US20050166846A1 - Large area deposition in high vacuum with high thickness uniformity - Google Patents

Large area deposition in high vacuum with high thickness uniformity Download PDF

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Publication number
US20050166846A1
US20050166846A1 US10/512,838 US51283804A US2005166846A1 US 20050166846 A1 US20050166846 A1 US 20050166846A1 US 51283804 A US51283804 A US 51283804A US 2005166846 A1 US2005166846 A1 US 2005166846A1
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United States
Prior art keywords
effusing
sources
source according
molecules
source
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Abandoned
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US10/512,838
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English (en)
Inventor
Giacomo Benvenuti
Simone Amorosi
Estelle Halary-Wagner
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Ecole Polytechnique Federale de Lausanne EPFL
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Ecole Polytechnique Federale de Lausanne EPFL
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Assigned to ECOLE POLYTECHNIQUE FEDERALE DE LAUSANNE (EPFL) reassignment ECOLE POLYTECHNIQUE FEDERALE DE LAUSANNE (EPFL) ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: AMOROSI, SIMONE, BENVENUTI, GIACOMO, HALARY-WAGNER, ESTELLE, HOFFMANN, PATRIK
Publication of US20050166846A1 publication Critical patent/US20050166846A1/en
Priority to US11/785,141 priority Critical patent/US20070193519A1/en
Priority to US13/280,131 priority patent/US8852344B2/en
Priority to US14/507,705 priority patent/US20150114566A1/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F4/00—Processes for removing metallic material from surfaces, not provided for in group C23F1/00 or C23F3/00
    • C23F4/02—Processes for removing metallic material from surfaces, not provided for in group C23F1/00 or C23F3/00 by evaporation
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/243—Crucibles for source material
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
    • C30B23/02—Epitaxial-layer growth
    • C30B23/06—Heating of the deposition chamber, the substrate or the materials to be evaporated
    • C30B23/066—Heating of the material to be evaporated

Definitions

  • the present invention relates to thermal or laser-assisted (electron or ion beam-assisted) film deposition with chemical precursors in the molecular regime.
  • the gas inlet system consisting in one or more effusive sources with given molecular angular distribution and relative position compared to the deposition area, can be assumed theoretically as the unique parameter influencing molecular impinging rate distribution on the deposition area [8, 9].
  • Sources flow angular distribution and their relative position to the deposition area can hence be assumed, practically and not only theoretically, as the key parameter to achieve high uniform thickness.
  • Effusive sources are defined as apertures between the main chamber, in which precursor molecules in the form of molecular beams will impinge on the deposition area, and a reservoir (in our case a single pre-chamber common to all the sources for a given precursor) in which higher-pressure conditions occur ranging from the viscous, through the transition, to the molecular regime.
  • Evaporation sources are used in physical vapour deposition processes and generally require very high temperatures necessary to reach sufficient vapour pressure, while gas sources use volatile chemical precursors resulting in high enough pressures even at temperatures as low as 100° C.
  • the difficulty in the molecular flow regime is to achieve simultaneously both high thickness uniformity and high growth rates [4], which are usually related to high efficiency use of precursor [4, 5], and high initial investment costs [1] as reducing the size of the reactor usually allows reduced equipment costs, but also leads to poor thickness uniformity.
  • the first quality of a source with respect to angular distribution is reproducibility and stability.
  • One of the problems in MBE sources is that the source angular distribution may vary to a large extent as a function of the filling level. This leads to poorly controllable angular distributions of effusing molecules with time [23].
  • Gas sources are generally more reliable, but care must be taken to control molecular angular distribution that can depend on pressure.
  • Another error that can account for different angular distributions is that the source dimension aperture can have a deep impact on the molecular distribution.
  • the source aperture geometry must now be compared to the distance between the source and the deposition area.
  • Point sources can arbitrarily be subdivided into three classes as reported by Cale [8]: cosine sources (Knudsen sources) over-cosine and under-cosine sources depending on their degree of collimation.
  • cosine sources Knudsen sources
  • over-cosine sources [22] [26] mainly because they can reach higher growth rates [4] and optimise precursor use.
  • collimated sources lead to several problems. Among these we can list a general increase in source-deposition area distance to keep uniform impinging rates and higher sensitivity to misalignments [10]. Under-cosine sources in opposition to more focused sources have been poorly discussed in literature.
  • the invention relates to a novel small point gas source (using chemical precursors) for vacuum deposition in the molecular regime able to lead to highly uniform thickness on large areas with small reactor size and high precursor efficiency use.
  • the source design is also compatible with light-assisted (electron or ion-assisted) deposition.
  • homogeneous etching can be achieved if it relies on impinging rate of etching chemical on a given area.
  • the reactor design is such that the source relative position and its angular distribution of effusing molecules are the only parameters accounting for their distribution on the substrate. Because of the line of sight propagation of the molecules in the molecular regime, the distribution of impinging molecules on the substrate can be calculated mathematically.
  • the reactor is composed of a precursor reservoir heated (for example by a thermo-regulated oil-bath up to temperatures of 200° C.) connected to a pre-chamber with a ring shape allowing irradiation of the substrate through its centre.
  • a precursor reservoir heated for example by a thermo-regulated oil-bath up to temperatures of 200° C.
  • a pre-chamber with a ring shape allowing irradiation of the substrate through its centre.
  • Four or more sources consisting in holes in a vacuum tight sheet separating the pre-chamber from the deposition chamber, where the substrate is positioned, are responsible of the molecular impinging distribution on the substrate.
  • the effusing rate is controlled by regulating the pressure and the temperature of the pre-chamber resulting in only one single cost efficient system control for all the sources. All the system is baked at a temperature at least 20° C. higher than the temperature of the precursor reservoir to avoid precursor condensation.
  • a cryo-panel is used to condense all the molecules effusing from the sources that do not collide directly on the substrate and of the by-products resulting from the chemical decomposition of the precursor.
  • a pumping system is used to achieve a vacuum between 10 ⁇ 12 and 10 ⁇ 3 mbar in the deposition chamber and a vacuum between 10 ⁇ 6 and 10 mbar in the pre-chamber.
  • a typical effusion source is a hole of 0.5 mm drilled in a foil of 0.05 mm of thickness between a reservoir (pre-chamber) with a pressure of 10 ⁇ 3 -10 ⁇ 2 mbar and the deposition chamber with a pressure below 10 ⁇ 3 mbar.
  • the hole dimensions however, depend on the pressure in the pre-chamber and on the substrate size, and could vary from 0.001 and 50 mm.
  • the thickness of the hole is about one order of magnitude (or more) smaller than the diameter, while the distance of the source to the deposition area is one order of magnitude (or more) larger than the diameter of the hole.
  • the second point discussed is how to achieve the desired distribution shaping of the sources required for the already discussed reasons in point 5 of the summary of the invention.
  • under-cosine distributions for small angles and over-cosine distributions for greater angles corresponding to regions outside the substrate are aimed at.
  • a tilt angle could be considered the first step in molecular beam modification (relative to the substrate), but this method is very limited.
  • Two other solutions are proposed, as examples, but should not be considered exhaustive.
  • the first design is based on selecting and promoting molecules escaping the source with a given angle. Two different types of molecules will escape the source: the molecules that had the last collision inside the pre-chamber with another molecule and those that had the last collision on a surface inside the source.
  • a volume below the effusing aperture is a forbidden region for gas phase collision.
  • a pumping aperture will act as a trap for surface scattered molecules. Counterbalancing both effects could lead to shaped distributions.
  • variable pressure configuration could lead to variable angular distributions without any moving part or modifications of the set-up.
  • FIG. 4 An example to reduce molecules effusing at small angles is reported in FIG. 4 with a cone-like shaped forbidden volume. Any kind of structure could serve to reach this purpose.
  • the apex may be cut and a hole provides a pumping aperture. If the cone is positioned under the hole at a distance b ⁇ 0, we will have a progressive increase of the volume, as angle will increase that will depend on the ratio between the distance b and the mean free path ⁇ .
  • variable pressure configuration will lead to variable effect of the cone as the mean free path is changed.
  • a particular case of this configuration could be a negative parameter b; i.e. the cone exits the pre-chamber through the hole.
  • mechanical complexity of multiple cones can be avoided by producing a continuous structure.
  • any kind of molecular angular distribution can be achieved by opportune disposition of several holes a 3-D surface.
  • these sources are dispatched close together compared to their distance to the deposition area we can consider them as a single point source with the advantage of easy mathematical modelling.
  • the total area of the holes should be small compared to the area separating the 3D surface from the pre-chamber to avoid gas depletion and pressure gradients.
  • each single hole must satisfy the rules introduced previously in the summary of the invention.
  • a particular shape of interest is a hemisphere (see FIG. 5 ).
  • asymmetric sources are easily produced leading to gas waste reduction.
  • FIG. 1 is a diagrammatic representation of FIG. 1 :
  • R is the radius of the ring on which are distributed the holes
  • r is the distance from the centre on the substrate ( 2 )
  • h is the distance of the substrate from the holes containing plane ( 3 ).
  • FIG. 2
  • ⁇ is the tilt angle of the surface on which is the source S and is oriented towards the z-axis.
  • FIG. 3 Shape of the ideal angular distribution ( 1 ), to achieve high impinging rate uniformity and small reactor size, compared to Knudsen effusion ( 2 ). Both curves are normalised to achieve same number of effusing molecules. In the ideal curve ( 1 ), 60° is assumed to be the cut-off plane that discriminates between deposition on and outside the deposition area. A rapid decrease of the molecules occurs after this critical angle and the under-cosine distribution ( 4 ) is modified resulting in an over-cosine distribution ( 3 ). Asymmetric sources could also prove useful.
  • FIG. 4 The source is composed of a hole ( 1 ), a volume ( 2 ) that reduce the region where gas phase collisions are allowed, and a pumping aperture ( 3 ) that reduce the surface from which scattered molecules can exit the source. Gas phase collisions are restricted to larger angles in FIG. 4 a . Surface scattered molecules are reduced for small angles FIG. 4 b . When the parameter b is not null, a variation in pressure induces a variation of the mean free path ⁇ . A different contribution of the cone to angular distribution is hence achievable as a function of pressure in FIG. 4 c . The structure can also exit the source as reported in FIG. 4 d.
  • FIG. 5 a Fractal source composed of a distribution of effusing holes on a hemispherical surface.
  • FIG. 5 b Asymmetric fractal source with preferential orientation of the molecular beam.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
  • Physical Vapour Deposition (AREA)
  • Chemical Vapour Deposition (AREA)
US10/512,838 2002-05-03 2003-05-02 Large area deposition in high vacuum with high thickness uniformity Abandoned US20050166846A1 (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
US11/785,141 US20070193519A1 (en) 2002-05-03 2007-04-16 Large area deposition in high vacuum with high thickness uniformity
US13/280,131 US8852344B2 (en) 2002-05-03 2011-10-24 Large area deposition in high vacuum with high thickness uniformity
US14/507,705 US20150114566A1 (en) 2002-05-03 2014-10-06 Large area deposition in high vacuum with high thickness uniformity

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
CH0200241 2002-05-03
WOPCT/CH02/00241 2002-05-03
PCT/CH2003/000285 WO2003093529A2 (en) 2002-05-03 2003-05-02 Large area deposition in high vacuum with high thickness uniformity

Related Parent Applications (1)

Application Number Title Priority Date Filing Date
PCT/CH2003/000285 A-371-Of-International WO2003093529A2 (en) 2002-05-03 2003-05-02 Large area deposition in high vacuum with high thickness uniformity

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US11/785,141 Continuation US20070193519A1 (en) 2002-05-03 2007-04-16 Large area deposition in high vacuum with high thickness uniformity

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US10/512,838 Abandoned US20050166846A1 (en) 2002-05-03 2003-05-02 Large area deposition in high vacuum with high thickness uniformity
US11/785,141 Abandoned US20070193519A1 (en) 2002-05-03 2007-04-16 Large area deposition in high vacuum with high thickness uniformity
US13/280,131 Expired - Fee Related US8852344B2 (en) 2002-05-03 2011-10-24 Large area deposition in high vacuum with high thickness uniformity
US14/507,705 Abandoned US20150114566A1 (en) 2002-05-03 2014-10-06 Large area deposition in high vacuum with high thickness uniformity

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US13/280,131 Expired - Fee Related US8852344B2 (en) 2002-05-03 2011-10-24 Large area deposition in high vacuum with high thickness uniformity
US14/507,705 Abandoned US20150114566A1 (en) 2002-05-03 2014-10-06 Large area deposition in high vacuum with high thickness uniformity

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US (4) US20050166846A1 (de)
EP (1) EP1504136A2 (de)
AU (1) AU2003226995A1 (de)
WO (1) WO2003093529A2 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120037077A1 (en) * 2002-05-03 2012-02-16 Giacomo Benvenuti Large area deposition in high vacuum with high thickness uniformity

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US20110239940A1 (en) * 2008-10-08 2011-10-06 Giacomo Benvenuti Vapor phase deposition system
FR2956869B1 (fr) 2010-03-01 2014-05-16 Alex Hr Roustaei Systeme de production de film flexible a haute capacite destine a des cellules photovoltaiques et oled par deposition cyclique des couches
US8087380B2 (en) * 2009-10-30 2012-01-03 Intevac, Inc. Evaporative system for solar cell fabrication
DE102012205615A1 (de) 2012-04-04 2013-10-10 Carl Zeiss Smt Gmbh Beschichtungsverfahren, Beschichtungsanlage und optisches Element mit Beschichtung
CN106978588B (zh) * 2017-03-31 2019-09-20 京东方科技集团股份有限公司 一种蒸镀罩、蒸镀源、蒸镀装置及蒸镀方法
DE102021206788A1 (de) 2021-06-30 2023-01-05 Carl Zeiss Smt Gmbh Verfahren zum Abscheiden einer Schicht, optisches Element und optische Anordnung für den DUV-Wellenlängenbereich
US20230399767A1 (en) * 2022-06-13 2023-12-14 Paul Colombo Systems and methods for pulsed beam deposition of epitaxial crystal layers

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US8852344B2 (en) * 2002-05-03 2014-10-07 Ecole Polytechnique Federale De Lausanne (Epfl) Large area deposition in high vacuum with high thickness uniformity

Also Published As

Publication number Publication date
US20120037077A1 (en) 2012-02-16
AU2003226995A1 (en) 2003-11-17
AU2003226995A8 (en) 2003-11-17
US20150114566A1 (en) 2015-04-30
WO2003093529A3 (en) 2004-03-18
EP1504136A2 (de) 2005-02-09
WO2003093529A2 (en) 2003-11-13
US8852344B2 (en) 2014-10-07
US20070193519A1 (en) 2007-08-23

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