WO2006114781A2 - Depot de materiaux - Google Patents

Depot de materiaux Download PDF

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Publication number
WO2006114781A2
WO2006114781A2 PCT/IE2006/000041 IE2006000041W WO2006114781A2 WO 2006114781 A2 WO2006114781 A2 WO 2006114781A2 IE 2006000041 W IE2006000041 W IE 2006000041W WO 2006114781 A2 WO2006114781 A2 WO 2006114781A2
Authority
WO
WIPO (PCT)
Prior art keywords
nano
layer
particles
spray
substrate
Prior art date
Application number
PCT/IE2006/000041
Other languages
English (en)
Other versions
WO2006114781A3 (fr
Inventor
Gabriel M. Crean
Gareth Redmond
Original Assignee
University College Cork - National University Of Ireland, Cork
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 University College Cork - National University Of Ireland, Cork filed Critical University College Cork - National University Of Ireland, Cork
Publication of WO2006114781A2 publication Critical patent/WO2006114781A2/fr
Publication of WO2006114781A3 publication Critical patent/WO2006114781A3/fr

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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • C23C18/1208—Oxides, e.g. ceramics
    • C23C18/1216—Metal oxides
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1229—Composition of the substrate
    • C23C18/1245—Inorganic substrates other than metallic
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/125—Process of deposition of the inorganic material
    • C23C18/1262—Process of deposition of the inorganic material involving particles, e.g. carbon nanotubes [CNT], flakes
    • C23C18/127—Preformed particles
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/125—Process of deposition of the inorganic material
    • C23C18/1291—Process of deposition of the inorganic material by heating of the substrate
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/14—Decomposition by irradiation, e.g. photolysis, particle radiation or by mixed irradiation sources
    • C23C18/143—Radiation by light, e.g. photolysis or pyrolysis

Definitions

  • the invention relates to deposition of a composite coating or layer on a substrate, the coating having particles embedded in a host material.
  • the invention is directed towards providing for more versatility in composition of coatings which are applied. Another object is to achieve this versatility with low- temperature processing and/or where the composite coating is to include nano- particles.
  • a method of forming a composite layer on a substrate comprising the steps of:
  • the nano-particles are chemically synthesised to provide the desired nano-particle size and composition in the layer.
  • the nano-particles are dispersed in the carrier liquid with a density chosen according to the desired density of nano-particles embedded in the layer.
  • control scheme times inclusion of the liquids to achieve a stratum of nano-particles in the layer.
  • the substrate is heated to a temperature of less than 500 0 C.
  • the substrate is a silicon wafer.
  • the deposit is treated by irradiation with UV radiation.
  • the radiation is generated by an excimer lamp.
  • the liquids are formed into a spray by an injection system and the spray is delivered to a spray head.
  • the host material is in a carrier liquid.
  • the host material comprises titanium isopropoxide solution.
  • the host material carrier liquid comprises hexane.
  • the nano-particle carrier liquid comprises hexane.
  • the invention provides an apparatus for forming a composite layer on a substrate, the layer comprising a host material in which nano-particles of a different material are embedded, the apparatus comprising:
  • spray means for forming the liquids into a spray and directing the spray so that it forms a deposit on the substrate, with relative proportions of the liquids contributing to the spray according to a control scheme to achieve a desired layer composition
  • the substrate support comprises a rotating stage.
  • the spray means comprises a plurality of injector systems, at least one per liquid.
  • the treatment means comprises an irradiation means.
  • the irradiation means comprises a UV source.
  • Fig. 1 is a schematic representation of a process of the invention
  • Figs 2 to 6 are diagrams illustrating process steps
  • Figs. 7(a) and 7(b) are 1OX bright-field and epifluorescence micrographs respectively (with 200ms integration) of portions of layers formed according to the invention.
  • the apparatus 1 comprises a rotating stage 2 in a processing chamber 3 at sub-atmospheric pressure.
  • the apparatus 1 also comprises a spray head 4 having an aperture for passage of UV light from a UV source 5 to a wafer on the stage 2.
  • the apparatus 1 also comprises a liquid injection system 10 for receiving a flow of host material in liquid precursor form.
  • the system 10 forms the liquid flow into a spray, which is delivered by the head 4 in the chamber 3.
  • the apparatus 1 also comprises nanocrystal injector systems 11 and 12. These receive a flow of nano-particles dispersed in a liquid carrier, and form the liquid into a spray which is also is delivered over the wafer by the spray head 4.
  • nano-crystal and “nano-particle” are interchangeable, and mean particles in the nano-particle size range.
  • the nano-particles may be solubilised as a colloidal sol. This may be achieved by a charged surface coating or by steric hindrance.
  • the method of manufacture includes the steps of maintaining the substrate at an appropriate temperature. This is preferably below 500 0 C.
  • the sprayed material forms a deposit on the substrate in the chamber.
  • the UV source 5 is operated so that the deposited material forms a layer on the substrate.
  • the layer comprises nano-particles embedded in the host material.
  • nano-particles may be chemically synthesised to have the precise chemical and physical properties desired.
  • the nano-particles are dispersed in the carrier liquid with a density chosen according to the desired density of nano-particles in the host material of the layer. As this is done “offline” in a highly controlled process there is very precise control over the nano- particle properties and their density. This is an advantageous departure from the prior art, in which the nano-particles are formed “inline” during the deposition process, such as in CVD processes.
  • the pattern of the nano-particles in the host material may be easily and precisely controlled. This is achieved by simply controlling the flows of the host and nano-particle/carrier streams.
  • the flows are pulsed with inter-leaving according to the desired patterns. There may, for example, be zero flow of the nano-particle stream for a period so that when it is started and subsequently stopped it forms a discrete stratum within the host material.
  • the deposited materials may be thermally decomposed at the heated substrate surface in order to form the layer.
  • stabilising moieties previously attached at the nano- particle surfaces, e.g. alkyl thiol molecules, by UV exposure to facilitate incorporation of the nano-particles in the host matrix.
  • Fig. 2. shows a substrate 20 onto which a layer 21 is formed.
  • the layer 21 comprises a host matrix 22 with embedded nano-particles 23.
  • the apparatus 1 may be used in a method of co-depositing a host matrix and nano-particles to form a stratum in a layer on a substrate, whereby the host material liquid precursor is introduced to form a host matrix 30 on a silicon substrate 20, and a nano-particle/carrier stream is pulsed for a defined period during the host matrix deposition resulting in the formation of a defined stratum 31 of nano-particles. Subsequent deposition of host material completes a layer 40 having a buried stratum 31 of nano-particles.
  • the apparatus 1 may alternatively be used to perform a method of co-depositing a host matrix and nano-particles to form a compositionally graded layer 50 on a substrate 20.
  • the second nano-particle injection system 12 is operated in a controlled fashion during the host matrix formation to allow a graded concentration of nano-particles 51 within the host matrix as shown in Fig. 4.
  • another method forms a sequentially varying multilayer structure 60 on a substrate 20 with parallel injection of the host liquid and a nano- particle/carrier liquid, but with sequential steps of the different nano-particle injections by the systems 11 and 12. This results in the formation of a multilayer, multifunctional thin film structure 60 on the substrate as shown in Fig. 5.
  • the apparatus 1 may be used in a method of forming a host layer 80 embedded with a plurality of different species of nano-particles 81 and 82 on a substrate. There is parallel injection of the host matrix and a plurality of different nano-particle carrier liquids. This results in the formation of randomly distributed nano-particles of different properties within a host matrix 83.
  • the host material liquid and the nano-particle carrier liquid or liquids may be pre- mixed and injected together for complete dispersion of the nano-particles in the host material in the layer.
  • the low temperature environment of this process is very well suited to deposition of nano-sized metallic and semiconductor nanocrystals since size effects such as suppression of melting point are well known. Low temperature deposition ensures that the risks of nano-crystal melting or phase change during deposition are minimised.
  • a 1:1 ratio of 0.1M titanium isopropoxide solution in hexane and a 2.5 mg/ml CdTe(ZnS) nanocrystal suspension (also in hexane) were mixed together.
  • the resulting mixture was agitated in an ultrasonic bath to ensure homogeneity.
  • the evaporation temperature was fixed at 200 0 C and the substrate temperature was maintained at 365 0 C.
  • Forming a host layer embedded with a plurality of different nano-particles on a substrate Forming a range of layer morphologies depending on the concentration of nano-particles injected, ranging from isolated islands through to discontinuous and ultimately continuous films.
  • hydrogen or another suitable agent may be incorporated into the reaction mixture during host Si NC deposition and incorporated into the SiO2 matrix in order to enhance the passivation of the surface and interface states between the Si NC and oxide host.

Abstract

Dans la présente invention, un système à injection de liquide (10) reçoit une charge de matériau hôte sous forme de précurseur liquide et produit à partir de cette charge liquide un brouillard qui est distribué par une tête (4) dans une chambre (3). Des systèmes d'injection (11, 12) de nanoparticules transportées en solution reçoivent les charges de nanoparticules dispersées dans les solutions et produisent un brouillard qui est également distribué au-dessus de la plaquette substrat par la tête de pulvérisation (4). Dans la chambre, le matériau pulvérisé forme un dépôt sur le substrat. Une source d'UV (5) est utilisée pour que le matériau forme une couche sur le substrat. Cette couche comprend des nanoparticules noyées dans le matériau hôte.
PCT/IE2006/000041 2005-04-26 2006-04-26 Depot de materiaux WO2006114781A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IE20050254 2005-04-26
IE2005/0254 2005-04-26

Publications (2)

Publication Number Publication Date
WO2006114781A2 true WO2006114781A2 (fr) 2006-11-02
WO2006114781A3 WO2006114781A3 (fr) 2007-11-15

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