JP2005091788A - Electrochromic element - Google Patents
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Abstract
Description
本発明は、表示素子や光学機器に用いられる調光素子の一つであるエレクトロクロミック素子に関する。 The present invention relates to an electrochromic element that is one of dimming elements used in display elements and optical devices.
従来、電圧を印加すると、可逆的に光の透過率、反射率を変化させることができる調光素子として、エレクトロクロミック素子（以下、ＥＣＤ）が、液晶素子などと共に研究されている。ＥＣＤは、液晶素子に比べて透過率が高い、光散乱の影響が少ない、偏光の影響を受けないなど調光素子として優れた性能を有している。
しかし、ＷＯ3を還元発色層、Ｉｒ酸化物を酸化発色層に用いたＥＣＤは、電圧を印加すると青色に着色されてしまうため、デジタルカメラなどの可視光域でのカラーバランスを重視する撮像素子の調光素子として使用する場合、色再現性、カラーバランスが大きく変化し、色付きが発生してしまい望ましくなかった。
2. Description of the Related Art Conventionally, an electrochromic element (hereinafter referred to as ECD) has been studied together with a liquid crystal element or the like as a dimming element capable of reversibly changing light transmittance and reflectance when a voltage is applied. ECD has excellent performance as a light control device, such as high transmittance compared to a liquid crystal device, little influence of light scattering, and no influence of polarized light.
However, an ECD using WO 3 as a reduction color layer and Ir oxide as an oxidation color layer is colored blue when a voltage is applied. Therefore, an image sensor that places importance on color balance in a visible light region such as a digital camera. When used as a light control device, color reproducibility and color balance are greatly changed, and coloring occurs, which is not desirable.
そこで、このような着色による色付きを無くすための方法として、還元発色層としてＷＯ3にＭｏＯ3を混ぜる方法などが公知となっている。さらに、ＷＯ3とＭｏＯ3の混合物を還元発色層として均一に成膜できる方法として、ＷＯ3とＭｏＯ3にＭｇＯ、ＺｒＯ2、Ｙ2Ｏ3、Ａｌ2Ｏ3などを混ぜた混合物材料を還元発色膜に用いる方法が、例えば、次の特許文献１に提案されている。
また、還元発色層だけでなく、酸化発色層にＩｒ酸化物、Ｎｉ酸化物、Ｓｎ酸化物などを用いると有効なことが、例えば、次の特許文献２に提案されている。
Further, for example, the following Patent Document 2 proposes that it is effective to use Ir oxide, Ni oxide, Sn oxide, or the like not only in the reduction coloring layer but also in the oxidation coloring layer.
しかし、ＷＯ3とＭｏＯ3を混ぜる方法は、これらの沸点が異なるため、成膜した還元発色層に色付きが生じたり、部分的に色むらができたりする問題があった。
また、特許文献１には、このＥＣＤの着色による色付きを無くす方法として、ＭｏＯ3の沸点よりも高い融点を有するＭｇＯ、ＺｒＯ2、Ｙ2Ｏ3、Ａｌ2Ｏ3などをＷＯ3とＭｏＯ3に混ぜた混合物材料を還元発色層に用いることが提案されているが、上記色付きの問題点を完全には解消できていない。
また、特許文献２では、Ｉｒ酸化物とＮｉ酸化物の混合材料を酸化発色層に用いる方法が公知技術として公開されているが、この方法も上記特許文献１の方法における還元発色層と同様に色付きが生じたり、部分的に色むらができたりする問題がある。
However, the method of mixing WO 3 and MoO 3 has a problem in that since the boiling points thereof are different, the formed reduced color layer is colored or partially uneven.
In Patent Document 1, a method of eliminating coloring due coloration of the ECD, MgO having a melting point higher than the boiling point of MoO 3, ZrO 2, Y 2 O 3, Al 2 O 3 and WO 3 and MoO 3 Although it has been proposed to use a mixture material mixed in the reductive coloring layer, the problem of coloring cannot be completely solved.
Further, in Patent Document 2, a method of using a mixed material of Ir oxide and Ni oxide for the oxidation coloring layer is disclosed as a known technique, but this method is also the same as the reduction coloring layer in the method of Patent Document 1 described above. There is a problem that coloring occurs or color unevenness occurs partially.
本発明は、上述の問題点に鑑みてなされたものであり、色付きが無く、複雑な混合材料を使うことなく簡単に再現性良く実現できる、ＥＣＤを提供することを目的とする。 The present invention has been made in view of the above-described problems, and an object of the present invention is to provide an ECD that is not colored and can be easily realized with good reproducibility without using a complicated mixed material.
上記目的を達成するため、本発明によるＥＣＤは、基板上に透明導電膜、酸化発色層、電解質層、還元発色層、透明導電膜が順次構成されているエレクトロクロミック素子において、前記還元発色層をＷＯ3とＴｉＯ2の多層膜で構成することを特徴としている。 In order to achieve the above object, the ECD according to the present invention includes an electrochromic device in which a transparent conductive film, an oxidation coloring layer, an electrolyte layer, a reduction coloring layer, and a transparent conductive film are sequentially formed on a substrate. It is characterized by comprising a multilayer film of WO 3 and TiO 2 .
また、本発明によるＥＣＤは、基板上に透明導電膜、酸化発色層、電解質層、還元発色層、透明導電膜が順次構成されているエレクトロクロミック素子において、前記酸化発色層をＩｒ酸化物とＮｉ酸化物の多層膜で構成することを特徴としている。 Further, the ECD according to the present invention is an electrochromic device in which a transparent conductive film, an oxidation coloring layer, an electrolyte layer, a reduction coloring layer, and a transparent conductive film are sequentially formed on a substrate. It is characterized by comprising a multilayer film of oxide.
また、本発明によるＥＣＤは、基板上に透明導電膜、酸化発色層、電解質層、還元発色層、透明導電膜が順次構成されているエレクトロクロミック素子において、前記還元発色層をＷＯ3とＴｉＯ2の多層膜で構成し、前記酸化発色層をＩｒ酸化物とＮｉ酸化物の多層膜で構成することを特徴としている。 Also, ECD according to the present invention, a transparent conductive film, oxidation color layer on the substrate, an electrolyte layer, reduction coloring layer, the electrochromic device transparent conductive film are sequentially configured, the reduction coloring layer WO 3 and TiO 2 And the oxidation coloring layer is composed of a multilayer film of Ir oxide and Ni oxide.
また、本発明によるＥＣＤにおいては、前記多層膜は、真空蒸着、イオンプレーティング、イオンアシスト蒸着、スパッタリング法で成膜されることを特徴としている。 In the ECD according to the present invention, the multilayer film is formed by vacuum deposition, ion plating, ion-assisted deposition, or sputtering.
本発明によれば色付きの無いＥＣＤを複雑な混合材料を使わず簡単に再現性良く実現できる。 According to the present invention, ECD without color can be realized easily and with good reproducibility without using complex mixed materials.
実施例の説明に先立ち、本発明の作用効果について説明する。
本発明のＥＣＤのように、ＷＯ3とＴｉＯ2を積層して多層膜の還元発色層を形成すれば、ＷＯ3の青い色付きを抑えて色付きをなくすことができ、安定して色付きの無いＥＣＤを作製することが可能になる。
また、本発明のＥＣＤのように、Ｉｒ酸化物とＮｉ酸化物を積層して多層膜の酸化発色層を形成すれば、安定して色付きの無いＥＣＤを作製することが可能になる。
なお、色付きの調整は、多層膜の層数、各層の膜厚を制御することで容易にできる。また多層膜の成膜時の膜厚、光学特性を安定させるために成膜手法としては、真空蒸着、イオンプレーティング、イオンアシスト蒸着、スパッタリング法で成膜することが望ましい。
Prior to the description of the embodiments, the effects of the present invention will be described.
By forming WO 3 and TiO 2 to form a multilayered reduction coloring layer as in the ECD of the present invention, the blue coloring of WO 3 can be suppressed and the coloring can be eliminated, and the ECD stably without coloring. Can be produced.
In addition, as in the case of the ECD of the present invention, if a multilayered oxide color-developing layer is formed by stacking Ir oxide and Ni oxide, it is possible to stably produce an ECD having no color.
Colored adjustment can be easily performed by controlling the number of layers of the multilayer film and the film thickness of each layer. Further, in order to stabilize the film thickness and optical characteristics when forming the multilayer film, it is desirable to form the film by vacuum deposition, ion plating, ion-assisted deposition, or sputtering.
図１は本発明の実施例１にかかるＥＣＤの概略構成図である。
実施例１のＥＣＤは次のような手順で作製する。
まず、ＩＴＯ（透明導電膜）２が１００ｎｍの膜厚に成膜された透明ガラス基板１を真空蒸着装置（図示省略）の中にセットする。
次に、第１層として、酸化発色層としてのＩｒ酸化膜３の成膜を行う。即ち、真空蒸着装置を１×１０-4ｐａまで排気する。排気の後、圧力が２×１０-2ｐａになるようＯ2を真空蒸着装置に導入し、基板に直接ＲＦ印加を行うイオンプレーティングの手法を用い、ＲＦパワーを３００Ｗに設定し、蒸着材料としてＩｒ酸化物を用いて電子銃で蒸発させ、Ｉｒ酸化物の膜厚が２０ｎｍになるまで成膜を行う。
FIG. 1 is a schematic configuration diagram of an ECD according to Embodiment 1 of the present invention.
The ECD of Example 1 is manufactured by the following procedure.
First, a transparent glass substrate 1 on which an ITO (transparent conductive film) 2 is formed to a thickness of 100 nm is set in a vacuum vapor deposition apparatus (not shown).
Next, as a first layer, an Ir oxide film 3 is formed as an oxidative coloring layer. That is, the vacuum evaporation apparatus is evacuated to 1 × 10 −4 pa. After evacuation, O 2 is introduced into the vacuum vapor deposition apparatus so that the pressure becomes 2 × 10 −2 pa, and the RF power is set to 300 W using an ion plating method in which RF is directly applied to the substrate. The film is deposited until the film thickness of the Ir oxide is 20 nm by evaporating with an electron gun using Ir oxide.
次に、第２層として、酸化発色層としてのＮｉ酸化膜４の成膜を行う。即ち、圧力が２×１０-2ｐａになるようＯ2を真空蒸着装置に導入し、基板に直接ＲＦ印加を行うイオンプレーティングの手法を用い、蒸着材料としてＮｉ酸化物を用いて電子銃で蒸発させ、Ｎｉ酸化物の膜厚が２０ｎｍになるまで成膜を行う。 Next, as the second layer, a Ni oxide film 4 is formed as an oxidative coloring layer. That is, using an ion plating method in which O 2 is introduced into a vacuum deposition apparatus so that the pressure becomes 2 × 10 −2 pa and RF is directly applied to the substrate, Ni oxide is used as a deposition material, and an electron gun is used. Evaporation is performed until the Ni oxide film thickness reaches 20 nm.
次に、第３層として、電解質層としてのＴａ2Ｏ5膜５の成膜を行う。即ち、圧力が２×１０-2ｐａになるようＯ2を真空蒸着装置に導入し、基板に直接ＲＦ印加を行うイオンプレーティングの手法を用い、蒸着材料としてＴａ2Ｏ5を用いて電子銃で蒸発させ、Ｔａ2Ｏ5の膜厚が２００ｎｍになるまで成膜を行う。 Next, a Ta 2 O 5 film 5 as an electrolyte layer is formed as a third layer. That is, using an ion plating method in which O 2 is introduced into a vacuum deposition apparatus so that the pressure becomes 2 × 10 −2 pa and RF is directly applied to the substrate, Ta 2 O 5 is used as a deposition material, and an electron gun is used. Evaporation is performed until film thickness of Ta 2 O 5 reaches 200 nm.
次に、第４層として、還元発色層としてのＴｉＯ2膜６の成膜を行う。即ち、第２層と同じ圧力条件、同じ手法を用い、蒸着材料としてＴｉＯ2を用いて電子銃で蒸発させ、ＴｉＯ2の膜厚が２００ｎｍになるまで成膜を行う。 Next, as the fourth layer, a TiO 2 film 6 is formed as a reducing color developing layer. That is, using the same pressure condition and the same method as the second layer, using TiO 2 as an evaporation material and evaporating with an electron gun, the film is formed until the film thickness of TiO 2 reaches 200 nm.
次に、第５層として、還元発色層としてのＷＯ3膜７の成膜を行う。即ち、第２層と同じ圧力条件、同じ手法を用い、蒸着材料としてＷＯ3を用いて電子銃で蒸発させ、ＷＯ3の膜厚が９００ｎｍになるまで成膜を行う。 Next, as a fifth layer, a WO 3 film 7 is formed as a reduction coloring layer. That is, using the same pressure condition and the same method as the second layer, evaporating with an electron gun using WO 3 as a deposition material, film formation is performed until the film thickness of WO 3 becomes 900 nm.
次に、第６層として、ＩＴＯ膜８の成膜を行う。即ち、第２層と同じ圧力条件、同じ手法を用い、蒸着材料としてＩＴＯを用いて電子銃で蒸発させ、ＩＴＯの膜厚が２００ｎｍになるまで成膜を行う。 Next, an ITO film 8 is formed as a sixth layer. That is, using the same pressure condition and the same method as the second layer, using ITO as a vapor deposition material and evaporating with an electron gun, film formation is performed until the ITO film thickness reaches 200 nm.
その後、このように構成された上記ＥＣＤの外周面を樹脂８で封止し、その上にガラス基板１０を貼り合わせた。樹脂８は、熱硬化型の２成分系エポキシ樹脂であり、例えば、主剤として常温では液状のビスフェノール型の樹脂と、硬化剤として常温で液状のアミン系の樹脂で組成されている。
このように作製された実施例１のＥＣＤにおける、上下のＩＴＯ２，８に＋２Ｖの電圧を印加したときと、電圧を印加しないとき（スルー状態）の夫々の分光透過率特性を図２に示す。
実施例１のＥＣＤでは、電圧の印加により着色したときにおいても色付きの無いニュートラルな分光特性が得られた。
Thereafter, the outer peripheral surface of the ECD configured as described above was sealed with a resin 8, and a glass substrate 10 was bonded thereon. The resin 8 is a thermosetting two-component epoxy resin, and is composed of, for example, a bisphenol-type resin that is liquid at room temperature as a main agent and an amine-based resin that is liquid at room temperature as a curing agent.
FIG. 2 shows the spectral transmittance characteristics of the ECD of Example 1 manufactured in this way when a voltage of +2 V is applied to the upper and lower ITO 2 and 8 and when no voltage is applied (through state).
In the ECD of Example 1, neutral spectral characteristics without coloring were obtained even when colored by applying a voltage.
図３は本発明の実施例２にかかるＥＣＤの概略構成図である。
実施例２のＥＣＤは次のような手順で作製する。
まず、ＩＴＯ（透明導電膜）２が１００ｎｍの膜厚に成膜された透明ガラス基板１を真空蒸着装置（図示省略）の中にセットする。
次に、第１層〜第３層までは、実施例１と同じ手順で同様の膜を作製する。
FIG. 3 is a schematic configuration diagram of an ECD according to the second embodiment of the present invention.
The ECD of Example 2 is manufactured by the following procedure.
First, a transparent glass substrate 1 on which an ITO (transparent conductive film) 2 is formed to a thickness of 100 nm is set in a vacuum vapor deposition apparatus (not shown).
Next, for the first layer to the third layer, similar films are produced in the same procedure as in the first embodiment.
次に、第４層として、還元発色層としてのＷＯ3膜７の成膜を行う。即ち、第３層と同じ圧力条件、同じ手法を用い、蒸着材料としてＷＯ3を用いて電子銃で蒸発させ、ＷＯ3の膜厚が４００ｎｍになるまで成膜を行う。 Next, as a fourth layer, a WO 3 film 7 is formed as a reduction coloring layer. That is, using the same pressure condition and the same method as the third layer, evaporating with an electron gun using WO 3 as an evaporation material, film formation is performed until the film thickness of WO 3 reaches 400 nm.
次に、第５層として、還元発色層としてのＴｉＯ2膜６の成膜を行う。即ち、第３層と同じ圧力条件、同じ手法を用い、蒸着材料としてＴｉＯ2を用いて電子銃で蒸発させ、ＴｉＯ2の膜厚が２００ｎｍになるまで成膜を行う。 Next, as a fifth layer, a TiO 2 film 6 is formed as a reducing color developing layer. That is, using the same pressure condition and the same method as the third layer, using TiO 2 as an evaporation material and evaporating with an electron gun, the film is formed until the film thickness of TiO 2 reaches 200 nm.
次に、第６層として、還元発色層としてのＷＯ3膜７’の成膜を行う。即ち、第３層と同じ圧力条件、同じ手法を用い、蒸着材料としてＷＯ3を用いて電子銃で蒸発させ、ＷＯ3の膜厚が４００ｎｍになるまで成膜を行う。 Next, as a sixth layer, a WO 3 film 7 ′ as a reduction coloring layer is formed. That is, using the same pressure condition and the same method as the third layer, evaporating with an electron gun using WO 3 as an evaporation material, film formation is performed until the film thickness of WO 3 reaches 400 nm.
次に、第７層として、ＩＴＯ膜８の成膜を行う。即ち、第３層と同じ圧力条件、同じ手法を用い、蒸着材料としてＩＴＯを用いて電子銃で蒸発させ、ＩＴＯの膜厚が２００ｎｍになるまで成膜を行う。 Next, an ITO film 8 is formed as a seventh layer. That is, using the same pressure condition and the same method as the third layer, using ITO as a vapor deposition material and evaporating with an electron gun, film formation is performed until the ITO film thickness reaches 200 nm.
その後、このように構成された上記ＥＣＤの外周面を実施例１と同様に樹脂８で封止し、その上にガラス基板１０を貼り合わせた。
このように作製された実施例２のＥＣＤにおける、上下のＩＴＯ２，８に＋２Ｖの電圧を印加したときと、電圧を印加しないとき（スルー状態）の夫々の分光透過率特性は、図２に示した実施例１と同様であり、電圧の印加により着色したときにおいても色付きの無いニュートラルな分光特性が得られた。
Thereafter, the outer peripheral surface of the ECD thus configured was sealed with the resin 8 in the same manner as in Example 1, and the glass substrate 10 was bonded thereon.
In the ECD of Example 2 manufactured in this way, the spectral transmittance characteristics when +2 V is applied to the upper and lower ITO 2 and 8 and when no voltage is applied (through state) are shown in FIG. As in Example 1, neutral spectral characteristics without coloring were obtained even when colored by application of voltage.
図４は本発明の実施例３にかかるＥＣＤの概略構成図である。
実施例３のＥＣＤは次のような手順で作製する。
まず、ＩＴＯ（透明導電膜）２が１００ｎｍの膜厚に成膜された透明ガラス基板１を真空蒸着装置（図示省略）の中にセットする。
次に、第１層〜第３層までは、実施例１と同じ手順で同様の膜を作製する。
FIG. 4 is a schematic configuration diagram of an ECD according to Embodiment 3 of the present invention.
The ECD of Example 3 is manufactured by the following procedure.
First, a transparent glass substrate 1 on which an ITO (transparent conductive film) 2 is formed to a thickness of 100 nm is set in a vacuum vapor deposition apparatus (not shown).
Next, for the first layer to the third layer, similar films are produced in the same procedure as in the first embodiment.
次に、第４層として、還元発色層としてのＷＯ3膜７の成膜を行う。即ち、第３層と同じ圧力条件、同じ手法を用い、蒸着材料としてＷＯ3を用いて電子銃で蒸発させ、ＷＯ3の膜厚が２００ｎｍになるまで成膜を行う。 Next, as a fourth layer, a WO 3 film 7 is formed as a reduction coloring layer. That is, using the same pressure condition and the same method as the third layer, using WO 3 as an evaporation material, evaporation is performed with an electron gun, and film formation is performed until the film thickness of WO 3 becomes 200 nm.
次に、第５層として、還元発色層としてのＴｉＯ2膜６の成膜を行う。即ち、第３層と同じ圧力条件、同じ手法を用い、蒸着材料としてＴｉＯ2を用いて電子銃で蒸発させ、ＴｉＯ2の膜厚が１００ｎｍになるまで成膜を行う。 Next, as a fifth layer, a TiO 2 film 6 is formed as a reducing color developing layer. That is, using the same pressure condition and the same method as the third layer, using TiO 2 as an evaporation material and evaporating with an electron gun, the film is formed until the film thickness of TiO 2 reaches 100 nm.
次に、第６層として、還元発色層としてのＷＯ3膜７’の成膜を行う。即ち、第３層と同じ圧力条件、同じ手法を用い、蒸着材料としてＷＯ3を用いて電子銃で蒸発させ、ＷＯ3の膜厚が２００ｎｍになるまで成膜を行う。 Next, as a sixth layer, a WO 3 film 7 ′ as a reduction coloring layer is formed. That is, using the same pressure condition and the same method as the third layer, using WO 3 as an evaporation material, evaporation is performed with an electron gun, and film formation is performed until the film thickness of WO 3 becomes 200 nm.
次に、第７層として、還元発色層としてのＴｉＯ2膜６’の成膜を行う。即ち、第３層と同じ圧力条件、同じ手法を用い、蒸着材料としてＴｉＯ2を用いて電子銃で蒸発させ、ＴｉＯ2の膜厚が１００ｎｍになるまで成膜を行う。 Next, as a seventh layer, a TiO 2 film 6 ′ as a reduction coloring layer is formed. That is, using the same pressure condition and the same method as the third layer, using TiO 2 as an evaporation material and evaporating with an electron gun, the film is formed until the film thickness of TiO 2 reaches 100 nm.
次に、第８層として、還元発色層としてのＷＯ3膜７”の成膜を行う。即ち、第３層と同じ圧力条件、同じ手法を用い、蒸着材料としてＷＯ3を用いて電子銃で蒸発させ、ＷＯ3の膜厚が２００ｎｍになるまで成膜を行う。 Next, as an eighth layer, a WO 3 film 7 ″ as a reduction coloring layer is formed. That is, using the same pressure condition and the same technique as those of the third layer, using WO 3 as an evaporation material, an electron gun is used. Evaporation is performed until the film thickness of WO 3 reaches 200 nm.
次に、第９層として、ＩＴＯ膜８の成膜を行う。即ち、第３層と同じ圧力条件、同じ手法を用い、蒸着材料としてＩＴＯを用いて電子銃で蒸発させ、ＩＴＯの膜厚が２００ｎｍになるまで成膜を行う。 Next, an ITO film 8 is formed as a ninth layer. That is, using the same pressure condition and the same method as the third layer, using ITO as a vapor deposition material and evaporating with an electron gun, film formation is performed until the ITO film thickness reaches 200 nm.
その後、このように構成された上記ＥＣＤの外周面を実施例１と同様に樹脂８で封止し、その上にガラス基板１０を貼り合わせた。
このように作製された実施例３のＥＣＤにおける、上下のＩＴＯ２，８に＋２Ｖの電圧を印加したときと、電圧を印加しないとき（スルー状態）の夫々の分光透過率特性は、図２に示した実施例１と同様であり、電圧の印加により着色したときにおいても色付きの無いニュートラルな分光特性が得られた。
Thereafter, the outer peripheral surface of the ECD thus configured was sealed with the resin 8 in the same manner as in Example 1, and the glass substrate 10 was bonded thereon.
In the ECD of Example 3 manufactured in this way, the spectral transmittance characteristics when +2 V is applied to the upper and lower ITO 2 and 8 and when no voltage is applied (through state) are shown in FIG. As in Example 1, neutral spectral characteristics without coloring were obtained even when colored by application of voltage.
図５は本発明の実施例４にかかるＥＣＤの概略構成図である。
実施例４のＥＣＤは次のような手順で作製する。
まず、ＩＴＯ（透明導電膜）２が１００ｎｍの膜厚に成膜された透明ガラス基板を真空蒸着装置（図示省略）の中にセットする。
FIG. 5 is a schematic configuration diagram of an ECD according to Embodiment 4 of the present invention.
The ECD of Example 4 is produced by the following procedure.
First, a transparent glass substrate on which ITO (transparent conductive film) 2 is formed to a thickness of 100 nm is set in a vacuum vapor deposition apparatus (not shown).
次に、第１層として、酸化発色層としてのＩｒ酸化膜３の成膜を行う。即ち、真空蒸着装置を１×１０-4ｐａまで排気した後、圧力が２×１０-2ｐａになるようＯ2を真空蒸着装置に導入し、基板に直接ＲＦ印加を行うイオンプレーティングの手法を用い、ＲＦパワーを３００Ｗに設定し、蒸着材料としてＩｒ酸化物を用いて電子銃で蒸発させ、Ｉｒ酸化物の膜厚が１０ｎｍになるまで成膜を行う。 Next, as a first layer, an Ir oxide film 3 is formed as an oxidative coloring layer. That is, after the vacuum deposition apparatus is evacuated to 1 × 10 −4 pa, O 2 is introduced into the vacuum deposition apparatus so that the pressure becomes 2 × 10 −2 pa, and RF plating is directly applied to the substrate. , The RF power is set to 300 W, Ir oxide is used as a vapor deposition material and evaporated by an electron gun, and film formation is performed until the film thickness of Ir oxide reaches 10 nm.
次に、第２層として、酸化発色層としてのＮｉ酸化膜４の成膜を行う。即ち、圧力が２×１０-2ｐａになるようＯ2を真空蒸着装置に導入し、基板に直接ＲＦ印加を行うイオンプレーティングの手法を用い、蒸着材料としてＮｉ酸化物を用いて電子銃で蒸発させ、Ｎｉ酸化膜の膜厚が３０ｎｍになるまで成膜を行う。 Next, as the second layer, a Ni oxide film 4 is formed as an oxidative coloring layer. That is, using an ion plating method in which O 2 is introduced into a vacuum deposition apparatus so that the pressure becomes 2 × 10 −2 pa and RF is directly applied to the substrate, Ni oxide is used as a deposition material, and an electron gun is used. Evaporation is performed until the Ni oxide film has a thickness of 30 nm.
次に、第３層として、酸化発色層としてのＩｒ酸化膜３’の成膜を行う。即ち、圧力が２×１０-2ｐａになるようＯ2を真空蒸着装置に導入し、基板に直接ＲＦ印加を行うイオンプレーティングの手法を用い、ＲＦパワーを３００Ｗに設定し、蒸着材料としてＩｒ酸化物を用いて電子銃で蒸発させ、Ｉｒ酸化物の膜厚が１０ｎｍになるまで成膜を行う。 Next, as a third layer, an Ir oxide film 3 ′ as an oxidation coloring layer is formed. That is, O 2 is introduced into a vacuum vapor deposition apparatus so that the pressure becomes 2 × 10 −2 pa, an ion plating method in which RF is directly applied to the substrate, an RF power is set to 300 W, and Ir is used as a vapor deposition material. The oxide is evaporated with an electron gun, and film formation is performed until the Ir oxide film thickness reaches 10 nm.
次に、第４層として、電解質層としてのＴａ2Ｏ5膜５の成膜を行う。即ち、圧力が２×１０-2ｐａになるようＯ2を真空蒸着装置に導入し、基板に直接ＲＦ印加を行うイオンプレーティングの手法を用い、蒸着材料としてＴａ2Ｏ5を用いて電子銃で蒸発させ、Ｔａ2Ｏ5の膜厚が２００ｎｍになるまで成膜を行う。 Next, a Ta 2 O 5 film 5 as an electrolyte layer is formed as a fourth layer. That is, using an ion plating method in which O 2 is introduced into a vacuum deposition apparatus so that the pressure becomes 2 × 10 −2 pa and RF is directly applied to the substrate, Ta 2 O 5 is used as a deposition material, and an electron gun is used. Evaporation is performed until film thickness of Ta 2 O 5 reaches 200 nm.
次に、第５層として、還元発色層としてのＷＯ3膜７の成膜を行う。即ち、第４層と同じ圧力条件、同じ手法を用い、蒸着材料としてＷＯ3を用いて電子銃で蒸発させ、ＷＯ3の膜厚が４００ｎｍになるまで成膜を行う。 Next, as a fifth layer, a WO 3 film 7 is formed as a reduction coloring layer. That is, using the same pressure condition and the same method as the fourth layer, using WO 3 as a vapor deposition material, evaporation is performed with an electron gun, and film formation is performed until the film thickness of WO 3 reaches 400 nm.
次に、第６層として、還元発色層としてのＴｉＯ2膜６の成膜を行う。即ち、第４層と同じ圧力条件、同じ手法を用い、蒸着材料としてＴｉＯ2を用いて電子銃で蒸発させ、ＴｉＯ2の膜厚が２００ｎｍになるまで成膜を行う。 Next, as a sixth layer, a TiO 2 film 6 is formed as a reducing color developing layer. That is, using the same pressure condition and the same method as the fourth layer, using TiO 2 as an evaporation material, evaporating with an electron gun, and forming the film until the thickness of TiO 2 reaches 200 nm.
次に、第７層として、還元発色層としてのＷＯ3膜７’の成膜を行う。即ち、第４層と同じ圧力条件、同じ手法を用い、蒸着材料としてＷＯ3を用いて電子銃で蒸発させ、ＷＯ3の膜厚が４００ｎｍになるまで成膜を行う。 Next, as a seventh layer, a WO 3 film 7 ′ is formed as a reduction coloring layer. That is, using the same pressure condition and the same method as the fourth layer, using WO 3 as a vapor deposition material, evaporation is performed with an electron gun, and film formation is performed until the film thickness of WO 3 reaches 400 nm.
次に、第８層として、ＩＴＯ膜８の成膜を行う。即ち、第４層と同じ圧力条件、同じ手法を用い、蒸着材料としてＩＴＯを用いて電子銃で蒸発させ、ＩＴＯの膜厚が２００ｎｍになるまで成膜を行う。 Next, an ITO film 8 is formed as an eighth layer. That is, using the same pressure condition and the same method as the fourth layer, using ITO as an evaporation material and evaporating with an electron gun, film formation is performed until the ITO film thickness reaches 200 nm.
その後、このように構成された上記ＥＣＤの外周面を実施例１と同様に樹脂８で封止し、その上にガラス基板１０を貼り合わせた。
このように作製された実施例４のＥＣＤにおける、上下のＩＴＯ２，８に＋２Ｖの電圧を印加したときと、電圧を印加しないとき（スルー状態）の夫々の分光透過率特性は、図２に示した実施例１と同様であり、電圧の印加により着色したときにおいても色付きの無いニュートラルな分光特性が得られた。
Thereafter, the outer peripheral surface of the ECD thus configured was sealed with the resin 8 in the same manner as in Example 1, and the glass substrate 10 was bonded thereon.
In the ECD of Example 4 manufactured in this way, the spectral transmittance characteristics when +2 V is applied to the upper and lower ITO 2 and 8 and when no voltage is applied (through state) are shown in FIG. As in Example 1, neutral spectral characteristics without coloring were obtained even when colored by application of voltage.
図６は本発明の実施例５にかかるＥＣＤの概略構成図である。
実施例５のＥＣＤは次のような手順で作製する。
まず、ＩＴＯ（透明導電膜）２が１００ｎｍの膜厚に成膜された透明ガラス基板を真空蒸着装置（図示省略）の中にセットする。
FIG. 6 is a schematic configuration diagram of an ECD according to Embodiment 5 of the present invention.
The ECD of Example 5 is produced by the following procedure.
First, a transparent glass substrate on which ITO (transparent conductive film) 2 is formed to a thickness of 100 nm is set in a vacuum vapor deposition apparatus (not shown).
次に、第１層として、酸化発色層としてのＩｒ酸化膜３の成膜を行う。即ち、真空蒸着装置を１×１０-4ｐａまで排気した後、圧力が２×１０-2ｐａになるようＯ2を真空蒸着装置に導入し、基板に直接ＲＦ印加を行うイオンプレーティングの手法を用い、ＲＦパワーを３００Ｗに設定し、蒸着材料としてＩｒ酸化物を用いて電子銃で蒸発させ、Ｉｒ酸化物の膜厚が１０ｎｍになるまで成膜を行う。 Next, as a first layer, an Ir oxide film 3 is formed as an oxidative coloring layer. That is, after the vacuum deposition apparatus is evacuated to 1 × 10 −4 pa, O 2 is introduced into the vacuum deposition apparatus so that the pressure becomes 2 × 10 −2 pa, and RF plating is directly applied to the substrate. , The RF power is set to 300 W, Ir oxide is used as the vapor deposition material and evaporated using an electron gun, and film formation is performed until the Ir oxide film thickness reaches 10 nm.
次に、第２層として、酸化発色層としてのＮｉ酸化膜４の成膜を行う。即ち、圧力が２×１０-2ｐａになるようＯ2を真空蒸着装置に導入し、基板に直接ＲＦ印加を行うイオンプレーティングの手法を用い、蒸着材料としてＮｉ酸化物を用いて電子銃で蒸発させ、Ｎｉ酸化膜の膜厚が２０ｎｍになるまで成膜を行う。 Next, as the second layer, a Ni oxide film 4 is formed as an oxidative coloring layer. That is, using an ion plating method in which O 2 is introduced into a vacuum deposition apparatus so that the pressure becomes 2 × 10 −2 pa and RF is directly applied to the substrate, Ni oxide is used as a deposition material, and an electron gun is used. Evaporation is performed until the Ni oxide film has a thickness of 20 nm.
次に、第３層として、酸化発色層としてのＩｒ酸化膜３’の成膜を行う。即ち、圧力が２×１０-2ｐａになるようＯ2を真空蒸着装置に導入し、基板に直接ＲＦ印加を行うイオンプレーティングの手法を用い、ＲＦパワーを３００Ｗに設定し、蒸着材料としてＩｒ酸化物を用いて電子銃で蒸発させ、Ｉｒ酸化物を膜厚が１０ｎｍになるまで成膜を行う。 Next, as a third layer, an Ir oxide film 3 ′ as an oxidation coloring layer is formed. That is, O 2 is introduced into a vacuum vapor deposition apparatus so that the pressure becomes 2 × 10 −2 pa, an ion plating method in which RF is directly applied to the substrate, an RF power is set to 300 W, and Ir is used as a vapor deposition material. The oxide is evaporated with an electron gun, and Ir oxide is deposited until the film thickness reaches 10 nm.
次に、第４層として、酸化発色層としてのＮｉ酸化膜４’の成膜を行う。即ち、圧力が２×１０-2ｐａになるようＯ2を真空蒸着装置に導入し、基板に直接ＲＦ印加を行うイオンプレーティングの手法を用い、蒸着材料としてＮｉ酸化物を用いて電子銃で蒸発させ、Ｎｉ酸化膜の膜厚が２０ｎｍになるまで成膜を行う。 Next, as a fourth layer, a Ni oxide film 4 ′ is formed as an oxidation coloring layer. That is, using an ion plating method in which O 2 is introduced into a vacuum deposition apparatus so that the pressure becomes 2 × 10 −2 pa and RF is directly applied to the substrate, Ni oxide is used as a deposition material, and an electron gun is used. Evaporation is performed until the Ni oxide film has a thickness of 20 nm.
次に、第５層として、電解質層としてのＴａ2Ｏ5膜５の成膜を行う。即ち、圧力が２×１０-2ｐａになるようＯ2を真空蒸着装置に導入し、基板に直接ＲＦ印加を行うイオンプレーティングの手法を用い、蒸着材料としてＴａ2Ｏ5を用いて電子銃で蒸発させ、Ｔａ2Ｏ5の膜厚が２００ｎｍになるまで成膜を行う。 Next, a Ta 2 O 5 film 5 as an electrolyte layer is formed as a fifth layer. That is, using an ion plating method in which O 2 is introduced into a vacuum deposition apparatus so that the pressure becomes 2 × 10 −2 pa and RF is directly applied to the substrate, Ta 2 O 5 is used as a deposition material, and an electron gun is used. Evaporation is performed until film thickness of Ta 2 O 5 reaches 200 nm.
次に、第６層として、還元発色層としてのＷＯ3膜７の成膜を行う。即ち、第５層と同じ圧力条件、同じ手法を用い、蒸着材料としてＷＯ3を用いて電子銃で蒸発させ、ＷＯ3の膜厚が４００ｎｍになるまで成膜を行う。 Next, as a sixth layer, a WO 3 film 7 is formed as a reduction coloring layer. That is, using the same pressure condition and the same method as the fifth layer, using WO 3 as an evaporation material, evaporation is performed with an electron gun, and film formation is performed until the film thickness of WO 3 reaches 400 nm.
次に、第７層として、還元発色層としてのＴｉＯ2膜６の成膜を行う。即ち、第５層と同じ圧力条件、同じ手法を用い、蒸着材料としてＴｉＯ2を用いて電子銃で蒸発させ、ＴｉＯ2の膜厚が２００ｎｍになるまで成膜を行う。 Next, as a seventh layer, a TiO 2 film 6 is formed as a reduction coloring layer. That is, using the same pressure condition and the same method as the fifth layer, using TiO 2 as a vapor deposition material and evaporating with an electron gun, the film is formed until the film thickness of TiO 2 reaches 200 nm.
次に、第８層として、還元発色層としてのＷＯ3膜７’の成膜を行う。即ち、第５層と同じ圧力条件、同じ手法を用い、蒸着材料としてＷＯ3を用いて電子銃で蒸発させ、ＷＯ3の膜厚が４００ｎｍになるまで成膜を行う。 Next, as an eighth layer, a WO 3 film 7 ′ as a reduction coloring layer is formed. That is, using the same pressure condition and the same method as the fifth layer, using WO 3 as an evaporation material, evaporation is performed with an electron gun, and film formation is performed until the film thickness of WO 3 reaches 400 nm.
次に、第９層として、ＩＴＯ膜８の成膜を行う。即ち、第５層と同じ圧力条件、同じ手法を用い、蒸着材料としてＩＴＯを用いて電子銃で蒸発させ、ＩＴＯの膜厚が２００ｎｍになるまで成膜を行う。 Next, an ITO film 8 is formed as a ninth layer. That is, using the same pressure condition and the same method as the fifth layer, using ITO as a vapor deposition material and evaporating with an electron gun, film formation is performed until the ITO film thickness reaches 200 nm.
その後、このように構成された上記ＥＣＤの外周面を実施例１と同様に樹脂８で封止し、その上にガラス基板１０を貼り合わせた。
このように作製された実施例５のＥＣＤにおける、上下のＩＴＯ２，８に＋２Ｖの電圧を印加したときと、電圧を印加しないとき（スルー状態）の夫々の分光透過率特性は、図２に示した実施例１と同様であり、電圧の印加により着色したときにおいても色付きの無いニュートラルな分光特性が得られた。
Thereafter, the outer peripheral surface of the ECD thus configured was sealed with the resin 8 in the same manner as in Example 1, and the glass substrate 10 was bonded thereon.
In the ECD of Example 5 manufactured in this way, the spectral transmittance characteristics when +2 V is applied to the upper and lower ITO 2 and 8 and when no voltage is applied (through state) are shown in FIG. As in Example 1, neutral spectral characteristics without coloring were obtained even when colored by application of voltage.
なお、上記各実施例において、他のイオンビームアシスト蒸着、スパッタリングで成膜してＥＣＤを作製した場合も、図２に示す分光透過率特性と同様な結果が得られた。 In each of the above examples, the same results as the spectral transmittance characteristics shown in FIG. 2 were obtained when the ECD was formed by film formation by other ion beam assisted vapor deposition or sputtering.
１，１０ ガラス基板
２，８ ＩＴＯ膜（透明導電膜）
３，３’ Ｉｒ酸化膜（酸化発色層）
４，４’ Ｎｉ酸化膜（酸化発色層）
５ Ｔａ2Ｏ5膜（電解質層）
６，６’ ＴｉＯ2膜（還元発色層）
７，７’，７” ＷＯ3膜（還元発色層）
９ 樹脂
1,10 glass substrate 2,8 ITO film (transparent conductive film)
3,3 'Ir oxide film (oxidation coloring layer)
4,4 'Ni oxide film (oxidation coloring layer)
5 Ta 2 O 5 film (electrolyte layer)
6,6 'TiO 2 film (reduction coloring layer)
7, 7 ', 7 "WO 3 film (reduction coloring layer)
9 Resin
Claims (4)
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| JP2018526665A (en) * | 2015-07-14 | 2018-09-13 | ビュー， インコーポレイテッド | Counter electrode for electrochromic devices |
| JP2020518004A (en) * | 2017-04-24 | 2020-06-18 | エルジー・ケム・リミテッド | Electrochromic film and electrochromic device including the same |
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