JP4547501B2 - Conductivity control method, device manufacturing method and device of transparent conductive material - Google Patents
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Description
本発明は、透明導電性材料の導電率制御法、デバイス作製法及びデバイスに係り、とくに透明導電性材料表面乃至は内部に、水素ガス又は水素を含む化合物を介して光照射することにより、従来困難とされてきた透明導電性材料表面乃至は内部の導電率制御を、位置選択的あるいは空間選択的に行うことが可能な透明導電性材料の導電率制御法、デバイス作製法及びデバイスに関する。 The present invention relates to a method for controlling the conductivity of a transparent conductive material, a device manufacturing method, and a device. In particular, the surface or the inside of a transparent conductive material is irradiated with light through a compound containing hydrogen gas or hydrogen. The present invention relates to a conductivity control method, a device manufacturing method, and a device of a transparent conductive material capable of controlling the conductivity of a surface or inside of a transparent conductive material, which has been considered difficult, in a position-selective or space-selective manner.
透明導電性材料は、ディスプレイや太陽電池など、エレクトロニクスやオプトエレクトロニクス分野のデバイスとして広く用いられている。また最近、透明導電性材料をシリカガラス基板上に形成し、それを電波吸収ガラスとして利用する要請が強い。しかし従来の技術では、透明導電性材料表面乃至は内部の導電率制御を、位置選択的あるいは空間選択的に行うことが困難であった。このことが、電波吸収ガラスを含むデバイスの高効率化を制限していた。 Transparent conductive materials are widely used as devices in the electronics and optoelectronic fields, such as displays and solar cells. Recently, there is a strong demand for forming a transparent conductive material on a silica glass substrate and using it as a radio wave absorbing glass. However, in the conventional technique, it has been difficult to control the conductivity of the surface of the transparent conductive material or the inside thereof in a position selective manner or a spatial selective manner. This has limited the high efficiency of devices including radio wave absorbing glass.
透明導電性材料表面乃至は内部の導電率制御を、位置選択的あるいは空間選択的に行うことにより、透明導電性材料を基礎とした高効率電波吸収ガラス等のデバイスの作製法の確立を課題とする。 Establishing a method for producing devices such as high-efficiency radio wave absorption glass based on transparent conductive materials by controlling the conductivity of the surface of the transparent conductive material or inside in a position-selective or space-selective manner. To do.
そこで、本発明は、上記の点に鑑み、透明導電性材料表面乃至は内部に、水素ガス又は水素を含む化合物を介して光照射することにより、位置選択的あるいは空間選択的に導電率を変化させることを可能とした透明導電性材料の導電率制御法、デバイス作製法及びデバイスを提供することを目的とする。 Therefore, in view of the above points, the present invention changes the conductivity selectively or spatially by irradiating the surface or inside of the transparent conductive material through hydrogen gas or a compound containing hydrogen. It is an object of the present invention to provide a conductivity control method, a device manufacturing method, and a device of a transparent conductive material that can be made to be made.
本発明のその他の目的や新規の特徴は後述の実施の形態において明らかにする。 Other objects and novel features of the present invention will be clarified in embodiments described later.
上記目的を達成するために、本発明のある態様の透明導電性材料の導電率制御法は、透明導電性材料としてのフッ素ドープＳｎＯ２表面乃至は内部に、光を吸収して水素原子又はイオンを放出する水素を含む化合物又は水素ガスを介して光照射することにより、導電率を低下させることを特徴としている。 In order to achieve the above object, a method for controlling the conductivity of a transparent conductive material according to an aspect of the present invention is to absorb light on a surface or inside of a fluorine-doped SnO 2 as a transparent conductive material to absorb hydrogen atoms or ions. The conductivity is lowered by irradiating light through a compound containing hydrogen or hydrogen gas that releases hydrogen .
前記透明導電性材料の導電率制御法において、前記透明導電性材料表面にマスクを配し、前記マスクの開口部に存在する前記水素を含む化合物又は水素ガスを通して光照射し、位置選択的に導電率を低下させてもよい。 In the method for controlling the conductivity of the transparent conductive material, a mask is disposed on the surface of the transparent conductive material, and light irradiation is performed through the hydrogen-containing compound or hydrogen gas present in the opening of the mask, thereby selectively conducting the position. The rate may be reduced.
前記透明導電性材料の導電率制御法において、前記透明導電性材料表面又は内部に光集束手段を通して光照射し、位置選択的又は空間選択的に導電率を低下させてもよい。
前記透明導電性材料の導電率制御法において、前記水素を含む化合物が固体又は液体であって、前記透明導電性材料表面に層状に形成されているか、あるいは前記透明導電性材料内部に浸透しているとよい。
In conductivity control method of the transparent conductive material, irradiated with light through the light focusing means to the inside or the transparent conductive material surface, it may reduce the regioselective or spatial selective conductivity.
In the conductivity control method of the transparent conductive material, the compound containing hydrogen is solid or liquid and is formed in a layer on the surface of the transparent conductive material, or penetrates into the transparent conductive material. It is good to be.
本発明の別の態様のデバイス作製法は、前記透明導電性材料の導電率制御法により、前記透明導電性材料表面乃至は内部の導電率を低下させることを特徴としている。 Device fabrication method of another aspect of the present invention, the conductivity control method of the transparent conductive material, the or transparent conductive material surface is characterized by reducing the internal conductivity.
本発明の別の態様のデバイスは、前記透明導電性材料のデバイス作製法により、前記透明導電性材料表面乃至は内部の導電率を低下させたことを特徴としている。 The device according to another aspect of the present invention is characterized in that the conductivity of the surface of the transparent conductive material or the inside thereof is lowered by the device manufacturing method of the transparent conductive material.
本発明によれば、透明導電性材料表面乃至は内部に、水素ガス又は水素を含む化合物を介して光照射することにより、従来困難とされてきた透明導電性材料表面乃至は内部の導電率を制御することが可能である。 According to the present invention, the surface of the transparent conductive material or the inside thereof is irradiated with light through a hydrogen gas or a compound containing hydrogen, so that the conductivity of the surface of the transparent conductive material or the internal conductivity, which has been conventionally difficult, is reduced. It is possible to control.
また、光を部分的に透過させるマスクや光集束手段等を用いることで、位置選択的（２次元選択的）あるいは空間選択的（３次元選択的）に導電率を変化させることが可能である。 Further, by using a mask that partially transmits light, light focusing means, or the like, it is possible to change the conductivity in a position-selective (two-dimensional selective) or space-selective (three-dimensional selective) manner. .
以下、本発明を実施するための最良の形態として、透明導電性材料の導電率制御法、デバイス作製法及びデバイスの実施の形態を図面に従って説明する。 Hereinafter, as the best mode for carrying out the present invention, a conductivity control method of a transparent conductive material, a device manufacturing method, and a device embodiment will be described with reference to the drawings.
図１で本発明に係る透明導電性材料の導電率制御法、デバイス作製法及びデバイスの実施の形態を示す。 FIG. 1 shows an embodiment of a conductivity control method, a device manufacturing method, and a device of a transparent conductive material according to the present invention.
図１（Ａ）は、透明導電性材料表面の導電率を制御する場合の実施の形態１で用いる実験概略構成であり、透明なシリカガラス基板１上の透明導電性材料としてのＳｎＯ２：Ｆ膜（フッ素ドープＳｎＯ２膜）２表面にはマスク４が密着配置されている。マスク４は開口部４ａを除きレーザー光３を遮断できる金属薄板あるいはシリカガラス基板１の表面に蒸着等で形成された金属膜等である。合成石英製入射窓６はマスク４上に密着して配置され（マスク４が薄板の場合、それを押さえる役目もある）、シリカガラス基板１と合成石英製入射窓６とで挟まれた開口部４ａ内には水素を含む化合物としての水（Ｈ２Ｏ）５が層状に形成されている。レーザー光３は、合成石英製入射窓６及び水５を介して透明導電性ＳｎＯ２：Ｆ膜２表面に照射される。
FIG. 1A is a schematic configuration of an experiment used in Embodiment 1 in the case of controlling the conductivity of the surface of a transparent conductive material, and SnO 2 : F as a transparent conductive material on a transparent silica glass substrate 1. A mask 4 is disposed in close contact with the surface of the film (fluorine-doped SnO 2 film) 2. The mask 4 is a thin metal plate that can block the laser light 3 except for the
レーザー光３の波長は、水５に吸収されて水素（原子又はイオン）を放出しかつ透明導電性ＳｎＯ２：Ｆ膜２にも吸収される紫外線領域の波長帯が望ましい。また、レーザー光３のエネルギー密度はレーザーアブレーションが起きない弱いレーザー光であることが好ましい。 The wavelength of the laser beam 3 is desirably a wavelength band in the ultraviolet region that is absorbed by the water 5 to release hydrogen (atoms or ions) and is also absorbed by the transparent conductive SnO 2 : F film 2. The energy density of the laser beam 3 is preferably a weak laser beam that does not cause laser ablation.
マスク４の開口部４ａを通してレーザー光３が照射された透明導電性ＳｎＯ２：Ｆ膜２の部分は電気抵抗が増大（導電率が低下）する。
The portion of the transparent conductive SnO 2 : F film 2 irradiated with the laser beam 3 through the
この実施の形態１によれば、次の通りの効果を得ることができる。 According to the first embodiment, the following effects can be obtained.
(1) 透明導電性材料としてのＳｎＯ２：Ｆ膜２の表面にマスク４を配し、マスク４の開口部４ａに存在する水素を含む化合物としての水５を通して光照射することで、位置選択的にＳｎＯ２：Ｆ膜２の導電率を変化させて、導電率制御が可能である。すなわち、所望の開口部形状のマスク４を用いることにより、開口部位置で規定された所望の位置に、開口部形状及び大きさで規定された所望の形状及び大きさの抵抗増大部分（導電率低下部分）を形成できる。 (1) Position selection by arranging a mask 4 on the surface of the SnO 2 : F film 2 as a transparent conductive material and irradiating light through water 5 as a compound containing hydrogen present in the opening 4a of the mask 4 In particular, it is possible to control the conductivity by changing the conductivity of the SnO 2 : F film 2. That is, by using the mask 4 having a desired opening shape, a resistance increasing portion (conductivity) having a desired shape and size defined by the opening shape and size is formed at a desired position defined by the opening position. Can be formed.
(2) 従って、所望の導電率パターンを有する透明導電膜を有するデバイス作製法を提供でき、また所望の導電率パターンを有する透明導電膜の透明デバイスを実現可能である。 (2) Therefore, a device manufacturing method having a transparent conductive film having a desired conductivity pattern can be provided, and a transparent device of a transparent conductive film having a desired conductivity pattern can be realized.
図１（Ｂ）は、透明導電性材料内部の導電率を制御する場合の実施の形態２で用いる実験概略構成であり、透明なシリカガラス基板１上の透明導電性ＳｎＯ２：Ｆナノ微粒子膜あるいは透明導電性ＳｎＯ２：Ｆ多孔性膜７と合成石英製入射窓６との間には水５が層状に形成されている。レーザー光３は、光集束手段としてのレンズ８を用い、合成石英製入射窓６及び水５を介して、透明導電性ＳｎＯ２：Ｆナノ微粒子膜あるいは透明導電性ＳｎＯ２：Ｆ多孔性膜７内部（又は表面）に集光照射される。
FIG. 1B is a schematic configuration of an experiment used in Embodiment 2 in the case of controlling the conductivity inside the transparent conductive material, and is a transparent conductive SnO 2 : F nanoparticle film on a transparent silica glass substrate 1. Alternatively, water 5 is formed in layers between the transparent conductive SnO 2 : F
ここで、透明導電性ＳｎＯ２：Ｆナノ微粒子膜あるいは透明導電性ＳｎＯ２：Ｆ多孔性膜７は、内部にも水５が浸透可能な材質である。
Here, the transparent conductive SnO 2 : F nanoparticulate film or the transparent conductive SnO 2 : F
また、透明導電性ＳｎＯ２：Ｆナノ微粒子膜あるいは透明導電性ＳｎＯ２：Ｆ多孔性膜７はレーザー光３の光源に対して、相対的に精密に三次元的に微動可能であり、結果的にレーザー光３が精密に三次元的に走査されるようになっている。
In addition, the transparent conductive SnO 2 : F nanoparticle film or the transparent conductive SnO 2 : F
この実施の形態２によれば、次の通りの効果を得ることができる。 According to the second embodiment, the following effects can be obtained.
(1) 透明導電性材料としての透明導電性ＳｎＯ２：Ｆナノ微粒子膜あるいは透明導電性ＳｎＯ２：Ｆ多孔性膜７の内部の導電率を、レーザー光３を走査することで、位置選択的及び空間選択的に制御することができる。
(1) A transparent conductive SnO 2 : F nanoparticle film or a transparent conductive SnO 2 : F
(2) レーザー光３の焦点位置を、透明導電性材料としての透明導電性ＳｎＯ２：Ｆナノ微粒子膜あるいは透明導電性ＳｎＯ２：Ｆ多孔性膜７の表面に合わせることにより、所望の位置に、所望の形状及び大きさで、透明導電性材料表面の導電性を制御することもできる。
(2) By aligning the focal position of the laser beam 3 with the surface of the transparent conductive SnO 2 : F nanoparticle film or the transparent conductive SnO 2 : F
(3) 従って、位置選択的及び空間選択的に透明導電性材料の導電率を制御したデバイス作製法を提供でき、また位置選択的及び空間選択的に透明導電性材料の導電率を制御した透明デバイスを実現可能である。 (3) Therefore, it is possible to provide a device manufacturing method in which the conductivity of the transparent conductive material is controlled in a position-selective and space-selective manner, and in which the conductivity of the transparent conductive material is controlled in a position-selective and space-selective manner. The device can be realized.
なお、上記の各実施の形態では、水素を含む化合物として水を例示したが、光を吸収して水素（原子又はイオン）を放出するものであればよく、メチルアルコール、エチルアルコール等も使用可能である。また、各実施の形態において、水素を含む化合物（液体又は固体）を使用する場合、周囲の雰囲気は大気（又は非反応性の気体）であればよいが、大気雰囲気の代わりに水素ガス雰囲気や水蒸気等の水素を含む化合物の気体雰囲気中としてもよく、この場合には水素を含む化合物（液体又は固体）を設ける必要はない。 In each of the above embodiments, water is exemplified as the compound containing hydrogen. However, any compound that absorbs light and releases hydrogen (atoms or ions) may be used, and methyl alcohol, ethyl alcohol, or the like can be used. It is. In each embodiment, when a compound containing hydrogen (liquid or solid) is used, the surrounding atmosphere may be air (or non-reactive gas), but a hydrogen gas atmosphere or A gas atmosphere of a compound containing hydrogen such as water vapor may be used. In this case, it is not necessary to provide a compound (liquid or solid) containing hydrogen.
前記透明導電性材料として、ＳｎＯ２：Ｆ以外の材料（例えば、Ｆ以外をドープしたＳｎＯ２等）も使用可能であり、水素（原子又はイオン）により導電率が変化する材料を使用可能である。 As the transparent conductive material, materials other than SnO 2 : F (for example, SnO 2 doped with other than F) can be used, and materials whose conductivity is changed by hydrogen (atoms or ions) can be used. .
水素ガス又は水素を含む化合物に吸収されて水素（原子又はイオン）を放出させ、かつ透明導電性材料にも吸収される紫外線領域の波長帯のランプ光源をレーザー光源の代わりに使用可能である（強力なエネルギー密度を必要としないため）。 A lamp light source having a wavelength band in the ultraviolet region that is absorbed by hydrogen gas or a compound containing hydrogen to release hydrogen (atoms or ions) and is also absorbed by the transparent conductive material can be used instead of the laser light source ( Because it does not require strong energy density).
以下、本発明に係る透明導電性材料の導電率制御法、デバイス作製法及びデバイスを実施例で詳述する。 Hereinafter, the conductivity control method, the device production method, and the device of the transparent conductive material according to the present invention will be described in detail in Examples.
図１（Ａ）の実験概略構成において、レーザー光３として、波長１９３ｎｍのＡｒＦエキシマレーザーを用いた。レーザー光照射部分でのエネルギー密度は、約２０ｍＪ／ｃｍ２／pulse一定とした。また、パルス繰り返し周波数は１０Ｈｚ一定とした。レーザー光照射時間は３０分及び４５分であった。シリカガラス基板１上の透明導電性ＳｎＯ２：Ｆ膜２の膜厚は、約１．２μｍであった。実験は大気中で行った。 1A, an ArF excimer laser having a wavelength of 193 nm was used as the laser beam 3. The energy density in the laser beam irradiation portion was fixed at about 20 mJ / cm 2 / pulse. The pulse repetition frequency was constant at 10 Hz. Laser light irradiation time was 30 minutes and 45 minutes. The film thickness of the transparent conductive SnO 2 : F film 2 on the silica glass substrate 1 was about 1.2 μm. The experiment was conducted in the atmosphere.
図２は、レーザー光照射時間と透明導電性ＳｎＯ２：Ｆ膜の抵抗との関係を示すグラフである。レーザー光照射前の透明導電性ＳｎＯ２：Ｆ膜の抵抗は、測定距離１０ｍｍ（膜に接触させた２本の針の距離）において約２０Ωであった。３０分のレーザー光照射後、その抵抗は約４００Ωまで上昇した。そして、レーザー光照射４５分後では約１０ｋΩを示すようになり、膜の平均可視透過率は概ね維持したまま、抵抗を約３桁の範囲で制御できることが判明した。 FIG. 2 is a graph showing the relationship between the laser light irradiation time and the resistance of the transparent conductive SnO 2 : F film. The resistance of the transparent conductive SnO 2 : F film before laser light irradiation was about 20Ω at a measurement distance of 10 mm (distance between two needles in contact with the film). After 30 minutes of laser light irradiation, the resistance increased to about 400Ω. Then, after 45 minutes of laser light irradiation, it showed about 10 kΩ, and it was found that the resistance can be controlled within a range of about 3 digits while maintaining the average visible transmittance of the film.
前記４５分でレーザー光照射された試料の膜厚を、触針式段差計により測定した結果、露光部分の膜厚変化は認められなかった。 As a result of measuring the film thickness of the sample irradiated with the laser beam in 45 minutes with a stylus type step meter, no change in the film thickness of the exposed portion was observed.
なお、比較のために、水を介在させず、前記同一条件でＡｒＦエキシマレーザーを照射した結果、透明導電性ＳｎＯ２：Ｆ膜の抵抗変化は認められなかった。 For comparison, as a result of irradiating ArF excimer laser under the same conditions without water, no change in resistance of the transparent conductive SnO 2 : F film was observed.
従って、実施例にて述べた導電率制御方法は、表面に段差の無い、所定の導電率パターンのデバイス作製法として利用でき、そのデバイス作製法により、表面に段差の無い、所定の導電率パターンの透明デバイスを得ることができる。 Therefore, the conductivity control method described in the embodiment can be used as a device manufacturing method of a predetermined conductivity pattern having no step on the surface, and the predetermined conductivity pattern having no step on the surface by the device manufacturing method. A transparent device can be obtained.
以上、本発明の実施の形態及び実施例について説明してきたが、本発明はこれに限定されることなく請求項の記載の範囲内において各種の変形、変更が可能なことは当業者には自明であろう。 Although the embodiments and examples of the present invention have been described above, the present invention is not limited to this, and it is obvious to those skilled in the art that various modifications and changes can be made within the scope of the claims. Will.
本発明によれば、透明導電性材料表面乃至は内部の導電率を、位置選択的あるいは空間選択的に変化させることにより、例えば透明導電性材料を基礎とした高効率電波吸収ガラスデバイスの作製法を確立でき、エレクトロニクス、オプトエレクトロニクス、フォトニクスあるいはバイオ/メディカル分野でのデバイス作製の基盤技術として利用可能であるなど多機能マイクロ/ナノデバイス作製のための必要不可欠な技術となる。また本発明は、これら分野にとどまらず、今後マイクロ・ナノマシーニング技術を利用して発展するデバイス作製の分野に多大に利用可能である。 According to the present invention, a method for producing a high-efficiency radio wave absorption glass device based on a transparent conductive material, for example, by changing the surface or internal conductivity of the transparent conductive material in a position-selective or space-selective manner. It can be used as a basic technology for device fabrication in the fields of electronics, optoelectronics, photonics or bio / medical, and is an indispensable technology for the fabrication of multifunctional micro / nano devices. The present invention is not limited to these fields, and can be used greatly in the field of device fabrication that will be developed using micro / nano machining techniques.
１ シリカガラス基板
２ 透明導電性ＳｎＯ２：Ｆ膜
３ レーザー光
４ マスク
５ 水（Ｈ２Ｏ）
６ 合成石英製入射窓
７ 透明導電性ＳｎＯ２：Ｆナノ微粒子膜あるいは透明導電性ＳｎＯ２：Ｆ多孔性膜
８ レンズ
1 silica glass substrate 2 transparent conductive SnO 2: F film 3 laser beam 4 mask 5 water (H 2 O)
6 Synthetic
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