EP0877099A1 - Couches électriquement conductrices comportant ZnO sur substrates et procédé de fabrication - Google Patents

Couches électriquement conductrices comportant ZnO sur substrates et procédé de fabrication Download PDF

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Publication number
EP0877099A1
EP0877099A1 EP98105597A EP98105597A EP0877099A1 EP 0877099 A1 EP0877099 A1 EP 0877099A1 EP 98105597 A EP98105597 A EP 98105597A EP 98105597 A EP98105597 A EP 98105597A EP 0877099 A1 EP0877099 A1 EP 0877099A1
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EP
European Patent Office
Prior art keywords
zno
layer
infiltration
sol
ωcm
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.)
Granted
Application number
EP98105597A
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German (de)
English (en)
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EP0877099B1 (fr
Inventor
Lubomir Dr.Rer.Nat. Spanhel
Michael Dip.-Chem. Hilgendorff
Gerd Prof. Dr. Müller
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.)
Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
Original Assignee
Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
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Publication of EP0877099A1 publication Critical patent/EP0877099A1/fr
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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
    • 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
    • C23C18/125—Process of deposition of the inorganic material
    • C23C18/1254—Sol or sol-gel processing
    • 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
    • C23C18/1275—Process of deposition of the inorganic material performed under inert atmosphere

Definitions

  • the invention relates to electrically conductive ZnO containing transparent layers on substrates that in the electronics industry or for various Sensors can be used and a process for their manufacture.
  • the layer thicknesses are between 200 and 1000 nm and the electrical properties are achieved by doping, high manufacturing temperatures or tempering in a vacuum or in a hydrogen atmosphere.
  • nanocrystalline ZnO layers with desired optical and electrical properties could not be produced so far.
  • this object is related to the ZnO layer by the features of claim 1, and in terms of the manufacturing process by the Features of claim 7 solved.
  • optically transparent, nanoporous and electrically conductive ZnO or aluminum-doped ZnO layers are thus proposed for the first time.
  • the great advantage of the layers according to the invention is that they can be produced in a relatively large thickness (from 0.4 to 3 ⁇ m) and that the electrical and optical properties can be influenced favorably by the doping and subsequent infiltration, so that the Layers according to the invention can be used in sensor technology.
  • the layers according to the invention are optically transparent under controlled conditions (T> 90%, 450 nm - 1200 nm) and have specific resistances in the range from ... to ....
  • the invention further relates to a method for Production of layers containing ZnO.
  • the method according to the invention is characterized in that that wet chemical, with a known Sol-Geltechnik made a concentrated ZnO-Sol and with at least one coating step Layer thickness of the dry layer of at least 0.4 ⁇ m is applied.
  • the method according to the invention can be further developed in which Al-doped ZnO layers on various Substrates can be applied.
  • a Zinc alkoxide precursor by base catalyzed hydrolysis synthesized a ZnO sol containing nanoparticles this is preferred by condensation in its concentration is increased.
  • the zinc alkoxide precursor can, for example, by Refluxing zinc acetate can be obtained in alcohol and hydrolysis can be done, for example, with TMAH (Tetramethyl ammonium hydroxide), LiOH, NaOH or KOH be performed.
  • TMAH Tetramethyl ammonium hydroxide
  • Al-doped ZnO layers can be applied in the same way if Al-containing zinc alkoxide precursors are used to synthesize the ZnO sol or if Al (sek-BuO) 3 is added to the ZnO sol. The synthesis takes place until 2-molar ZnO or Al-containing ZnO sols containing nanoparticles are obtained.
  • Additional infiltration can reduce the nanoporosity of the layers produced and thus both the electrical, as well as the optical properties targeted be influenced, so that the possible area of application and in particular expanded that for sensors can be.
  • the procedure is now such that a Zinc alkoxide precursor by refluxing zinc acetate or zinc acetate with some at% aluminum alkoxide in Alcohols, e.g. Ethanol, 1-propanol, 2-propanol, 1-butanol i.a. done in air.
  • Alcohols e.g. Ethanol, 1-propanol, 2-propanol, 1-butanol i.a. done in air.
  • the still wet layer is Temperatures between 200 and 500 ° C, preferably at 300 ° C annealed in air and a transparent Received layer.
  • an aftertreatment can be carried out, the layers being subjected to a thermal treatment in the temperature range between 200 and 500 ° C. in air, in an inert atmosphere (argon) and preferably in reducing atmosphere (H 2 / N 2 mixture).
  • argon inert atmosphere
  • H 2 / N 2 mixture reducing atmosphere
  • the result is optically transparent layers, the smallest specific resistance of which is 4 x 10 -3 ⁇ cm, measured with a 2-point or 4-point DC measurement. It is only through this aftertreatment of the coated substrates, preferably in the reducing atmosphere already described, in combination with the relatively high layer thickness that the unexpectedly large increase in conductivity of the layer or layers produced is achieved.
  • the surface resistance can thus be reduced from above 20 M ⁇ / ⁇ before this thermal post-treatment to values far below 50 ⁇ / ⁇ after the thermal treatment.
  • optical transparent layers T> 90% in the wavelength range between 450 nm to 1200 nm for layer thicknesses to 2 microns can be achieved, as in the in the figure 1 shown diagram for a 1.5 ⁇ m thick Al-doped ZnO layer made after double infiltration and has a sheet resistance of 27 ⁇ / ⁇ , is shown.
  • a 0.65 M zinc alkoxide precursor is synthesized by refluxing Zn (Ac) 2 x 2H 2 O in 1-propanol. With simultaneous heating, hydrolysis takes place with TMAH.
  • the ZnO / Al sol obtained in this way is then cleaned Glass substrate applied with a dip coating, drawing speeds from 20 to 30 cm / min have been observed.
  • the Al-doped ZnO layer obtained in this way is nanoporous and optically transparent and has a layer thickness between 0.8 ⁇ m to 2 ⁇ m.
  • the coated substrate is subsequently immersed over a period of about 5 minutes in a hot 0.1 M zinc alkoxide precursor which contains 2 at% Al (sec-BuO) 3 in order to carry out a first infiltration. Furthermore, taking into account the stoichiometric equilibrium TMAH, the zinc alkoxide precursor was added and after a further approx. 5 min immersion time the substrate was removed from this infiltration solution at a speed of approx. 2.5 cm / min and immediately afterwards over a period of 15 min at a Temperature annealed to 300 ° C in air.
  • TMAH stoichiometric equilibrium
  • the applied optically transparent Al-doped Layer structure showed a sheet resistance above 20 M ⁇ / ⁇ on.
  • a thermal aftertreatment was carried out at 400 ° C. in a reducing forming gas atmosphere (10% H 2 , 90% N 2 ) over a period of approx. 4 h and a specific resistance between 6 ⁇ 10 for the layers treated accordingly -3 ⁇ cm and 4 x 10 -3 ⁇ cm reached.
  • the Al-free ZnO layers have specific resistances of 2 x 10 -1 - 8 x 10 -2 ⁇ cm.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Thermal Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Nanotechnology (AREA)
  • Chemically Coating (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
EP98105597A 1997-05-06 1998-03-27 Procédé de fabrication d'une couche électriquement conductrice comportant ZnO sur un substrat Expired - Lifetime EP0877099B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19719162 1997-05-06
DE19719162A DE19719162C2 (de) 1997-05-06 1997-05-06 Verfahren zur Herstellung einer elektrisch leitenden ZnO enthaltenden Schicht auf einem Substrat

Publications (2)

Publication Number Publication Date
EP0877099A1 true EP0877099A1 (fr) 1998-11-11
EP0877099B1 EP0877099B1 (fr) 2003-07-09

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EP98105597A Expired - Lifetime EP0877099B1 (fr) 1997-05-06 1998-03-27 Procédé de fabrication d'une couche électriquement conductrice comportant ZnO sur un substrat

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EP (1) EP0877099B1 (fr)
DE (2) DE19719162C2 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000026923A1 (fr) * 1998-10-29 2000-05-11 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Materiau electro-conducteur et transparent, son procede de production et son utilisation
DE102005046450A1 (de) * 2005-09-28 2007-04-05 Osram Opto Semiconductors Gmbh Optoelektronischer Halbleiterchip, Verfahren zu dessen Herstellung und optoelektronisches Bauteil
DE102005047168A1 (de) * 2005-09-30 2007-04-12 Osram Opto Semiconductors Gmbh Optoelektronischer Halbleiterchip

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102006023685A1 (de) 2005-09-29 2007-04-05 Osram Opto Semiconductors Gmbh Optoelektronischer Halbleiterchip
DE102015118417A1 (de) * 2015-10-28 2017-05-04 Osram Oled Gmbh Optoelektronisches Bauelement und Verfahren zum Herstellen eines optoelektronischen Bauelements

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0336574A1 (fr) * 1988-04-06 1989-10-11 Imperial Chemical Industries Plc Préparation d'une couche conductrice transparente d'oxyde de zinc
US5252356A (en) * 1991-02-22 1993-10-12 The Honjo Chemical Corporation Method of producing transparent zinc oxide films

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0336574A1 (fr) * 1988-04-06 1989-10-11 Imperial Chemical Industries Plc Préparation d'une couche conductrice transparente d'oxyde de zinc
US5252356A (en) * 1991-02-22 1993-10-12 The Honjo Chemical Corporation Method of producing transparent zinc oxide films

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
DATABASE INSPEC INSTITUTE OF ELECTRICAL ENGINEERS, STEVENAGE, GB; KAMAT P V: "Nanocrystalline semiconductor thin films for microelectronic and optoelectronic applications", XP002071586 *
KAMALASANAN M N ET AL: "SOL-GEL SYNTHESIS OF ZNO THIN FILMS", THIN SOLID FILMS, vol. 288, no. 1/02, 15 November 1996 (1996-11-15), pages 112 - 115, XP000691282 *
MATERIALS TECHNOLOGY, JULY-AUG. 1994, USA, vol. 9, no. 7-8, ISSN 1066-7857, pages 147 - 149 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000026923A1 (fr) * 1998-10-29 2000-05-11 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Materiau electro-conducteur et transparent, son procede de production et son utilisation
DE102005046450A1 (de) * 2005-09-28 2007-04-05 Osram Opto Semiconductors Gmbh Optoelektronischer Halbleiterchip, Verfahren zu dessen Herstellung und optoelektronisches Bauteil
EP1770794A3 (fr) * 2005-09-28 2008-07-09 OSRAM Opto Semiconductors GmbH Puce optoélectronique semiconductrice, procédé de fabrication et dispositif optoélectronique
US7838876B2 (en) 2005-09-28 2010-11-23 Osram Opto Semiconductors Gmbh Optoelectronic semiconductor device in which current spreading layer of sol gel material mixed with nanoparticles is mixed with wavelength conversion dyes
DE102005047168A1 (de) * 2005-09-30 2007-04-12 Osram Opto Semiconductors Gmbh Optoelektronischer Halbleiterchip

Also Published As

Publication number Publication date
DE59808946D1 (de) 2003-08-14
EP0877099B1 (fr) 2003-07-09
DE19719162A1 (de) 1998-11-12
DE19719162C2 (de) 2001-02-08

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