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WO2017014083A1 - Film fonctionnel et dispositif électronique le comportant - Google Patents

Film fonctionnel et dispositif électronique le comportant Download PDF

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Publication number
WO2017014083A1
WO2017014083A1 PCT/JP2016/070392 JP2016070392W WO2017014083A1 WO 2017014083 A1 WO2017014083 A1 WO 2017014083A1 JP 2016070392 W JP2016070392 W JP 2016070392W WO 2017014083 A1 WO2017014083 A1 WO 2017014083A1
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WIPO (PCT)
Prior art keywords
containing layer
layer
metal
transition metal
functional film
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Ceased
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PCT/JP2016/070392
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English (en)
Japanese (ja)
Inventor
千代子 竹村
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.)
Konica Minolta Inc
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Konica Minolta Inc
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Filing date
Publication date
Application filed by Konica Minolta Inc filed Critical Konica Minolta Inc
Publication of WO2017014083A1 publication Critical patent/WO2017014083A1/fr
Anticipated expiration legal-status Critical
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin

Definitions

  • Quantum dots are vulnerable to water and oxygen, so they are used by dispersing them in a curable resin such as epoxy resin or acrylic resin.
  • the quantum dot (QD) -containing resin layer should be laminated with two gas barrier films.
  • a method for producing a QD sheet that is more resistant to water and oxygen is generally known (for example, see Patent Document 1).
  • the functional film of the present invention can obtain higher adhesion and gas barrier property improving effects between the transition metal (M1) -containing layer and the organosilicon compound-containing layer. This is presumed to be because a stronger bond is likely to be formed between the transition metal (M1) (preferably a transition metal of Group 5-11, particularly preferably Nb of Group 5) and Si.
  • M1 transition metal of Group 5-11, particularly preferably Nb of Group 5
  • aminosilane compound examples include 3-aminopropyltrimethoxysilane, 3-aminopropyldimethylethoxysilane, 3-arylaminopropyltrimethoxysilane, propylethylenediaminesilane, N- [3- (trimethoxysilyl) propyl] ethylenediamine, 3 -Butylaminopropyltrimethylsilane, 3-dimethylaminopropyldiethoxymethylsilane, 2- (2-aminoethylthioethyl) triethoxysilane, bis (butylamino) dimethylsilane, and the like.
  • the content of polysilazane in the metal (M2) -containing layer before the modification treatment may be 100% by mass when the total mass of the metal (M2) -containing layer is 100% by mass.
  • the polysilazane content in the layer is preferably in the range of 10 to 99% by mass, and in the range of 40 to 95% by mass. More preferably, it is in the range of 70 to 95% by mass.
  • a plasma treatment capable of a conversion reaction at a lower temperature or a conversion reaction by ultraviolet irradiation treatment is preferable.
  • the modification treatment can be efficiently performed by heat-treating the coating film containing the silicon compound in combination with another modification treatment, preferably an excimer irradiation treatment described later.
  • any commonly used ultraviolet ray generator can be used.
  • the irradiation intensity and the irradiation time in a range in which the substrate carrying the irradiated metal (M2) -containing layer is not damaged.
  • Examples of such ultraviolet ray generating means include metal halide lamps, high pressure mercury lamps, low pressure mercury lamps, xenon arc lamps, carbon arc lamps, and excimer lamps (single wavelengths of 172 nm, 222 nm, and 308 nm, for example, USHIO INC. Manufactured by MD Excimer Co., Ltd.), UV light laser, and the like, but are not particularly limited.
  • the ultraviolet ray from the generation source is reflected by the reflecting plate and then the metal (M2) -containing layer is contained. It is preferred to hit the layer.
  • a dry inert gas is preferable as a gas satisfying the irradiation atmosphere used at the time of vacuum ultraviolet irradiation, and dry nitrogen gas is particularly preferable from the viewpoint of cost.
  • the oxygen concentration can be adjusted by measuring the flow rate of oxygen gas and inert gas introduced into the irradiation chamber and changing the flow rate ratio.
  • the amount of irradiation energy (integrated light amount) of vacuum ultraviolet rays on the coating surface is preferably within the range of 10 to 10000 mJ / cm 2 , more preferably within the range of 100 to 8000 mJ / cm 2 , and 200 to 6000 mJ. More preferably within the range of / cm 2 . If it is 10 mJ / cm 2 or more, the modification can proceed sufficiently. If it is 10,000 mJ / cm 2 or less, cracking due to over-reformation and thermal deformation of the substrate are unlikely to occur.
  • the vacuum ultraviolet light used for the modification may be generated by plasma formed of a gas containing at least one of CO, CO 2 and CH 4 .
  • a gas containing at least one of CO, CO 2 and CH 4 hereinafter also referred to as carbon-containing gas
  • a carbon-containing gas may be used alone, but a rare gas or H 2 is used as a main gas. It is preferable to add a small amount of carbon-containing gas.
  • the plasma generation method include capacitively coupled plasma.
  • the film density of the metal (M2) -containing layer is appropriately set depending on the purpose, but is preferably in the range of 1.5 to 2.6 g / cm 3 . Within this range, the density of the film becomes higher, and the gas barrier property deterioration and the oxidation deterioration of the film due to humidity hardly occur.
  • the oxygen deficiency composition of the composite oxide of the transition metal (M1) and the metal (M2) is more than a predetermined thickness. It represents that it is included.
  • the minimum value in the mixed region is preferably (2y + 3z) / (a + bx) ⁇ 0.2, and (2y + 3z) / ( a + bx) ⁇ 0.3 is more preferable, and (2y + 3z) / (a + bx) ⁇ 0.4 is further preferable.
  • the thickness of the mixed region where good gas barrier properties can be obtained is preferably 5 nm or more, more preferably 8 nm or more, and more preferably 10 nm or more as the sputtering thickness in terms of SiO 2. More preferably, it is more preferably 20 nm or more.
  • a transition metal (M1) -containing layer containing a compound (oxide) containing a transition metal (M1) as a main component and a metal (M2) containing a compound (oxide) containing a metal (M2) as a main component
  • the gas barrier increases as the degree of oxygen deficiency increases. It has been found that the properties are further improved. This is because, as described above, the transition metal (M1) and the metal (M2) are more easily bonded than the transition metal (M1) and the metal (M2). This is probably because a dense and high-density structure is formed in the mixed region by making the region have an oxygen deficient composition.
  • a co-evaporation method can be preferably used as a method for producing the mixed region described above.
  • the co-evaporation method is preferably a co-sputtering method.
  • the co-sputtering method employed in the present invention includes, for example, a composite target made of an alloy containing both transition metal (M1) and metal (M2), or a composite oxide of transition metal (M1) and metal (M2). It can be a single sputtering using a composite target as a sputtering target.
  • the co-sputtering method in the present invention is multi-source simultaneous sputtering using a plurality of sputtering targets including a single element of transition metal (M1) or its oxide and a single element of metal (M2) or its oxide.
  • Examples include one or more conditions selected from the group consisting of the gas supply amount, the degree of vacuum during film formation, and the power during film formation, and these film formation conditions (preferably oxygen partial pressure) ) Can be adjusted to form a thin film made of a complex oxide having an oxygen-deficient composition. That is, by forming the transition metal (M1) -containing layer and the metal (M2) -containing layer using the co-evaporation method as described above, almost all regions in the thickness direction can be mixed regions. For this reason, according to such a method, a desired gas barrier property can be realized by an extremely simple operation of controlling the thickness of the mixed region. In addition, what is necessary is just to adjust the film-forming time at the time of implementing a co-evaporation method, for example, in order to control the thickness of a mixing area
  • the organosilicon compound-containing layer according to the present invention is formed on the side opposite to the base material of the transition metal (M1) -containing layer.
  • the functional film of the present invention is organic silicon so that the transition metal (M1) contained in the transition metal (M1) -containing layer and the UV curable resin constituting the QD-containing resin layer are bonded via a chemical bond.
  • a compound-containing layer is formed.
  • the thickness of the organic silicon compound-containing layer is preferably 30 nm or less, more preferably 25 nm or less, still more preferably 20 nm or less, and particularly preferably less than 20 nm.
  • the thickness of the organosilicon compound-containing layer is measured by a transmission electron microscope (TEM).
  • a functional group such as a (meth) acryloyl group is exposed on the exposed surface of the transition metal (M1) -containing layer as a method of thinly forming the organosilicon compound-containing layer.
  • M1 transition metal
  • the method of forming an organosilicon compound content layer is mentioned.
  • the exposed functional groups can be sufficiently oriented on the surface of the organosilicon compound-containing layer, Moreover, the possibility that the organosilicon compound-containing layer is peeled off due to cohesive failure is also reduced.
  • the organic silicon compound-containing layer is formed in detail so that a functional group such as a (meth) acryloyl group is exposed on the exposed surface of the transition metal (M1) -containing layer.
  • the acryloyl group is an acyl group derived from acrylic acid represented by “CH 2 ⁇ CH—C ( ⁇ O) —”
  • the methacryloyl group is “CH 2 ⁇ C (CH 3 ) —C ( ⁇ O) — ”
  • an acyl group derived from methacrylic acid and“ (meth) acryloyl group ”is a collective name.
  • a reactive group for example, (meth) acryloyl group-containing compound (for example, (meth) acryloyl group-containing silane coupling agent) other than (meth) acryloyl group.
  • the alkoxysilyl group in the acryloyl group-containing silane coupling agent forms a chemical bond (covalent bond) with the constituent material of the transition metal (M1) -containing layer.
  • the (meth) acryloyl group becomes a transition metal ( M1)
  • an organosilicon compound-containing layer is formed on the surface of the containing layer.
  • the functional group such as (meth) acryloyl group is exposed on the surface of the transition metal (M1) -containing layer” means that the surface layer is scraped and measured by pyrolysis gas chromatography. It is possible to confirm by collating.
  • Examples of the (meth) acryloyl group-containing compound used in the “form in which the (meth) acryloyl group is exposed” include compounds containing a (meth) acryloyl group and an alkoxysilyl group in one molecule.
  • the alkoxysilyl moiety contained in the compound forms a bond with the transition metal (M1). can do.
  • the (meth) acryloyl group contained in the (meth) acryloyl group-containing compound forms a chemical bond with the transition metal (M1) via another atom.
  • the (meth) acryloyl group can be more firmly connected to the transition metal (M1) -containing layer, and as a result, the ultraviolet curable resin is adjacent to the transition metal (M1) -containing layer.
  • Examples of such compounds include vinyl group-containing silane coupling agents such as KBM-1003 (manufactured by Shin-Etsu Silicone) and epoxy group-containing silane coupling agents such as KBM-403 (manufactured by Shin-Etsu Silicone). That is, as a preferred embodiment of the present invention, “a reactive group capable of forming a bond with the transition metal (M1) constituting the transition metal (M1) -containing layer and a raw material for the ultraviolet curable resin constituting the QD-containing resin layer” 1 or 2 or more types selected from the group consisting of an alkoxysilyl group, a (meth) acryloyl group, a vinyl group, and an epoxy group. It is a preferable embodiment that the silane coupling agent contains a functional group (polymerizable substituent).
  • a compound capable of forming the organosilicon compound-containing layer for example, the above-described (meth) acryl group-containing silane coupling agent, etc. 1 reactive group capable of forming a bond with the transition metal compound constituting the transition metal (M1) -containing layer and 1 reactive group capable of forming a bond with the raw material of the ultraviolet curable resin constituting the QD-containing resin layer
  • a solution in which the compound “) in the molecule” is dissolved in an appropriate solvent is applied to the surface of the transition metal (M1) -containing layer and dried.
  • Examples of materials other than the above-described (meth) acryloyl group-containing silane coupling agent include compounds containing a (meth) acryloyl group.
  • Examples of the (meth) acryloyl group-containing compound other than the (meth) acryloyl group-containing silane coupling agent include polyol poly (meth) acrylate, epoxy (meth) acrylate, urethane (meth) acrylate, and (meth) acrylic monomer. .
  • the said solution may contain a filler for the purpose of slipperiness and winding-up property.
  • the filler include silica-based inorganic fillers such as quartz, fumed silica, precipitated silica, anhydrous silica, fused silica, crystalline silica, and ultrafine powder amorphous silica, titanium oxide, zinc oxide, zirconium oxide, and niobium oxide.
  • metal oxide inorganic fillers such as aluminum oxide, cerium oxide, and yttrium oxide.
  • silica-based inorganic fillers are particularly preferable.
  • the shape of the filler is preferably spherical, and the particle size is preferably in the range of 10 to 50 ⁇ m.
  • UV curable organic / inorganic hybrid hard coating material manufactured by JSR Corporation OPSTAR (registered trademark) series (polymerizable unsaturated group on silica fine particles) And a compound obtained by bonding an organic compound having a compound (a).
  • the surface roughness is calculated from an uneven cross-sectional curve continuously measured by an atomic force microscope (AFM) with a detector having a stylus with a minimum tip radius, and measured with a stylus with a minimum tip radius. This is the roughness related to the amplitude of fine irregularities, measured many times in a section whose direction is several tens of ⁇ m.
  • AFM atomic force microscope
  • the thickness of the bleed-out prevention layer is in the range of 1 to 10 ⁇ m, preferably in the range of 2 to 7 ⁇ m.
  • transition metal (M1) -containing layer A transition metal (M1) -containing layer is formed on the metal (M2) -containing layer by a vapor phase method / sputtering (magnetron sputtering apparatus, manufactured by Canon Anelva: Model EB1100 (hereinafter, the same apparatus is used for sputtering)). A film was formed.
  • the used sputtering apparatus can set a plurality of types of targets, and can continuously form a plurality of layers having different metal types while maintaining a predetermined vacuum state.
  • a functional film 106 was produced in the same manner except that KBM-403, which is an epoxy group-containing silane coupling agent, was used instead of KBM-803, which is a silane coupling agent.
  • the functional film 114 was produced in the same manner except that the transition metal (M1) -containing layer was formed as follows.
  • the functional film 117 was produced in the same manner except that the metal (M2) -containing layer was not formed.
  • PET polyethylene terephthalate
  • UH13 manufactured by Toray Industries, Inc.
  • the said base material (UH13) was provided with the high-refractive-index easy-adhesion layer on the single side
  • the functional film 118 was subjected to the following composition analysis. Specifically, the composition distribution profile was measured in the thickness direction from the surface side (organosilicon compound-containing layer side) of the functional film 118 by XPS analysis. XPS analysis conditions are as follows.
  • the composition in the mixed region (region where the transition metal (M1) -containing layer and the metal (M2) -containing layer are adjacent) is (M2) (M1) x O y N z (0.02 ⁇ x ⁇ 50, y > 0, z ⁇ 0), it was confirmed that the region satisfying the following formula (1) had a thickness of 25 nm in the thickness direction.
  • (M2) is Si and (M1) is Nb. In this region, Al was not detected.
  • a functional film 119 was produced in the same manner except that the transition metal (M1) -containing layer was not formed.
  • a functional film 121 was produced in the same manner except that the organic silicon compound-containing layer was not formed.
  • the functional film 122 was produced in the same manner except that the metal (M2) -containing layer, the transition metal (M1) -containing layer, and the organosilicon compound-containing layer were not formed.
  • semiconductor nanoparticles (CdSe / ZnS) emitting red and green light were respectively synthesized.
  • the semiconductor nanoparticles were dispersed in a toluene solvent so that the red component and the green component were 0.75 mg and 4.12 mg, respectively.
  • the resin A prepared above was added to this dispersion to prepare a coating solution for forming an acrylic resin-containing light emitting layer in which the content of semiconductor nanoparticles was 1% (solid content).
  • This acrylic resin-containing light-emitting layer-forming coating solution was applied on each organosilicon compound-containing layer of each functional film thus produced to form a quantum dot (QD) -containing coating film. Subsequently, it arrange
  • An acrylic resin-containing light emitting layer corresponding to each of the functional films 101 to 122 is obtained by curing the quantum dot-containing coating film by applying ultraviolet irradiation with a high-pressure mercury lamp under the conditions of / cm 2 and 300 mJ / cm 2.
  • the functional film of the present invention is superior in water vapor barrier property and adhesiveness as compared with the functional film of the comparative example.
  • the transition metal (M1) -containing layer and the organosilicon compound-containing layer are sequentially laminated on the base material to provide a functional film having high adhesion to the QD-containing resin layer. It was confirmed that it was useful.

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  • Laminated Bodies (AREA)

Abstract

La présente invention aborde le problème de la fourniture d'un film fonctionnel qui adhère fermement à une couche de résine contenant un point quantique. Ce film fonctionnel (1) est caractérisé en ce qu'une couche (4) contenant un métal de transition (M1) et une couche contenant un composé d'organosilicium (6) sont stratifiées dans l'ordre indiqué sur un matériau de base (2).
PCT/JP2016/070392 2015-07-23 2016-07-11 Film fonctionnel et dispositif électronique le comportant Ceased WO2017014083A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2015-145474 2015-07-23
JP2015145474A JP2018140494A (ja) 2015-07-23 2015-07-23 機能性フィルム及びこれを備えた電子デバイス

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WO2017014083A1 true WO2017014083A1 (fr) 2017-01-26

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TW (1) TW201718253A (fr)
WO (1) WO2017014083A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114934355A (zh) * 2022-05-09 2022-08-23 东营俊富净化科技有限公司 一种高通量pp熔喷纳微孔折叠液体过滤材料的制备方法

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112469758B (zh) 2018-07-26 2025-10-28 三菱瓦斯化学株式会社 固化性组合物、预浸料、树脂片、覆金属箔层叠板和印刷电路板
WO2021176543A1 (fr) * 2020-03-03 2021-09-10 シャープ株式会社 Élément électroluminescent et son procédé de production

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003094548A (ja) * 2001-09-26 2003-04-03 Sony Corp 反射防止フィルム
WO2009093318A1 (fr) * 2008-01-24 2009-07-30 Yuken Industry Co., Ltd. Élément à film de revêtement résistant à la corrosion, son procédé de production, et composition de revêtement pour sa production
JP2015003439A (ja) * 2013-06-20 2015-01-08 コニカミノルタ株式会社 ガスバリアフィルムの製造方法、有機エレクトロルミネッセンス素子の製造方法、及び、有機エレクトロルミネッセンス素子
JP2015099636A (ja) * 2013-11-18 2015-05-28 コニカミノルタ株式会社 有機エレクトロルミネッセンス素子
JP2015116807A (ja) * 2013-12-19 2015-06-25 エスケー イノベーション カンパニー リミテッドSk Innovation Co., Ltd. ナノ構造体

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003094548A (ja) * 2001-09-26 2003-04-03 Sony Corp 反射防止フィルム
WO2009093318A1 (fr) * 2008-01-24 2009-07-30 Yuken Industry Co., Ltd. Élément à film de revêtement résistant à la corrosion, son procédé de production, et composition de revêtement pour sa production
JP2015003439A (ja) * 2013-06-20 2015-01-08 コニカミノルタ株式会社 ガスバリアフィルムの製造方法、有機エレクトロルミネッセンス素子の製造方法、及び、有機エレクトロルミネッセンス素子
JP2015099636A (ja) * 2013-11-18 2015-05-28 コニカミノルタ株式会社 有機エレクトロルミネッセンス素子
JP2015116807A (ja) * 2013-12-19 2015-06-25 エスケー イノベーション カンパニー リミテッドSk Innovation Co., Ltd. ナノ構造体

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114934355A (zh) * 2022-05-09 2022-08-23 东营俊富净化科技有限公司 一种高通量pp熔喷纳微孔折叠液体过滤材料的制备方法

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JP2018140494A (ja) 2018-09-13

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