JP5351559B2 - Sheet-like luminescent member, electroluminescent sheet, method for producing sheet-like luminescent member, and method for producing electroluminescent sheet - Google Patents
Sheet-like luminescent member, electroluminescent sheet, method for producing sheet-like luminescent member, and method for producing electroluminescent sheet Download PDFInfo
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- JP5351559B2 JP5351559B2 JP2009046592A JP2009046592A JP5351559B2 JP 5351559 B2 JP5351559 B2 JP 5351559B2 JP 2009046592 A JP2009046592 A JP 2009046592A JP 2009046592 A JP2009046592 A JP 2009046592A JP 5351559 B2 JP5351559 B2 JP 5351559B2
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- LKKPNUDVOYAOBB-UHFFFAOYSA-N naphthalocyanine Chemical compound N1C(N=C2C3=CC4=CC=CC=C4C=C3C(N=C3C4=CC5=CC=CC=C5C=C4C(=N4)N3)=N2)=C(C=C2C(C=CC=C2)=C2)C2=C1N=C1C2=CC3=CC=CC=C3C=C2C4=N1 LKKPNUDVOYAOBB-UHFFFAOYSA-N 0.000 description 1
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Images
Abstract
Description
本発明は、シート状発光性部材、電界発光シート、電界発光層の製造方法及び電界発光シートの製造方法に関する。さらに詳しくは、本発明は、商業ビルの窓や自動車などへ設置する広告媒体、装飾用媒体、あるいは防犯用シートなどに用いられる電界発光シートを、高い生産性のもとに、低コストで効率よく与えることのできるシート状発光性部材、この部材を用いてなる電界発光層の製造方法及び電界発光シートの製造方法に関するものである。 The present invention relates to a sheet-like luminescent member, an electroluminescent sheet, a method for manufacturing an electroluminescent layer, and a method for manufacturing an electroluminescent sheet. More specifically, the present invention provides an electroluminescent sheet used for advertising media, decorative media, security sheets, etc. installed in commercial building windows and automobiles, with high productivity and low cost. The present invention relates to a sheet-like luminescent member that can be provided well, a method for producing an electroluminescent layer using this member, and a method for producing an electroluminescent sheet.
電気・電子分野、あるいは光学分野における機能素子として、電圧を印加することにより発光する電界発光素子が知られている。この電界発光素子は、一般に発光層に、無機系電界発光材料を用いた無機電界発光素子と、有機系電界発光材料を用いた有機電界発光素子に大別することができる。
特に、電流を通じることによって励起され発光する薄膜材料を用いた有機電界発光素子は、低電圧で高輝度の発光が得られるために、携帯電話ディスプレイ、パーソナルデジタルアシスタント（ＰＤＡ）、コンピュータディスプレイ、自動車の情報ディスプレイ、ＴＶモニター、あるいは一般照明を含む広い分野で幅広い潜在用途を有している。
As a functional element in the electric / electronic field or the optical field, an electroluminescent element that emits light when a voltage is applied is known. In general, the electroluminescent element can be roughly classified into an inorganic electroluminescent element using an inorganic electroluminescent material and an organic electroluminescent element using an organic electroluminescent material.
In particular, organic electroluminescent devices using thin-film materials that emit light when excited by electric current can emit light with high brightness at low voltage, so mobile phone displays, personal digital assistants (PDAs), computer displays, automobiles It has a wide range of potential applications in a wide range of fields including information displays, TV monitors, or general lighting.
一方、無機系電界発光材料は、有機系電界発光材料に比べて、高輝度の発光は得られにくいものの、長期安定性に優れていると共に、高温などの苛酷な条件下でも安定して発光するという利点を有しており、この無機系電界発光材料を発光層に用いた無機電界発光素子は、耐候性、耐熱性、長期安定性などが要求される分野での利用が研究されている。 On the other hand, inorganic electroluminescent materials, while it is difficult to obtain high luminance light emission compared to organic electroluminescent materials, are excellent in long-term stability and emit light stably even under severe conditions such as high temperatures. The inorganic electroluminescent element using this inorganic electroluminescent material for the light emitting layer has been studied for use in fields that require weather resistance, heat resistance, long-term stability, and the like.
ところで、電界発光素子の一つとして、電界発光シートが知られている。この電界発光シートの基本構成は、第１基材、第１電極、電界発光層、第２電極及び第２基材が、この順に積層された構成であり、そして、第１基材及び第１電極は透明である。また、電界発光層には、一般に無機系電界発光材料が好ましく用いられている。
このような電界発光シートは、例えば商業ビルの窓や自動車などへ設置する広告媒体、装飾用媒体、あるいは防犯用シートなどのバックライト用等として用いられる。
By the way, an electroluminescent sheet is known as one of electroluminescent elements. The basic configuration of the electroluminescent sheet is a configuration in which a first base, a first electrode, an electroluminescent layer, a second electrode, and a second base are stacked in this order, and the first base and the first base The electrode is transparent. In general, an inorganic electroluminescent material is preferably used for the electroluminescent layer.
Such an electroluminescent sheet is used, for example, as a backlight for an advertising medium, a decorative medium, a security sheet, or the like installed in a commercial building window or an automobile.
例えば、特許文献１には、フィルム状発光体の表面に、広告対象を示す画像を配した看板を用いて行う広告方法、及びフィルム状発光体の表面に、広告対象を示す画像を配して構成される広告用の看板が提案されている。そして、前記フィルム状発光体は、一対の電極層と、その電極間に挿入されるとともに、電界を印可することで発光する電界発光層とを備えた電界発光素子であることが開示されており、該電界発光層には、硫化亜鉛、酸化亜鉛などの無機系電界発光材料が用いられている。 For example, in Patent Document 1, an advertisement method is performed using a signboard in which an image indicating an advertisement target is arranged on the surface of the film-like light emitter, and an image showing the advertisement object is arranged on the surface of the film-like light emitter. A billboard for advertising composed has been proposed. And it is disclosed that the said film-form light-emitting body is an electroluminescent element provided with a pair of electrode layer and the electroluminescent layer inserted between the electrodes and light-emitted by applying an electric field. In the electroluminescent layer, an inorganic electroluminescent material such as zinc sulfide or zinc oxide is used.
無機系電界発光材料を用いて電界発光層を形成する方法としては、一般に、焼結法、レーザアブレーション法、分子エピタキシー（ＭＢＥ）法、又はスパッタリング法や真空蒸着法などの物理的気相蒸着（ＰＶＤ）法、化学的気相蒸着（ＣＶＤ）法などが用いられる（例えば、特許文献２参照）。しかしながら、これらの方法は操作が煩雑であったり、高価な装置を用いたりするため、得られる電界発光素子はコスト高になるのを免れないという欠点を有している。 In general, as a method of forming an electroluminescent layer using an inorganic electroluminescent material, a physical vapor deposition method such as a sintering method, a laser ablation method, a molecular epitaxy (MBE) method, or a sputtering method or a vacuum evaporation method ( PVD method, chemical vapor deposition (CVD) method, etc. are used (for example, refer patent document 2). However, since these methods are complicated in operation or use an expensive apparatus, the obtained electroluminescent device has a disadvantage that it is inevitable that the cost is increased.
そこで、このような欠点を改良する方法として、例えば、硫化亜鉛を銅で活性化してなる無機系電界発光材料及びチタン酸バリウムなどの高誘電体材料を、それぞれ有機バインダー中に分散させてなるコーティング材料を用い、透明フィルム上に形成された透明電極上に、スクリーン印刷法などにより、電界発光層、誘電体層及び背面電極を順に設けてなる電界発光灯が開示されている（例えば、特許文献３参照）。
しかしながら、この技術においては、前記特許文献２に示す技術に比べて、高価な装置や煩雑な操作を必要としないが、工程数が多く、大量生産には適していないといった欠点がある。
Therefore, as a method for improving such a defect, for example, a coating in which an inorganic electroluminescent material obtained by activating zinc sulfide with copper and a high dielectric material such as barium titanate are dispersed in an organic binder, respectively. An electroluminescent lamp is disclosed in which an electroluminescent layer, a dielectric layer, and a back electrode are provided in this order on a transparent electrode formed on a transparent film using a material by a screen printing method or the like (for example, Patent Documents). 3).
However, this technique does not require an expensive apparatus or complicated operation as compared with the technique shown in Patent Document 2, but has a drawback that it has many steps and is not suitable for mass production.
本発明は、このような状況下になされたものであり、広告媒体や装飾用媒体、あるいは防犯用シートなどに用いられる電界発光シートを、高い生産性のもとに、低コストで効率よく与えることができるシート状発光性部材、該部材を用いて形成された大量生産が可能な電界発光シート、シート状発光性部材の製造方法及び電界発光シートの製造方法を提供することを目的とするものである。 The present invention has been made under such circumstances, and efficiently provides an electroluminescent sheet used for an advertising medium, a decoration medium, a security sheet, etc. at a low cost with high productivity. An object of the present invention is to provide a sheet-like luminescent member that can be produced, an electroluminescent sheet that can be mass-produced using the member, a method for producing a sheet-like luminescent member, and a method for producing an electroluminescent sheet It is.
本発明者らは、前記目的を達成するために鋭意研究を重ねた結果、下記の知見を得た。
熱可塑性樹脂、好ましくは軟化点が特定の範囲にある熱可塑性樹脂中に、電界発光体を分散させてなるシート状発光性部材は、それを電界発光層に用いることで、電界発光シートを、高い生産性のもとに、低コストで効率よく与えることができ、該電界発光シートの大量生産が可能になることを見出した。
また、前記の熱可塑性樹脂と電界発光体とを混練したのち、押出機などでシート状に押出すことにより、シート状発光性部材を容易に形成し得ることを見出した。
さらに、それぞれ特定の構成を有する第１積層体と第２積層体を作製し、これらを熱ラミネートによって接合することにより、目的の電界発光シートが効率よく得られることを見出した。
本発明は、かかる知見に基づいて完成したものである。
As a result of intensive studies to achieve the above object, the present inventors have obtained the following knowledge.
A sheet-like light-emitting member obtained by dispersing an electroluminescent material in a thermoplastic resin, preferably a thermoplastic resin having a softening point in a specific range, can be used for an electroluminescent layer, whereby an electroluminescent sheet is obtained. It has been found that the electroluminescent sheet can be efficiently produced at a low cost under high productivity, and the electroluminescent sheet can be mass-produced.
Further, it has been found that a sheet-like luminescent member can be easily formed by kneading the thermoplastic resin and the electroluminescent material and then extruding it into a sheet with an extruder or the like.
Furthermore, it discovered that the target electroluminescent sheet could be obtained efficiently by producing the 1st laminated body and the 2nd laminated body which each have a specific structure, and joining these by heat | fever lamination.
The present invention has been completed based on such findings.
すなわち、本発明は、
［１］熱可塑性樹脂と、その中に分散状態で存在する電界発光体とを含むことを特徴とするシート状発光性部材、
［２］熱可塑性樹脂の軟化点が３０〜２７０℃である上記［１］に記載のシート状発光性部材、
［３］厚さが１０〜１０００μｍである上記［１］又は［２］に記載のシート状発光性部材、
［４］電界発光体の含有量が、熱可塑性樹脂１００質量部に対して、２０〜９００質量部である上記［１］〜［３］のいずれかに記載のシート状発光性部材、
［５］上記［１］〜［４］のいずれかに記載のシート状発光性部材を、電界発光層として有することを特徴とする電界発光シート、
［６］少なくとも第１基材、第１電極、電界発光層、第２電極及び第２基材がこの順に積層されてなり、かつ第１基材及び第１電極が透明である上記［５］に記載の電界発光シート、
［７］誘電体層を第１電極と電界発光層の間及び／又は電界発光層と第２電極の間に有する上記［６］に記載の電界発光シート、
［８］熱可塑性樹脂と電界発光体を混練したのち、押出機によりシート状に押出すことを特徴とする上記［１］〜［４］のいずれかに記載のシート状発光性部材の製造方法、
That is, the present invention
[1] A sheet-like light-emitting member comprising a thermoplastic resin and an electroluminescent material present in a dispersed state therein,
[2] The sheet-like light-emitting member according to [1], wherein the thermoplastic resin has a softening point of 30 to 270 ° C.
[3] The sheet-like luminescent member according to [1] or [2], having a thickness of 10 to 1000 μm,
[4] The sheet-like luminescent member according to any one of [1] to [3], wherein the content of the electroluminescent material is 20 to 900 parts by mass with respect to 100 parts by mass of the thermoplastic resin.
[5] An electroluminescent sheet comprising the sheet-like luminescent member according to any one of [1] to [4] as an electroluminescent layer,
[6] The above [5], wherein at least the first substrate, the first electrode, the electroluminescent layer, the second electrode, and the second substrate are laminated in this order, and the first substrate and the first electrode are transparent. The electroluminescent sheet according to claim 1,
[7] The electroluminescent sheet according to the above [6], having a dielectric layer between the first electrode and the electroluminescent layer and / or between the electroluminescent layer and the second electrode,
[8] The method for producing a sheet-like light-emitting member according to any one of [1] to [4], wherein the thermoplastic resin and the electroluminescent material are kneaded and then extruded into a sheet shape by an extruder. ,
［９］下記（１）又は（２）の工程により第１積層体及び第２積層体を作製し、第１積層体のシート状発光性部材側と第２積層体の第２電極側、又は第１積層体の第１電極側と第２積層体のシート状発光性部材側とを、それぞれ熱ラミネートによって接合することを特徴とする上記［５］〜［７］のいずれかに記載の電界発光シートの製造方法、及び
（１）第１基材上に少なくとも第１電極及び上記［１］〜［４］のいずれかに記載のシート状発光性部材を電界発光層として順に形成して第１積層体を作製し、別に第２基材上に少なくとも第２電極を形成することで第２積層体を作製する工程。
（２）第１基材上に少なくとも第１電極を形成することで第１積層体を作製し、別に第２基材上に少なくとも第２電極及び上記［１］〜［４］のいずれかに記載のシート状発光性部材を電界発光層として順に形成して第２積層体を作製する工程。
［１０］第１基材上に少なくとも第１電極を形成して第１積層体を作成し、別に第２基材上に少なくとも第２電極を形成して第２積層体を作製し、第１積層体の第１電極側と第２積層体の第２電極側とを、上記［１］〜［４］のいずれかに記載のシート状発光性部材を電界発光層として用いて接合することを特徴とする上記［５］〜［７］のいずれかに記載の電界発光シートの製造方法、
を提供するものである。
[9] A first laminate and a second laminate are produced by the following step (1) or (2), and the sheet-like luminescent member side of the first laminate and the second electrode side of the second laminate, or The electric field according to any one of [5] to [7], wherein the first electrode side of the first laminate and the sheet-like light-emitting member side of the second laminate are joined by thermal lamination, respectively. A method for producing a light-emitting sheet, and (1) forming at least a first electrode and a sheet-like light-emitting member according to any one of [1] to [4] as an electroluminescent layer in order on a first base material The process of producing a 2nd laminated body by producing 1 laminated body and forming a 2nd electrode at least on a 2nd base material separately.
(2) A first laminate is produced by forming at least a first electrode on a first substrate, and at least a second electrode and any one of the above [1] to [4] on a second substrate. The process of forming the sheet-like luminescent member of description as an electroluminescent layer in order, and producing a 2nd laminated body.
[10] At least a first electrode is formed on the first substrate to create a first laminate, and at least a second electrode is formed on the second substrate to produce a second laminate. The first electrode side of the laminate and the second electrode side of the second laminate are joined using the sheet-like luminescent member according to any one of [1] to [4] as an electroluminescent layer. The method for producing an electroluminescent sheet according to any one of [5] to [7] above,
Is to provide.
本発明によれば、商業ビルの窓や自動車などへ設置する広告媒体、装飾用媒体、あるいは防犯用シートなどに用いられる電界発光シートを、高い生産性のもとに、低コストで効率よく与えることのできるシート状発光性部材を提供することができる。
また、前記シート状発光性部材を用いて電界発光層を形成することにより、大量生産が可能な電界発光シートを提供することができる。さらに、本発明によれば、シート状発光性部材の効率的な製造方法、及び該電界発光シートの大量生産が可能な電界発光シートの製造方法を提供することができる。
According to the present invention, an electroluminescent sheet used for an advertising medium, a decorative medium, a security sheet or the like installed in a commercial building window or an automobile is efficiently provided at low cost with high productivity. The sheet-like luminescent member which can be provided can be provided.
Moreover, the electroluminescent sheet which can be mass-produced can be provided by forming an electroluminescent layer using the said sheet-like luminescent member. Furthermore, according to the present invention, it is possible to provide an efficient method for producing a sheet-like luminescent member and a method for producing an electroluminescent sheet capable of mass production of the electroluminescent sheet.
まず、本発明のシート状発光性部材について説明する。
［シート状発光性部材］
本発明のシート状発光性部材は、熱可塑性樹脂と、その中に分散状態で存在する電界発光体とを含むことを特徴とする。
（熱可塑性樹脂）
本発明のシート状発光性部材に用いられる熱可塑性樹脂としては、熱可塑性の性質を有するものであればよく、特に制限はないが、電界発光体の分散性、シート状発光性部材のラミネート性などの観点から、軟化点が３０〜２７０℃の範囲にあるものが好ましく、３２〜２５０℃の範囲にあるものがより好ましく、８０〜２４０℃の範囲にあるものがさらに好ましい。
First, the sheet-like luminescent member of the present invention will be described.
[Sheet-like luminescent member]
The sheet-like luminescent member of the present invention is characterized by containing a thermoplastic resin and an electroluminescent material present in a dispersed state therein.
(Thermoplastic resin)
The thermoplastic resin used in the sheet-like light-emitting member of the present invention is not particularly limited as long as it has a thermoplastic property, and the dispersibility of the electroluminescent material and the laminate property of the sheet-like light-emitting member are not particularly limited. In view of the above, those having a softening point in the range of 30 to 270 ° C are preferred, those in the range of 32 to 250 ° C are more preferred, and those in the range of 80 to 240 ° C are more preferred.
このような熱可塑性樹脂としては、例えばポリエチレンテレフタレート、ポリブチレンテレフタレートなどのポリエステル、ポリエステル系熱可塑性エラストマー、エポキシ化などにより変性した各種熱可塑性エラストマー、ポリ塩化ビニル、エチレン−酢酸ビニル共重合樹脂、アクリル系樹脂、アクリル−ウレタン共重合体、アクリル−ウレタングラフト共重合体、エチレン−（メタ）アクリル酸共重合樹脂、ポリプロピレンなどのポリオレフィン類、ポリオレフィン系熱可塑性エラストマーなどを挙げることができる。これらの中で、エチレン−酢酸ビニル共重合体や、エチレン−（メタ）アクリル酸共重合体が好適である。
これらの熱可塑性樹脂は１種を単独で用いてもよく、２種以上を組み合わせて用いてもよい。
Examples of such thermoplastic resins include polyesters such as polyethylene terephthalate and polybutylene terephthalate, polyester-based thermoplastic elastomers, various thermoplastic elastomers modified by epoxidation, polyvinyl chloride, ethylene-vinyl acetate copolymer resins, acrylics, and the like. Resin, acrylic-urethane copolymer, acrylic-urethane graft copolymer, ethylene- (meth) acrylic acid copolymer resin, polyolefins such as polypropylene, and polyolefin-based thermoplastic elastomers. Among these, an ethylene-vinyl acetate copolymer and an ethylene- (meth) acrylic acid copolymer are preferable.
These thermoplastic resins may be used individually by 1 type, and may be used in combination of 2 or more type.
（電界発光体）
本発明のシート状発光性部材において、前述した熱可塑性樹脂に混練分散させる電界発光体としては、無機系電界発光材料及び有機系電界発光材料のいずれも用いることができるが、本発明の電界発光シートの用途の観点から、長期安定性に優れる無機系電界発光材料が好ましい。
(Electroluminescent)
In the sheet-like luminescent member of the present invention, as the electroluminescent material kneaded and dispersed in the thermoplastic resin described above, both inorganic electroluminescent materials and organic electroluminescent materials can be used. From the viewpoint of use of the sheet, an inorganic electroluminescent material having excellent long-term stability is preferable.
＜無機系電界発光材料＞
本発明で用いる無機系電界発光材料に特に制限はなく、従来公知の無機系電界発光材料の中から、任意のものを適宜選択して用いることができる。この無機系電界発光材料としては、例えば硫化亜鉛（ＺｎＳ）を母材とし、発光中心材料として銅、マンガン、フッ化テルビウム、フッ化サマリウム、フッ化ツリウムを各々添加したＺｎＳ：Ｃｕ、ＺｎＳ：Ｍｎ、ＺｎＳ：ＴｂＦ3、ＺｎＳ：ＳｍＦ3、ＺｎＳ：ＴｍＦ3；硫化カルシウム（ＣａＳ）を母材とし、発光中心材料としてユーロピウムを添加したＣａＳ：Ｅｕ；硫化ストロンチウム（ＳｒＳ）を母材とし、発光中心材料としてセリウムを添加したＳｒＳ：Ｃｅ；あるいはＣａＣａ2Ｓ4、ＳｒＣａ2Ｓ4のようなアルカリ土類カルシウム硫化物などを母材とし、発光中心材料としてマンガンなどの遷移金属や、ユーロピウム、セリウム、テルビウムなどの希土類元素を添加したものなどを好ましく挙げることができる。
なかでも、緑色に発光するものとしてＺｎＳ：ＣｕやＺｎＳ：ＴｂＦ3が、黄橙色に発光するものとしてＺｎＳ：Ｍｎが、赤色に発光するものとしてＺｎＳ：ＳｍＦ3、及びＣａＳ：Ｅｕが、青色に発光するものとしてＺｎＳ：ＴｍＦ3、ＳｒＳ：Ｃｅが好ましい。
<Inorganic electroluminescent material>
There is no restriction | limiting in particular in the inorganic type electroluminescent material used by this invention, Arbitrary things can be suitably selected and used from conventionally well-known inorganic type electroluminescent material. As this inorganic electroluminescent material, for example, zinc sulfide (ZnS) is used as a base material, and copper, manganese, terbium fluoride, samarium fluoride, and thulium fluoride are added as emission center materials, respectively, ZnS: Cu, ZnS: Mn. ZnS: TbF 3 , ZnS: SmF 3 , ZnS: TmF 3 ; CaS: Eu containing calcium sulfide (CaS) as a base material and europium added as a luminescent center material; strontium sulfide (SrS) as a base material, luminescent center SrS: Ce with cerium added as a material; or alkaline earth calcium sulfide such as CaCa 2 S 4 and SrCa 2 S 4 as a base material; transition metal such as manganese as a luminescent center material; europium, cerium, Preferable examples include those added with rare earth elements such as terbium.
Among them, ZnS: Cu or ZnS: TbF 3 emits green light, ZnS: Mn emits yellow orange light, ZnS: SmF 3 emits red light, and CaS: Eu turns blue. ZnS: TmF 3 and SrS: Ce are preferable for emitting light.
さらには、Ｓｃ以外の希土類元素、例えばＹ、Ｌａ、Ｃｅ、Ｐｒ、Ｎｄ、Ｓｍ、Ｅｕ、Ｇｄ、Ｔｂ、Ｄｙ、Ｈｏ、Ｅｒ、Ｔｍ、Ｙｂ、ＬｕなどをドープしたＳｃ2Ｏ3からなる酸化物発光材料も挙げることができる。ドープする希土類元素としては、Ｃｅ、Ｓｍ、Ｅｕ、Ｔｂ、Ｔｍが好ましい。ドープする希土類元素の種類により、黄色、黄色より長波長側の赤色、黄色より短波長側の緑色や青色に発光する。
本発明においては、これらの無機系電界発光材料は１種を単独で用いてもよく、必要に応じ２種以上を組み合わせて用いてもよい。
Furthermore, an oxide composed of Sc 2 O 3 doped with rare earth elements other than Sc, such as Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, etc. A light emitting material can also be mentioned. As the rare earth element to be doped, Ce, Sm, Eu, Tb, and Tm are preferable. Depending on the kind of rare earth element to be doped, light is emitted in yellow, red on the longer wavelength side from yellow, and green or blue on the shorter wavelength side from yellow.
In the present invention, these inorganic electroluminescent materials may be used alone or in combination of two or more as necessary.
＜有機系電界発光材料＞
本発明における有機系電界発光材料に特に制限はなく、低分子型及び高分子型のいずれも使用することができ、また蛍光発光材料及び燐光発光材料のいずれも使用することができる。
低分子型有機系電界発光材料の中で、蛍光発光材料としては、例えばベンゾオキサゾール誘導体、ベンゾイミダゾール誘導体、ベンゾチアゾール誘導体、スチリルベンゼン誘導体、ポリフェニル誘導体、ジフェニルブタジエン誘導体、テトラフェニルブタジエン誘導体、ナフタルイミド誘導体、クマリン誘導体、ペリレン誘導体、ペリノン誘導体、オキサジアゾール誘導体、アルダジン誘導体、ピラリジン誘導体、シクロペンタジエン誘導体、ビススチリルアントラセン誘導体、キナクリドン誘導体、ピロロピリジン誘導体、チアジアゾロピリジン誘導体、スチリルアミン誘導体、芳香族ジメチリデン化合物、８−キノリノール誘導体の金属錯体や希土類錯体に代表される各種金属錯体などが好ましく挙げられる。
<Organic electroluminescent material>
There is no restriction | limiting in particular in the organic electroluminescent material in this invention, Both a low molecular type and a high molecular type can be used, and both a fluorescent luminescent material and a phosphorescent luminescent material can be used.
Among the low-molecular organic electroluminescent materials, examples of fluorescent light-emitting materials include benzoxazole derivatives, benzimidazole derivatives, benzothiazole derivatives, styrylbenzene derivatives, polyphenyl derivatives, diphenylbutadiene derivatives, tetraphenylbutadiene derivatives, and naphthalimide. Derivatives, coumarin derivatives, perylene derivatives, perinone derivatives, oxadiazole derivatives, aldazine derivatives, pyrazine derivatives, cyclopentadiene derivatives, bisstyryl anthracene derivatives, quinacridone derivatives, pyrrolopyridine derivatives, thiadiazolopyridine derivatives, styrylamine derivatives, aromatic Preferable examples include dimethylidene compounds, metal complexes of 8-quinolinol derivatives, and various metal complexes represented by rare earth complexes.
また、燐光発光材料としては、オルトメタル化金属錯体［例えば山本明夫著「有機金属化学−基礎と応用−」１５０頁〜２３２頁、裳華房社（１９８２年発行）やＨ．Ｙｅｒｓｉｎ著「Ｐｈｏｔｏｃｈｅｍｉｓｔｒｙ ａｎｄ Ｐｈｏｔｏｐｈｙｓｉｃｓ ｏｆ Ｃｏｏｒｄｉｎａｔｉｏｎ Ｃｏｍｐｏｕｎｄｓ」、７１頁〜７７頁、１３５頁〜１４６頁、Ｓｐｒｉｎｇｅｒ−Ｖｅｒｌａｇ社（１９８７年発行）等に記載されている化合物群の総称］、又はポリフィリン金属錯体などを好ましく挙げることができる。 Examples of phosphorescent materials include ortho-metalated metal complexes [for example, Akio Yamamoto, “Organic Metal Chemistry: Fundamentals and Applications”, pages 150 to 232; Yersin's “Photochemistry and Photophysics of Coordination Compounds”, pages 71-77, pages 135-146, Springer-Verlag (published in 1987), etc., or a polyphyllin metal complex Preferable examples can be given.
一方、高分子型有機系電界発光材料としては、蛍光発光材料であるポリチオフェン誘導体、ポリフェニレン誘導体、ポリフェニレンビニレン誘導体、ポリフルオレン誘導体などを好ましく挙げることができる。
本発明においては、有機系電界発光材料として、前記の低分子型及び高分子型の中から、１種を選び用いてもよく、２種以上を選び組み合わせて用いてもよい。
なお、後述の電界発光層が、このような有機系電界発光材料からなる層である場合、該電界発光層の陽極側に、正孔注入・輸送層を、陰極側に電子注入・輸送層を積層することが好ましい。
On the other hand, preferred examples of the polymer organic electroluminescent material include polythiophene derivatives, polyphenylene derivatives, polyphenylene vinylene derivatives, and polyfluorene derivatives that are fluorescent materials.
In the present invention, one type of organic electroluminescent material may be selected and used from the low molecular types and high molecular types, and two or more types may be selected and used in combination.
When the electroluminescent layer described later is a layer made of such an organic electroluminescent material, a hole injection / transport layer is provided on the anode side of the electroluminescent layer, and an electron injection / transport layer is provided on the cathode side. It is preferable to laminate.
本発明のシート状発光性部材においては、前記電界発光体が粒子である場合には、熱可塑性樹脂中への均一分散性の観点から、平均粒径が１〜１００μｍであることが好ましく、１０〜６０μｍであることがより好ましく、２０〜５０μｍであることがさらに好ましい。
また、当該電界発光体の含有量は、無機系、有機系で異なるが、無機系の場合、発光性及び経済性のバランスなどの観点から、熱可塑性樹脂１００質量部に対して、通常２０〜９００質量部程度、好ましくは１００〜９００質量部、より好ましくは１００〜７００質量部、さらに好ましくは１００〜５００質量部であり、特に好ましくは１５０〜３５０質量部である。
In the sheet-like luminescent member of the present invention, when the electroluminescent material is a particle, the average particle size is preferably 1 to 100 μm from the viewpoint of uniform dispersibility in the thermoplastic resin. It is more preferably ˜60 μm, and further preferably 20-50 μm.
Further, the content of the electroluminescent material is different depending on whether it is inorganic or organic, but in the case of inorganic, the content is usually 20 to 100 parts by mass with respect to 100 parts by mass of the thermoplastic resin from the viewpoint of balance between light emission and economy. About 900 parts by mass, preferably 100 to 900 parts by mass, more preferably 100 to 700 parts by mass, still more preferably 100 to 500 parts by mass, and particularly preferably 150 to 350 parts by mass.
《沈降防止剤》
本発明のシート状発光性部材には、電界発光体の沈降を防止し、後述する電界発光層における電界発光体の分散を良好なものにするために、沈降防止剤を好ましく含有させることができる。この沈降防止剤としては、例えば酸化ポリエチレン系、水素添加ひまし油、高級脂肪酸アミド等が挙げられ、好ましい沈降防止剤はオレイン酸アミド、ステアリン酸アミド、カプロン酸アミド、リノール酸アミド、Ｎ，Ｎ′−メチレンビスステアリン酸アミド、Ｎ，Ｎ′−エチレンビスステアリン酸アミドなどの高級脂肪酸アミド類である。
沈降防止剤の含有量は、沈降防止効果と経済性のバランスなどの観点から、熱可塑性樹脂１００質量部に対して、固形分として通常０．１〜５質量部程度、好ましくは０．２〜４質量部である。これらの沈降防止剤は１種類を単独で使用してもよいし、２種以上を組み合わせて用いてもよい。
<Anti-settling agent>
The sheet-like luminescent member of the present invention can preferably contain an anti-settling agent in order to prevent sedimentation of the electroluminescent body and to improve the dispersion of the electroluminescent body in the electroluminescent layer described later. . Examples of the anti-settling agent include polyethylene oxide, hydrogenated castor oil, higher fatty acid amide and the like, and preferable anti-settling agents include oleic acid amide, stearic acid amide, caproic acid amide, linoleic acid amide, N, N′-. Higher fatty acid amides such as methylenebisstearic acid amide and N, N'-ethylenebisstearic acid amide;
The content of the anti-settling agent is usually about 0.1 to 5 parts by mass, preferably about 0.2 to about 100 parts by mass with respect to 100 parts by mass of the thermoplastic resin, from the viewpoint of the balance between anti-settling effect and economy. 4 parts by mass. One of these antisettling agents may be used alone, or two or more thereof may be used in combination.
《発光色調整剤》
本発明のシート状発光性部材には、発光色を調整する目的で、発光色調整剤を好ましく含有させることができる。発光色調整剤としては、蛍光体及び顔料から選ばれる少なくとも一種を好ましく挙げることができる。
<Luminescent color modifier>
The sheet-like luminescent member of the present invention can preferably contain a luminescent color adjusting agent for the purpose of adjusting the luminescent color. Preferable examples of the emission color adjusting agent include at least one selected from phosphors and pigments.
（蛍光体）
本発明のシート状発光性部材に用いられる蛍光体は、発光色をどのように調整するかにより、公知の蛍光体のなかから適宜選択して使用することができる。例えば、発光体から発する青色ないし青緑色領域の光を吸収して、緑色領域の蛍光を発する蛍光色素としては、２，３，５，６−１Ｈ，４Ｈ−テトラヒドロ−８−トリフルオロメチルキノリジン（９，９ａ，１−ｇｈ）クマリン（クマリン１５３）、３−（２′−ベンゾチアゾリル）−７−ジエチルアミノクマリン（クマリン６）、３−（２′−ベンゾイミダゾリル）−７−Ｎ，Ｎ−ジエチルアミノクマリン（クマリン７）、３−（２′−Ｎ−メチルベンゾイミダゾリル）−７−Ｎ，Ｎ−ジエチルアミノクマリン（クマリン３０）などのクマリン系色素、ソルベントイエロー１１、ソルベントイエロー１１６などのナフタルイミド系色素などが好ましく挙げられる。
(Phosphor)
The phosphor used in the sheet-like luminescent member of the present invention can be used by appropriately selecting from known phosphors depending on how the emission color is adjusted. For example, as a fluorescent dye that absorbs light in a blue to blue-green region emitted from a light emitter and emits fluorescence in a green region, 2,3,5,6-1H, 4H-tetrahydro-8-trifluoromethylquinolidine (9,9a, 1-gh) coumarin (coumarin 153), 3- (2'-benzothiazolyl) -7-diethylaminocoumarin (coumarin 6), 3- (2'-benzimidazolyl) -7-N, N-diethylaminocoumarin (Coumarin 7), 3- (2′-N-methylbenzimidazolyl) -7-N, N-diethylaminocoumarin (coumarin 30) and other coumarin dyes, naphthalimide dyes such as solvent yellow 11 and solvent yellow 116, etc. Preferably mentioned.
発光体から発する青色ないし青緑色領域の光を吸収して、赤色領域の蛍光を発する蛍光色素としては、例えば４−ジシアノメチレン−２−メチル−６−（ｐ−ジメチルアミノスチリル）−４Ｈ−ピラン（ＤＣＭ）などのシアニン系色素、１−エチル−２−〔４−（ｐ−ジメチルアミノフェニル）−１，３−ブタジエニル）−ピリジウム−パークロレート（ピリジン１）などのピリジン系色素、ローダミンＢ，ローダミン６Ｇ，ローダミン３Ｂ，ローダミン１０１，ローダミン１１０，スルホローダミン，ベーシックバイオレット１１，ベーシックレッド２などのローダミン系色素、あるいはオキサジン系色素などが好ましく挙げられる。また、蛍光色素は、ポリメタクリル酸エステル，ポリ塩化ビニル，塩化ビニル−酢酸ビニル共重合樹脂，アルキッド樹脂，芳香族スルホンアミド樹脂，ユリア樹脂，メラミン樹脂，ベンゾグアナミン樹脂及びこれらの樹脂混合物などに予め練り込んで顔料化して蛍光顔料としたものであってもよい。
蛍光体の含有量は、電界発光体１００質量部に対して１〜５０質量部が好ましく、３〜２０質量部がより好ましい。これらの蛍光色素や蛍光顔料は単独で用いてもよく、必要に応じ二種以上を組み合わせて用いてもよい。
As a fluorescent dye that absorbs light in a blue or blue-green region emitted from a light emitter and emits fluorescence in a red region, for example, 4-dicyanomethylene-2-methyl-6- (p-dimethylaminostyryl) -4H-pyran Cyanine dyes such as (DCM), pyridine dyes such as 1-ethyl-2- [4- (p-dimethylaminophenyl) -1,3-butadienyl) -pyridium-perchlorate (pyridine 1), rhodamine B, Preferred examples include rhodamine dyes such as rhodamine 6G, rhodamine 3B, rhodamine 101, rhodamine 110, sulforhodamine, basic violet 11, and basic red 2, or oxazine dyes. Fluorescent dyes are pre-kneaded in polymethacrylic acid esters, polyvinyl chloride, vinyl chloride-vinyl acetate copolymer resins, alkyd resins, aromatic sulfonamide resins, urea resins, melamine resins, benzoguanamine resins, and mixtures of these resins. The pigment may be made into a fluorescent pigment.
1-50 mass parts is preferable with respect to 100 mass parts of electroluminescent bodies, and, as for content of fluorescent substance, 3-20 mass parts is more preferable. These fluorescent dyes and fluorescent pigments may be used alone or in combination of two or more as necessary.
（顔料）
本発明のシート状発光性部材に用いられる顔料は、発光色をどのように調整するかにより、公知の顔料のなかから適宜選択して使用することができる。例えば、チタン白、亜鉛華、弁柄、朱、群青、コバルトブルー、チタン黄、黄鉛などの無機顔料、イソインドリノン、ハンザイエローＡ、キナクリドン、パーマネントレッド４Ｒ、フタロシアニンブルー、インダスレンブリーＲＳなどの有機顔料などが好ましく挙げられる。
顔料の含有量は、電界発光体１００質量部に対して１〜５０質量部が好ましく、３〜２０質量部がより好ましい。
(Pigment)
The pigment used for the sheet-like luminescent member of the present invention can be appropriately selected from known pigments depending on how the luminescent color is adjusted. For example, titanium white, zinc white, petal, vermilion, ultramarine, cobalt blue, titanium yellow, yellow lead, and other inorganic pigments, isoindolinone, Hansa Yellow A, quinacridone, permanent red 4R, phthalocyanine blue, Induslenbury RS, etc. Of these, organic pigments are preferred.
1-50 mass parts is preferable with respect to 100 mass parts of electroluminescent bodies, and, as for content of a pigment, 3-20 mass parts is more preferable.
《紫外線吸収剤及び赤外線吸収剤》
本発明のシート状発光性部材には、発光性部材の耐候性の向上を目的として、紫外線吸収剤及び赤外線吸収剤から選ばれる少なくとも一種を好ましく含有させることができる。
<Ultraviolet absorber and infrared absorber>
The sheet-like luminescent member of the present invention can preferably contain at least one selected from an ultraviolet absorber and an infrared absorber for the purpose of improving the weather resistance of the luminescent member.
（紫外線吸収剤）
紫外線吸収剤は、公知の紫外線吸収剤のなかから適宜選択して使用することができる。例えば、紫外線吸収剤としては、２−（２'−ヒドロキシ−３'，５'−ジ−ｔｅｒｔ−ブチルフェニル）−５−クロロベンゾトリアゾール、２−（２'−ヒドロキシ−３'−ｔｅｒｔ−ブチル−５'−メチルフェニル）−５−クロロベンゾトリアゾール、２−（２'−ヒドロキシ−３'−ｔｅｒｔ−アミル−５'−イソブチルフェニル）−５−クロロベンゾトリアゾール、２−（２'−ヒドロキシ−３'−イソブチル−５'−メチルフェニル）−５−クロロベンゾトリアゾール、２−（２'−ヒドロキシ−３'−イソブチル−５'−プロピルフェニル）−５−クロロベンゾトリアゾールなどの２'−ヒドロキシフェニル−５−クロロベンゾトリアゾール系紫外線吸収剤；２−（２'−ヒドロキシ−３'，５'−ジ−ｔｅｒｔ−ブチルフェニル）ベンゾトリアゾール、２−（２'−ヒドロキシ−５'−メチルフェニル）ベンゾトリアゾールなどの２'−ヒドロキシフェニルベンゾトリアゾール系紫外線吸収剤；２，２'−ジヒドロキシ−４−メトキシベンゾフェノン、２，２'−ジヒドロキシ−４，４'−ジメトキシベンゾフェノン、２，２'，４，４'−テトラヒドロキシベンゾフェノンなどの２，２'−ジヒドロキシベンゾフェノン系紫外線吸収剤；２−ヒドロキシ−４−メトキシベンゾフェノン、２，４−ジヒドロキシベンゾフェノンなどの２−ヒドロキシベンゾフェノン系紫外線吸収剤；サリチル酸フェニル、４−ｔｅｒｔ−ブチル−フェニル−サリシレートなどのサリチル酸エステル系紫外線吸収剤；２−エチル−ヘキシル−２−シアノ−３，３−ジフェニルアクリレート、エチル−２−シアノ−３，３−ジフェニルアクリレート、オクチル−２−シアノ−３，３−ジフェニルアクリレートなどのシアノアクリレート系紫外線吸収剤；及び２−（４，６−ビス（２，４−ジメチルフェニル）−１，３，５−トリアジン−２−イル）−５−ヒドロキシフェニル、２−（２，４−ジヒドロキシフェニル）−４，６−ビス−（２，４−ジメチルフェニル）−１，３−５−トリアジン、２，４−ビス［２−ヒドロキシ−4−ブトキシフェニル］−６（２，４−ジブトキシフェニル）−１，３，５−トリアジン、トリス（ヒドロキシフェニル）トリアジンなどのトリアジン系紫外線吸収剤などが好ましく挙げられる。その他、ベンゾトリアゾール骨格にアクリロイル基又はメタクリロイル基を導入した反応型紫外線吸収剤なども好ましく挙げられる。
紫外線吸収剤の含有量は、熱可塑性樹脂１００質量部に対して０．５〜２０質量部が好ましく、１〜１０質量部がより好ましい。
(UV absorber)
The ultraviolet absorber can be used by appropriately selecting from known ultraviolet absorbers. For example, as an ultraviolet absorber, 2- (2′-hydroxy-3 ′, 5′-di-tert-butylphenyl) -5-chlorobenzotriazole, 2- (2′-hydroxy-3′-tert-butyl) -5'-methylphenyl) -5-chlorobenzotriazole, 2- (2'-hydroxy-3'-tert-amyl-5'-isobutylphenyl) -5-chlorobenzotriazole, 2- (2'-hydroxy- 2'-hydroxyphenyl such as 3'-isobutyl-5'-methylphenyl) -5-chlorobenzotriazole, 2- (2'-hydroxy-3'-isobutyl-5'-propylphenyl) -5-chlorobenzotriazole -5-chlorobenzotriazole ultraviolet absorber; 2- (2'-hydroxy-3 ', 5'-di-tert-butylphenyl) benzotriazole, 2 -2'-hydroxyphenylbenzotriazole ultraviolet absorbers such as (2'-hydroxy-5'-methylphenyl) benzotriazole; 2,2'-dihydroxy-4-methoxybenzophenone, 2,2'-dihydroxy-4, 2,2′-dihydroxybenzophenone ultraviolet absorbers such as 4′-dimethoxybenzophenone and 2,2 ′, 4,4′-tetrahydroxybenzophenone; 2-hydroxy-4-methoxybenzophenone, 2,4-dihydroxybenzophenone and the like 2-hydroxybenzophenone UV absorbers; salicylic acid ester UV absorbers such as phenyl salicylate, 4-tert-butyl-phenyl-salicylate; 2-ethyl-hexyl-2-cyano-3,3-diphenyl acrylate, ethyl-2 -Cyano-3,3-diphe Cyanoacrylate-based ultraviolet absorbers such as polyacrylate, octyl-2-cyano-3,3-diphenylacrylate; and 2- (4,6-bis (2,4-dimethylphenyl) -1,3,5-triazine- 2-yl) -5-hydroxyphenyl, 2- (2,4-dihydroxyphenyl) -4,6-bis- (2,4-dimethylphenyl) -1,3-5-triazine, 2,4-bis [ Preferable examples include triazine-based ultraviolet absorbers such as 2-hydroxy-4-butoxyphenyl] -6 (2,4-dibutoxyphenyl) -1,3,5-triazine and tris (hydroxyphenyl) triazine. In addition, a reactive ultraviolet absorber having an acryloyl group or a methacryloyl group introduced into the benzotriazole skeleton is also preferred.
0.5-20 mass parts is preferable with respect to 100 mass parts of thermoplastic resins, and, as for content of a ultraviolet absorber, 1-10 mass parts is more preferable.
（赤外線吸収剤）
赤外線吸収剤は、有機赤外線吸収剤や無機赤外線吸収剤などの公知の赤外線吸収剤のなかから適宜選択して使用することができる。
有機赤外線吸収剤としては、フタロシアニン、ナフタロシアニン、アントラキノン、シアニン化合物、スクワリリウム化合物、チオールニッケル錯体化合物、トリアリルメタン、ナフトキノン、アントラキノン、及びＮ，Ｎ，Ｎ'，Ｎ'−テトラキス（ｐ−ジ−ｎ−ブチルアミノフェニル）−ｐ−フェニレンジアミニウムパークロレート、フェニレンジアミニウムクロラート、フェニレンジアミニウムヘキサフルオロアンチモンネート、フェニレンジアミニウムフルオロボレート、フェニレンジアミニウムフルオレートなどのアミン化合物などが挙げられる。
(Infrared absorber)
The infrared absorber can be appropriately selected and used from known infrared absorbers such as an organic infrared absorber and an inorganic infrared absorber.
Organic infrared absorbers include phthalocyanine, naphthalocyanine, anthraquinone, cyanine compound, squarylium compound, thiol nickel complex compound, triallylmethane, naphthoquinone, anthraquinone, and N, N, N ′, N′-tetrakis (p-di- n-Butylaminophenyl) -p-phenylenediaminium perchlorate, phenylenediaminium chloride, phenylenediaminium hexafluoroantimonate, phenylenediaminiumfluoroborate, phenylenediaminiumfluorate, and other amine compounds.
無機赤外線吸収剤としては、Ｓｎ、Ｔｉ、Ｓｉ、Ｚｎ、Ｚｒ、Ｆｅ、Ａｌ、Ｃｒ、Ｃｏ、Ｃｅ、Ｉｎ、Ｎｉ、Ａｇ、Ｃｕ、Ｐｔ、Ｎｎ、Ｔａ、Ｗ、Ｖ及びＭｏなどの金属の酸化物、窒化物、炭化物、酸窒化物、硫化物が好ましく挙げられる。なかでもＩＴＯ（インジウムスズ酸化物）、ＡＴＯ（アンチモンスズ酸化物）、ＳｎＯ2、ＴｉＯ2、ＳｉＯ2、ＺｒＯ2、ＺｎＯ、Ｆｅ2Ｏ3、Ａ１2Ｏ3、ＦｅＯ、Ｃｒ2Ｏ3、Ｃｏ2Ｏ3、ＣｅＯ2、Ｉｎ2Ｏ3、ＮｉＯ、ＭｎＯ、ＣｕＯ、ＷＯ3などの金属酸化物が好ましく挙げられる。金属酸化物には、赤外線吸収能の向上等を目的としてセシウム（Ｃｅ）などの添加剤をくわえてもよい。
赤外線吸収剤の含有量は、熱可塑性樹脂１００質量部に対して０．５〜２０質量部が好ましく、１〜１０質量部がより好ましい。
Inorganic infrared absorbers include metals such as Sn, Ti, Si, Zn, Zr, Fe, Al, Cr, Co, Ce, In, Ni, Ag, Cu, Pt, Nn, Ta, W, V, and Mo. Preferred examples include oxides, nitrides, carbides, oxynitrides, and sulfides. Among them, ITO (indium tin oxide), ATO (antimony tin oxide), SnO 2 , TiO 2 , SiO 2 , ZrO 2 , ZnO, Fe 2 O 3 , A1 2 O 3 , FeO, Cr 2 O 3 , Co Preferable examples include metal oxides such as 2 O 3 , CeO 2 , In 2 O 3 , NiO, MnO, CuO, and WO 3 . An additive such as cesium (Ce) may be added to the metal oxide for the purpose of improving infrared absorption ability.
0.5-20 mass parts is preferable with respect to 100 mass parts of thermoplastic resins, and, as for content of an infrared absorber, 1-10 mass parts is more preferable.
また、本発明のシート状発光性部材には、本発明の目的が損なわれない範囲で、前記した以外の各種添加剤、例えば酸化防止剤、光安定剤、粘着付与剤などを、必要に応じて含有させることができる。 Further, the sheet-like luminescent member of the present invention may contain various additives other than those described above, for example, an antioxidant, a light stabilizer, a tackifier, and the like, as long as the object of the present invention is not impaired. Can be contained.
（シート状発光性部材の作製）
本発明のシート状発光性部材の作製方法としては、シート状であって、熱可塑性樹脂中に、電界発光体及び必要に応じて用いられる沈降防止剤をはじめ、その他各種添加剤が均質に分散し得る方法であればよく、特に制限はないが、例えば所定の割合の熱可塑性樹脂と電界発光体と必要に応じて用いられる沈降防止剤をはじめ、その他各種添加剤とを、混練したのち、押出機を用いて、そのダイより、シート状に押出すことにより、所望のシート状発光性部材を作製することができる。この際、本発明のシート状発光性部材を、所定の部材にラミネートしたい場合には、前記押出機より、被ラミネート部材上に、本発明のシート状発光性部材をラミネートすることができる。
(Production of sheet-like luminescent member)
As a method for producing the sheet-like luminescent member of the present invention, the sheet-like luminescent member is homogeneously dispersed in a thermoplastic resin, including an electroluminescent material and an anti-settling agent used as needed, and other various additives. There is no particular limitation as long as it is a method that can be performed, for example, after kneading a predetermined proportion of a thermoplastic resin, an electroluminescent material, an anti-settling agent used as necessary, and other various additives, A desired sheet-like luminescent member can be produced by extruding into a sheet form from the die using an extruder. At this time, when the sheet-like luminescent member of the present invention is to be laminated on a predetermined member, the sheet-like luminescent member of the present invention can be laminated on the member to be laminated by the extruder.
このようにして得られた本発明のシート状発光性部材の厚さは、発光性（輝度、照度）及び実用性の観点から、１０〜１０００μｍが好ましく、２０〜５００μｍがより好ましく、３０〜１００μｍがさらに好ましい。
また、シート状発光性部材の破断強度は、１〜１００ＭＰａであることが好ましい。破断強度がこの範囲にあると張力が加わっても切断しにくく、効率よく電界発光シートを製造することができる。
The thickness of the sheet-like light-emitting member of the present invention thus obtained is preferably 10 to 1000 μm, more preferably 20 to 500 μm, and more preferably 30 to 100 μm from the viewpoints of light emission (brightness and illuminance) and practicality. Is more preferable.
Moreover, it is preferable that the breaking strength of a sheet-like luminescent member is 1-100 Mpa. When the breaking strength is within this range, it is difficult to cut even if tension is applied, and an electroluminescent sheet can be produced efficiently.
本発明のシート状発光性部材は、後述の電界発光シートにおける電界発光層の形成に好適に用いられる。このシート状発光性部材を上記電界発光層に用いることにより、大量生産が可能な電界発光シートを効率よく製造することができる。 The sheet-like luminescent member of the present invention is suitably used for forming an electroluminescent layer in an electroluminescent sheet described later. By using this sheet-like luminescent member for the electroluminescent layer, an electroluminescent sheet capable of mass production can be efficiently produced.
次に、本発明の電界発光シートについて説明する。
［電界発光シート］
本発明の電界発光シートは、前述した本発明のシート状発光性部材を、電界発光層として有することを特徴とする。
本発明の電界発光シートの好ましい態様として、少なくとも第１基材、第１電極、電界発光層、第２電極及び第２基材がこの順に積層されてなり、かつ第１基材及び第１電極が透明であるものを挙げることができる。
Next, the electroluminescent sheet of the present invention will be described.
[Electroluminescent sheet]
The electroluminescent sheet of the present invention has the above-described sheet-like luminescent member of the present invention as an electroluminescent layer.
As a preferred embodiment of the electroluminescent sheet of the present invention, at least a first base material, a first electrode, an electroluminescent layer, a second electrode, and a second base material are laminated in this order, and the first base material and the first electrode Is transparent.
（第１基材及び第２基材）
本発明の電界発光シートにおいては、第１基材及び第２基材として、プラスチックフィルムが用いられる。このプラスチックフィルムは、第１基材及び第２基材共に、水分を透過させないフィルム又は水分透過率の極めて低いフィルムが好ましく、また第１基材は、さらに透明性を有することが肝要である。このようなフィルム材料としては、コストや汎用性の点からポリエステル、ポリアミドなどが好ましく、ポリエステルとしては、ポリエチレンテレフタレート、ポリブチレンテレフタレート、ポリエチレンナフタレート、ポリアリレートなどが挙げられる。またポリアミドとしては、全芳香族ポリアミド：ナイロン６、ナイロン６６、ナイロン共重合体などが好ましく挙げられる。用いる基材フィルムの厚さとしては特に制約はなく、通常１〜１０００μｍ、好ましくは５〜５００μｍ、実用性の面から５０〜２００μｍである。
なお、第２基材は特に透明である必要はなく、上記基材の他にアルミ箔、銅箔等の金属箔等も用いることができる。
(First base material and second base material)
In the electroluminescent sheet of the present invention, plastic films are used as the first base material and the second base material. The plastic film is preferably a film that does not transmit moisture or a film that has a very low moisture permeability for both the first substrate and the second substrate, and it is important that the first substrate further has transparency. As such a film material, polyester, polyamide, and the like are preferable from the viewpoint of cost and versatility, and examples of the polyester include polyethylene terephthalate, polybutylene terephthalate, polyethylene naphthalate, and polyarylate. Preferred examples of the polyamide include wholly aromatic polyamides: nylon 6, nylon 66, nylon copolymers, and the like. There is no restriction | limiting in particular as thickness of the base film to be used, Usually, 1-1000 micrometers, Preferably it is 5-500 micrometers, and is 50-200 micrometers from the surface of practical use.
The second substrate need not be particularly transparent, and a metal foil such as an aluminum foil or a copper foil can be used in addition to the above-described substrate.
第１基材は無色透明であってもよいし、有色透明であってもよいが、後述の電界発光層から発せられる光を散乱あるいは減衰等させることがない点で、無色透明であるのが好ましい。
また、第１基材及び第２基材は、その表面又は裏面に、必要により透湿防止層（ガスバリア層）を設けることができる。前記透湿防止層（ガスバリア層）の材料としては、窒化珪素、酸化珪素などの無機物が好適に用いられる。該透湿防止層（ガスバリア層）は、例えば、高周波スパッタリング法などにより形成することができる。
The first substrate may be colorless and transparent, or may be colored and transparent, but is colorless and transparent in that it does not scatter or attenuate light emitted from the electroluminescent layer described below. preferable.
Moreover, the 1st base material and the 2nd base material can provide a moisture-permeable prevention layer (gas barrier layer) on the surface or the back surface as needed. As the material for the moisture permeation preventive layer (gas barrier layer), inorganic materials such as silicon nitride and silicon oxide are preferably used. The moisture permeation preventing layer (gas barrier layer) can be formed by, for example, a high frequency sputtering method.
（第１電極）
本発明の電界発光シートにおける第１電極（陽極）としては、陽極としての機能を有し、透明電極であればよく、特に制限されず、電界発光シートの用途に応じて、公知の陽極の中から適宜選択することができる。その材料としては、例えば、金属、合金、金属酸化物、有機導電性化合物、またはこれらの混合物を好適に挙げられ、仕事関数が４．０ｅＶ以上の材料が好ましい。具体例としては、アンチモンやフッ素等をドープした酸化錫（ＡＴＯ、ＦＴＯ）、酸化錫、酸化亜鉛、酸化インジウム、酸化インジウム錫（ＩＴＯ）、酸化亜鉛インジウム（ＩＺＯ）等の半導性金属酸化物、金、銀、クロム、ニッケル等の金属、さらにこれらの金属と導電性金属酸化物との混合物または積層物、ヨウ化銅、硫化銅などの無機導電性物質、ポリアニリン、ポリチオフェン、ポリピロールなどの有機導電性材料、およびこれらとＩＴＯとの積層物などが好ましく挙げられる。
(First electrode)
The first electrode (anode) in the electroluminescent sheet of the present invention is not particularly limited as long as it has a function as an anode and is a transparent electrode, and may be a known anode according to the use of the electroluminescent sheet. Can be appropriately selected. As the material, for example, a metal, an alloy, a metal oxide, an organic conductive compound, or a mixture thereof can be preferably cited, and a material having a work function of 4.0 eV or more is preferable. Specific examples include semiconducting metal oxides such as tin oxide (ATO, FTO) doped with antimony or fluorine, tin oxide, zinc oxide, indium oxide, indium tin oxide (ITO), indium zinc oxide (IZO), etc. Metals such as gold, silver, chromium and nickel, and mixtures or laminates of these metals and conductive metal oxides, inorganic conductive materials such as copper iodide and copper sulfide, organics such as polyaniline, polythiophene and polypyrrole Preferable examples include conductive materials and laminates of these with ITO.
第１電極は、例えば印刷方式、コーティング方式等の湿式方式、真空蒸着法、スパッタリング法、イオンプレーティング法等の物理的方式、ＣＶＤ、プラズマＣＶＤ法等の化学的方式、などの中から前記材料との適性を考慮して適宜選択した方法に従って前記第１基材上に形成することができる。例えば、第１電極の材料として、ＩＴＯを選択する場合には、該第１電極の形成は、直流あるいは高周波スパッタリング法、真空蒸着法、イオンプレーティング法等に従って行うことができる。また第１電極の材料として有機導電性化合物を選択する場合には湿式製膜法に従って行うことができる。 The first electrode is made of, for example, a printing method, a wet method such as a coating method, a physical method such as a vacuum deposition method, a sputtering method, or an ion plating method, a chemical method such as a CVD method or a plasma CVD method, or the like. In view of the suitability, it can be formed on the first substrate according to a method appropriately selected. For example, when ITO is selected as the material for the first electrode, the first electrode can be formed according to a direct current or high frequency sputtering method, a vacuum deposition method, an ion plating method, or the like. Moreover, when selecting an organic electroconductive compound as a material of a 1st electrode, it can carry out according to the wet film forming method.
第１電極の厚さとしては、前記材料により適宜選択することができ、一概に規定することはできないが、通常１０〜１０００ｎｍであり、２０〜５００ｎｍが好ましく、５０〜２００ｎｍがより好ましい。
第１電極の抵抗値としては、１０3Ω／□以下が好ましく、１０2Ω／□以下がより好ましい。
The thickness of the first electrode can be appropriately selected depending on the material and cannot be generally defined, but is usually 10 to 1000 nm, preferably 20 to 500 nm, and more preferably 50 to 200 nm.
The resistance value of the first electrode is preferably 10 3 Ω / □ or less, and more preferably 10 2 Ω / □ or less.
第１電極は、無色透明であっても、有色透明であってもよいが、無色透明が好ましい。また、該第１電極側から発光を取り出すためには、第１基材と第１電極の積層体の透過率が、６０％以上が好ましく、７０％以上がより好ましい。この透過率は、分光光度計を用いた公知の方法に従って測定することができる。
本発明においては、生じた発光を導光部材となる第１基材に効率良く導光させるために、第１基材にあらかじめ設けられる第１電極は光透過性電極であることが好ましい。特に好ましい第１電極はＩＴＯである。
The first electrode may be colorless and transparent or colored and transparent, but is preferably colorless and transparent. Moreover, in order to take out light emission from the first electrode side, the transmittance of the laminate of the first base material and the first electrode is preferably 60% or more, and more preferably 70% or more. This transmittance can be measured according to a known method using a spectrophotometer.
In the present invention, the first electrode provided in advance on the first base material is preferably a light-transmitting electrode in order to efficiently guide the generated light emission to the first base material serving as the light guide member. A particularly preferred first electrode is ITO.
（第２電極）
本発明の電界発光シートにおける第２電極（陰極）としては、陰極としての機能を有していればよく、特に制限されず、電界発光シートの用途に応じて、公知の陰極の中から適宜選択することができる。
その材料としては、例えば、金属、合金、金属酸化物、および電気伝導性化合物、これらの混合物などが挙げられ、仕事関数が４．５ｅＶ以下のものが好ましい。具体例としてはアルカリ金属（たとえば、Ｌｉ、Ｎａ、Ｋ、またはＣｓ等）、アルカリ土類金属（たとえばＭｇ、Ｃａ等）、金、銀、鉛、アルミニウム、ナトリウム−カリウム合金、リチウム−アルミニウム合金、マグネシウム−銀合金、インジウム、およびイッテルビウム等の希土類金属などが好ましく挙げられる。これらは、単独で使用してもよく、２種以上を組み合わせて使用してもよい。
これらの中で、保全安定性に優れる点で、アルミニウムを主体とする材料が好ましい。アルミニウムを主体とする材料とは、アルミニウム単独、又はアルミニウムと０．０１〜１０質量％程度のアルカリ金属若しくはアルカリ土類金属との合金若しくは混合物（例えば、リチウム−アルミニウム合金、マグネシウム−アルミニウム合金など）をいう。
(Second electrode)
The second electrode (cathode) in the electroluminescent sheet of the present invention is not particularly limited as long as it has a function as a cathode, and is appropriately selected from known cathodes according to the use of the electroluminescent sheet. can do.
Examples of the material include metals, alloys, metal oxides, electrically conductive compounds, mixtures thereof, and the like, and those having a work function of 4.5 eV or less are preferable. Specific examples include alkali metals (for example, Li, Na, K, or Cs), alkaline earth metals (for example, Mg, Ca, etc.), gold, silver, lead, aluminum, sodium-potassium alloys, lithium-aluminum alloys, Preferred are rare earth metals such as magnesium-silver alloy, indium and ytterbium. These may be used alone or in combination of two or more.
Among these, a material mainly composed of aluminum is preferable from the viewpoint of excellent maintenance stability. The material mainly composed of aluminum is aluminum alone or an alloy or mixture of aluminum and an alkali metal or alkaline earth metal of about 0.01 to 10% by mass (for example, lithium-aluminum alloy, magnesium-aluminum alloy, etc.) Say.
第２電極の形成方法に特に制限はなく、公知の方法に従って行うことができる。例えば、印刷方式、コーティング方式等の湿式方式、真空蒸着法、スパッタリング法、イオンプレーティング法等の物理的方式、ＣＶＤ、プラズマＣＶＤ法等の化学的方式、などの中から前記材料との適性を考慮して適宜選択した方法に従って前記第２基材上に形成することができる。例えば、第２電極の材料として、金属等を選択する場合には、その１種又は２種以上を同時又は順次にスパッタ法等に従って行うことができる。 There is no restriction | limiting in particular in the formation method of a 2nd electrode, According to a well-known method, it can carry out. For example, suitability with the above materials from among wet methods such as printing methods, coating methods, physical methods such as vacuum deposition methods, sputtering methods and ion plating methods, chemical methods such as CVD and plasma CVD methods, etc. It can be formed on the second base material according to a method appropriately selected in consideration. For example, when a metal or the like is selected as the material for the second electrode, one or more of them can be simultaneously or sequentially performed according to a sputtering method or the like.
第２電極の厚さとしては、前記材料により適宜選択することができ、一概に規定することはできないが、通常１０〜１０００ｎｍであり、２０〜５００ｎｍが好ましく、５０〜２００ｎｍがより好ましい。なお、この第２電極は、透明であってもよいし、不透明であってもよい。 The thickness of the second electrode can be appropriately selected depending on the material and cannot be generally defined, but is usually 10 to 1000 nm, preferably 20 to 500 nm, and more preferably 50 to 200 nm. The second electrode may be transparent or opaque.
（電界発光層）
本発明の電界発光シートにおける電界発光層は、前述した本発明のシート状発光性部材により形成されたものであり、本発明においては、第１電極、第２電極又は後述の誘導体層に上記シート状発光性部材をラミネートして電界発光層を形成することができる。
上記シート状発光性部材のラミネート法については特に制限はないが、以下に示す本発明のシート状発光性部材の製造方法によれば、効率よくシート状発光性部材を製造することができ、それを用いて電界発光層を形成することができる。
本発明のシート状発光性部材の製造方法によれば、前述の熱可塑性樹脂と電界発光体を混練したのち、押出機を用いてシート状に押出すことにより、シート状発光性部材が効率よく形成される。
(Electroluminescent layer)
The electroluminescent layer in the electroluminescent sheet of the present invention is formed by the above-described sheet-like luminescent member of the present invention. In the present invention, the sheet is formed on the first electrode, the second electrode, or a later-described derivative layer. The electroluminescent layer can be formed by laminating the luminescent member.
The method for laminating the sheet-like luminescent member is not particularly limited. However, according to the method for producing a sheet-like luminescent member of the present invention shown below, the sheet-like luminescent member can be efficiently produced. Can be used to form an electroluminescent layer.
According to the method for producing a sheet-like light-emitting member of the present invention, the sheet-like light-emitting member is efficiently obtained by kneading the above-described thermoplastic resin and the electroluminescent body and then extruding it into a sheet using an extruder. It is formed.
この際、混練機としては、従来公知のリボンブレンダ、ヘンシェルミキサー、バンバリーミキサー、ドラムタンブラー、単軸スクリュー押出機、２軸スクリュー押出機、コニーダ、多軸スクリュー押出機等を用いることができる。混練温度は、使用する熱可塑性樹脂の軟化点よりも通常７０〜１１０℃程度、好ましくは８０〜１００℃高い温度である。なお、この混練時に、本発明の目的が損なわれない範囲で、所望により各種添加剤、例えば酸化防止剤、紫外線吸収剤、光安定剤などを添加することができる。
得られた混練物は、通常ペレット化したのち、押出成形機などを用いて、ダイスよりシート状に押し出す。ダイス温度は、使用する熱可塑性樹脂の軟化点よりも、通常３０〜１２０℃程度、好ましくは７０〜９０℃高い温度である。
At this time, as the kneading machine, a conventionally known ribbon blender, Henschel mixer, Banbury mixer, drum tumbler, single screw extruder, twin screw extruder, conida, multi-screw extruder or the like can be used. The kneading temperature is usually about 70 to 110 ° C., preferably 80 to 100 ° C. higher than the softening point of the thermoplastic resin to be used. In addition, during the kneading, various additives such as an antioxidant, an ultraviolet absorber, a light stabilizer and the like can be added as desired within a range that does not impair the object of the present invention.
The obtained kneaded product is usually pelletized and then extruded into a sheet form from a die using an extruder or the like. The die temperature is usually about 30 to 120 ° C., preferably 70 to 90 ° C. higher than the softening point of the thermoplastic resin to be used.
このようにして得られた電界発光層の厚さは、他層との接合性及び発光性などの観点から、通常１０〜１０００μｍ程度、好ましくは２０〜５００μｍ、より好ましくは３０〜１００μｍである。
なお、前述したように、電界発光層が有機系電界発光材料を含む場合、該電界発光層の第１電極側に正孔注入・輸送層を、第２電極側に電子注入・輸送層を設け、一体化させたものを本発明の電界発光シートに用いることが好ましい。
The thickness of the electroluminescent layer thus obtained is usually about 10 to 1000 μm, preferably 20 to 500 μm, and more preferably 30 to 100 μm, from the viewpoints of bondability with other layers and light emitting properties.
As described above, when the electroluminescent layer contains an organic electroluminescent material, a hole injection / transport layer is provided on the first electrode side of the electroluminescent layer, and an electron injection / transport layer is provided on the second electrode side. It is preferable to use an integrated sheet for the electroluminescent sheet of the present invention.
（誘電体層）
本発明の電界発光シートにおいては、発光効率を高めるために、第１電極と電界発光層との間及び／又は電界発光層と第２電極との間に誘電体材料を含む誘電体層を設けることができる。
誘電体材料としては、例えばＳｉＯ2、ＢａＴｉＯ3、ＳｉＯＮ、Ａｌ2Ｏ3、ＴｉＯ2、Ｓｉ3Ｎ4、ＳｉＡｌＯＮ、Ｙ2Ｏ3、Ｓｍ2Ｏ3、Ｔａ2Ｏ5、ＢａＴａ2Ｏ3、ＰｂＮｂ2Ｏ3、Ｓｒ（Ｚｒ，Ｔｉ）Ｏ3、ＳｒＴｉＯ3、ＰｂＴｉＯ3、ＨｆＯ3などを好ましく挙げることができる。これらは１種を単独で用いてもよく、２種以上を組み合わせて用いてもよい。
(Dielectric layer)
In the electroluminescent sheet of the present invention, in order to increase luminous efficiency, a dielectric layer containing a dielectric material is provided between the first electrode and the electroluminescent layer and / or between the electroluminescent layer and the second electrode. be able to.
Examples of the dielectric material include SiO 2 , BaTiO 3 , SiON, Al 2 O 3 , TiO 2 , Si 3 N 4 , SiAlON, Y 2 O 3 , Sm 2 O 3 , Ta 2 O 5 , BaTa 2 O 3 , PbNb 2 O 3 , Sr (Zr, Ti) O 3 , SrTiO 3 , PbTiO 3 , HfO 3 and the like can be preferably exemplified. These may be used individually by 1 type and may be used in combination of 2 or more type.
誘電体層は、例えば適当なバインダー樹脂中に、前記誘電体材料を均質分散させたものを、従来公知の塗工法、例えばスプレー法やナイフコート法、ロールコート法、バーコート法、ブレードコート法、ダイコート法、グラビアコート法などにより塗工する方法、あるいは押出し機を用いて形成することができる。 For example, the dielectric layer is obtained by uniformly dispersing the dielectric material in a suitable binder resin, and a conventionally known coating method such as a spray method, a knife coating method, a roll coating method, a bar coating method, a blade coating method, or the like. It can be formed by using a die coating method, a gravure coating method or the like, or using an extruder.
誘電体層は、本発明の電界発光シートを交流で駆動させる場合において、電界発光層の電気伝導度が高すぎて電界発光層に十分な電圧を印加しにくい場合、あるいは過大電流により絶縁破壊が起こるおそれがある場合等において、それらを制御する効果を発揮する。当該誘電体層の厚さは、上記効果を良好に発揮させる観点から、通常０．１〜１００μｍ程度、好ましくは１０〜５０μｍである。 In the case where the electroluminescent sheet of the present invention is driven with an alternating current, the dielectric layer is subject to dielectric breakdown due to excessive electric current when the electric conductivity of the electroluminescent layer is too high or a sufficient voltage cannot be applied to the electroluminescent layer. In the case where there is a possibility of occurrence, the effect of controlling them is exhibited. The thickness of the dielectric layer is usually about 0.1 to 100 μm, preferably 10 to 50 μm, from the viewpoint of satisfactorily exhibiting the above effects.
なお、誘電体層は、後述の電界発光シートの製造方法において詳しく説明するが、それが設けられる位置によっては、熱ラミネート性を有することが、電界発光シートの製造の簡便さなどから、有利である。この場合、バインダー樹脂として、熱ラミネート性を有する前述の熱可塑性樹脂を用いることができる。 The dielectric layer will be described in detail in a method for manufacturing an electroluminescent sheet, which will be described later. However, depending on the position where the dielectric layer is provided, it is advantageous to have thermal laminating properties because of the ease of manufacturing the electroluminescent sheet. is there. In this case, the above-mentioned thermoplastic resin having heat laminating properties can be used as the binder resin.
次に、前述した本発明の電界発光シートを製造する方法について説明する。
［電界発光シートの製造方法］
本発明に係る電界発光シートの製造方法の一態様によれば、下記（１）又は（２）の工程で第１積層体及び第２積層体を作製し、第１積層体のシート状発光性部材側と第２積層体の第２電極側、又は第１積層体の第１電極側と第２積層体のシート状発光性部材側とを、それぞれ熱ラミネートにより接合することにより、前述した本発明の電界発光シートが得られる。
（１）第１基材上に少なくとも第１電極及び本発明のシート状発光性部材を電界発光層として順に形成することで第１積層体を作製し、別に第２基材上に少なくとも第２電極を形成することで第２積層体を作製する工程。
（２）第１基材上に少なくとも第１電極を形成することで第１積層体を作製し、別に第２基材上に少なくとも第２電極及び本発明のシート状発光性部材を電界発光層として順に形成することで第２積層体を作製する工程。
Next, a method for producing the above-described electroluminescent sheet of the present invention will be described.
[Method for producing electroluminescent sheet]
According to one aspect of the method for producing an electroluminescent sheet according to the present invention, the first laminate and the second laminate are produced in the following step (1) or (2), and the sheet-like light emitting property of the first laminate is obtained. By joining the member side and the second electrode side of the second laminated body, or the first electrode side of the first laminated body and the sheet-like luminescent member side of the second laminated body, respectively by thermal lamination, the above-described book The electroluminescent sheet of the invention is obtained.
(1) A first laminate is produced by sequentially forming at least a first electrode and a sheet-like luminescent member of the present invention as an electroluminescent layer on a first substrate, and separately at least a second layer on a second substrate. The process of producing a 2nd laminated body by forming an electrode.
(2) A first laminate is produced by forming at least a first electrode on a first substrate, and at least the second electrode and the sheet-like luminescent member of the present invention are separately provided on an electroluminescent layer on a second substrate. The process of producing a 2nd laminated body by forming in order.
本発明の製造方法においては、第１積層体及び第２積層体の構成を、それぞれ下記のように記号で表す。
すなわち、第１基材を「１」、第２基材を「２」で表し、第１電極を「Ｅ1」、第２電極を「Ｅ2」で表し、電界発光層を「Ｌ」で表す。また、後述の誘電体層は「Ｄ」で表す。
In the manufacturing method of this invention, the structure of a 1st laminated body and a 2nd laminated body is each represented with a symbol as follows.
That is, the first substrate is represented by “1”, the second substrate is represented by “2”, the first electrode is represented by “E 1 ”, the second electrode is represented by “E 2 ”, and the electroluminescent layer is represented by “L”. Represent. Further, a dielectric layer to be described later is represented by “D”.
上記（１）の工程を経る方法においては、第１積層体として、１−Ｅ1−Ｌの構成のものが得られ、第２積層体として、２−Ｅ2の構成のものが得られる。この第１積層体と第２積層体を、ＬとＥ2を対面させて熱ラミネートによって接合することにより、１−Ｅ1−Ｌ−Ｅ2−２の構成の電界発光シート（ａ）が得られる。 In the method through the step (1), a 1-E 1 -L configuration is obtained as the first laminate, and a 2-E 2 configuration is obtained as the second laminate. The first laminated body and the second laminated body are joined by thermal lamination with L and E 2 facing each other, thereby obtaining an electroluminescent sheet (a) having a configuration of 1-E 1 -LE 2 -2. It is done.
また、上記（２）の工程を経る方法においては、第１積層体として、１−Ｅ1の構成のものが得られ、第２積層体として、２−Ｅ2−Ｌの構成のものが得られる。この第１積層体と第２積層体を、Ｅ1とＬを対面させて熱ラミネートによって接合することにより、１−Ｅ1−Ｌ−Ｅ2−２の構成の電界発光シート（ａ）が得られる。
上記電界発光シート（ａ）の構成を示す断面模式図を図１に示す。また、上記（１）、（２）の工程を経て得られる第１積層体の構成、第２積層体の構成及び得られた電界発光シートの構成を表１に示す。
Further, in the method using the above step (2), first laminate obtained having a structure of 1-E 1, the second laminate obtained those 2-E 2 -L configuration It is done. The first laminated body and the second laminated body are bonded by thermal lamination with E 1 and L facing each other, whereby an electroluminescent sheet (a) having a configuration of 1-E 1 -LE 2 -2 is obtained. It is done.
FIG. 1 is a schematic cross-sectional view showing the configuration of the electroluminescent sheet (a). Table 1 shows the configuration of the first laminate obtained through the steps (1) and (2), the configuration of the second laminate, and the configuration of the obtained electroluminescent sheet.
本発明の製造方法においては、下記（３）〜（１２）のいずれかの工程により第１積層体及び第２積層体を作製し、第１積層体の誘電体層側、電界発光層側又は第１電極側と、第２積層体の第２電極側、電界発光層側又は誘電体層側とを、それぞれ熱ラミネートによって接合することにより、前述した本発明の電界発光シートを得ることができる。 In the production method of the present invention, the first laminated body and the second laminated body are produced by any one of the following steps (3) to (12), and the dielectric layer side, the electroluminescent layer side or the first laminated body The electroluminescent sheet of the present invention described above can be obtained by joining the first electrode side and the second electrode side, the electroluminescent layer side or the dielectric layer side of the second laminate by thermal lamination. .
（３）第１基材上に少なくとも第１電極、誘電体層及び本発明の電界発光層をこの順に形成することで第１積層体を作製し、別に第２基材上に少なくとも第２電極を形成することで第２積層体を作製する工程。
（４）第１基材上に少なくとも第１電極及び誘電体層を順に形成することで第１積層体を作製し、別に第２基材上に少なくとも第２電極及び本発明の電界発光層を順に形成することで第２積層体を作製する工程。
（５）第１基材上に少なくとも第１電極を形成することで第１積層体を作製し、別に第２基材上に少なくとも第２電極、本発明の電界発光層及び誘電体層をこの順で形成することで第２積層体を作製する工程。
（６）第１基材上に少なくとも第１電極、本発明の電界発光層及び誘電体層をこの順に形成することで第１積層体を作製し、別に第２基材上に少なくとも第２電極を形成することで第２積層体を作製する工程。
（７）第１基材上に少なくとも第１電極及び本発明の電界発光層を順に形成することで第１積層体を作製し、別に第２基材上に少なくとも第２電極及び誘電体層を順に形成することで第２積層体を作製する工程。
（８）第１基材上に少なくとも第１電極を形成することで第１積層体を作製し、別に第２基材上に少なくとも第２電極、誘電体層及び本発明の電界発光層をこの順に形成することで第２積層体を作製する工程。
（９）第１基材上に少なくとも第１電極、誘電体層、本発明の電界発光層及び誘電体層をこの順に形成することで第１積層体を作製し、別に第２基材上に少なくとも第２電極を形成することで第２積層体を作製する工程。
（１０）第１基材上に少なくとも第１電極、誘電体層及び本発明の電界発光層をこの順に形成することで第１積層体を作製し、別に第２基材上に少なくとも第２電極及び誘電体層を順に形成することで第２積層体を作製する工程。
（１１）第１基材上に少なくとも第１電極及び誘電体層を順に形成することで第１積層体を作製し、別に第２基材上に少なくとも第２電極、誘電体層及び本発明の電界発光層をこの順に形成することで第２積層体を作製する工程。
（１２）第１基材上に少なくとも第１電極を形成することで第１積層体を作製し、別に第２基材上に少なくとも第２電極、誘電体層、本発明の電界発光層及び誘電体層をこの順に形成することで第２積層体を作製する工程。
ここで、（９）〜（１２）における第１電極側と第２電極側の誘電体層は同一であっても異なってもよい。
(3) A first laminate is produced by forming at least a first electrode, a dielectric layer, and an electroluminescent layer of the present invention in this order on a first substrate, and separately at least a second electrode on the second substrate. The process of producing a 2nd laminated body by forming.
(4) A first laminate is produced by sequentially forming at least a first electrode and a dielectric layer on a first substrate, and at least a second electrode and an electroluminescent layer of the present invention are separately formed on a second substrate. The process of producing a 2nd laminated body by forming in order.
(5) A first laminate is produced by forming at least a first electrode on a first substrate, and at least a second electrode, an electroluminescent layer and a dielectric layer of the present invention are separately provided on a second substrate. The process of producing a 2nd laminated body by forming in order.
(6) A first laminate is produced by forming at least the first electrode, the electroluminescent layer of the present invention, and the dielectric layer in this order on the first base material, and separately at least the second electrode on the second base material. The process of producing a 2nd laminated body by forming.
(7) A first laminate is produced by sequentially forming at least a first electrode and an electroluminescent layer of the present invention on a first substrate, and at least a second electrode and a dielectric layer are separately formed on a second substrate. The process of producing a 2nd laminated body by forming in order.
(8) A first laminated body is produced by forming at least a first electrode on a first substrate, and at least a second electrode, a dielectric layer and an electroluminescent layer of the present invention are formed on the second substrate. The process of producing a 2nd laminated body by forming in order.
(9) A first laminate is produced by forming at least the first electrode, the dielectric layer, the electroluminescent layer of the present invention, and the dielectric layer in this order on the first substrate, and separately on the second substrate. The process of producing a 2nd laminated body by forming a 2nd electrode at least.
(10) A first laminate is produced by forming at least a first electrode, a dielectric layer, and an electroluminescent layer of the present invention in this order on a first substrate, and separately at least a second electrode on the second substrate. And a step of forming the second stacked body by sequentially forming the dielectric layers.
(11) A first laminate is produced by sequentially forming at least a first electrode and a dielectric layer on a first substrate, and at least a second electrode, a dielectric layer and the present invention are separately formed on a second substrate. The process of producing a 2nd laminated body by forming an electroluminescent layer in this order.
(12) A first laminate is produced by forming at least a first electrode on a first substrate, and separately at least a second electrode, a dielectric layer, an electroluminescent layer and a dielectric according to the present invention on a second substrate. The process of producing a 2nd laminated body by forming a body layer in this order.
Here, the dielectric layers on the first electrode side and the second electrode side in (9) to (12) may be the same or different.
上記（３）の工程を経る方法においては、第１積層体として、１−Ｅ1−Ｄ−Ｌの構成のものが得られ、第２積層体として、２−Ｅ2の構成のものが得られる。この第１積層体と第２積層体を、ＬとＥ2を対面させて熱ラミネートによって接合することにより、１−Ｅ1−Ｄ−Ｌ−Ｅ2−２の構成の電界発光シート（ｂ）が得られる。
上記（４）の工程を経る方法においては、第１積層体として、１−Ｅ1−Ｄの構成のものが得られ、第２積層体として、２−Ｅ2−Ｌの構成のものが得られる。この第１積層体と第２積層体を、ＤとＬを対面させて熱ラミネートによって接合することにより、１−Ｅ1−Ｄ−Ｌ−Ｅ2−２の構成の電界発光シート（ｂ）が得られる。
上記（５）の工程を経る方法においては、第１積層体として、１−Ｅ1の構成のものが得られ、第２積層体として、２−Ｅ2−Ｌ−Ｄの構成のものが得られる。この第１積層体と第２積層体を、Ｅ1とＤを対面させて熱ラミネートによって接合することにより、１−Ｅ1−Ｄ−Ｌ−Ｅ2−２の構成の電界発光シート（ｂ）が得られる。この場合、誘電体層Ｄは第１電極Ｅ1と接合するため、熱ラミネート性を有することが好ましい。
上記（６）の工程を経る方法においては、第１積層体として、１−Ｅ1−Ｌ−Ｄの構成のものが得られ、第２積層体として、２−Ｅ2の構成のものが得られる。この第１積層体と第２積層体を、ＤとＥ2を対面させて熱ラミネートによって接合することにより、１−Ｅ1−Ｌ−Ｄ−Ｅ2−２の構成の電界発光シート（ｃ）が得られる。この場合、誘電体Ｄは第２電極と接合するため、熱ラミネート性を有することが好ましい。
In the method through the step (3), a 1-E 1 -DL configuration is obtained as the first laminate, and a 2-E 2 configuration is obtained as the second laminate. It is done. The first laminated body and the second laminated body are joined by thermal lamination with L and E 2 facing each other, whereby an electroluminescent sheet having a configuration of 1-E 1 -DLE 2 -2 (b) Is obtained.
In the method through the step (4), a 1-E 1 -D configuration is obtained as the first laminate, and a 2-E 2 -L configuration is obtained as the second laminate. It is done. The first laminate and the second laminate are joined by thermal lamination with D and L facing each other, whereby an electroluminescent sheet (b) having a configuration of 1-E 1 -DLE 2 -2 is obtained. can get.
In the method through the step (5), a 1-E 1 structure is obtained as the first laminate, and a 2-E 2 -LD structure is obtained as the second laminate. It is done. The first laminated body and the second laminated body are joined by thermal lamination with E 1 and D facing each other, whereby an electroluminescent sheet having a configuration of 1-E 1 -DLE 2 -2 (b) Is obtained. In this case, since the dielectric layer D is bonded to the first electrode E 1 , it is preferable to have a heat laminating property.
In the method through the step (6), a 1-E 1 -LD configuration is obtained as the first laminate, and a 2-E 2 configuration is obtained as the second laminate. It is done. The first laminated body and the second laminated body are joined by thermal lamination with D and E 2 facing each other, thereby forming an electroluminescent sheet (c) having a configuration of 1-E 1 -LDE 2 -2. Is obtained. In this case, since the dielectric D is bonded to the second electrode, it preferably has a heat laminating property.
上記（７）の工程を経る方法においては、第１積層体として、１−Ｅ1−Ｌの構成のものが得られ、第２積層体として、２−Ｅ2−Ｄの構成のものが得られる。この第１積層体と第２積層体を、ＬとＤを対面させて熱ラミネートによって接合することにより、１−Ｅ1−Ｌ−Ｄ−Ｅ2−２の構成の電界発光シート（ｃ）が得られる。
上記（８）の工程を経る方法においては、第１積層体として、１−Ｅ1の構成のものが得られ、第２積層体として、２−Ｅ2−Ｄ−Ｌの構成のものが得られる。この第１積層体と第２積層体を、Ｅ1とＬを対面させて熱ラミネートによって接合することにより、１−Ｅ1−Ｌ−Ｄ−Ｅ2−２の構成の電界発光シート（ｃ）が得られる。
上記（９）の工程を経る方法においては、第１積層体として、１−Ｅ1−Ｄ−Ｌ−Ｄ’の構成のものが得られ、第２積層体として、２−Ｅ2の構成のものが得られる。この第１積層体と第２積層体を、Ｄ’とＥ2を対面させて熱ラミネートによって接合することにより、１−Ｅ1−Ｄ−Ｌ−Ｄ’−Ｅ2−２の構成の電界発光シート（ｄ）が得られる。この場合、誘電体層Ｄと誘電体層Ｄ’は、同一でも異なっていてもよく、また誘電体層Ｄ’は第２電極Ｅ2と接合するため、熱ラミネート性を有することが好ましい。
In the method through the step (7), a 1-E 1 -L configuration is obtained as the first laminate, and a 2-E 2 -D configuration is obtained as the second laminate. It is done. The first laminate and the second laminate are joined by thermal lamination with L and D facing each other, whereby an electroluminescent sheet (c) having a configuration of 1-E 1 -LDE 2 -2 is obtained. can get.
In the method through the step (8), a first laminate having a configuration of 1-E 1 is obtained, and a second laminate having a configuration of 2-E 2 -DL is obtained. It is done. The first laminated body and the second laminated body are joined by thermal lamination with E 1 and L facing each other, whereby an electroluminescent sheet (c) having a configuration of 1-E 1 -LDE 2 -2 Is obtained.
In the method through the step (9), a first laminate having a configuration of 1-E 1 -DLD ′ is obtained, and a second laminate having a configuration of 2-E 2 is obtained. Things are obtained. The first laminated body and the second laminated body are joined by thermal lamination with D ′ and E 2 facing each other, whereby electroluminescence having a configuration of 1-E 1 -DLD′-E 2 -2 is obtained. A sheet (d) is obtained. In this case, the dielectric layer D and the dielectric layer D ′ may be the same or different, and since the dielectric layer D ′ is bonded to the second electrode E 2 , it is preferable to have a heat laminating property.
上記（１０）の工程を経る方法においては、第１積層体として、１−Ｅ1−Ｄ−Ｌの構成のものが得られ、第２積層体として、２−Ｅ2−Ｄ’の構成のものが得られる。この第１積層体と第２積層体を、ＬとＤ’を対面させて熱ラミネートによって接合することにより、１−Ｅ1−Ｄ−Ｌ−Ｄ’−Ｅ2−２の構成の電界発光シート（ｄ）が得られる。この場合、誘電体層Ｄと誘電体層Ｄ’は、同一でも異なっていてもよい。
上記（１１）の工程を経る方法においては、第１積層体として、１−Ｅ1−Ｄの構成のものが得られ、第２積層体として、２−Ｅ2−Ｄ’−Ｌの構成のものが得られる。この第１積層体と第２積層体を、ＤとＬを対面させて熱ラミネートによって接合することにより、１−Ｅ1−Ｄ−Ｌ−Ｄ’−Ｅ2−２の構成の電界発光シート（ｄ）が得られる。この場合、誘電体層Ｄ及び誘電体層Ｄ’は同一でも異なっていてもよい。
上記（１２）の工程を経る方法においては、第１積層体として、１−Ｅ1の構成のものが得られ、第２積層体として、２−Ｅ2−Ｄ’−Ｌ−Ｄの構成のものが得られる。この第１積層体と第２積層体を、Ｅ1とＤを対面させて熱ラミネートによって接合することにより、１−Ｅ1−Ｄ−Ｌ−Ｄ’−Ｅ2−２の構成の電界発光シート（ｄ）が得られる。この場合、誘電体層Ｄと誘電体層Ｄ’は同一でも異なっていてもよく、また誘電体層Ｄは第１電極Ｅ1と接合するため、熱ラミネート性を有することが好ましい。
In the method through the step (10), a first laminate having a configuration of 1-E 1 -DL is obtained, and a second laminate having a configuration of 2-E 2 -D ′. Things are obtained. The first laminated body and the second laminated body are joined by thermal lamination with L and D ′ facing each other, thereby forming an electroluminescent sheet having a configuration of 1-E 1 -DLD′-E 2 -2. (D) is obtained. In this case, the dielectric layer D and the dielectric layer D ′ may be the same or different.
In the method through the step (11), a first laminate having a configuration of 1-E 1 -D is obtained, and a second laminate having a configuration of 2-E 2 -D′-L. Things are obtained. The first laminated body and the second laminated body are joined by thermal lamination with D and L facing each other, whereby an electroluminescent sheet having a configuration of 1-E 1 -DLD′-E 2 -2 ( d) is obtained. In this case, the dielectric layer D and the dielectric layer D ′ may be the same or different.
In the method through the step (12), a 1-E 1 structure is obtained as the first laminated body, and a 2-E 2 -D′-LD structure is obtained as the second laminated body. Things are obtained. The first laminated body and the second laminated body are joined by thermal lamination with E 1 and D facing each other, thereby forming an electroluminescent sheet having a configuration of 1-E 1 -DLD′-E 2 -2. (D) is obtained. In this case, the dielectric layer D and the dielectric layer D ′ may be the same or different, and since the dielectric layer D is bonded to the first electrode E 1 , it is preferable to have a heat laminating property.
上記電界発光シート（ｂ）、（ｃ）及び（ｄ）の構成を示す断面模式図を、それぞれ図２、図３及び図４に示す。
また、上記（３）〜（１２）の工程を経る方法における第１積層体の構成、第２積層体の構成及び得られる電界発光シートの構成を表１に示す。
Cross-sectional schematic diagrams showing the configurations of the electroluminescent sheets (b), (c), and (d) are shown in FIGS. 2, 3, and 4, respectively.
Table 1 shows the configuration of the first laminate, the configuration of the second laminate, and the configuration of the electroluminescent sheet obtained in the method through the steps (3) to (12).
本発明の電界発光シートの製造方法は前記のように各層を第１積層体と第２積層体から製造する方法に制限されず、前記の製造方法を利用して、３つ以上の積層体を用いることよっても電界発光シートを製造することも可能である。 The method for producing the electroluminescent sheet of the present invention is not limited to the method for producing each layer from the first laminate and the second laminate as described above, and three or more laminates can be formed using the production method. Even if it uses, it is also possible to manufacture an electroluminescent sheet.
本発明に係る電界発光シートの製造方法の別の態様によれば、第１基材上に少なくとも第１電極を形成して第１積層体を作成し、別に第２基材上に少なくとも第２電極を形成して第２積層体を作製し、第１積層体の第１電極側と第２積層体の第２電極側とを、本発明のシート状発光性部材を電界発光層として用いて接合して電界発光シートを製造することができる。第１基材、第２基材、第１電極、第２電極及びシート状発光性部材は前記と同様のものを使用することができる。本態様においては、熱可塑性樹脂と電界発光体を混練したあと、押出機によりシート状に押出されて形成されたシート状発光性部材を、第１積層体の第１電極側と第２積層体の第２電極側との間に載置し、２本の加熱されたロールの間を通すことにより熱ラミネートして接合してもよいし、押出機により熱可塑性樹脂と電界発光体との混練物を押出して第１積層体の第１電極側と第２積層体の第２電極側とを接合してもよい。 According to another aspect of the method for producing an electroluminescent sheet according to the present invention, at least a first electrode is formed on a first base material to form a first laminate, and separately on at least a second base material. An electrode is formed to produce a second laminated body, and the first electrode side of the first laminated body and the second electrode side of the second laminated body are used using the sheet-like luminescent member of the present invention as an electroluminescent layer. An electroluminescent sheet can be manufactured by bonding. The same thing as the above can be used for the 1st substrate, the 2nd substrate, the 1st electrode, the 2nd electrode, and the sheet-like luminous member. In this aspect, after kneading the thermoplastic resin and the electroluminescent body, the sheet-like luminescent member formed by being extruded into a sheet shape by an extruder is used as the first electrode side and the second laminated body of the first laminated body. It may be placed between the second electrode side and thermally laminated by passing between two heated rolls, or the thermoplastic resin and electroluminescent material may be kneaded by an extruder The product may be extruded to join the first electrode side of the first laminate and the second electrode side of the second laminate.
このような本発明の製造方法によれば、（ｉ）電界発光層を、熱ラミネート性を有するシート状発光性部材を用いて形成することにより、（ｉｉ）さらに必要に応じて、誘電体層を熱ラミネート性を有するものにすることにより、所望の構成の電界発光シートを、極めて簡便に、生産性よく、製造することができる。したがって、本発明の製造方法は、電界発光シートの大量生産に適している。
本発明の電界発光シートは、大量生産が可能であり、例えば商業ビルの窓や自動車などへ設置する広告媒体、装飾用媒体、あるいは防犯用シートなどのバックライト等として好適に用いられる。
According to such a production method of the present invention, (i) the electroluminescent layer is formed by using a sheet-like luminescent member having a heat laminating property, and (ii) further, if necessary, a dielectric layer By having a heat laminating property, it is possible to manufacture an electroluminescent sheet having a desired configuration extremely simply and with high productivity. Therefore, the manufacturing method of the present invention is suitable for mass production of electroluminescent sheets.
The electroluminescent sheet of the present invention can be mass-produced, and is suitably used as a backlight for advertisement media, decoration media, security sheets, etc. installed in commercial building windows and automobiles, for example.
次に、本発明を実施例によりさらに詳細に説明するが、本発明は、これらの例によってなんら限定されるものではない。
なお、熱可塑性樹脂の軟化点は、下記のようにして測定した。
＜熱可塑性樹脂の軟化点の測定＞
ＪＩＳ Ｋ ６８６３に準拠し、測定を行った。
また、各実施例における輝度及び照度、電界発光シートの破断強度測定は、下記のようにして測定した。
＜輝度の測定＞
輝度測定装置（コニカミノルタ社製「ＬＳ−１００」）を用いて、電界発光シートを２００Ｖ、２０００Ｈｚの条件で駆動させた時の発光輝度を測定した。
＜照度の測定＞
電界発光シートを２００Ｖ、２０００Ｈｚの条件で駆動させ、発光面から１０ｃｍ離れた距離の照度を照度測定装置（コニカミノルタ社製「ＣＬ−２００」）を用いて測定した。
＜シート状発光性部材の破断強度の測定＞
ＪＩＳ Ｋ ７１２７に準拠し、万能引張試験機（島津製作所社製、精密万能試験機「島津オートグラフ ＡＧ−１ ２０ｋＮ」）を用いて、試験速度２００ｍ／ｍｉｎの条件で、破断強度を測定した。
EXAMPLES Next, although an Example demonstrates this invention further in detail, this invention is not limited at all by these examples.
The softening point of the thermoplastic resin was measured as follows.
<Measurement of softening point of thermoplastic resin>
Measurement was performed in accordance with JIS K 6863.
Moreover, the brightness | luminance and illuminance in each Example, and the breaking strength measurement of an electroluminescent sheet | seat were measured as follows.
<Measurement of brightness>
Using a luminance measuring device (“LS-100” manufactured by Konica Minolta Co., Ltd.), the emission luminance was measured when the electroluminescent sheet was driven under the conditions of 200 V and 2000 Hz.
<Measurement of illuminance>
The electroluminescent sheet was driven under the conditions of 200 V and 2000 Hz, and the illuminance at a distance of 10 cm from the light emitting surface was measured using an illuminance measuring device (“CL-200” manufactured by Konica Minolta).
<Measurement of breaking strength of sheet-like luminescent member>
In accordance with JIS K 7127, the breaking strength was measured using a universal tensile testing machine (manufactured by Shimadzu Corporation, precision universal testing machine “Shimadzu Autograph AG-1 20 kN”) at a test speed of 200 m / min.
製造例１ 基材付き第１電極の作製
巾３００ｍｍ、厚さ１００μｍのポリエチレンナフタレート（ＰＥＮ）フィルム（帝人デュポン社製、「Ｑ６５ＦＡ」）に、巻き取り式スパッタ装置を用いて、ライン速度０．２ｍ／分、アルゴン・酸素雰囲気下におけるチャンバー内圧力２．０×１０-1Ｐａ、円筒型ＩＴＯターゲットに１５００Ｗの電力を印加し、スパッタリングにより、厚さ１００ｎｍのＩＴＯ透明導電膜を形成し、基材付き第１電極を作製した。なお、巻き取り式スパッタ装置は、ロック技研工業（株）製マグネトロン型スパッタ装置を用いた。
Production Example 1 Production of First Electrode with Base Material A polyethylene naphthalate (PEN) film having a width of 300 mm and a thickness of 100 μm (“Q65FA” manufactured by Teijin DuPont Co., Ltd.) was used to form a line speed of 0. An ITO transparent conductive film having a thickness of 100 nm is formed by sputtering by applying 1500 W of power to a cylindrical ITO target at a pressure of 2 m / min in an atmosphere of argon and oxygen in an atmosphere of oxygen and oxygen of 2.0 × 10 −1 Pa. A first electrode with a material was produced. Note that a magnetron type sputtering apparatus manufactured by Rock Giken Co., Ltd. was used as the winding type sputtering apparatus.
製造例２ 基材付き第２電極の作製
巾３００ｍｍ、厚さ１００μｍのＰＥＮフィルム（帝人デュポン社製、「Ｑ６５ＦＡ」）に、巻き取り式スパッタ装置（ロック技研工業（株）製マグネトロン型スパッタ装置）を用いて、ライン速度０．２ｍ／分、アルゴン雰囲気下におけるチャンバー内圧力２．０×１０-1Ｐａ、円筒型Ａｌターゲットに２５００Ｗの電力を印加し、スパッタリングにより、厚さ１００ｎｍのＡｌ薄膜を形成し、基材付き第２電極を作製した。
Production Example 2 Production of Second Electrode with Base Material A PEN film having a width of 300 mm and a thickness of 100 μm (“Q65FA” manufactured by Teijin DuPont Co., Ltd.) and a take-up type sputtering device (magnetron type sputtering device manufactured by Rock Giken Co., Ltd.) , A line speed of 0.2 m / min, a pressure in a chamber of 2.0 × 10 −1 Pa in an argon atmosphere, a power of 2500 W is applied to a cylindrical Al target, and an Al thin film having a thickness of 100 nm is formed by sputtering. Then, a second electrode with a base material was produced.
実施例１
エチレン−酢酸ビニル共重合樹脂（三井・デュポンポリケミカル社製、「ＥＶＡＦＬＥＸ ＥＶ１５０」、軟化点３４℃）１００質量部と、ＺｎＳ・ＣｕからなるＥＬ蛍光体（オスラムシルバニア社製、「ＧＧＳ４２Ｇｒｅｅｎ」、平均粒径２５μｍ）４００質量部とを、二軸押出混練機（テクノベル社製、「ＫＺＷ２５ＴＷＩＮ−３０ＭＧ−ＳＴＭ」）により、１３０℃にて混練して、ペレットを作製した。次いで、押出試験機（東洋精機製作所製、「ラボプラストミル３０Ｃ１５０」）を用いダイス温度１１５℃とし、膜厚５０μｍのシート状発光性部材を、製造例２で得た基材付き第２電極上に押出し、該第２電極にラミネートされた電界発光層を形成し、第２積層体を作製した。
次に、この第２積層体の電界発光層面と、製造例１で得た基材付き第１電極（第１積層体）とを、該第２積層体の巻取り部にて１５０℃での熱ラミネートにより、接合し、電界発光シートを作製した。
この電界発光シートの性能評価結果を表２に示す。
Example 1
100 mass parts of ethylene-vinyl acetate copolymer resin (Mitsui / DuPont Polychemical Co., Ltd., “EVAFLEX EV150”, softening point 34 ° C.) and ZnS / Cu EL phosphor (manufactured by OSRAM Sylvania Co., “GGS42Green”, average 400 parts by mass of a particle size of 25 μm was kneaded at 130 ° C. by a twin-screw extrusion kneader (manufactured by Technobell, “KZW25TWIN-30MG-STM”) to prepare pellets. Next, a sheet-like luminescent member having a film thickness of 50 μm was obtained on the second electrode with a base material obtained in Production Example 2 using an extrusion tester (“Labo Plast Mill 30C150” manufactured by Toyo Seiki Seisakusho Co., Ltd.). And an electroluminescent layer laminated on the second electrode was formed to produce a second laminate.
Next, the surface of the electroluminescent layer of the second laminate and the first electrode with the base material (first laminate) obtained in Production Example 1 at 150 ° C. at the winding portion of the second laminate. Bonding was performed by heat lamination to produce an electroluminescent sheet.
Table 2 shows the performance evaluation results of the electroluminescent sheet.
実施例２
実施例１において、エチレン−酢酸ビニル共重合樹脂１００質量部に対して、ＺｎＳ・ＣｕからなるＥＬ蛍光体を３００質量部混練したこと以外は、実施例１と同様にして、電界発光シートを作製した。その性能評価結果を表２に示す。
Example 2
In Example 1, an electroluminescent sheet was produced in the same manner as in Example 1, except that 300 parts by mass of EL phosphor made of ZnS · Cu was kneaded with 100 parts by mass of ethylene-vinyl acetate copolymer resin. did. The performance evaluation results are shown in Table 2.
実施例３
実施例１において、エチレン−酢酸ビニル共重合樹脂１００質量部に対して、ＺｎＳ・ＣｕからなるＥＬ蛍光体を２００質量部混練したこと以外は、実施例１と同様にして、電界発光シートを作製した。その性能評価結果を表２に示す。
Example 3
In Example 1, an electroluminescent sheet was produced in the same manner as in Example 1, except that 200 parts by mass of EL phosphor made of ZnS · Cu was kneaded with 100 parts by mass of ethylene-vinyl acetate copolymer resin. did. The performance evaluation results are shown in Table 2.
実施例４
実施例１において、エチレン−酢酸ビニル共重合樹脂１００質量部に対して、ＺｎＳ・ＣｕからなるＥＬ蛍光体を１００質量部混練したこと以外は、実施例１と同様にして、電界発光シートを作製した。その性能評価結果を表２に示す。
Example 4
In Example 1, an electroluminescent sheet was produced in the same manner as in Example 1 except that 100 parts by mass of an EL phosphor made of ZnS · Cu was kneaded with 100 parts by mass of an ethylene-vinyl acetate copolymer resin. did. The performance evaluation results are shown in Table 2.
実施例５
実施例１において、エチレン−酢酸ビニル共重合樹脂１００質量部に対して、ＺｎＳ・ＣｕからなるＥＬ蛍光体を５０質量部混練したこと以外は、実施例１と同様にして、電界発光シートを作製した。その性能評価結果を表２に示す。
Example 5
In Example 1, an electroluminescent sheet was prepared in the same manner as in Example 1 except that 50 parts by mass of EL phosphor made of ZnS · Cu was kneaded with 100 parts by mass of ethylene-vinyl acetate copolymer resin. did. The performance evaluation results are shown in Table 2.
実施例６
実施例１において、エチレン−酢酸ビニル共重合樹脂の代わりに、エチレン−メタクリル酸共重合体（三井・デュポンポリケミカル社製、「ＮＵＣＲＥＬ ＡＮ４９０２１Ｃ」、軟化点９２℃）を用いて混練温度を２００℃、ダイス温度を１８５℃とした以外は、実施例１と同様にして、電界発光シートを作製した。その性能評価結果を表２に示す。
Example 6
In Example 1, instead of the ethylene-vinyl acetate copolymer resin, an ethylene-methacrylic acid copolymer (Mitsui DuPont Polychemical Co., Ltd., “NUCREL AN49021C”, softening point 92 ° C.) was used, and the kneading temperature was 200 ° C. An electroluminescent sheet was produced in the same manner as in Example 1 except that the die temperature was 185 ° C. The performance evaluation results are shown in Table 2.
実施例７
実施例６において、エチレン−メタクリル酸共重合体１００質量部に対して、ＺｎＳ・ＣｕからなるＥＬ蛍光体を３００質量部混練した以外は、実施例６と同様にして、電界発光シートを作製した。その性能評価結果を表２に示す。
Example 7
In Example 6, an electroluminescent sheet was produced in the same manner as in Example 6, except that 300 parts by mass of EL phosphor made of ZnS · Cu was kneaded with 100 parts by mass of ethylene-methacrylic acid copolymer. . The performance evaluation results are shown in Table 2.
実施例８
実施例６において、エチレン−メタクリル酸共重合体１００質量部に対して、ＺｎＳ・ＣｕからなるＥＬ蛍光体を２００質量部混練した以外は、実施例６と同様にして、電界発光シートを作製した。その性能評価結果を表２に示す。
Example 8
In Example 6, an electroluminescent sheet was produced in the same manner as in Example 6 except that 200 parts by mass of an EL phosphor made of ZnS · Cu was kneaded with 100 parts by mass of the ethylene-methacrylic acid copolymer. . The performance evaluation results are shown in Table 2.
実施例９
実施例６において、エチレン−メタクリル酸共重合体１００質量部に対して、ＺｎＳ・ＣｕからなるＥＬ蛍光体を１００質量部混練した以外は、実施例６と同様にして、電界発光シートを作製した。その性能評価結果を表２に示す。
Example 9
In Example 6, an electroluminescent sheet was produced in the same manner as in Example 6, except that 100 parts by mass of an EL phosphor composed of ZnS · Cu was kneaded with 100 parts by mass of the ethylene-methacrylic acid copolymer. . The performance evaluation results are shown in Table 2.
実施例１０
実施例６において、エチレン−メタクリル酸共重合体１００質量部に対して、ＺｎＳ・ＣｕからなるＥＬ蛍光体を５０質量部混練した以外は、実施例６と同様にして、電界発光シートを作製した。その性能評価結果を表２に示す。
Example 10
In Example 6, an electroluminescent sheet was produced in the same manner as in Example 6 except that 50 parts by mass of an EL phosphor made of ZnS · Cu was kneaded with 100 parts by mass of an ethylene-methacrylic acid copolymer. . The performance evaluation results are shown in Table 2.
実施例１１
製造例２で得た第２電極上に誘電体層を形成し、該誘電体層上に電界発光層を形成した以外は、実施例１と同様にして電界発光シートを作製した。誘電体層は
次のようにして形成した。
（誘電体層の形成）
エチレン−酢酸ビニル共重合樹脂（三井・デュポンポリケミカル社製、「ＥＶＡＦＬＥＸ ＥＶ１５０」、軟化点３４℃）１００質量部と、ＳｉＯ2２００質量部とを、二軸押出混練機（テクノベル社製、「ＫＺＷ２５ＴＷＩＮ−３０ＭＧ−ＳＴＭ」）により、１３０℃にて混練して、ペレットを作製し、押出試験機（東洋精機製作所製、「ラボプラストミル３０Ｃ１５０」）を用いダイス温度１１５℃で、膜厚４０μｍの誘電体層を形成した。
Example 11
An electroluminescent sheet was produced in the same manner as in Example 1 except that a dielectric layer was formed on the second electrode obtained in Production Example 2 and an electroluminescent layer was formed on the dielectric layer. The dielectric layer was formed as follows.
(Formation of dielectric layer)
100 parts by mass of ethylene-vinyl acetate copolymer resin (Mitsui / DuPont Polychemical Co., Ltd., “EVAFLEX EV150”, softening point 34 ° C.) and 200 parts by mass of SiO 2 were mixed with a twin-screw extruder kneader (Technobel, “ KZW25TWIN-30MG-STM ”), kneaded at 130 ° C. to produce pellets, using an extrusion tester (“ Toyo Seiki Seisakusho, “Lab Plast Mill 30C150”) at a die temperature of 115 ° C. and a film thickness of 40 μm. A dielectric layer was formed.
実施例１２
エチレン−酢酸ビニル共重合樹脂の代わりに、ポリエチレンテレフタレート（クラレ社製、「クラペットＫＳ７１０Ｂ」、軟化点２３０℃）を用いて混練温度を３１５℃、ダイス温度を３０５℃とした以外は、実施例１と同様にして、電界発光シートを作製した。その性能評価結果を表２に示す。
Example 12
Example 1 except that polyethylene terephthalate (“Kurapet KS710B”, softening point 230 ° C.) was used instead of ethylene-vinyl acetate copolymer resin and the kneading temperature was 315 ° C. and the die temperature was 305 ° C. In the same manner, an electroluminescent sheet was produced. The performance evaluation results are shown in Table 2.
実施例１３
製造例１及び２で得た基材付き第１電極と基材付第２電極の間に、実施例１と同様のペレットを使用し、押出試験機（東洋精機製作所製、「ラボプラストミル３０Ｃ１５０」）を用いダイス温度１１５℃とし、製造例１及び２で得た基材付き第１電極と基材付き第２電極の間に、膜厚が５０μｍとなるようにシート状発光性部材を押出し、基材付き第１電極と基材付き第２電極を接合して電界発光シートを作製した。その性能評価結果を表２に示す。
Example 13
Between the first electrode with the base material and the second electrode with the base material obtained in Production Examples 1 and 2, the same pellets as in Example 1 were used, and an extrusion tester (“Labo Plast Mill 30C150, manufactured by Toyo Seiki Seisakusho Co., Ltd.) was used. )) And a die temperature of 115 ° C., and a sheet-like luminescent member is extruded between the first electrode with the base material and the second electrode with the base material obtained in Production Examples 1 and 2 so that the film thickness becomes 50 μm. The 1st electrode with a base material and the 2nd electrode with a base material were joined, and the electroluminescent sheet | seat was produced. The performance evaluation results are shown in Table 2.
比較例１
製造例１で得た基材付き第１電極上に、シアノエチルセルロース１００質量部と、ＺｎＳ・ＣｕからなるＥＬ蛍光体（オスラムシルバニア社製、「ＧＧＳ４２Ｇｒｅｅｎ」、平均粒径２５μｍ）４００質量部、溶剤としてブチルセロソルブを混合し、スクリーン印刷を１０回繰り返して、厚さ５０μｍの発光層を形成し、接着剤（東洋モートン社製、「ＴＭ−３０」）を用いて製造例２で得た基材付き第２電極層と発光層を貼り合わせて電界発光シートを作製した。その性能評価結果を表２に示す。
比較例１の電界発光シートは、スクリーン印刷を１０回行わなければならず。実施例の電界発光シートに比べて作成に長時間を要した。
Comparative Example 1
On the first electrode with the base material obtained in Production Example 1, 100 parts by mass of cyanoethyl cellulose, 400 parts by mass of an EL phosphor made of ZnS · Cu (manufactured by OSRAM Sylvania, “GGS42Green”, average particle size 25 μm), solvent Butyl cellosolve was mixed, and screen printing was repeated 10 times to form a light emitting layer with a thickness of 50 μm, and with a base material obtained in Production Example 2 using an adhesive (“TM-30” manufactured by Toyo Morton Co., Ltd.) The electroluminescent sheet was produced by bonding the second electrode layer and the light emitting layer. The performance evaluation results are shown in Table 2.
The electroluminescent sheet of Comparative Example 1 must be screen printed 10 times. Compared with the electroluminescent sheet of the example, it took a long time to prepare.
本発明のシート状発光性部材は、商業ビルの窓や自動車などへ貼付する広告媒体、装飾用媒体あるいは防犯用シートなどのバックライト等として用いられる電界発光シートにおける電界発光層などに用いることができ、上記電界発光シートを高い生産性のもとに、低コストで効率よく与えることができる。 The sheet-like luminescent member of the present invention can be used for an electroluminescent layer in an electroluminescent sheet used as a backlight for advertising media, decorative media or security sheets to be attached to commercial building windows, automobiles, and the like. The electroluminescent sheet can be efficiently provided at low cost with high productivity.
Claims (7)
下記（１）又は（２）の工程により第１積層体及び第２積層体を作製し、第１積層体のシート状発光性部材と第２積層体の第２電極側、又は第１積層体の第１電極側と第２積層体のシート状発光性部材とを、それぞれ熱ラミネートによって接合し、
前記シート状発光性部材が、前記熱可塑性樹脂と前記電界発光体とを混練したのち、押出機によりシート状に押出すことにより得られるものであり、
前記熱可塑性樹脂が、ポリエステルであることを特徴とする電界発光シートの製造方法。
（１）第１基材上に少なくとも第１電極及び前記シート状発光性部材を順に形成して第１積層体を作製し、別に第２基材上に少なくとも第２電極を形成することで第２積層体を作製する工程。
（２）第１基材上に少なくとも第１電極を形成することで第１積層体を作製し、別に第２基材上に少なくとも第２電極及び前記シート状発光性部材を順に形成して第２積層体を作製する工程。 A method for producing an electroluminescent sheet having a sheet-like luminescent member as an electroluminescent layer , comprising a thermoplastic resin and an electroluminescent material present in a dispersed state therein ,
The first laminate and the second laminate are produced by the following step (1) or (2), and the sheet-like luminescent member of the first laminate and the second electrode side of the second laminate, or the first laminate. The first electrode side and the sheet-like luminescent member of the second laminate are joined by thermal lamination,
The sheet-like luminescent member is obtained by kneading the thermoplastic resin and the electroluminescent body and then extruding it into a sheet with an extruder,
The method for producing an electroluminescent sheet, wherein the thermoplastic resin is polyester.
(1) At least a first electrode and the sheet-like luminescent member are sequentially formed on a first substrate to produce a first laminate, and at least a second electrode is formed on a second substrate. The process of producing 2 laminated bodies.
(2) A first laminate is produced by forming at least a first electrode on a first substrate, and separately forming at least a second electrode and the sheet-like luminescent member in order on a second substrate. The process of producing 2 laminated bodies.
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