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WO2008145098A2 - PROCÉDÉ DE GRAVURE CHIMIQUE EN MILIEU HUMIDE SUR COUCHES MINCES DE TiO2 ET SUR PARTICULES DE TiO2, ET AGENT DE GRAVURE CHIMIQUE - Google Patents

PROCÉDÉ DE GRAVURE CHIMIQUE EN MILIEU HUMIDE SUR COUCHES MINCES DE TiO2 ET SUR PARTICULES DE TiO2, ET AGENT DE GRAVURE CHIMIQUE Download PDF

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Publication number
WO2008145098A2
WO2008145098A2 PCT/DE2008/000875 DE2008000875W WO2008145098A2 WO 2008145098 A2 WO2008145098 A2 WO 2008145098A2 DE 2008000875 W DE2008000875 W DE 2008000875W WO 2008145098 A2 WO2008145098 A2 WO 2008145098A2
Authority
WO
WIPO (PCT)
Prior art keywords
tio
particles
concentration
etching
etchant
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/DE2008/000875
Other languages
German (de)
English (en)
Other versions
WO2008145098A3 (fr
Inventor
Abdelhak Belaidi
Thomas Dittrich
Martha Christina Lux-Steiner
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.)
Helmholtz Zentrum Berlin fuer Materialien und Energie GmbH
Original Assignee
Helmholtz Zentrum Berlin fuer Materialien und Energie GmbH
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 Helmholtz Zentrum Berlin fuer Materialien und Energie GmbH filed Critical Helmholtz Zentrum Berlin fuer Materialien und Energie GmbH
Priority to EP08758115A priority Critical patent/EP2164813A2/fr
Publication of WO2008145098A2 publication Critical patent/WO2008145098A2/fr
Publication of WO2008145098A3 publication Critical patent/WO2008145098A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • 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
    • C03C17/245—Oxides by deposition from the vapour phase
    • C03C17/2456—Coating containing TiO2
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • 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
    • C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
    • 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
    • C03C17/256—Coating containing TiO2
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K13/00—Etching, surface-brightening or pickling compositions
    • C09K13/02—Etching, surface-brightening or pickling compositions containing an alkali metal hydroxide
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/20—Light-sensitive devices
    • H01G9/2027—Light-sensitive devices comprising an oxide semiconductor electrode
    • H01G9/2031—Light-sensitive devices comprising an oxide semiconductor electrode comprising titanium oxide, e.g. TiO2
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • 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
    • C03C2217/21—Oxides
    • C03C2217/212—TiO2
    • 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
    • C03C2218/328—Partly or completely removing a coating
    • C03C2218/33—Partly or completely removing a coating by etching
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/542—Dye sensitized solar cells

Definitions

  • the invention relates to a method for wet-chemical etching of TiO 2 thin films and TiO 2 particles and an etchant.
  • TiO 2 thin films have become increasingly important due to their applicability in photovoltaics, sensors and biomedicine.
  • TiO 2 thin films In order to produce defined TiO 2 thin films for a specific application, the TiO 2 thin films produced by known processes are often subjected to a wet-chemical process. It must be remembered that TiO 2 is one of the most stable materials and insoluble in most acids and also in basic solutions.
  • H 2 SO 4 is used in the photoelectrochemical etching of TiO 2 electrodes.
  • n-TiO 2 electrodes in H 2 SO 4 exposed during a voltage cycle exhibit increased photocurrent and increased intensity of photoluminescence. It is stated that during the etching process in H 2 SO 4 a large number of micropores are formed on the electrode surface, whereby an active n-TiO 2 surface is formed.
  • Thin film or a reduction of the particle size allows and no toxic and readily degradable etching products arise.
  • the object is achieved by a method according to claim 1, comprising the method steps producing an etchant having a pH> 13, containing an alkali in a concentration of> 0.1 mol, selected from the liquors NH 4 OH, NaOH, KOH or mixtures of these, and H 2 O 2 in low concentration compared to the lye concentration, setting a temperature equal to or greater than room temperature, immersing the TiO 2 thin-films or particles in the etchant and lingering the layers or particles as a function of the temperature and composition of the etchant, taking out the etched TiO 2 films, rinsing with distilled water and drying, or according to claim 3, comprising the steps of immersing the TiO 2 films in a liquor having a concentration> 0 , 1 mol and a temperature equal to or greater than room temperature, wherein the liquor is selected from NH 4 OH, NaOH, KOH or mixtures thereof, and adding H 2 O 2 in a low concentration compared to the lye concentration in such an amount
  • H 2 O 2 is added to maintain the initial composition of the etchant during the etching process. Namely, it has been found that H 2 O 2 is consumed during the etching process and then the etching process stops.
  • H 2 O 2 is used in a concentration of about 1 mmol, the residence time of the TiO 2 thin films to be etched in the etchant is up to 60 min.
  • the etchant according to the invention contains an alkali with a concentration> 0.1 mol and H 2 O 2 with a low concentration compared to the lye concentration and has a pH> 13, wherein the lye is selected from NH 4 OH, NaOH or KOH or Mixtures thereof.
  • the concentration of H 2 O 2 is about 1 mmol.
  • FIGS. 1 to 8 show SEM images of TiO 2 thin layers in different etching stages, see above
  • FIG. 1 the surface of an untreated TiO 2 thin film
  • FIG. 2 this untreated TiO 2 thin film in cross section
  • FIG. 3 the surface of a TiO 2 thin film after 10 minutes etching
  • FIG. 4 etched for 10 minutes TiO 2 thin film in cross section
  • FIG. 5 shows the surface of a TiO 2 thin film after 20 min etching
  • Figure 6 by the surface of a TiO 2 thin film. this 20 min etched TiO 2 thin film in cross section
  • FIG. 8 the surface of this TiO 2 thin film etched for 40 min and then treated with HCl.
  • Fig. 9 is a graph showing the dependence of the thickness of the TiO 2 thin film on the etching time.
  • the TiO 2 thin film on which the exemplary embodiment is based was produced on an FTO glass substrate (F: SnO 2 -coated glass) by immersing this substrate in tetraisopropyl orthotitanate dissolved in isopropanol. The resulting thin film was sintered at 500 ° C. for 2 hours.
  • the TiO 2 thin film consists of nanoparticles with a diameter of approx. 20 nm.
  • Fig. 1 shows the SEM image of the untreated surface of the TiO 2 thin film produced and Fig. 2 of this surface in cross section. It can be seen that the TiO 2 thin film completely covers the FTO glass substrate and is relatively flat. From the cross-sectional image a layer thickness of 250 nm could be determined.
  • H 2 O 2 hydrogen peroxide
  • sodium hydroxide solution having a concentration of 8 mol
  • the TiO 2 thin film is immersed.
  • H 2 O 2 was recognized to be very important because the process stops as soon as H 2 O 2 is consumed by the reactions taking place. If H 2 O 2 is supplied again, the reaction starts again.
  • FIG. 3 and 4 now show the corresponding SEM images of the 10 min etched TiO 2 thin film. It can be seen that the roughness has increased and holes have emerged. However, these changes are not distributed homogeneously in the surface. It was found that less rough areas occurred where the FTO glass substrate underlying the TiO 2 thin film has large crystal grains. A change in the size of the nanoparticles in the TiO 2 layer could not be determined.
  • FIG. 4 shows a decrease in the thickness of the TiO 2 thin layer, which is only 123 nm here. After 20 minutes etching time, the FTO grains are already visible on the surface (see Fig. 5 and 6), other areas of the surface of the treated TiO 2 - thin film are further covered with TiO 2 , whose thickness is now about 50 nm.
  • TiO 2 thin-film sample is etched for 40 minutes, only a few areas of the surface of the treated TiO 2 thin film are covered with TiO 2 (see FIG. That is, during the etching process, the morphology of the TiO 2 thin film has changed. The TiO 2 thin film is even completely destroyed by immersion in a 1 mol HCL solution, as can be seen in Fig. 8.
  • FIG. 9 is a graph showing the reduction of the thickness of the TiO 2 thin film with the etching time. It can be seen that no linear dependence could be observed.
  • the dissolution rate of TiO 2 can reach 10 nm / min. The curve was measured with the parameters given above. A change in concentration and temperature causes - as is well known to those skilled in the art - a change in the etching rate and thus a different removal in the thickness.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Power Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • ing And Chemical Polishing (AREA)

Abstract

La présente invention concerne un procédé et un agent de gravure pour gravure chimique en milieu humide de couches minces et de particules de TiO2, permettant un enlèvement défini de matière de la couche mince de TiO2, voire une diminution de calibre particulaire. Le procédé comporte plusieurs opérations. On commence par confectionner un agent de gravure d'un pH supérieur à 13 et contenant à une concentration supérieure à 0,1 mole une base prise dans le groupe NH4OH, NaOH et KOH ou l'un de leurs mélanges, et H2O2 à une concentration inférieure à celle de la base. On établit une température qui ne soit pas inférieure à la température ambiante. On plonge les couches minces ou les particules de TiO2 dans l'agent de gravure et on les y laisse tremper pendant une durée qui est fonction de la température et de la composition de l'agent de gravure. On retire du bain de gravure les couches minces ou les particules de TiO2 gravées. On les rince à l'eau distillée et on les fait sécher. Pour conserver la composition initiale de l'agent de gravure, on ajoute du H2O2 pendant le traitement de gravure.
PCT/DE2008/000875 2007-05-30 2008-05-23 PROCÉDÉ DE GRAVURE CHIMIQUE EN MILIEU HUMIDE SUR COUCHES MINCES DE TiO2 ET SUR PARTICULES DE TiO2, ET AGENT DE GRAVURE CHIMIQUE Ceased WO2008145098A2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP08758115A EP2164813A2 (fr) 2007-05-30 2008-05-23 PROCÉDÉ DE GRAVURE CHIMIQUE EN MILIEU HUMIDE SUR COUCHES MINCES DE TiO2 ET SUR PARTICULES DE TiO2, ET AGENT DE GRAVURE CHIMIQUE

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE200710025136 DE102007025136A1 (de) 2007-05-30 2007-05-30 Verfahren zum nasschemischen Ätzenvon TiO2-Dünnschichten und TiO2-Partikeln sowie Ätzmittel
DE102007025136.1 2007-05-30

Publications (2)

Publication Number Publication Date
WO2008145098A2 true WO2008145098A2 (fr) 2008-12-04
WO2008145098A3 WO2008145098A3 (fr) 2009-02-12

Family

ID=39941784

Family Applications (1)

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PCT/DE2008/000875 Ceased WO2008145098A2 (fr) 2007-05-30 2008-05-23 PROCÉDÉ DE GRAVURE CHIMIQUE EN MILIEU HUMIDE SUR COUCHES MINCES DE TiO2 ET SUR PARTICULES DE TiO2, ET AGENT DE GRAVURE CHIMIQUE

Country Status (3)

Country Link
EP (1) EP2164813A2 (fr)
DE (1) DE102007025136A1 (fr)
WO (1) WO2008145098A2 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013010612A1 (fr) * 2011-07-18 2013-01-24 Merck Patent Gmbh Formation de structures sur des couches antistatiques et anti-réfléchissantes et sur des couches empilées correspondantes

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4110595C1 (en) 1991-04-02 1992-11-26 Thyssen Edelstahlwerke Ag, 4000 Duesseldorf, De Wet-chemical removal of hard coatings from workpiece surfaces - comprises using hydrogen peroxide soln. stabilised by complex former e.g. potassium-sodium tartrate-tetra:hydrate
DE4339502C2 (de) 1993-11-24 1999-02-25 Thoene Carl Stefan Entschichtungslösung zum naßchemischen Entfernen von Hartstoffschichten und Verfahren zu deren Anwendung

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FR2334770A1 (fr) * 1975-12-09 1977-07-08 Radiotechnique Compelec Procede d'attaque d'une couche metallique oxydable servant de masque de photogravure
US5223081A (en) * 1991-07-03 1993-06-29 Doan Trung T Method for roughening a silicon or polysilicon surface for a semiconductor substrate
JPH0710606A (ja) * 1993-06-29 1995-01-13 Asahi Glass Co Ltd 熱線反射ガラスのエッチング方法
NL1014360C2 (nl) * 2000-02-11 2001-08-16 Weterings B V H Ruit, voorzien van een aanslag en/of aantasting tegengaande bekleding alsmede werkwijze voor het vervaardigen daarvan.
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KR100624089B1 (ko) * 2005-07-12 2006-09-15 삼성전자주식회사 패턴 형성 방법, 이를 이용한 다중게이트 산화막 및 플래쉬메모리 셀의 제조 방법

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4110595C1 (en) 1991-04-02 1992-11-26 Thyssen Edelstahlwerke Ag, 4000 Duesseldorf, De Wet-chemical removal of hard coatings from workpiece surfaces - comprises using hydrogen peroxide soln. stabilised by complex former e.g. potassium-sodium tartrate-tetra:hydrate
DE4339502C2 (de) 1993-11-24 1999-02-25 Thoene Carl Stefan Entschichtungslösung zum naßchemischen Entfernen von Hartstoffschichten und Verfahren zu deren Anwendung

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JOURNAL OF SOL-GEL SCIENCE AND TECHNOLOGY, vol. 10, 1997, pages 193 - 202
See also references of EP2164813A2
WIE IN COLLOIDS AND SURFACES A: PHYSICOCHEM. ENG. ASPECTS, vol. 241, 2004, pages 173 - 183

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013010612A1 (fr) * 2011-07-18 2013-01-24 Merck Patent Gmbh Formation de structures sur des couches antistatiques et anti-réfléchissantes et sur des couches empilées correspondantes
CN103688600A (zh) * 2011-07-18 2014-03-26 默克专利股份有限公司 抗静电和抗反射涂层及相应的堆叠层的结构化
US20140166613A1 (en) * 2011-07-18 2014-06-19 Merck Patent Gmbh Structuring of antistatic and antireflection coatings and of corresponding stacked layers

Also Published As

Publication number Publication date
WO2008145098A3 (fr) 2009-02-12
DE102007025136A1 (de) 2008-12-11
EP2164813A2 (fr) 2010-03-24

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