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`9
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`PATENT ABSTRACTS OF JAPAN
`
`(11)Publication number :
`
`2000-026138
`
`(43)Date of publication of application : 25.01.2000
`
`
`(51)Int.Cl.
`
`coac 17/27
`AOIN 59/16
`3010 53/86
`BOIJ 35/02
`3050
`5/00
`B323
`9/00
`003C 17/25
`
`
`
`(21)Application number : 11—118406
`
`(71)App|icant : TOTO LTD
`
`(22)Date of filing :
`
`26.04.1999
`
`'
`
`(72)lnventor : TSUJIMICHI KAZUYA
`HASUO HIROTO
`KOBAYASHI HIDENORI
`SAEKI YOSHIMITSU
`
`(30)Priority
`
`Priority number : 10131179
`
`Priority date : 24.04.1998
`
`Priority country : JP
`
`
`(54) PHOTOCATALYST THIN FILM HAVING DEPOSITED FOULING REMOVAL ACTIVITY,
`LAMINATE AND FORMATION OF THE SAME
`
`(57)Abstract:
`
`PROBLEM TO BE SOLVED: To form the photocatalyst thin film exhibiting excellent fouling
`preventive activity and superior durability by placing a titanium alkoxide solution on the surface
`of a base material and heating the titanium alkoxide to subject it to thermal decomposition and
`polymerization to obtain a titanium oxide thin film formed on the base material.
`SOLUTION: The formation of this photocatalyst thin film comprises: diluting a titanium alkoxide
`preferably such as titanium tetraisopropoxide, with ethanol or the like, to obtain a solution
`having an about 0.5'to 20 wt.% alkoxide concn.; vaporizing this solution to generate a vapor;
`spraying the surface of a base material with the vapor directly or with a gaseous mixture of the
`vapor and an appropriate carrier gas, wherein the surface of the base material is heated to
`about 50 to 600° C beforehand; and subjecting a part or the whole of titanium alkoxide placed
`on the surface of the base material to decomposition and polymerization with heat of the
`surface of the base material to form a titanium oxide thin film. Thus, the objective photocatalyst
`thin film having high smoothness, high hardness, hydrophilicity-enhancing properties effected by
`photoexcitation and organic matter decomposition activity, can be formed on the surface of the
`base material.
`
`
`
`
`LEGAL STATUS
`
`[Date of request for examination]
`
`06.04.2000
`
`[Date of sending the examiner’s decision of
`rejection]
`
`[Kind of final disposal of application other than
`the examiner’s decision of rejection or
`application converted registration]
`
`[Date of final disposal for application]
`
`file://C:¥Documents and Settings¥oonishi¥My Documents¥JPOEn¥JP-A-2000-2...
`
`2007/10/01
`
`a {<
`
`

`

`JP-A-2000-26138
`
`2/10 4’49“: .
`
`[Patent number]
`
`[Date of registration]
`
`3219076
`
`10.08.2001
`
`[Number of appeal against examiner’s decision
`of rejection]
`
`[Date of requesting appeal against examiner’s
`decision of rejection]
`
`[Date of extinction of right]
`* NOTICES *
`
`JPO and INPIT are not responsible for any
`damages caused by the use of this translation.
`
`1.This document has been translated by computer. So the translation may not reflect the original
`precisely.
`2.**** shows the word which can not be translated.
`
`3.In the drawings, any words are not translated.
`
`CLAIMS
`
`[Claim(s)]
`[Claim 1] The adhesion dirt clearance nature photocatalyst thin film characterized by having high
`smooth nature and a degree of hardness, and having the property that a hydrophilic property
`increases by optical pumping. and the resolving power over the organic substance.
`[Claim 2] The adhesion dirt clearance nature photocatalyst thin film according to claim 1
`characterized by the arithmetical mean deviation of profile having smooth 2nm or more nature it
`is [ nature ] 15nm or less in the field of 5 micrometer of the adhesion dirt clearance nature
`photocatalyst thin film front face of said adhesion dirt clearance nature photocatalyst thin film
`around.
`
`[Claim 3] An adhesion dirt clearance nature photocatalyst thin film given in either claim 1
`characterized by discovering the hydrophilic property to which the contact angle of the water of
`the adhesion dirt clearance nature photocatalyst thin film front face which carried out optical
`pumping becomes smaller in [ 5 degree or more ] 30 degrees or less than the contact angle of
`the water in front of optical pumping, and claim 2.
`[Claim 4] An adhesion dirt clearance nature photocatalyst thin film given in either of claim 1 to
`claims 3 to which said adhesion dirt clearance nature photocatalyst thin film is characterized by
`generating active oxygen under existence of oxygen and moisture by optical pumping.
`[Claim 5] An adhesion dirt clearance nature photocatalyst thin film given in either of claim 1 to
`claims 4 characterized by consisting of titanium oxide said whose adhesion dirt clearance nature
`photocatalyst thin film is the semi-conductor oxide which presents a photocatalyst function, tin
`oxide. and at least one oxide of a zinc oxide.
`
`[Claim 6] The adhesion dirt clearance nature photocatalyst thin film according to claim 5
`characterized by for said adhesion dirt clearance nature photocatalyst thin film blending an
`insulator oxide with said semi-conductor oxide, and constituting it.
`[Claim 7] An adhesion dirt clearance nature photocatalyst thin film given in either claim 6
`characterized by for said adhesion dirt clearance nature photocatalyst thin film blending
`transition metals or a transition-metals oxide, and constituting it, and claim 6.
`[Claim 8] An adhesion dirt clearance nature photocatalyst thin film given in either of claims 1-7
`characterized by a photocatalyst particle coming to expose in said adhesion dirt clearance
`nature photocatalyst thin film.
`[Claim 9] The layered product characterized by coming to form said adhesion dirt clearance
`nature photocatalyst thin film given in either of claims 1-8 in a base material front face.
`[Claim 10] The layered product according to claim 9 characterized by having the degree of
`
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`3/10 ’\°—°/°
`
`hardness whose Mohs hardness of the front face of said layered product is four or more.
`[Claim 11] A layered product given in either claim 9 characterized by being the ceramics with
`which the base material of said layered product consists of oxides, such as pottery, such as
`glass and a tile, cement, or precast concrete, and claim 10.
`[Claim 12] The formation approach of a layered product given in either claim 9 characterized by
`** including the process which covers a metal alkoxide on said base material front face, and the
`process which carries out heating baking at this, and claim 11.
`[Claim 13] The formation approach of a layered product given in either claim 9 characterized by
`including the process which carries out preheating so that the temperature on the front face of a
`base material may become 50 degrees C or more beforehand before covering a metal alkoxide on
`said base material front face, and the process heated so that it may be the temperature beyond
`after that and preheating and may become 600 degrees C or less, and claim 11.
`[Claim 14] The formation approach of a layered product given in either claim 9 characterized by
`including the process which covers a metal alkoxide on said base material front face, and the
`process which heat—treats the base material which covered this metal alkoxide under 300-
`degree—C or more temperature ambient atmosphere 700 degrees C or less, and claim 11.
`[Claim 15] The formation approach of a layered product given in either of claims 12-14
`characterized by changing a metal alkoxide to a metallic oxide by heat-treatment of the metal
`alkoxide covered by said base material front face.
`[Claim 16] The formation approach of a layered product given in either of claims 12-15
`characterized by changing a titanium alkoxide to anatase mold titanium oxide by heat-treatment
`of the titanium alkoxide covered by said base material front face.
`
`
`[Translation done]
`
`* NOTICES *
`
`.IPO and INPIT are not responsible for any
`damages caused by the use of
`this translation.
`
`1.This document has been translated by computer. So the translation may not reflect the original
`precisely.
`2.**** shows the word which can not be translated.
`
`3.In the drawings, any words are not translated.
`
`DETAILED DESCRIPTION
`WWW—V“......m..vv......v.,..._.......s..._..ga............,.....«...mwvm«_.m._.............._........~............._..................w~.......,..._._.ww.............»......................,........................,......,...........«.....,...........,..,.,........,,......_..,,.....«........._...,....______
`
`[Detailed Description of the Invention]
`[0001]
`[Field of the Invention] This invention relates to the adhesion dirt clearance nature photocatalyst
`thin film which demonstrates the outstanding antifouling force and endurance, and its
`manufacture approach.
`[0002]
`[Description of the Prior Art] Titanium oxide is widely known as an ingredient excellent in
`photocatalyst activity, and various photocatalyses are known. In recent years, it became clear to
`discover a hydrophilic property with the expensive titanium oxide thin film which carried out
`optical pumping by UV irradiation. The antifouling force in which the titanium oxide thin film
`[ matter / adhering to a titanium oxide thin film front face / dirt / rinsing] easily of being
`removable was expensive was shown using the property.
`[0003] Conventionally, the following approaches have been used as a technique which produces
`the titanium oxide thin film which was equipped with the antifouling force of the above-
`mentioned publication, and was excellent in endurance on a base material front face.
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`file://C:¥Documents and Settings¥oonishi¥My Documents¥JPOEn¥JP-A-2000-2...
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`JP-A-2000-26138
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`4/10 /\°-—°/°~ .
`
`[0004] Homogeneity and a detailed titanium oxide thin film can be produced on a front face by
`applying the titanium oxide sol which distributed the titanium oxide particle to the solvent to the
`base material front face which has a binder layer on a base material front face, and calcinating it
`at elevated temperature about 700 degrees C or more. without burying a titanium oxide particle
`in the interior of a base material or a binder layer. Thus. the produced titanium oxide thin film
`discovers a high hydrophilic property according to a photocatalyst operation of titanium oxide
`under UV irradiation. According to this effectiveness, a titanium oxide thin film demonstrates the
`high antifouling force in which the dirt for organic adhering to that front face is easily removable
`with rinsing.
`[0005] However, since these approaches fixed a spherical titanium oxide particle on a base
`material front face, the opening between particles and the granularity of the front face resulting
`from condensation of particles existed in the front face. For this reason, there was a problem
`that clearance of the dirt matter which entered into surface irregularity was not necessarily
`easy.
`
`[0006] moreover -- in order to fulfill the surface degree of hardness and the pair abrasiveness
`which are required of a ceramic product front face -- a titanium oxide thin film -- elevated
`temperature about 700 degrees C or more -- it is -- in addition -- and there was a problem that
`it was necessary to fix in base materials, such as a ceramic, through a binder layer.
`[0007]
`[Problem(s) to be Solved by the Invention] It is what was made in order that this invention might
`solve the above-mentioned technical problem. The object of this invention More whenever
`[ stoving temperature / which immobilization takes ], setting fixing a photocatalyst thin film on a
`base material front face, and maintaining the resolving power over about the same degree of
`hardness as the conventional technique, buildup of the hydrophilic property by UV irradiation,
`and the organic substance at low temperature a binder layer -- not needing -- in addition -- and
`it is in offering the higher adhesion dirt clearance nature photocatalyst thin film and its
`manufacture approach of smooth nature.
`[0008]
`[Means for Solving the Problem] The solution which contains the titanium alkoxide which is a
`kind of a metal alkoxide as a result of repeating research, in order to solve the above-mentioned
`technical problem is used as a film production raw material. Arrange it in a base material front
`face, and a titanium alkoxide with the heat on the front face of a base material, or the heat by
`low-temperature heat-treatment of a base material a pyrolysis and by carrying out a
`polymerization (dealcoholization reaction) and forming a titanium oxide thin film in a base material
`front face More whenever [ stoving temperature / which immobilization takes ] maintaining the
`resolving power over about the same degree of hardness as the conventional technique, buildup
`of the hydrophilic property by UV irradiation, and the organic substance at low temperature a
`binder layer -- not needing -- in addition -- and since [ of smooth nature ] it is higher, the high
`adhesion dirt clearance nature' photocatalyst thin film and its manufacture approach of the
`antifouling property that it is rare for the dirt matter to enter into surface irregularity are found
`out, and it came to make this invention.
`[0009] As a titanium alkoxide used for this invention, it is Ti-(OR) 4. (R expresses an alkyl group
`here) Although either is usable if expressed with a chemical formula, it is desirable to use
`especially titanium tetraisopropoxide.
`[0010] The organic solvent which it is also possible to dilute and use it for a solvent, and a
`titanium alkoxide and compatibility are good as a solvent [ as opposed to a titanium alkoxide in
`this case ], and does not hydrolyze a titanium alkoxide can use the titanium alkoxide used for
`this invention. Especially ethanol, isopropanol, and isobutanol are desirable.
`[0011] Although especially the concentration to the solvent of a titanium alkoxide used for this
`invention is not limited, its 0.5 - 20 % of the weight is desirable.
`[0012] What added other metal alkoxides can be used for the titanium alkoxide solution diluted to
`the solvent as a film production raw material used for this invention. In this case, as for the
`metal alkoxide kind to add, what has a good titanium alkoxide and compatibility is desirable. As
`such a metal alkoxide, the alt.silicic-acid tetraethyl which is a kind of a silicon alkoxide is
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`5/10 ,\°_:;
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`mentioned.
`
`[0013] It is especially suitable, in order not to spoil the shape of surface type of a base material
`after film production as an approach of arranging the metal alkoxide of this invention in a base
`material front face if the chemical vapor deposition which sprays the steam of a metal alkoxide
`on a base material front face is used although what kind of approach may be used.
`[0014] With the chemical vapor deposition which sprays the steam of said metal alkoxide on a
`base material front face, when a titanium alkoxide is used as a metal alkoxide kind, more
`
`specifically, the following approaches are taken. It carries out by spraying on a base material
`what mixed with direct or carrier gas the steam generated by evaporation of the solution
`containing a titanium alkoxide. Moreover, the approach of spraying the thing which the drop of a
`titanium alkoxide was sent [ thing] in into carrier gas with the sufficiently large rate of flow, and
`made it evaporating as a simpler approach using the equipment of an atomizing process on a
`base material can be used. Also in which approach, it is desirable to heat the solution containing
`a titanium alkoxide and to raise the vapor pressure so that evaporation of a titanium alkoxide
`may be performed promptly.
`[0015] By the approach of said publication, after arranging the solution containing a titanium
`alkoxide in a base material front face by approaches, such as chemical vapor deposition, one of
`the approaches of of (a) of a publication and (b) or both can be suitably chosen below as an
`approach of forming a titanium oxide thin film in a base material front face. By these approaches,
`inclusion of a binder layer may not be needed for an anatase mold titanium oxide thin film with
`high smooth nature and a high degree of hardness on a base material. (a) How to heat the base
`material front face beforehand, so that the skin temperature may become 50-600 degrees C. to
`decompose, make carry out the polymerization of all the titanium all [ a part or ] arranged in the
`base material front face with the heat on the front face of a base material, and form a titanium
`
`oxide thin film in a base material front face, before arranging the solution containing a titanium
`alkoxide in a base material front face by approaches, such as said chemical vapor deposition. (b)
`They are a pyrolysis and the approach of making carry out a polymerization and'forming a
`titanium oxide thin film in a base material front face in all the titanium all [ a part or] that heat-
`treated the base material which arranged the solution containing a titanium alkoxide in the base
`material front face by approaches, such as said chemical vapor deposition, under the 300-600-
`degree C temperature environment, and was arranged in the base material front face.
`[0016] The thin film with which the semi-conductor oxide particle and the insulator oxide were
`intermingled can be formed in a base material front face by using as a film production raw
`material the solution which mixed the alkoxide of the metal kind of a semi-conductor oxide and
`
`an insulator oxide, and using the film production approach of the above—mentioned publication
`for production of the adhesion dirt clearance nature photocatalyst thin film blended and equipped
`
`with both semi-conductor oxide and insulator oxides, such as titanium oxide, (refer to drawing
`1 ). thus, although it comes out not to mention maintaining the photocatalyst property of a semi-
`conductor oxide since the semi-conductor oxide and the insulator oxide have exposed both the
`produced thin films to a front face, many chemical properties of an insulator oxide can be further
`given to a front face. Moreover, it is also possible by arranging the alkoxide of the metal kind of a
`semi-conductor oxide, and the alkoxide of the metal kind of an insulator oxide in a front face by
`turns, and forming the target oxide thin film by heat-treatment to form a semi-conductor oxide
`thin film and an insulator oxide thin film on a base material front face in the shape of a layer
`(refer to drawingg ). In this case, the count of formation of an oxide and the formation sequence
`
`of an oxide are not limited. Thus, an example of the produced thin film is shown in drawing_2 . As
`
`shown in drawing__2_ , when the good insulator oxide layer of adhesion is prepared for said both
`and chemistry target at the interface of a base material and a semi-conductor oxide layer, it
`becomes possible to prepare a semi—conductor oxide layer firmly by the base material top.
`Moreover, the diffusion to the semi-conductor oxide layer of the element which constitutes a
`base material by the insulator oxide layer is controlled, and many properties of a semi-conductor
`oxide are maintained.
`
`[0017] By equipping the adhesion dirt clearance nature photocatalyst thin film of this invention
`with transition metals, the resolving power over the bigger organic substance can also be given
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`6/10 /\°—’~‘} ,
`
`to an adhesion dirt clearance nature photocatalyst thin film. Spreading and UV irradiation are
`performed for the solution with which the ion of said transition metals is