JP2007118112A - Method for preparing nano-tree/nano-particle composite structure, and nano-tree/nano-particle composite structure - Google Patents
Method for preparing nano-tree/nano-particle composite structure, and nano-tree/nano-particle composite structure Download PDFInfo
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本願発明は、ナノ樹木状構造物とナノ微粒子の複合構造物の作製方法と作製されるナノ樹木状構造物とナノ微粒子の複合構造物に関する。 The present invention relates to a method for producing a composite structure of nano-dendritic structures and nano-fine particles and a composite structure of nano-dendritic structures and nano-particles to be produced.
これまでに数多くのナノメートルサイズの構造物（ナノ構造物）が創生され、実用化が展望されている。本発明者らも新しい形態を有するナノ構造物を実現している（特許文献１）。 Many nanometer-sized structures (nanostructures) have been created so far, and their practical application is expected. The present inventors have also realized a nanostructure having a new form (Patent Document 1).
本発明者らが提案しているナノ構造物は、ナノメートルサイズの樹木状構造物（ナノ樹木状構造物）であり、このナノ樹木状構造物は、真空中かつ電磁場中に配置された絶縁体基板の表面付近に原料ガスを導入し、収束かつ走査可能な電子ビームを絶縁体基板の表面に照射することにより絶縁体基板の表面に形成するものである。電子ビームの走査によりナノメートルの精度で絶縁体基板上に描かれるパターンに形成する。ナノ樹木状構造物は、他のナノ構造物に比べ表面積が大きく、したがって、触媒、センサー、量子素子などへの応用が期待されている。
本願発明は、先に提案したナノ樹木状構造物を発展させ、機能性材料としての応用に新たな展望を切り拓く新しいナノ構造物を創生することを課題としている。 This invention makes it a subject to develop the nano tree-like structure proposed previously and to create a new nano structure that opens up a new perspective for application as a functional material.
本願発明は、上記の課題を解決するものとして、第１に、ナノメートルサイズの樹木状構造物の表面にナノメートルサイズの微粒子を付着させることを特徴としている。 In order to solve the above problems, the present invention is characterized in that, firstly, nanometer-sized fine particles are adhered to the surface of a nanometer-sized tree-like structure.
本願発明は、第２に、イオンスパッタリング法によりナノメートルサイズの微粒子を付着させることを特徴としている。 Second, the present invention is characterized in that nanometer-sized fine particles are deposited by ion sputtering.
本願発明は、第３に、第１または第２の発明により作製される、ナノメートルサイズの樹木状構造物の表面にナノメートルサイズの微粒子が付着しているナノ樹木状構造物とナノ微粒子の複合構造物であることを特徴としている。 Thirdly, the present invention relates to a nano dendritic structure and a nano fine particle in which nanometer size fine particles are attached to the surface of a nanometer size dendritic structure produced according to the first or second invention. It is a composite structure.
本願の第１の発明によれば、ナノ樹木状構造物の表面にナノ微粒子が付着した全く新しい形態のナノ構造物が提供される。 According to 1st invention of this application, the nanostructure of the completely new form with which nanoparticle adhered to the surface of a nano dendritic structure is provided.
本願の第２の発明によれば、ナノ微粒子が効率的に発生し、ナノ樹木状構造物の表面に高い密度で付着する。 According to the second invention of the present application, nanoparticles are efficiently generated and adhere to the surface of the nano-dendritic structure at a high density.
本願の第３の発明によれば、より機能的なナノメートルサイズの触媒として、また、センサーや量子素子などとしての適用が考えられ、また、化学、生物、製薬などの分野での利用も考えられる新しいナノ構造物が提供される。 According to the third invention of the present application, it can be applied as a more functional nanometer-sized catalyst, as a sensor, a quantum device, or the like. New nanostructures are provided.
ナノ樹木状構造物は、たとえば、前記特許文献１に記載された方法で作製することができる。すなわち、セラミックス、ガラス、樹脂またはこれらの複合物から形成された絶縁体基板を真空中かつ電磁場中に置き、図１ａに示したように、真空を保ったまま、原料ガスを絶縁体基板の表面に導入する。たとえば、絶縁体基板の表面に向けて配置されたノズルなどを通じて原料ガスを導入することができる。原料ガス導入時の真空度は１×１０−２Ｐａ程度を目安にすることができる。電磁場の強度は、通常、１Ｔ〜１０Ｔの範囲にすることができる。原料ガスには、Ｗ、Ｍｏ、Ｔｉ、Ｔａ、Ｇａ、Ｃｕ、Ｚｎ、Ｉｎ、Ａｌ、Ｆｅ、Ｎｉ、Ｃｏなどの金属元素やＳｉ、Ｂなどの半導体元素もしくは半金属元素を含む化合物のガスが例示される。原料ガスは単一のガスまたは複数種の混合ガスとすることができる。 The nano-dendritic structure can be produced, for example, by the method described in Patent Document 1. That is, an insulator substrate formed of ceramics, glass, resin, or a composite thereof is placed in a vacuum and an electromagnetic field, and the source gas is supplied to the surface of the insulator substrate while maintaining the vacuum as shown in FIG. 1a. To introduce. For example, the source gas can be introduced through a nozzle or the like arranged toward the surface of the insulator substrate. The degree of vacuum when introducing the raw material gas can be about 1 × 10 −2 Pa. The intensity of the electromagnetic field can usually be in the range of 1T to 10T. The source gas includes a compound gas containing a metal element such as W, Mo, Ti, Ta, Ga, Cu, Zn, In, Al, Fe, Ni, Co, or a semiconductor element or a semimetal element such as Si or B. Illustrated. The source gas can be a single gas or a mixed gas of a plurality of types.
そして、原料ガスを絶縁体基板の表面付近に導入しながら、収束電子ビームを絶縁体基板の表面に照射する。収束電子ビームが照射された絶縁体基板の表面にナノ樹木状構造物が形成する。収束電子ビームについては、加速電圧２００ｋＶ、エネルギー２００ｋｅＶを標準的な条件として例示することができる。照射時間は数秒〜数十分程度とすることができる。絶縁体基板の温度は、通常、室温（５℃〜２２℃）とすることができる。ナノ樹木状構造物は、走査される収束電子イオンビームが照射された絶縁体基板の表面に形成する。したがって、ナノ樹木状構造物の形成はナノメートルの精度で可能である。 Then, the surface of the insulator substrate is irradiated with a focused electron beam while introducing the source gas near the surface of the insulator substrate. A nano dendritic structure is formed on the surface of the insulator substrate irradiated with the focused electron beam. As for the focused electron beam, an acceleration voltage of 200 kV and an energy of 200 keV can be exemplified as standard conditions. The irradiation time can be about several seconds to several tens of minutes. The temperature of the insulator substrate can usually be room temperature (5 ° C. to 22 ° C.). The nano dendritic structure is formed on the surface of the insulator substrate irradiated with the focused focused electron ion beam. Therefore, the formation of nano dendritic structures is possible with nanometer accuracy.
この他、ナノ樹木状構造物の作製は、化学合成方法、電気化学蒸着方法などによって行うこともできる。 In addition, the production of the nano-dendritic structure can also be performed by a chemical synthesis method, an electrochemical deposition method, or the like.
ナノ樹木構造物の表面にナノ微粒子を付着させる際には、ナノ微粒子の原料となるターゲット材を用い、ターゲット材に対してイオンスパッタリング、真空蒸着などを行うことができる。ナノ微粒子は単一の元素よりなるものの他、複数の元素を含むものなどとすることができる。生成するナノ微粒子は、図１ｂに示したように、ナノ樹木状構造物の表面に分布して付着する。ナノ樹木状構造物とナノ微粒子との複合構造物（ナノ樹木/ナノ微
粒子複合構造物）が得られる。ナノ樹木/ナノ微粒子複合構造物は、より機能的なナノメ
ートルサイズの触媒として、また、センサーや量子素子などとして有効であると考えられ、応用が期待される。また、化学、生物、製薬などの分野での利用も考えられる。
When the nano fine particles are attached to the surface of the nano tree structure, a target material that is a raw material of the nano fine particles is used, and ion sputtering, vacuum deposition, or the like can be performed on the target material. The nano fine particles may be composed of a single element or may include a plurality of elements. As shown in FIG. 1b, the generated nano fine particles are distributed and attached to the surface of the nano dendritic structure. A composite structure of nano-dendritic structures and nano-particles (nano-tree / nano-particle composite structure) is obtained. The nano-tree / nano-particle composite structure is considered to be effective as a more functional nanometer-sized catalyst, and as a sensor or quantum device, and is expected to be applied. It can also be used in fields such as chemistry, biology, and pharmaceuticals.
なお、ナノ微粒子の付着をイオンスパッタリング法により行うと、ナノ微粒子の生成が効率よく行われ、高い密度でナノ樹木状構造物の表面にナノ微粒子が付着する。 In addition, when nanoparticle adhesion is performed by ion sputtering, nanoparticle generation is efficiently performed, and the nanoparticle adheres to the surface of the nano-dendritic structure at a high density.
アルミナ（Ａｌ２Ｏ３）から形成された絶縁体基板を密閉容器内に配置し、室温に保った。密閉容器内を排気した後、密閉容器内にＷ（ＣＯ）６ガスを導入し、絶縁体基板の表面にＷ（ＣＯ）６ガスを流した。密閉容器内の圧力は１×１０−２Ｐａ以下であった。約１．５Ｔの磁場をかけ、広がりを抑えた電子ビームを絶縁体基板の表面に照射した。電子ビームは、加速電圧２００ｋＶ、エネルギー２００ｋｅＶとして発生させた。照射時間は１５０秒とした。図２の透過電子顕微鏡写真に示されるようなナノメートルサイズの樹木状構造物（ナノ樹木状構造物）が絶縁体基板の表面に形成した。細い枝の直径は３ｎｍ以下であった。形成したナノ樹木状構造物をエネルギー分散型分析装置（ＥＤＳ）を用いて分析した。その結果は図３に示した通りである。原料ガス中に含まれていたＷのピークが主に現れている。このことから、ナノ樹木状構造物はＷから形成されていると判定される。 An insulator substrate formed of alumina (Al 2 O 3 ) was placed in a sealed container and kept at room temperature. After evacuating the sealed container, introducing the W (CO) 6 gas into the sealed vessel was flushed the W (CO) 6 gas to the surface of the insulating substrate. The pressure in the sealed container was 1 × 10 −2 Pa or less. An approximately 1.5 T magnetic field was applied to irradiate the surface of the insulator substrate with an electron beam with reduced spread. The electron beam was generated with an acceleration voltage of 200 kV and an energy of 200 keV. The irradiation time was 150 seconds. A nanometer-sized tree-like structure (nano-dendritic structure) as shown in the transmission electron micrograph of FIG. 2 was formed on the surface of the insulator substrate. The diameter of the thin branch was 3 nm or less. The formed nano-dendritic structure was analyzed using an energy dispersive analyzer (EDS). The result is as shown in FIG. The peak of W contained in the source gas mainly appears. From this, it is determined that the nano-dendritic structure is formed of W.
次いで、密閉容器内にＡｕから形成されたターゲット材を配置し、イオンスパッタリングを行った。イオンスパッタリング装置として日本電子製QUICK Auto Coater JFC 1500を用い、真空度１×１０−１Ｐａ、陽極電圧１ｋＶ、陽極電流７ｍＡ、スパッタリング時間
７秒の条件で行った。
Subsequently, the target material formed from Au was arrange | positioned in the airtight container, and ion sputtering was performed. A QUICK Auto Coater JFC 1500 manufactured by JEOL Ltd. was used as the ion sputtering apparatus, and the conditions were such that the degree of vacuum was 1 × 10 −1 Pa, the anode voltage was 1 kV, the anode current was 7 mA, and the sputtering time was 7 seconds.
図４の透過電子顕微鏡写真に示されているように、ナノ樹木状構造物の表面に直径約２．１ｎｍのナノ微粒子が分布して付着していることが確認された。付着密度は２．７×１０１２/ｃｍ２であった。得られたナノ樹木状構造物とナノ微粒子との複合構造物をエネ
ルギー分散型分析装置（ＥＤＳ）により分析した。図５はその結果であり、ナノ樹木状構造物を形成するＷに加え、Ａｕのピークが現れている。ナノ樹木状構造物の表面に付着したナノ微粒子はＡｕのナノ微粒子であると判定される。
As shown in the transmission electron micrograph of FIG. 4, it was confirmed that nanoparticles having a diameter of about 2.1 nm were distributed and adhered to the surface of the nano-dendritic structure. The adhesion density was 2.7 × 10 12 / cm 2 . The obtained composite structure of nano dendritic structure and nano fine particles was analyzed by an energy dispersive analyzer (EDS). FIG. 5 shows the result, and an Au peak appears in addition to W forming the nano-dendritic structure. The nano fine particles attached to the surface of the nano dendritic structure are determined to be Au nano fine particles.
以上詳しく説明した通り、本願発明によって、全く新しい形態のナノ構造物が提供される。 As explained in detail above, the present invention provides a completely new form of nanostructure.
Claims (3)
、ナノメートルサイズの樹木状構造物の表面にナノメートルサイズの微粒子が付着しているナノ樹木/ナノ微粒子複合構造物。 A nano-tree / nanoparticle composite comprising nanometer-size fine particles attached to the surface of a nanometer-size dendritic structure produced by the method for producing a nano-tree / nanoparticle composite structure according to claim 1 or 2. Structure.
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