JP3873126B2 - Method for producing indium phosphide nanowires and nanotubes - Google Patents
Method for producing indium phosphide nanowires and nanotubes Download PDFInfo
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- JP3873126B2 JP3873126B2 JP2003378896A JP2003378896A JP3873126B2 JP 3873126 B2 JP3873126 B2 JP 3873126B2 JP 2003378896 A JP2003378896 A JP 2003378896A JP 2003378896 A JP2003378896 A JP 2003378896A JP 3873126 B2 JP3873126 B2 JP 3873126B2
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- indium phosphide
- indium
- nanotubes
- nanowires
- weight ratio
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- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 title claims description 42
- 239000002071 nanotube Substances 0.000 title claims description 18
- 239000002070 nanowire Substances 0.000 title claims description 18
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 229910003437 indium oxide Inorganic materials 0.000 claims description 16
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 16
- 239000010453 quartz Substances 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 239000011261 inert gas Substances 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 229910052738 indium Inorganic materials 0.000 description 5
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000000945 filler Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000004093 laser heating Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Description
この出願の発明は、リン化インジウムナノワイヤーとリン化インジウムナノチューブの製造方法に関するものである。さらに詳しくは、この出願の発明は、エレクトロニクスやオプトエレクトロニクスの分野において応用が期待されているリン化インジウムのナノワイヤー及びナノチューブの新しい製造方法に関するものである。
The invention of this application relates to a method for producing indium phosphide nanowires and indium phosphide nanotubes . More specifically, the invention of this application relates to a new method for producing indium phosphide nanowires and nanotubes that are expected to be applied in the fields of electronics and optoelectronics.
リン化インジウムのナノワイヤーの合成には次の２つの方法が採用されている。 The following two methods are employed for the synthesis of indium phosphide nanowires.
一つは、金等の金属を含んだリン化インジウムをレーザー加熱する方法であり（たとえば、非特許文献１、２参照）、他の一つは、インジウム、ガリウム等の低融点金属のナノ粒子を触媒としてナノワイヤーを成長させる方法（たとえば、非特許文献３参照）である。
この出願の発明は、リン化インジウムのナノワイヤーやナノチューブといったナノ構造物を製造する新しい方法を提供することを解決すべき課題としている。 The invention of this application is to provide a new method for producing nanostructures such as indium phosphide nanowires and nanotubes.
この出願の発明は、上記の課題を解決するものとして、リン化インジウムと酸化インジウムの混合物を不活性ガスの気流中で石英管状炉により1000℃〜1500℃に加熱することを特徴とするリン化インジウムナノワイヤーとリン化インジウムナノチューブの製造方法を提供する。
In order to solve the above-mentioned problems, the invention of this application is characterized in that a mixture of indium phosphide and indium oxide is heated to 1000 ° C. to 1500 ° C. in a quartz tube furnace in an inert gas stream. A method for producing indium nanowires and indium phosphide nanotubes is provided.
この出願の発明のリン化インジウムナノワイヤーとリン化インジウムナノチューブの製造方法によれば、リン化インジウムナノワイヤーとリン化インジウムナノチューブの今までにない新しい製造方法が提供される。
According to the manufacturing method of indium phosphide nanowires and indium phosphide nanotubes of the invention of this application, an unprecedented new manufacturing method of indium phosphide nanowires and indium phosphide nanotubes is provided.
以下、実施例を示しつつ、この出願の発明のリン化インジウムナノワイヤーとリン化インジウムナノチューブについてさらに詳しく説明する。
Hereinafter, the indium phosphide nanowire and the indium phosphide nanotube of the invention of this application will be described in more detail with reference to examples.
この出願の発明のリン化インジウムナノワイヤーとリン化インジウムナノチューブの製造方法は、たとえば次のようにしてリン化インジウムナノワイヤーとリン化インジウムナノチューブを製造することができる。
The method for producing indium phosphide nanowires and indium phosphide nanotubes invention application can be prepared, for example, indium phosphide nanowires and indium phosphide nanotubes as follows.
まず、リン化インジウムと酸化インジウムの混合物を微粉化し、アルミナボートに入れる。次いで、アルミナボートを石英管状炉に取り付け、アルゴン等の不活性ガスを流しながらアルミナボートを1000℃〜1500℃に加熱する。加熱時間は、0.5時間〜２時間程度と
することができる。そして、出発物質である原料混合物が完全に蒸発すると、石英管の内壁の500℃〜600℃に維持された部分に灰色の粉末が堆積する。この粉末が、リン化インジウムのナノワイヤー及びナノチューブである。
First, a mixture of indium phosphide and indium oxide is pulverized and placed in an alumina boat. Next, the alumina boat is attached to a quartz tubular furnace, and the alumina boat is heated to 1000 ° C. to 1500 ° C. while flowing an inert gas such as argon. The heating time can be about 0.5 hour to 2 hours. When the raw material mixture as the starting material is completely evaporated, a gray powder is deposited on the portion of the inner wall of the quartz tube maintained at 500 ° C. to 600 ° C. This powder is indium phosphide nanowires and nanotubes.
原料混合物におけるリン化インジウムと酸化インジウムの重量比は、１０：0.5〜１０
：４の間とすることができる。酸化インジウムが、リン化インジウムを１０とする重量比で0.5を下回ると、触媒的な作用が弱まり、リン化インジウムナノワイヤーの収量が低下
する。酸化インジウムは、上記の重量比で４で十分にリン化インジウムナノチューブが生成するので、これより多く用いる必要はない。
The weight ratio of indium phosphide to indium oxide in the raw material mixture is 10: 0.5 to 10
: Between 4 When indium oxide is less than 0.5 by weight ratio with indium phosphide being 10, the catalytic action is weakened and the yield of indium phosphide nanowires is reduced. Indium oxide is sufficient to produce indium phosphide nanotubes at a weight ratio of 4 described above, and it is not necessary to use more than this.
加熱温度については、温度が高いほど生成する反応ガスの蒸発が十分に行われるようになるが、温度が高すぎると石英管状炉の劣化が起こり、好ましくないため、上限は1500℃とする。下限は、1000℃であり、その理由は、1000℃未満では反応性ガスの蒸発が遅くなるからである。 As for the heating temperature, the higher the temperature, the more the generated reaction gas evaporates. However, if the temperature is too high, the quartz tube furnace deteriorates, which is not preferable, so the upper limit is set to 1500 ° C. The lower limit is 1000 ° C., because the evaporation of the reactive gas is slowed below 1000 ° C.
加熱時間は、出発物質である原料混合物が蒸発し、完全に消失する時間であればよく、おおむね0.5時間〜２時間程度である。 The heating time should just be the time which the raw material mixture which is a starting material evaporates, and lose | disappears completely, and is about 0.5 to 2 hours in general.
加熱時の不活性ガスの流量は、500ml/min〜2000ml/minの範囲とすることができる。500mi/min未満であると生成ガスの移行に時間がかかり、2000ml/minを超えると移送ガスとしての不活性ガスが余分となる。 The flow rate of the inert gas during heating can be in the range of 500 ml / min to 2000 ml / min. If it is less than 500 mi / min, it takes time to transfer the product gas, and if it exceeds 2000 ml / min, an inert gas as a transfer gas becomes redundant.
レアメタリック社製のリン化インジウム片（純度99.999％）0.5ｇと和光純薬工業（株
）製の酸化インジウム粉末（純度99.9％）0.05ｇの混合物（重量比１０：１）をボールミルを用いて８時間かけて粉砕し、粒子径およそ数ミクロンの微粉にした。この混合粉末をアルミナボートに入れ、アルミナボートを長さ1.2ｍ、直径５cmの石英管状炉の端に挿入
した。アルゴンガスを1000ml/minの流量で石英管の中に流しながら、加熱した。温度が1150℃になった時、アルミナボートを石英管の中央部に移動させた。２時間加熱した後、石英管状炉を室温に冷却した。アルミナボートから２０cm〜２５cm離れた石英管の内壁に灰色の粉末が約２５mg堆積した。粉末が堆積した石英管の内壁の温度は、アルミナボートが1150℃の時、500℃〜600℃であった。
A ball mill was used to mix 0.5 g of indium phosphide pieces (purity 99.999%) manufactured by Rare Metallic and 0.05 g of indium oxide powder (purity 99.9%) manufactured by Wako Pure Chemical Industries, Ltd. (weight ratio 10: 1). The powder was pulverized over 8 hours to obtain a fine powder having a particle size of about several microns. This mixed powder was put into an alumina boat, and the alumina boat was inserted into the end of a quartz tubular furnace having a length of 1.2 m and a diameter of 5 cm. Heating was performed while flowing argon gas into the quartz tube at a flow rate of 1000 ml / min. When the temperature reached 1150 ° C., the alumina boat was moved to the center of the quartz tube. After heating for 2 hours, the quartz tube furnace was cooled to room temperature. About 25 mg of gray powder was deposited on the inner wall of the quartz tube 20 cm to 25 cm away from the alumina boat. The temperature of the inner wall of the quartz tube on which the powder was deposited was 500 ° C. to 600 ° C. when the alumina boat was 1150 ° C.
酸化インジウムを0.1ｇ（重量比１０：２）、0.2ｇ（重量比１０：４）に変えた以外はすべて上記と同一の条件で同一の操作を行った。いずれの場合にも、石英管の内壁の500
℃〜600℃に保たれた部分に灰色の粉末が25mg堆積した。
The same operation was performed under the same conditions as above except that indium oxide was changed to 0.1 g (weight ratio 10: 2) and 0.2 g (weight ratio 10: 4). In either case, the inner wall of the quartz tube
25 mg of a gray powder was deposited on the portion kept at a temperature of from 600C to 600C.
図１、図２、図３に、リン化インジウムと酸化インジウムの重量比を１０：１、１０：２、１０：４にした時に得られた生成物の走査型顕微鏡による観察像を示した。原料混合物の重量比が１０：１及び１０：２の場合の生成物は、図１及び図２に確認されるように、わずかに曲がったナノワイヤーである。その直径は１０ナノメートル〜３０ナノメートルで均一であり、長さは数十マイクロメートルである。原料混合物の重量比を１０：４とした時に得られた生成物は、図３に示したように、直径は約200ナノメートルと太い。ま
た、この生成物には、観察像において暗く写っている部分があり、このことから、充填物が内含されているナノチューブであると理解される。
FIGS. 1, 2 and 3 show images observed with a scanning microscope of the product obtained when the weight ratio of indium phosphide to indium oxide was 10: 1, 10: 2, and 10: 4. The product when the weight ratio of the raw material mixture is 10: 1 and 10: 2 is a slightly bent nanowire, as can be seen in FIGS. Its diameter is uniform from 10 nanometers to 30 nanometers, and its length is several tens of micrometers. As shown in FIG. 3, the product obtained when the weight ratio of the raw material mixture is 10: 4 is as thick as about 200 nanometers. In addition, this product has a dark portion in the observed image, which is understood to be a nanotube including a filler.
図４に、原料混合物の重量比を１０：２にした時に得られた生成物のＸ線回折パターンを示した。格子定数ａ＝1.022nmの立方晶系の酸化インジウム、格子定数ａ＝0.588nmの立方晶系のリン化インジウム及び正方晶系のインジウムのピークが見られ、最も強いピークはリン化インジウムである。このことから、生成物はリン化インジウムのナノワイヤーであると判定される。 FIG. 4 shows the X-ray diffraction pattern of the product obtained when the weight ratio of the raw material mixture was 10: 2. Peaks of cubic indium oxide having a lattice constant a = 1.02 nm, cubic indium phosphide and tetragonal indium having a lattice constant a = 0.588 nm are observed, and the strongest peak is indium phosphide. From this, it is determined that the product is an indium phosphide nanowire.
図５に、原料混合物の重量比が１０：４の時に得られた生成物の透過型電子顕微鏡像を示した。およそ５０％の充填率でナノチューブの内部に充填物が存在している。この充填
物を含む部分のナノチューブのＸ線エネルギー拡散スペクトルを図６に示した。この図６より、充填物はインジウムであると確認される。このことから、原料混合物の重量比が１０：４の時に得られた生成物は、インジウムが内含されているリン化インジウムナノチューブであると理解される。
FIG. 5 shows a transmission electron microscope image of the product obtained when the weight ratio of the raw material mixture was 10: 4. There is a filler inside the nanotube with a filling factor of approximately 50%. FIG. 6 shows an X-ray energy diffusion spectrum of the nanotube including the filler. From FIG. 6, it is confirmed that the filling is indium. From this, it is understood that the product obtained when the weight ratio of the raw material mixture is 10: 4 is indium phosphide nanotubes containing indium.
もちろん、この出願の発明は、以上の実施例によって限定されるものではない。細部については様々な態様が可能であることはいうまでもない。 Of course, the invention of this application is not limited by the above embodiments. Needless to say, various details are possible.
以上詳しく説明したとおり、この出願の発明によって、リン化インジウムナノワイヤーとリン化インジウムナノチューブの新しい製造方法が提供される。 As described in detail above, the present invention provides a new method for producing indium phosphide nanowires and indium phosphide nanotubes .
Claims (1)
A method for producing indium phosphide nanowires and indium phosphide nanotubes , wherein a mixture of indium phosphide and indium oxide is heated to 1000 ° C to 1500 ° C in a quartz tube furnace in an inert gas stream.
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| JP2003378896A JP3873126B2 (en) | 2003-11-07 | 2003-11-07 | Method for producing indium phosphide nanowires and nanotubes |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2003378896A JP3873126B2 (en) | 2003-11-07 | 2003-11-07 | Method for producing indium phosphide nanowires and nanotubes |
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| Publication Number | Publication Date |
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| JP2005139043A JP2005139043A (en) | 2005-06-02 |
| JP3873126B2 true JP3873126B2 (en) | 2007-01-24 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101760604B1 (en) | 2016-02-16 | 2017-07-31 | 조선대학교산학협력단 | Method for synthesizing horizontal ITO nanowires |
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| JP4576603B2 (en) * | 2004-05-26 | 2010-11-10 | 独立行政法人物質・材料研究機構 | Method for producing indium phosphide nanotubes |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101760604B1 (en) | 2016-02-16 | 2017-07-31 | 조선대학교산학협력단 | Method for synthesizing horizontal ITO nanowires |
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