JP2005008431A - Production method for monolayered boron nitride nanotube by laser ablation method - Google Patents
Production method for monolayered boron nitride nanotube by laser ablation method Download PDFInfo
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- JP2005008431A JP2005008431A JP2003170919A JP2003170919A JP2005008431A JP 2005008431 A JP2005008431 A JP 2005008431A JP 2003170919 A JP2003170919 A JP 2003170919A JP 2003170919 A JP2003170919 A JP 2003170919A JP 2005008431 A JP2005008431 A JP 2005008431A
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- boron nitride
- monolayered
- walled
- laser ablation
- nitride nanotube
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Abstract
Description
【0001】
【発明の属する技術分野】
この出願の発明は、単層窒化ホウ素ナノチューブの製造方法に関する。さらに詳しくは、この出願の発明は、半導体材料、エミッター材料、耐熱性充填材料、高強度材料、触媒等の分野において従来にない特性を有する材料として見込まれる窒化ホウ素の単層ナノチューブを高純度で製造することのできる単層窒化ホウ素ナノチューブの製造方法に関する。
【0002】
【従来の技術】
炭素原子が筒状に並んだナノメートルサイズのチューブ状炭素物質、カーボンナノチューブが知られている。このカーボンナノチューブは、アーク放電法、レーザー加熱法、化学的気相成長法等により合成されており、直径、巻き方、層数等によって導体あるいは半導体の性質を示す。
【0003】
近年、窒化ホウ素が、グラファイトと構造的な類似性があることから、窒化ホウ素ナノチューブもまた、上記と同様な方法により合成されている。この他、窒化ホウ素ナノチューブの製造方法については、ホウ化ニッケルを触媒に使用し、ボラジンを原料として合成する方法(たとえば、非特許文献1参照)やカーボンを鋳型として使用し、酸化ホウ素と窒素を高周波誘導加熱炉中で反応させて合成する方法(たとえば、特許文献1、2参照)が提案されている。窒化ホウ素ナノチューブには、カーボンナノチューブと比較して熱的、化学的に安定であるという大きな利点がある。このことから、窒化ホウ素は、半導体材料、エミッター材料、耐熱性充填材料、高強度材料、触媒等の分野において従来にない特性を有する材料として見込まれている。
【0004】
【非特許文献1】
O.R.Lourie外,ケミカル・マテリアルズ(Chem.Mater.),2000年,第12巻,p.1808
【特許文献1】
特開2000−109306号公報
【特許文献2】
特開2002−97004号公報
【0005】
【発明が解決しようとする課題】
しかしながら、上述の窒化ホウ素ナノチューブの製造方法には、安全性において、また、カーボン等の不純物を含む等の問題があり、窒化ホウ素ナノチューブの半導体特性や強度等の物理的特性を測定することは困難であった。
【0006】
この出願の発明は、このような事情に鑑みてなされたものであり、炭素等の不純物を含まない高純度の単層窒化ホウ素ナノチューブを製造することのできる単層窒化ホウ素ナノチューブの製造方法を提供することを解決すべき課題としている。
【0007】
【課題を解決するための手段】
この出願の発明は、上記の課題を解決するものとして、100Torrの窒素雰囲気中で、波長1.064μm、パルス幅60ps、繰り返し回数2×105パルス/秒、強度2.7×1011W/cm2のレーザー光を、ターゲットとしての窒化ホウ素に照射することを特徴とする単層窒化ホウ素ナノチューブの製造方法を提供する(請求項1)。
【0008】
【発明の実施の形態】
この出願の発明の単層窒化ホウ素ナノチューブの製造方法では、窒素の減圧下で短時間−超高繰り返し回数のパルスレーザーを、ターゲットとしての窒化ホウ素に照射することにより、レーザー光の焦点付近にすす状の生成物を堆積させる。この生成物の中に、不純物のきわめて少ない高純度の単層窒化ホウ素ナノチューブが含まれる。
【0009】
短時間−超高繰り返し回数のレーザー照射法により単層窒化ホウ素ナノチューブが得られることは、従来技術にはない画期的なことである。
【0010】
以下、実施例を示し、この出願の発明の単層窒化ホウ素ナノチューブの製造方法についてさらに詳しく説明する。
【0011】
【実施例】
100Torrの窒素減圧中で、波長1.064μm、パルス幅60ps、繰り返し回数2×105パルス/秒、レーザー強度2.7×1011W/cm2の短時間−超高繰り返し回数のレーザーを、ターゲットとしての窒化ホウ素に照射した。レーザー光の焦点付近にすす状の生成物が堆積した。生成物は、質量分析装置を用いて測定した結果、不純物の総量が220ppm以下の高純度であった。この生成物を四塩化炭素に分散して超音波処理し、カーボン膜の付いた銅グリッドに滴下して透過型電子顕微鏡観察のための試料を作製した。
【0012】
図1は、高分解能透過型電子顕微鏡を用いて観察した像の写真である。
【0013】
単層のナノチューブが確認された。このチューブの巻き方はジグザグ状であった。
【0014】
図2は、得られた単層のナノチューブの電子エネルギー損失スペクトルを示した図である。
【0015】
この図2には、188eVと401evにホウ素と窒素のピークがそれぞれ現れており、B/N比は0.9±0.2である。このことから、化学量論的窒化ホウ素が生成していることが確認された。また、図2には、ホウ素、窒素以外のピークはなく、生成物である単層窒化ホウ素ナノチューブは高純度であることも確認された。
【0016】
【発明の効果】
以上詳しく説明したとおり、この出願の発明によって、炭素等の不純物を含まない高純度の単層窒化ホウ素ナノチューブが製造される。
【図面の簡単な説明】
【図1】単層窒化ホウ素ナノチューブの高分解能透過型電子顕微鏡像の写真である。
【図2】単層窒化ホウ素ナノチューブの電子エネルギー損失スペクトルを示した図である。[0001]
BACKGROUND OF THE INVENTION
The invention of this application relates to a method for producing single-walled boron nitride nanotubes. More specifically, the invention of this application relates to boron nitride single-walled nanotubes, which are expected as materials having unprecedented properties in the fields of semiconductor materials, emitter materials, heat-resistant filling materials, high-strength materials, catalysts, etc., with high purity. The present invention relates to a method for producing single-walled boron nitride nanotubes that can be produced.
[0002]
[Prior art]
A carbon nanotube, a nanometer-sized tubular carbon material in which carbon atoms are arranged in a cylindrical shape, is known. These carbon nanotubes are synthesized by an arc discharge method, a laser heating method, a chemical vapor deposition method, or the like, and exhibit the properties of a conductor or a semiconductor depending on the diameter, winding method, number of layers, and the like.
[0003]
In recent years, since boron nitride has structural similarity with graphite, boron nitride nanotubes have also been synthesized by the same method as described above. In addition, as for the method for producing boron nitride nanotubes, nickel boride is used as a catalyst, borazine is used as a raw material (see, for example, Non-Patent Document 1), carbon is used as a template, boron oxide and nitrogen are used. A method of synthesizing by reacting in a high-frequency induction heating furnace (for example, see Patent Documents 1 and 2) has been proposed. Boron nitride nanotubes have the great advantage of being thermally and chemically stable compared to carbon nanotubes. For this reason, boron nitride is expected as a material having unprecedented characteristics in the fields of semiconductor materials, emitter materials, heat-resistant filling materials, high-strength materials, catalysts, and the like.
[0004]
[Non-Patent Document 1]
O. R. Lourie et al., Chemical Materials, 2000, Vol. 12, p. 1808
[Patent Document 1]
JP 2000-109306 A [Patent Document 2]
Japanese Patent Laid-Open No. 2002-97004
[Problems to be solved by the invention]
However, the above-described method for producing boron nitride nanotubes has problems such as safety and inclusion of impurities such as carbon, and it is difficult to measure physical properties such as semiconductor properties and strength of boron nitride nanotubes. Met.
[0006]
The invention of this application was made in view of such circumstances, and provides a method for producing single-walled boron nitride nanotubes that can produce high-purity single-walled boron nitride nanotubes that do not contain impurities such as carbon. It is a problem to be solved.
[0007]
[Means for Solving the Problems]
In order to solve the above problems, the invention of this application has a wavelength of 1.064 μm, a pulse width of 60 ps, a repetition rate of 2 × 10 5 pulses / second, and an intensity of 2.7 × 10 11 W / second in a nitrogen atmosphere of 100 Torr. A method for producing a single-walled boron nitride nanotube, characterized by irradiating boron nitride as a target with a laser beam of cm 2 (claim 1).
[0008]
DETAILED DESCRIPTION OF THE INVENTION
In the method for producing single-walled boron nitride nanotubes of the invention of this application, a boron laser as a target is irradiated with a pulse laser of a short time-ultra high repetition number under a reduced pressure of nitrogen, so that the laser light is made close to the focal point of the laser light. The product is deposited. Among these products are high purity single-walled boron nitride nanotubes with very few impurities.
[0009]
The single-walled boron nitride nanotubes can be obtained by a short-time and ultra-high repetition number of laser irradiation methods, which is an epoch-making that is not found in the prior art.
[0010]
Hereinafter, an Example is shown and the manufacturing method of the single layer boron nitride nanotube of invention of this application is demonstrated in more detail.
[0011]
【Example】
In a nitrogen decompression of 100 Torr, a laser with a wavelength of 1.064 μm, a pulse width of 60 ps, a repetition rate of 2 × 10 5 pulses / second, and a laser intensity of 2.7 × 10 11 W / cm 2 for a short time-ultra high repetition rate, Irradiated to boron nitride as a target. Soot-like product was deposited near the focal point of the laser beam. As a result of measuring the product using a mass spectrometer, the product had a high purity with the total amount of impurities being 220 ppm or less. This product was dispersed in carbon tetrachloride, subjected to ultrasonic treatment, and dropped onto a copper grid with a carbon film to prepare a sample for observation with a transmission electron microscope.
[0012]
FIG. 1 is a photograph of an image observed using a high-resolution transmission electron microscope.
[0013]
Single-walled nanotubes were confirmed. The tube was wound in a zigzag shape.
[0014]
FIG. 2 is a diagram showing an electron energy loss spectrum of the obtained single-walled nanotube.
[0015]
In FIG. 2, peaks of boron and nitrogen appear at 188 eV and 401 ev, respectively, and the B / N ratio is 0.9 ± 0.2. From this, it was confirmed that stoichiometric boron nitride was generated. In addition, in FIG. 2, there are no peaks other than boron and nitrogen, and it was confirmed that the single-walled boron nitride nanotube as a product has high purity.
[0016]
【The invention's effect】
As described above in detail, according to the invention of this application, high-purity single-walled boron nitride nanotubes that do not contain impurities such as carbon are produced.
[Brief description of the drawings]
FIG. 1 is a photograph of a high-resolution transmission electron microscope image of single-walled boron nitride nanotubes.
FIG. 2 is a diagram showing an electron energy loss spectrum of single-walled boron nitride nanotubes.
Claims (1)
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN100347079C (en) * | 2005-04-20 | 2007-11-07 | 中国科学院金属研究所 | Production of boron nitride nanometer tube with water as growth improver |
US9782565B2 (en) | 2008-10-01 | 2017-10-10 | Covidien Lp | Endoscopic ultrasound-guided biliary access system |
US10076316B2 (en) | 2008-10-01 | 2018-09-18 | Covidien Lp | Needle biopsy device |
-
2003
- 2003-06-16 JP JP2003170919A patent/JP3921537B2/en not_active Expired - Lifetime
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN100347079C (en) * | 2005-04-20 | 2007-11-07 | 中国科学院金属研究所 | Production of boron nitride nanometer tube with water as growth improver |
US9782565B2 (en) | 2008-10-01 | 2017-10-10 | Covidien Lp | Endoscopic ultrasound-guided biliary access system |
US10076316B2 (en) | 2008-10-01 | 2018-09-18 | Covidien Lp | Needle biopsy device |
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