WO1997012082A1 - Preparation of a semiconductor thin film - Google Patents

Preparation of a semiconductor thin film Download PDF

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Publication number
WO1997012082A1
WO1997012082A1 PCT/US1996/015267 US9615267W WO9712082A1 WO 1997012082 A1 WO1997012082 A1 WO 1997012082A1 US 9615267 W US9615267 W US 9615267W WO 9712082 A1 WO9712082 A1 WO 9712082A1
Authority
WO
WIPO (PCT)
Prior art keywords
nanoparticles
film
cadmium telluride
temperature
preparation
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.)
Ceased
Application number
PCT/US1996/015267
Other languages
English (en)
French (fr)
Inventor
Martin Pehnt
Douglas L. Schulz
Calvin J. Curtis
David S. Ginley
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.)
Midwest Research Institute
Original Assignee
Midwest Research Institute
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 Midwest Research Institute filed Critical Midwest Research Institute
Priority to AU73698/96A priority Critical patent/AU7369896A/en
Publication of WO1997012082A1 publication Critical patent/WO1997012082A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/20—Methods for preparing sulfides or polysulfides, in general
    • 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
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00—Selenium; Tellurium; Compounds thereof
    • C01B19/007—Tellurides or selenides of metals
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • 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
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
    • 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
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
    • C30B29/48—AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te
    • 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
    • C30B5/00—Single-crystal growth from gels
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
    • H10P14/20—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials
    • H10P14/26—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials using liquid deposition
    • H10P14/265—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials using liquid deposition using solutions
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
    • H10P14/20—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials
    • H10P14/29—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials characterised by the substrates
    • H10P14/2901—Materials
    • H10P14/2922—Materials being non-crystalline insulating materials, e.g. glass or polymers
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
    • H10P14/20—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials
    • H10P14/34—Deposited materials, e.g. layers
    • H10P14/3402—Deposited materials, e.g. layers characterised by the chemical composition
    • H10P14/3424—Deposited materials, e.g. layers characterised by the chemical composition being Group IIB-VIA materials
    • H10P14/3432—Tellurides
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
    • H10P14/20—Formation of materials, e.g. in the shape of layers or pillars of semiconductor materials
    • H10P14/34—Deposited materials, e.g. layers
    • H10P14/3451—Structure
    • H10P14/3452—Microstructure
    • H10P14/3461—Nanoparticles
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/02—Amorphous compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/20—Materials for coating a single layer on glass
    • C03C2217/28—Other inorganic materials
    • C03C2217/287—Chalcogenides
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/11—Deposition methods from solutions or suspensions
    • C03C2218/113—Deposition methods from solutions or suspensions by sol-gel processes

Definitions

  • the present invention relates to a process for the preparation of a semiconductor film such as cadmium telluride by depositing nanoparticles of a semiconductor material onto a substrate whose surface temperature after nanoparticle deposition thereon is sufficient to thereby cause simultaneous fusion of the nanoparticles to thereby coalesce with each other and effectuate film growth.
  • a semiconductor film such as cadmium telluride
  • Thin-film semiconductor material such as cadmium telluride is a usual component found in solar cell construction.
  • cadmium telluride is a spray pyrolysis methodology in which aqueous solutions of cadmium chloride and tellurium oxide are deposited on a substrate at deposition temperatures between about 425 °C and 500 °C for subsequent growth of a cadmium telluride film.
  • a major disadvantage to the spray-pyrolysis process is its energy inefficiency because of the required relatively-high working temperatures.
  • a second approach for producing a semiconductor film is described by Alivisatos et aL in U.S. Patent No. 5,262,357.
  • the patentees teach a two-step process wherein (1) nanoparticles of a semiconductor material are deposited on a solid support surface; and (2) the deposited nanoparticles and support surface thereafter are subjected to a temperature sufficient to melt and form a film.
  • Alivisatos et al. state that their methodology cannot produce thicker layers (e.g. 20 or 30 particles deep) since such thicknesses so foimed act as if they are bulk materials without proper fusion.
  • a primary object of the present invention is to provide a one-step process for the production of a semiconductor film.
  • the present invention is a process for the preparation of a semiconductor film.
  • the process comprises depositing nanoparticles of a semiconductor material onto a substrate whose surface temperature after nanoparticle deposition thereon is sufficient to cause substantially simultaneous fusion ofthe nanoparticles to thereby coalesce with each other and effectuate film growth.
  • Colloidal suspensions comprising nanoparticles of the semiconductor material can be sprayed using a carrier gas onto a susceptor having a relatively high temperature such that, even after any cooling effect caused by the spray, the temperature ofthe nanoparticles is high enough to cause their fusion with each other.
  • the present invention is a process for the preparation of a semiconductor film.
  • An example of such a film is a cadmium telluride film that can be employed in the construction of ceratin solar-energy collecting apparatus.
  • the Examples that follow describe in detail the formation of cadmium telluride films .
  • Example I In order to prepare cadmium telluride nanoparticles for spray deposition onto a substrate for ultimate growth of a cadmium telluride film, a nearly stoichiometric ratio of Cd(CH 3 ) 2 (dimethylcadmium) in (n-C 8 H I7 ) 3 P (tri-n-octylphosphine or "TOP") and (tri-n-octylphosphinetelluride or "TOPTe”) in TOP were mixed together in a controlled-atmosphere glove box.
  • TOP tri-n-octylphosphine
  • TOPTe tri-n-octylphosphinetelluride
  • This room-temperature mixture was injected as rapidly as possible into liquified (n-C 8 H 17 ) 3 PO (tri-n-octylphosphine oxide or "TOPO") solvent maintained at the desired reaction temperature from 54 °C to about 125°C under N 2 .
  • TOPO-capped cadmium telluride nanoparticles were precipitated and washed with methanol, centrifuged, and the TOPO-and TOP-containing methanol solution was decanted. The nanoparticles then were isolated from insoluble byproducts by preferential dissolution in butanol, centrifugation, and separation via cannula.
  • the cadmium telluride nanoparticles Prior to spray deposition, the cadmium telluride nanoparticles were suspended in an organic dispersant, here butanol, and introduced into a controlled-atmosphere glove box to thereby provide a precursor spray.
  • an organic dispersant here butanol
  • a SnO 2 -coated Corning 7059 glass was provided as the substrate situated on the susceptor and upon which the cadmium telluride nanoparticles were to be deposited.
  • the cadmium telluride precursor spray was gravity fed into an atomizing spray nozzle using N 2 carrier gas flowing at a rate of 7.21/min. and deposited as "Film A" onto the substrate using typical spray flow rates of 0.8 to 1.3 ⁇ 0.1 mVmin. Films sprayed accordingly were typically 10-1,000 nm in thickness.
  • the susceptor temperature (T s ) was 350°C ⁇ 2°C as measured by a thermocouple located beneath the surface thereof. Careful calibrations were carried out to determine the effective surface temperature of the substrate due to gas, liquid and radiative cooling effects.
  • the effective growth temperature (T g .) at the surface of the substrate was measured by mounting a low mass thermocouple onto the substrate surface using silver paint with high thermal conductivity and confirmed by template temperature recorders and a surface probe thermometer.
  • the T g . for Film A was 240°C. After film deposition, the substrate was kept under N 2 flow and removed from the susceptor within 10 seconds.
  • Example II In the same manner as in Example I, except employing a susceptor temperature of 400°C ⁇ 2°C, the precursor spray was deposited on the substrate as "Film B.” The T p for Film B was 270 °C.
  • Example III In the same manner as in Example I, except employing a susceptor temperature of 400°C ⁇ 2°C, the precursor spray was deposited on the substrate as "Film B.” The T p for Film B was 270 °C.
  • Example III Example III
  • the precursor spray was deposited on the substrate as "Film C.”
  • the T ⁇ for Film C was 300 °C.
  • Atomic Force Microscopy also supported the dependence of morphological development of the cadmium telluride thin films on growth temperatures with larger grains forming at higher T ⁇
  • cadmium telluride nanoparticle precursors simply coalesce to form a cadmium telluride thin film upon interaction with a heated substrate.
  • T g . 270 ⁇ C.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Metallurgy (AREA)
  • Nanotechnology (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Composite Materials (AREA)
  • Dispersion Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Chemical Vapour Deposition (AREA)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
PCT/US1996/015267 1995-09-29 1996-09-24 Preparation of a semiconductor thin film Ceased WO1997012082A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU73698/96A AU7369896A (en) 1995-09-29 1996-09-24 Preparation of a semiconductor thin film

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US08/536,348 1995-09-29
US08/536,348 US5711803A (en) 1995-09-29 1995-09-29 Preparation of a semiconductor thin film

Publications (1)

Publication Number Publication Date
WO1997012082A1 true WO1997012082A1 (en) 1997-04-03

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PCT/US1996/015267 Ceased WO1997012082A1 (en) 1995-09-29 1996-09-24 Preparation of a semiconductor thin film

Country Status (6)

Country Link
US (1) US5711803A (cg-RX-API-DMAC7.html)
AR (1) AR003731A1 (cg-RX-API-DMAC7.html)
AU (1) AU7369896A (cg-RX-API-DMAC7.html)
IN (1) IN189239B (cg-RX-API-DMAC7.html)
WO (1) WO1997012082A1 (cg-RX-API-DMAC7.html)
ZA (1) ZA968080B (cg-RX-API-DMAC7.html)

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US5986206A (en) * 1997-12-10 1999-11-16 Nanogram Corporation Solar cell

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US6126740A (en) * 1995-09-29 2000-10-03 Midwest Research Institute Solution synthesis of mixed-metal chalcogenide nanoparticles and spray deposition of precursor films
US6607829B1 (en) 1997-11-13 2003-08-19 Massachusetts Institute Of Technology Tellurium-containing nanocrystalline materials
US6207392B1 (en) 1997-11-25 2001-03-27 The Regents Of The University Of California Semiconductor nanocrystal probes for biological applications and process for making and using such probes
US6294401B1 (en) 1998-08-19 2001-09-25 Massachusetts Institute Of Technology Nanoparticle-based electrical, chemical, and mechanical structures and methods of making same
US6139626A (en) * 1998-09-04 2000-10-31 Nec Research Institute, Inc. Three-dimensionally patterned materials and methods for manufacturing same using nanocrystals
CA2374337C (en) * 1999-07-26 2009-04-14 Massachusetts Institute Of Technology Tellurium-containing nanocrystalline materials
AU777998B2 (en) * 1999-10-05 2004-11-11 Commonwealth Scientific And Industrial Research Organisation Three dimensional array films
AUPQ326499A0 (en) * 1999-10-05 1999-10-28 Commonwealth Scientific And Industrial Research Organisation Nanoparticle films
AU1942401A (en) * 1999-12-03 2001-06-12 Rurromed Inc. Thermal immobilization of colloidal metal nanoparticles
GB0026382D0 (en) * 2000-10-27 2000-12-13 Nanox Ltd Production of metal chalcogenide nanoparticles
US20020110180A1 (en) * 2001-02-09 2002-08-15 Barney Alfred A. Temperature-sensing composition
US6819845B2 (en) * 2001-08-02 2004-11-16 Ultradots, Inc. Optical devices with engineered nonlinear nanocomposite materials
US6710366B1 (en) 2001-08-02 2004-03-23 Ultradots, Inc. Nanocomposite materials with engineered properties
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US7005669B1 (en) 2001-08-02 2006-02-28 Ultradots, Inc. Quantum dots, nanocomposite materials with quantum dots, devices with quantum dots, and related fabrication methods
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AU2002326920B2 (en) * 2001-09-17 2007-09-13 Massachusetts Institute Of Technology Semiconductor nanocrystal composite
RU2206503C1 (ru) * 2001-12-28 2003-06-20 Федеральное государственное унитарное предприятие Государственный научный центр РФ "Научно-исследовательский физико-химический институт им. Л.Я. Карпова" Способ электрофоретического получения нитей из твердых наночастиц
US7344491B1 (en) 2003-11-26 2008-03-18 Nanobiomagnetics, Inc. Method and apparatus for improving hearing
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US7879696B2 (en) * 2003-07-08 2011-02-01 Kovio, Inc. Compositions and methods for forming a semiconducting and/or silicon-containing film, and structures formed therefrom
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US8134175B2 (en) 2005-01-11 2012-03-13 Massachusetts Institute Of Technology Nanocrystals including III-V semiconductors
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US20120132272A1 (en) 2010-11-19 2012-05-31 Alliance For Sustainable Energy, Llc. Solution processed metal oxide thin film hole transport layers for high performance organic solar cells
CN102249549B (zh) * 2011-04-01 2013-05-22 中南大学 一种太阳能电池用铜铟硒光伏薄膜、粉体、涂料及制备方法
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Patent Citations (5)

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US5363798A (en) * 1993-09-29 1994-11-15 The United States Of America As Represented By The Secretary Of The Navy Large area semiconductor wafers
US5491114A (en) * 1994-03-24 1996-02-13 Starfire Electronic Development & Marketing, Ltd. Method of making large-area semiconductor thin films formed at low temperature using nanocrystal presursors
US5576248A (en) * 1994-03-24 1996-11-19 Starfire Electronic Development & Marketing, Ltd. Group IV semiconductor thin films formed at low temperature using nanocrystal precursors
US5537000A (en) * 1994-04-29 1996-07-16 The Regents, University Of California Electroluminescent devices formed using semiconductor nanocrystals as an electron transport media and method of making such electroluminescent devices

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5986206A (en) * 1997-12-10 1999-11-16 Nanogram Corporation Solar cell

Also Published As

Publication number Publication date
ZA968080B (en) 1997-04-21
IN189239B (cg-RX-API-DMAC7.html) 2003-01-11
AU7369896A (en) 1997-04-17
AR003731A1 (es) 1998-09-09
US5711803A (en) 1998-01-27

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