WO2008046588A1 - procédé de quantification de l'activité photocatalytique de surfaces et utilisation du procédé - Google Patents

procédé de quantification de l'activité photocatalytique de surfaces et utilisation du procédé Download PDF

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Publication number
WO2008046588A1
WO2008046588A1 PCT/EP2007/008973 EP2007008973W WO2008046588A1 WO 2008046588 A1 WO2008046588 A1 WO 2008046588A1 EP 2007008973 W EP2007008973 W EP 2007008973W WO 2008046588 A1 WO2008046588 A1 WO 2008046588A1
Authority
WO
WIPO (PCT)
Prior art keywords
mbar
substrate
organic
layer
photocatalytic
Prior art date
Application number
PCT/EP2007/008973
Other languages
German (de)
English (en)
Inventor
Thomas Neubert
Frank Neumann
Michael Vergöhl
Original Assignee
Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V.
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 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. filed Critical Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V.
Priority to EP07819041A priority Critical patent/EP2080011A1/fr
Priority to JP2009532716A priority patent/JP5043118B2/ja
Publication of WO2008046588A1 publication Critical patent/WO2008046588A1/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/47—Scattering, i.e. diffuse reflection
    • G01N21/4738—Diffuse reflection, e.g. also for testing fluids, fibrous materials
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/8422—Investigating thin films, e.g. matrix isolation method

Definitions

  • the invention describes a quantifying measuring method for measuring the photocatalytic activity of surfaces.
  • a thin stearic acid layer is vapor-deposited onto the photocatalytic surface to be measured.
  • the measurement of the photocatalytic degradation reaction with an organic test substance is already at a standstill of the technique.
  • the organic test substance can be present as gas, liquid or solid layer on the photocatalytic substrate.
  • the degradation reaction is analyzed by quantitative analysis of the chemical degradation products. This requires appropriate know-how for chemical analysis as well as cost-intensive equipment (gas chromatographs, infrared spectrometers, etc.).
  • an organic test substance In order to be able to measure a photocatalytic degradation reaction in a practical manner, an organic test substance must first be applied to the surface to be measured. The quality of the measurement is closely linked to the homogeneity of the applied test substance layer. In principle, the larger and more homogeneous the test substance can be applied, the more reproducible and more accurate are the measurement results.
  • the organic test substance methyl stearate, stearic acid, etc.
  • the organic solvent e.g., hexane
  • DE 10 2004 027 118 A1 discloses a method for the quantitative determination of the photocatalytic degradation of organic dyes on photocatalytically active surfaces by means of fluorescence analysis.
  • the object of the present invention is to specify a simple measuring method which makes possible an efficient, economical and accurate determination of the photocatalytic activity of a substrate.
  • a method for quantifying the photocatalytic activity of a surface of a substrate in which a thermally vapor deposited layer in direct contact with the surface of the substrate containing at least one light scattering organic compound is irradiated with short wavelength electromagnetic radiation and by optical measurement methods the time course of the decrease in the amount of the compound caused by photocatalytic degradation is determined.
  • test substance layers (stearic acid) to be applied very homogeneously over a surface area of several square centimeters.
  • the layer thickness and the coated surface can be freely selected over a large area. • The application is simple, reproducible and requires only a small technical effort.
  • the layer containing at least one light-scattering organic compound is vapor-deposited directly onto the surface of the substrate.
  • An alternative embodiment of the method provides that the layer is applied to a further, for electromagnetic radiation in the optical measuring method at least partially transparent substrate and this further substrate is brought into contact with the coated surface of the substrate to be measured.
  • the contact can be non-positive and / or positive.
  • the stearic acid can be evaporated on a UV-transparent quartz glass substrate, wel The coated side is placed on a photocatalytically active surface. The degradation reaction can be measured here by scattered light measurements of the reflected light.
  • the measuring method can also be used for smooth substrates, which can not be directly coated with stearic acid (built-in photocatalytic product, products with too large dimensions).
  • the vapor deposition under reduced pressure of between 10 -6 mbar and 10 mbar is preferably carried out between 10 -3 mbar and 1 mbar, more preferably between 10 -3 mbar and 10 "1 mbar.
  • the organic compound is preferably selected from the group consisting of vaporizable organic compounds and / or organic fatty acids and their derivatives.
  • derivatives are understood as meaning inorganic and / or organic fatty acid derivatives. These include, for example, esters, ethers and / or salts.
  • any known organic fatty acid can be used for the process.
  • the fatty acid is selected from the saturated, monounsaturated and / or polyunsaturated fatty acids.
  • stearic acid and / or methyl stearate are biologically completely harmless and very inexpensive.
  • the layer thickness produced in the process does not play an essential role in carrying out the process, but preferably a coating is produced which has a thickness of from 1 to 1000 nm, preferably from 50 to 300 nm.
  • the irradiation of the coating takes place over a period of 1 minute to 48 hours, preferably from 10 minutes to 12 hours, particularly preferably from 30 minutes to 6 hours.
  • the irradiation may be continuous, i. throughout the period, but it is also possible to perform the irradiation at intervals.
  • the measurement of the decrease in the amount of the applied compound can be carried out simultaneously with the irradiation, but also after completion of irradiation and / or in the breaks, if the irradiation is carried out at intervals.
  • UV light is preferably used during the irradiation, in particular radiation having a wavelength between 100 nm and 800 nm, preferably 300 nm and 500 nm, particularly preferably between 360 nm and 420 nm.
  • the coating is irradiated on the substrate, the only factor being that the irradiation takes place with a sufficiently high power, so that the most efficient degradation of the organic substance takes place.
  • the irradiation is applied in an intensity of 0.1 mW / cm 2 to 10 mW / cm 2 inclusive, preferably from 0.5 mW / cm 2 to 5 mW inclusive / cm 2 , more preferably from 0.8 mW / cm 2 to 1.5 mW / cm 2 takes place.
  • the determination of the residual amount is carried out with optical measurement methods in the visible and / or infrared spectral range.
  • the optical measurement methods are selected from the group consisting of determination of the absorption, fluorescence, spectral lipometry and / or scattered light measurement.
  • the scattered light measurement is preferred.
  • a further light source may be used, but in particular when determining the residual amount via fluorescence, the UV light source used in the irradiation may be the only light source required for carrying out the method, which in this case is another advantageous simplification of the experimental setup leads.
  • the method is suitable for quantifying the photocatalytic activity of substrates.
  • the substrates are selected from the group consisting of support structures which are coated with TiO 2 , ZnO, SrTiO 3 , and / or K 4 NbO 7 , glass, ceramics, metal, plastics, wood and / or paper.
  • the method finds use for the analytical observation of optical changes of organic layers as a result of chemical reactions, eg oxidation and / or crystallization.
  • a substrate 1 which is fixed on a fixing device 2, introduced into a coating chamber 3, to which a reduced pressure can be applied via a vacuum port 4.
  • the coating chamber 3 has a heating device 5.
  • the heater can be made electrically and heated by a transformer 7.
  • a crucible 8 with the organic compound used in this case, stearic acid is brought into thermal contact with the heating device.
  • the organic compound eg stearic acid
  • the boiling point of the organic compound is thereby lowered.
  • Crucible and heater should be such that the heat radiation emitted by this is minimal and the evaporation temperature of the organic test substance can be achieved very quickly.
  • the organic compound is then precipitated on the cool substrate by condensation / resublimation processes as a homogeneous layer with a uniform thickness. Processes that work with dissolved organic substances do not produce such a layer.
  • irradiation is carried out with a UV lamp having a defined spectrum (as narrow as possible) and known intensity (eg UVA at 366 nm and 1.0 mW / cm 2 ).
  • the measurement of the layer quantity of the test substance is carried out using suitable optical measuring methods. These can be measurements of the absorption in the visible and in the infrared spectral range as well as measurements of the fluorescence or by means of spectral ellipsometry.
  • optical scattered light measurements haze
  • these correlation are performed.
  • H ( ⁇ ) H max - (H max -H substrate ) 'exp (-B' ⁇ ) (Eq. 1)
  • a photocatalytic activity PA as a number N mo ieküi the destroyed stearic acid molecules per area A 7 radiation intensity ⁇ and time t. This can be determined by Equation 4 r from the degradation rate D / of the radiation intensity ⁇ and the molecular mass m e i mo Kuei of stearic acid.
  • equation 5 can be used to determine a quantum efficiency Q, which is defined as the number of destroyed bonds per incident photon ,

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  • Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Mathematical Physics (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
  • Catalysts (AREA)

Abstract

L'invention concerne un procédé de mesure de quantification qui permet de mesurer l'activité photocatalytique de surfaces. On vaporise une mince couche d'acide stéarique sur la surface photocatalytique à mesurer. La surface est ensuite irradiée par de la lumière UV et la partie de la lumière diffusée par la couche d'acide stéarique (= voile optique) est mesurée à des intervalles de temps définis. Si la surface est photocatalytique, la couche d'acide stéarique se décompose sans laisser de résidus de sorte que le voile optique descende jusqu'à la valeur de la surface non revêtue. A partir de l'évolution de la courbe du voile optique en fonction du temps, on peut alors déterminer quantitativement l'activité photocatalytique de la surface.
PCT/EP2007/008973 2006-10-17 2007-10-16 procédé de quantification de l'activité photocatalytique de surfaces et utilisation du procédé WO2008046588A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP07819041A EP2080011A1 (fr) 2006-10-17 2007-10-16 Procédé de quantification de l'activité photocatalytique de surfaces et utilisation du procédé
JP2009532716A JP5043118B2 (ja) 2006-10-17 2007-10-16 表面の光触媒活性を定量化する方法およびその使用

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE200610049009 DE102006049009B3 (de) 2006-10-17 2006-10-17 Verfahren zur Quantifizierung der photokatalytischen Aktivität von Oberflächen und dessen Verwendung
DE102006049009.6 2006-10-17

Publications (1)

Publication Number Publication Date
WO2008046588A1 true WO2008046588A1 (fr) 2008-04-24

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2007/008973 WO2008046588A1 (fr) 2006-10-17 2007-10-16 procédé de quantification de l'activité photocatalytique de surfaces et utilisation du procédé

Country Status (4)

Country Link
EP (1) EP2080011A1 (fr)
JP (1) JP5043118B2 (fr)
DE (1) DE102006049009B3 (fr)
WO (1) WO2008046588A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2286916A1 (fr) * 2009-08-13 2011-02-23 Technische Universität Braunschweig Procédé et utilisation de liaisons luminescentes pour la mesure d'une activité de surface photocatalytique

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009000293A1 (fr) 2007-06-25 2008-12-31 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Appareil de mesure et procédé de détermination des caractéristiques optiques pour la détection de réactions de décomposition photochimiques et électrochimiques
DE102009032608A1 (de) 2009-07-10 2011-01-20 Erdinger, Lothar, Priv.-Doz. Dr. Verfahren und Vorrichtung zur Messung der photokatalytischen Aktivität einer Probe
DE102010014632A1 (de) 2010-04-12 2011-10-13 Lothar Erdinger Verfahren und Vorrichtung zur Bestimmung der photokatalytischen Aktivität photokatalytisch aktiver Substanzen
KR102088244B1 (ko) 2018-02-05 2020-03-12 고려대학교 산학협력단 무전력 화학물질 감지센서 및 센싱방법

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004027118A1 (de) * 2004-06-03 2005-12-29 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Verfahren zum Nachweis des photokatalytischen Abbaus organischer Farbstoffe mittels Fluoreszenzanalyse
DE102005003878B3 (de) * 2005-01-24 2006-07-13 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Messvorrichtung zum Messen photokatalytischer Aktivität einer photokatalytischen Schicht

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JP3595996B2 (ja) * 1998-10-01 2004-12-02 株式会社豊田中央研究所 光触媒組成物及びその製造方法
JP2000162129A (ja) * 1998-11-30 2000-06-16 Shinku Riko Kk 光触媒機能評価方法及び評価装置

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004027118A1 (de) * 2004-06-03 2005-12-29 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Verfahren zum Nachweis des photokatalytischen Abbaus organischer Farbstoffe mittels Fluoreszenzanalyse
DE102005003878B3 (de) * 2005-01-24 2006-07-13 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Messvorrichtung zum Messen photokatalytischer Aktivität einer photokatalytischen Schicht

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
MILLS ET AL: "Simultaneous monitoring of the destruction of stearic acid and generation of carbon dioxide by self-cleaning semiconductor photocatalytic films", JOURNAL OF PHOTOCHEMISTRY AND PHOTOBIOLOGY, A: CHEMISTRY, ELSEVIER SEQUOIA, LAUSANNE, CH, vol. 182, no. 2, 31 August 2006 (2006-08-31), pages 181 - 186, XP005574986, ISSN: 1010-6030 *
See also references of EP2080011A1 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2286916A1 (fr) * 2009-08-13 2011-02-23 Technische Universität Braunschweig Procédé et utilisation de liaisons luminescentes pour la mesure d'une activité de surface photocatalytique

Also Published As

Publication number Publication date
DE102006049009B3 (de) 2008-06-05
EP2080011A1 (fr) 2009-07-22
JP2010507077A (ja) 2010-03-04
JP5043118B2 (ja) 2012-10-10

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