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WO1992019391A1 - Procede de formation de revetements en oxydes metalliques - Google Patents

Procede de formation de revetements en oxydes metalliques Download PDF

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Publication number
WO1992019391A1
WO1992019391A1 PCT/US1992/003505 US9203505W WO9219391A1 WO 1992019391 A1 WO1992019391 A1 WO 1992019391A1 US 9203505 W US9203505 W US 9203505W WO 9219391 A1 WO9219391 A1 WO 9219391A1
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WIPO (PCT)
Prior art keywords
metal
coating
substrate
metal oxide
oxide
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Ceased
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PCT/US1992/003505
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English (en)
Inventor
Benmin Gong
James C. W. Chien
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Publication of WO1992019391A1 publication Critical patent/WO1992019391A1/fr
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
    • H01L21/02227—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process
    • H01L21/0223—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate
    • H01L21/02244—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate of a metallic layer
    • 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
    • C03C17/23—Oxides
    • C03C17/25—Oxides by deposition from the liquid phase
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    • C04B41/455—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application the coating or impregnating process including a chemical conversion or reaction
    • C04B41/4554—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application the coating or impregnating process including a chemical conversion or reaction the coating or impregnating material being an organic or organo-metallic precursor of an inorganic material
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    • 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
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    • C23C18/1216—Metal oxides
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    • 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
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    • C23C18/1225—Deposition of multilayers of inorganic material
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    • 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
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    • C23C18/125—Process of deposition of the inorganic material
    • C23C18/1279—Process of deposition of the inorganic material performed under reactive atmosphere, e.g. oxidising or reducing atmospheres
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    • 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
    • C03C2218/30—Aspects of methods for coating glass not covered above
    • C03C2218/32—After-treatment
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
    • H01L21/02205—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition

Definitions

  • the present invention relates to methods of forming thermally stable metal oxide coatings upon substrates as of conducting, semiconducting and insulating surfaces; being more particularly directed to the formation of thin uniform and hole-free high temperature thermally stable metal oxide coatings for such purposes as (1) providing fractional to multi-micron insulating coating surfaces to conducting (and semiconducting) substrates and the like, including hard high-temperature thermally stable ceramic barrier coatings capable of resisting rust and other oxidation effects and acids, and having excellent hard wear characteristics; and (2) providing relatively conductive metal oxide coatings for
  • magnesium, lanthanum, strontium, and other metal salts to provide, as by spin coating, a coated solution upon the desired substrates ⁇ in that case, a semiconductor wafer surface.
  • the resulting micron thick film of polymer metal complex precursor thus applied to the substrate was then heated under an air atmosphere from room temperature to about 700 C for about 2 hours and then maintained at that temperature for another half hour, resulting in a smooth, continuous, pin-hole free insulating metal oxide layer of the order of 0.2
  • conductive metal oxide coatings of uniform, pinhole free properties may be desired on insulating substrates, as of glass or the like, or on semiconducting substrates as in solar cell construction.
  • An object of the invention is to provide a new and improved method of forming thin uniform and aberration-resistant and hole-free high temperature thermally stable metal oxide coatings upon substrates, including metal and other conducting
  • a further object is to provide such a novel coating method for such purposes as inhibiting rust or attack by acids or other elements upon metal and similar surfaces, providing a high temperature thermally stable ceramic barrier, providing a hard insulating thin micron range coating for conducting substrates, and/or providing a hard and excellent wear-resistant surface coating for various substrates.
  • Still an additional object is to provide novel coatings having the above-described properties that may be produced on a wide variety of substrate surfaces in accordance with the methodology underlying the
  • Another object is to provide a method of producing a conducting metal oxide coating for insulating
  • Another object is to provide a method of producing a conducting metal oxide coating for semiconducting surfaces, as of silicon or the like and novel coated products produced thereby.
  • the invention embraces a method of forming thin uniform and aberration-resistant and hole-free high- temperature thermally stable metal oxide coatings upon a substrate, that comprises, dissolving a metal salt in a polymer solution to form a polymer-metal-complex
  • precursor solution containing ions of the metal, the oxide of which is desired as a coating on the substrate; coating the precursor solution after filtration upon the surface of the substrate and insuring uniformity of application over such surface; firing the coated
  • the invention provides an entirely different and less complex and costly technique for enabling the desired types of metal oxide coatings.
  • Prior techniques have involved, for example, sputtering or chemical vapor deposition to deposit coatings having some of the properties above described.
  • the before-described methacrylic acid-vinyl acetate copolymer was dissolved in N,N-dimethylformarnide in the ratio of about fifty percent copolymer and fifty percent dimethylformarnide.
  • the resulting copolymer solution then received a metal salt in the form of indium nitrate pentahydrate in the proportion of 75% cop ⁇ lymer and 25% ⁇ f.etal salt to form a p ⁇ lymer-metal-complex precursor solution wherein indium oxide was desired as the
  • the precursor solution was filtered with 0.4 micron filtering to remove foreign particles and then to enable spin coating on an acetone-cleaned silicon substrate surface. This resulted in a coating of about 2 microns thinness, as measured by interferometer measurements, producing uniformity over the surface.
  • the coated substrate was then introduced into an air (or oxygen) oven with the temperature increased from room temperature to 400 C for about 40 minutes, resulting in substantially complete burn-off of the polymer
  • Example 1 The experiment of Example 1 was repeated and the amount of indium nitrate compound relative to the amountof polymer solution was varied from the 25 grams of the metal salt and 75 grams of the copolymer of Example 1. It was noted that control of the concentration could be effected by increasing the amount of the copolymer, resulting in thinning of the coating,
  • Example 1 of metal oxide salt and the copolymer were repeated for zirconium acetyl acetonate with about 3% yittrium nitrate added, instead of indium nitrate pentahydrate. The same process was effected, this time on a conducting
  • Example 1 The process and proportions set forth in Example 1 was repeated on a steel plate for an aluminum nitrate salt, producing an excellent insulating coating of aluminum oxide of the order of a few tenths of a micron.
  • Example 1 The building up of this layer to the order of amicron and higher was then effected by recycling or repeating the steps of Example 1 (namely the spinning and heating) five times, each time adding 0.2 micron thickness to the coating.
  • Example 2 The same process as in Example 1 was repeated on a steel plate with a chromium nitrate metal salt,
  • Example 1 The steps of Example 1 were also repeated for a titanium nitrate salt providing an excellent titanium dioxide film, again on a steel substrate.
  • the color of coatings is distinctly related to the coating thickness, which not only enables verification of thickness and uniformity of coating, but also enables a selection of a desired color of the coating surface. It has been found that all metal oxides tested produce the same color for the same thickness; namely, at 1 micron thickness, the coating is clear and has no color; at 0.2 micron
  • metal oxides can, with a further modification of the method, be rendered substantially conducting, and well adapted for providing a conducting metal oxide coating on insulation substrates, such as glass or a ceramic, such as alumina, ZrO 2 or YSZ, a high temperature polymer, such as a polyimide or polysulfone and the like.
  • the substrates may be flat surfaces, wafers or fibers such as glass or alumina fibers. This technique has been found to be effectable through the adding in the polymer metal complex precursor solution containing the dissolved metal salt, the oxide of which metal it is desired to use as the coating, an
  • the indium oxide-to-tin oxide ratio was about 10:1.
  • the resulting polymer metal complex precursor solution was spin coated upon the surface of a glass substrate, insuring uniformity of application over the whole surface, and the coated glass was then fired in an air or oxygen furnace at a temperature of about 400 C for about 40 minutes, raising the temperature from about room temperature about 5 degrees per minute. At about 300 C the polymer substantially completely burned off with no residue, leaving the oxidized doped indium oxide.
  • the glass coated element was then kept in the oven at the 400 C temperature for about 10 to 20 minutes and then it was removed and cooled, providing a coating, that was found to be conducting, of about 91% indium oxide and 9% tin oxide.
  • Example 7 The same technique of Example 7 was repeated with the process of coating and firing recycled five times, producing a one micron thick conducting indium oxide film.
  • Example 7 The process of Example 7 was repeated, but instead of spin-coating the glass, it was dip-coated again, producing a uniform, aberration-resistant and hole-free high temperature thermally stable conducting metal oxide coating of the order of 0.2 mircon.
  • the metal or other substrate surface may be dipped or sprayed with the polymer metal complex, again, however, enduring uniformity of application over the entire surface.
  • the polymer metal complex may, if desired, be drawn into a fiber or other shape as before stated.
  • metal oxides such as Al 2 O 3 , TiO 2 , ZrO 2 , MgO and Cr 2 O 3 ; and mixed metal oxides such as ZrO 2 ⁇ Y 2 O 3 (YSZ), SrTiO 3 , LaAlO 3 ,
  • the polymer of the polymer metal complex precursors used in the methods of the invention may as explained in part in said copending application, be a carboxly, amide, amic acid, ester, anhydride, nitrile or amine-containing homopolymer, copolymer or terpolymer or the like.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Thermal Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Chemically Coating (AREA)

Abstract

Procédé de formation de revêtements fins, uniformes, de l'ordre du micron et du sous-micron, en oxydes métalliques thermiquement stables à haute température, résistants aux aberrations et exempts de trous, sur des substrats métalliques, isolants et autres, comprenant l'application d'une solution de précurseur complexe de métal et de polymère sur le substrat et une cuisson appropriée en vue de l'oxydation du métal et du revêtement, ainsi que d'une élimination par brûlage de toutes les traces de polymère. On produit des revêtements en oxydes métalliques isolants sur des surfaces conductrices et semi-conductrices et, si on le désire, des revêtements en oxydes métalliques conducteurs sur des substrats isolants et semi-conducteurs.
PCT/US1992/003505 1991-04-29 1992-04-28 Procede de formation de revetements en oxydes metalliques Ceased WO1992019391A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US69343191A 1991-04-29 1991-04-29
US693,431 1991-04-29

Publications (1)

Publication Number Publication Date
WO1992019391A1 true WO1992019391A1 (fr) 1992-11-12

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012024019A1 (fr) * 2010-08-19 2012-02-23 Caterpillar Inc. Préoxydation de soupapes de moteur et sièges rapportés pour durée de vie améliorée
CN115125596A (zh) * 2021-03-24 2022-09-30 中国科学院苏州纳米技术与纳米仿生研究所 表面处理方法及应用

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4303554A (en) * 1979-06-22 1981-12-01 Hitachi, Ltd. Composition and process for producing transparent conductive film
US4636440A (en) * 1985-10-28 1987-01-13 Manville Corporation Novel process for coating substrates with glass-like films and coated substrates
US4666742A (en) * 1983-05-11 1987-05-19 Nissan Chemical Industries Ltd. Polymer composition containing an organic metal complex and method for producing a metallized polymer from the polymer composition
US4946710A (en) * 1987-06-02 1990-08-07 National Semiconductor Corporation Method for preparing PLZT, PZT and PLT sol-gels and fabricating ferroelectric thin films

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4303554A (en) * 1979-06-22 1981-12-01 Hitachi, Ltd. Composition and process for producing transparent conductive film
US4666742A (en) * 1983-05-11 1987-05-19 Nissan Chemical Industries Ltd. Polymer composition containing an organic metal complex and method for producing a metallized polymer from the polymer composition
US4636440A (en) * 1985-10-28 1987-01-13 Manville Corporation Novel process for coating substrates with glass-like films and coated substrates
US4946710A (en) * 1987-06-02 1990-08-07 National Semiconductor Corporation Method for preparing PLZT, PZT and PLT sol-gels and fabricating ferroelectric thin films

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012024019A1 (fr) * 2010-08-19 2012-02-23 Caterpillar Inc. Préoxydation de soupapes de moteur et sièges rapportés pour durée de vie améliorée
CN115125596A (zh) * 2021-03-24 2022-09-30 中国科学院苏州纳米技术与纳米仿生研究所 表面处理方法及应用

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