WO2014118019A1 - Procédé de dépôt de silicium polycristallin - Google Patents

Procédé de dépôt de silicium polycristallin Download PDF

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Publication number
WO2014118019A1
WO2014118019A1 PCT/EP2014/050880 EP2014050880W WO2014118019A1 WO 2014118019 A1 WO2014118019 A1 WO 2014118019A1 EP 2014050880 W EP2014050880 W EP 2014050880W WO 2014118019 A1 WO2014118019 A1 WO 2014118019A1
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WO
WIPO (PCT)
Prior art keywords
pptw
ppbw
silicon
copper
metal
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PCT/EP2014/050880
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German (de)
English (en)
Inventor
Dieter Knerer
Piotr Filar
Original Assignee
Wacker Chemie Ag
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Filing date
Publication date
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Publication of WO2014118019A1 publication Critical patent/WO2014118019A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B01J23/755—Nickel
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/02—Silicon
    • C01B33/021—Preparation
    • C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
    • C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/32—Manganese, technetium or rhenium
    • B01J23/34—Manganese
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/48—Silver or gold
    • B01J23/50—Silver
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/48—Silver or gold
    • B01J23/52—Gold
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B01J23/745—Iron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B01J23/75—Cobalt
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/85—Chromium, molybdenum or tungsten
    • B01J23/86—Chromium

Definitions

  • the invention relates to a method for the deposition of polycrystalline silicon.
  • High purity polycrystalline silicon serves as a starting material for the production of single crystal silicon for Czochralski (CZ) or zone melting (FZ) semiconductor, for the production of single or multicrystalline silicon by various drawing and casting processes
  • Polysilicon is usually produced by means of the Siemens process.
  • a reaction gas comprising one or more silicon-containing components and optionally hydrogen in a reactor comprising by direct
  • silicon-containing components are preferably silane (SiH4), monochlorosilane (SiH 3 Cl), dichlorosilane (DCS, SiH 2 Cl 2 ), trichlorosilane (TCS, SiHCl 3 ), tetrachlorosilane (SiCl 4 ) or
  • the Siemens procedure is usually in one
  • the reactor comprises a metallic base plate and a coolable bell which is placed on the base plate, so that a reaction space in the
  • the baseplate is provided with one or more gas inlet openings and one or more
  • Each carrier body usually consists of two thin ones
  • Filament rods and a bridge which usually connects adjacent rods at their free ends.
  • the filament rods are made of single or polycrystalline silicon
  • the filament rods are mounted vertically in electrodes located at the bottom of the reactor, via which the connection to the power supply takes place. High-purity precipitates on the heated filament rods and the horizontal bridge
  • the deposition process is usually controlled by the specification of rod temperature and reaction gas stream or composition.
  • the measurement of the rod temperature is carried out with
  • the rod temperature is controlled by controlling the electrical power
  • Reaction gases are given as a function of time or bar diameter.
  • the deposition with TCS or its mixture with DCS and / or STC is usually carried out at rod temperatures between 900 and 1100 ° C, a supply of silicon-containing component (s) (in total) of 0.5 to 10 kMol / h per 1 m 2 the rod surface, wherein the mole fraction of this component (s) in the feed stream (in total) is between 10% and 50% (the remainder 90% to 50%
  • US 4759830 and US 4773973 relate to processes for the production of thin layers of elemental silicon on an electrically conductive material suitable as an electrode by electrolytic deposition of silicon from a
  • halides of a transition metal are disclosed chromium (II) iodide (CrJ 2), manganese (II) iodide (MnJ 2),
  • the electrolytic deposition of the silicon can be cathodic, wherein the cathode material such as copper, chromium, molybdenum, nickel, platinum, iron or stainless steels, preferably of aluminum, silicon or graphite and as
  • Anode material such as platinum, silicon or graphite used.
  • the electrolytic deposition of the silicon may be carried out anodically from a melt comprising a silicon halide
  • the electrolytic deposition of the silicon may e.g. from a melt containing silicon tetraiodide, aluminum triiodide and lithium iodide.
  • the halide of a transition metal represents the so-called catalyst, which controls the silicon deposition and the quality of the silicon layers on e.g. Copper, chromium, molybdenum, nickel, iron and chromium steel or inorganic glasses e.g. from tin dioxide or tin dioxide / indium oxide mixtures
  • Silicon carrier under the conditions of that method in the first place. Namely, no silicon deposition is observed without this catalyst.
  • the Müller-Rochow synthesis is a process for
  • Catalyst is copper, which elementary or z. B. is used in the form of copper oxide. Zinc, tin, phosphorus and other elements also act as promoters. The reaction takes place at about 300 ° C and 0.5-2 bar (ü).
  • EP2036117 AI discloses that according to conventional technique
  • Metal layer to be grown on a substrate Metal layer to be grown on a substrate.
  • metal it may e.g. to trade gold on one
  • silicon from a silicon source is used to effect growth of silicon nanowires at the metal islands.
  • EP2082419 A2 discloses a process for metal catalyzed nanowire growth in which as metal catalysts
  • Transition metals from the periodic table u.a. Copper, silver, gold, nickel, palladium, platinum, cobalt, rhodium, iridium, indium, iron, ruthenium, tin, osmium, manganese, chromium,
  • Molybdenum tungsten, vanadium, niobium, tantalum, titanium, zirconium and Gallium, including mixtures of one or more of these metals.
  • the object of the present invention was to provide a more economical method for the separation of
  • the object is achieved by a method for depositing polycrystalline silicon, wherein a silicon-containing gas is introduced into a reactor and by reduction of the silicon-containing gas polycrystalline silicon is deposited on a by direct current passage to a temperature of at least 550 ° C heated carrier body, characterized characterized in that during the reduction of the silicon-containing gas at least one first metal selected from the group consisting of titanium, chromium, manganese, iron, cobalt, nickel, copper and zinc is present as a first metal selected from the group consisting of titanium, chromium, manganese, iron, cobalt, nickel, copper and zinc is present as a first
  • Catalyst acts and also at least one different from the first metal second metal selected from the group
  • the silicon-containing gas is preferably a halosilane, preferably trichlorosilane.
  • trichlorosilane is used in the presence of hydrogen.
  • the at least first and at least second metals shall be present in such quantities during the reduction of the silicon-containing gas that in the deposited polycrystalline silicon at least one element selected from the group consisting of titanium, chromium, manganese, iron, cobalt, nickel, copper and Zinc at a concentration of 18 pptw - 40 ppbw titanium, 0.2 pptw - 5 ppbw chromium, 0.5 pptw - 15 ppbw manganese, 7 pptw - 50 ppbw iron, 0.012 pptw - 25 ppbw cobalt, 0.9 pptw - 8 ppbw nickel, 3 pptw - 12 ppbw copper or 0.6 pptw - 11 ppbw zinc;
  • the invention therefore also relates to polycrystalline silicon containing at least one first metal selected from the group consisting of titanium, chromium, manganese, iron, cobalt, nickel, copper and zinc; and at least one second metal other than the first metal selected from the group consisting of copper, silver and gold;
  • the at least two selected metals are present in polycrystalline silicon in the following amounts: 18 pptw - 40 ppbw titanium, 0.2 pptw - 5 ppbw chromium, 7 pptw - 50 ppbw iron, 0.012 pptw - 25 ppbw cobalt, 0.9 pptw - 8 ppbw nickel, 3 pptw - 12 ppbw copper, 0.6 pptw - 11 ppbw zinc, 0.15 pptw - 21 ppbw silver, 0.001 pptw - 0.3 ppbw gold, 0.5 pptw - 15 ppbw manganese.
  • Table 1 shows the minimum and maximum concentrations of metals in the deposited polycrystalline silicon.
  • the metal (s) are used in combination with carbon. It is particularly preferred if copper, nickel and
  • the concentration of methane in the silicon-containing gas should be 2-18 ppm.
  • the process is associated with an immense economic advantage.
  • investigations of the deposition rates in reactors of the type shown in Fig. 1 has been shown that by the presence of the two catalyst metals compared
  • Polysilicon should be usually too high. However, it has been shown that even the smallest amounts of the existing metals, which have no negative impact on the quality of polycrystalline silicon, have a positive effect. It is essential that the catalytically active substances in solid, deposited polycrystalline silicon are effective. Disintegration of the silanes in the gas phase is undesirable. This would lead to gas phase nucleation and dusting, which is undesirable. The reaction mechanism must therefore be effective in the surface of the polycrystalline silicon. This is ensured by the fact that the metals are predominantly dissolved in solid silicon and do not remain free in the gas phase. The introduced metals can freely diffuse in already deposited polycrystalline silicon. As soon as they reach a surface and they are asymmetrically surrounded by silicon, stronger bonds form
  • Pseudosilicide deprives the environment hydrogen, probably as a proton.
  • the silicon-containing gas especially trichlorosilane, releases hydrogen. This is a first
  • Partial reaction The so-destabilized silane decomposes, thereby depositing silicon. This is a second partial reaction.
  • both partial reactions are accelerated by catalysts, wherein the first partial reaction is accelerated by a first catalyst and the second partial reaction by a second catalyst, which can not be clarified the first and second partial reactions are each accelerated by the ferrous metals or by the noble metals. Copper is obviously suitable for both
  • Partial reactions act as a catalyst.
  • methane or other carbon-containing gases are used, such as ethane, propane, butane, pentane, ethene, solvent vapors, the iso-forms of the
  • Carbon in the exhaust stream can be determined.
  • Polysilicon layer which becomes 20 times thicker with maximum catalyst action.
  • polysilicon is deposited on the silicon core in the experimental reactor of FIG. 1.
  • the same process conditions are temperature, pressure, gas flows and heating current. Only the metal addition by the catalyst source 9 in FIG. 1 is changed
  • Aluminum as an impurity not. However, on the n-side, the doping is counteracted by aluminum.
  • Metals that occupy lattice sites are generally active as p- or n-doping.
  • the effect is generally active as p- or n-doping.
  • B, C, Mg, Ca, Zn, Pt are unsuitable while Li, O, Cr, Mn, Fe, Ni, Cu, Ag, Au are interstitial impurities.
  • Diffusion coefficient has copper.
  • the charge carriers In order to enable the function of the pn junction, the charge carriers must be separated. This is all the more easily possible the longer the charge carrier lifetime. Some of the metals act on and as recombination centers.
  • Particularly advantageous are copper and silver.
  • the release of the metals in the reactor is preferably carried out by arc in the cold gas phase, namely in the silanes, preferably in an inert gas.
  • the metals can be incorporated in other ways in the reaction gases.
  • the metals may already be incorporated into the chlorosilane in an upstream process, e.g. Trichlorosilane, be introduced. It is also possible that metals are added to the hydrogen in a process upstream of the deposition.
  • the metals are introduced by means of a gas-tight, temperature-resistant and temperature and pressure swing-resistant spark plug.
  • a high voltage pulse leads to an arc in the
  • the spark plug comprises two electrodes, each one
  • Both electrodes can be completely made of one
  • Consist catalyst metal Alternatively, a
  • Catalyst metal attached to the electrode tip e.g. be soldered or welded, be.
  • the discharged amount of catalyst metal is through
  • FIG. 1 shows an apparatus for carrying out the method.
  • Fig. 2 shows a detail view of the spark plug. List of reference numbers used
  • a device for carrying out the method is shown schematically.
  • the reaction vessel 8 is a
  • the holder consists of two graphite power supply 11, which are mounted so that they are suitable to supply heating current to the silicon core.
  • the electrical connection is made by means of power connections 12.
  • Silicone gasket 4 to protect against high process temperatures, the graphite power supply with a water cooling 3
  • the silicon core 81 Since the silicon core 81 is not electrically conductive at room temperature, it must be brought by means of an infrared heater 72 to a temperature at which the heating current from the graphite power supply lines 11 is effective.
  • reaction vessel 8 For this heating, the reaction vessel 8 with a
  • Infrared radiation window 71 provided. After swinging out the HIR heating device, the IR radiation window 71 is used to observe the processes inside the reaction vessel, in particular by means of an IR pyrometer 72 to monitor the temperature.
  • process gases for the deposition of polysilicon are process gases
  • the supply of silanes 21 takes place at the bottom of the chamber, as well as the supply of the auxiliary gases 22.
  • the discharge of the exhaust gas 23 takes place in the upper region of the process chamber.
  • the catalysts are in the flow of auxiliary gases 22
  • the catalytically active metals are released by means of a slightly changed spark plug 9.
  • the spark plug serves as a catalyst source.
  • Fig. 2 the spark plug 9 is shown in more detail.
  • the distance between the electrodes can be adjusted and readjusted with a set screw 92 for adjusting the arc length.
  • the amount and the proportion of the released metals are adjusted by the electrode spacing, the ignition voltage, the charge, and the tip angles of the electrodes. If discharges are carried out under the same conditions until the detection limit of the metals has been far exceeded, the amount of metal can be assigned to a single discharge and thus quantitative ratios below the detection limits can be set.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Catalysts (AREA)

Abstract

L'invention concerne un procédé de dépôt de silicium polycristallin selon lequel un gaz contenant du silicium est introduit dans un réacteur et par réduction du gaz contenant du silicium, du silicium polycristallin est déposé sur un corps support chauffé à une température d'au moins 550 °C par passage direct du courant. Le procédé est caractérisé en ce qu'au cours de la réduction du gaz contenant du silicium, au moins un premier métal choisi dans le groupe composé de titane, chrome, manganèse, fer, cobalt, nickel, fer et zinc est présent et agit comme premier catalyseur, et au moins un second métal différent du premier, choisi dans le groupe composé de cuivre, argent et or est présent, et agit comme second catalyseur.
PCT/EP2014/050880 2013-01-31 2014-01-17 Procédé de dépôt de silicium polycristallin WO2014118019A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102013201608.5A DE102013201608A1 (de) 2013-01-31 2013-01-31 Verfahren zur Abscheidung von polykristallinem Silicium
DE102013201608.5 2013-01-31

Publications (1)

Publication Number Publication Date
WO2014118019A1 true WO2014118019A1 (fr) 2014-08-07

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PCT/EP2014/050880 WO2014118019A1 (fr) 2013-01-31 2014-01-17 Procédé de dépôt de silicium polycristallin

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DE (1) DE102013201608A1 (fr)
TW (1) TW201429870A (fr)
WO (1) WO2014118019A1 (fr)

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4481232A (en) 1983-05-27 1984-11-06 The United States Of America As Represented By The Department Of Energy Method and apparatus for producing high purity silicon
US4759830A (en) 1986-08-19 1988-07-26 Ciba-Geigy Ag Process for the production of polycrystalline silicon coatings by electrolytic deposition of silicon
WO2006094714A1 (fr) * 2005-03-05 2006-09-14 Joint Solar Silicon Gmbh & Co. Kg Reacteur et procede de production de silicium
EP2036117A1 (fr) 2006-06-15 2009-03-18 Electronics and Telecommunications Research Institute Procédé de fabrication de nanofils de silicium au moyen d'une pellicule mince à points quantiques de silicium
EP2077252A2 (fr) 2007-11-28 2009-07-08 Mitsubishi Materials Corporation Appareil de fabrication de silicium polycristallin et procédé de fabrication
EP2082419A2 (fr) 2006-11-07 2009-07-29 Nanosys, Inc. Systèmes et procédés de croissance de nanofils
WO2010074674A1 (fr) * 2008-12-23 2010-07-01 Arise Technologies Corporation Procédé et appareil pour le raffinage de silicium
EP2431329A1 (fr) * 2010-09-15 2012-03-21 Wacker Chemie AG Procédé de fabrication de tiges fines de silicium
EP2607310A1 (fr) * 2011-12-21 2013-06-26 Wacker Chemie AG Silicium polycristallin

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4481232A (en) 1983-05-27 1984-11-06 The United States Of America As Represented By The Department Of Energy Method and apparatus for producing high purity silicon
US4759830A (en) 1986-08-19 1988-07-26 Ciba-Geigy Ag Process for the production of polycrystalline silicon coatings by electrolytic deposition of silicon
US4773973A (en) 1986-08-19 1988-09-27 Ciba-Geigy Ag Process for the production of polycrystalline silicon coatings by electrolytic deposition of silicon
WO2006094714A1 (fr) * 2005-03-05 2006-09-14 Joint Solar Silicon Gmbh & Co. Kg Reacteur et procede de production de silicium
EP2036117A1 (fr) 2006-06-15 2009-03-18 Electronics and Telecommunications Research Institute Procédé de fabrication de nanofils de silicium au moyen d'une pellicule mince à points quantiques de silicium
EP2082419A2 (fr) 2006-11-07 2009-07-29 Nanosys, Inc. Systèmes et procédés de croissance de nanofils
EP2077252A2 (fr) 2007-11-28 2009-07-08 Mitsubishi Materials Corporation Appareil de fabrication de silicium polycristallin et procédé de fabrication
WO2010074674A1 (fr) * 2008-12-23 2010-07-01 Arise Technologies Corporation Procédé et appareil pour le raffinage de silicium
EP2431329A1 (fr) * 2010-09-15 2012-03-21 Wacker Chemie AG Procédé de fabrication de tiges fines de silicium
EP2607310A1 (fr) * 2011-12-21 2013-06-26 Wacker Chemie AG Silicium polycristallin

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TW201429870A (zh) 2014-08-01
DE102013201608A1 (de) 2014-07-31

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