the gas inlet member 1 is cooled to a maximum temperature 100 ° C, preferably at most 70 ° C.
  • Nitrogen or another inert gas is passed through the process gas supply lines 7, 9, 11, which flows into the process chamber 21 through the associated process gas inlet openings 8, 10, 12.
  • the isotherm shown in dashed lines in FIG. 2 is formed, in which the gas phase temperature is 100.degree.
  • the surface temperature of the metal component 20 is less than 100 ° C, there is no reaction of the cleaning gas with the applied passivation layer.
  • the volatile metal chlorides which are in the gas phase during the purification step may also contribute to the generation or stabilization of the passivation layer.
  • the pointing to the process chamber 21 surface of the susceptor 2 has a sufficiently high temperature that there, the cleaning gas can chemically react with the assignments, so that form volatile components that can be removed with the carrier gas.
  • the surfaces of the metal component 20 are between two cooled sections of the process chamber 21.
  • a cooled section locally assigned to the susceptor 2.
  • Another cooled section is spatially associated with the process chamber ceiling 19.
  • the metal component 20 has a first end portion which is cooled by a first cooling means and a second portion which is preferably also an end portion which is also cooled.
  • a gas inlet surface which has a plurality of gas inlet openings 8, 10, 12, wherein the gas inlet openings 8, 10, 12 may be arranged on a cylinder jacket surface or on a circular disk surface.
  • a CVD reactor characterized in that at least one metal surface has a passivation layer obstructing the detachment of the metal components of the metal surfaces by one or more reactive gases, and that the cooling channels 14, 17 are arranged so that the passivation layer at a Cleaning step in which a cleaning gas is introduced into the process chamber 21 and in which the susceptor 2 is heated to a first temperature of at least 700 ° C, heated to a maximum of a second temperature of 100 ° C.
  • a method characterized in that, in a conditioning step prior to the first deposition step, a passivation layer is formed on the metal surface which has the effect of detaching metal constituents from the metal surface by the at least one reactive gas and in the cleaning step, the temperature of the metal surface is cooled to a second temperature which is lower than the first temperature, at which the cleaning gas does not react with the passivation layer in a manner impairing the action of the passivation layer.
  • a CVD reactor or a method which is characterized in that the passivation layer is produced in a conditioning step, in which for a first treatment period, first an organometallic compound is fed together with a carrier gas in the process chamber 21 and then for a second Treatment period is brought oxygen, water vapor and / or carbon dioxide having gas or gas mixture in contact with the metal component.
  • a CVD reactor or a process characterized in that the surface of the metal component (20) is electropolished and in particular is an electropolished stainless steel surface.
  • a CVD reactor or a method which are characterized in that the cleaning gas inlet openings (6) at an angle (a) of 0 to 60 degrees, preferably 25 degrees with respect to a transverse axis to the flow direction, in particular vertical axis inclined are. All disclosed features are essential to the invention (individually, but also in combination with one another).
  • the disclosure of the associated / attached priority documents (copy of the prior application) is hereby also incorporated in full in the disclosure of the application, also for the purpose of including features of these documents in claims of the present application.
  • the subclaims characterize with their features independent inventive developments of the prior art, in particular to make on the basis of these claims divisional applications.

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)
  • Inorganic Chemistry (AREA)

Abstract

L'invention concerne un procédé de purge et un réacteur CVD avec un organe d'admission de gaz (1) pour introduire un gaz de traitement dans une chambre de traitement (21) agencée entre un plafond de chambre de traitement (19) et le suscepteur (2), l'organe d'admission de gaz (1) contenant au moins un composant métallique (20) qui présente au moins une surface métallique, en particulier en acier inoxydable, venant en contact avec le gaz de traitement. La surface métallique présente une couche de passivation empêchant tout décollement des composants métalliques de la surface métallique par l'intermédiaire d'un ou de plusieurs gaz réactifs. Les canaux réfrigérants (14, 17) sont agencés de telle sorte que la couche de passivation, lors d'une étape de purge, dans laquelle du chlore est introduit comme gaz de purge dans la chambre de traitement (21) et dans laquelle le suscepteur (2) est chauffé à une première température d'au moins 700 °C, soit chauffée à une seconde température maximale de 100 °C. La couche de passivation est formée en parallèle avec une réaction chimique d'un composé organométallique avec les atomes métalliques de la surface métallique et les orifices d'admission (6) du gaz de purge sont agencée de telle sorte que le gaz de purge vienne en contact avec la surface métallique présentant la couche de passivation. La couche de passivation est obtenue lors d'une étape de conditionnement dans laquelle, pendant une première durée de traitement, un composé organométallique est d'abord introduit en même temps qu'un gaz porteur dans la chambre de traitement (21) et ensuite, pendant une seconde durée de traitement, amené en contact avec le composant métallique.
EP17769005.4A 2016-09-09 2017-09-08 Réacteur cvd et procédé de purge d'un réacteur cvd Pending EP3510178A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE102016116953 2016-09-09
DE102017100725.3A DE102017100725A1 (de) 2016-09-09 2017-01-16 CVD-Reaktor und Verfahren zum Reinigen eines CVD-Reaktors
PCT/EP2017/072565 WO2018046650A1 (fr) 2016-09-09 2017-09-08 Réacteur cvd et procédé de purge d'un réacteur cvd

Publications (1)

Publication Number Publication Date
EP3510178A1 true EP3510178A1 (fr) 2019-07-17

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CN109844174B (zh) 2022-07-05
DE102017100725A1 (de) 2018-03-15
JP2019530224A (ja) 2019-10-17
KR102474132B1 (ko) 2022-12-02
WO2018046650A1 (fr) 2018-03-15
JP7402041B2 (ja) 2023-12-20
CN109844174A (zh) 2019-06-04
US10883171B2 (en) 2021-01-05
US20190226082A1 (en) 2019-07-25
TWI763707B (zh) 2022-05-11
KR20190046985A (ko) 2019-05-07

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