JP2005139044A - Single crystal silicon nanotube and its manufacturing method - Google Patents
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- 239000002620 silicon nanotube Substances 0.000 title claims abstract description 20
- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 239000005083 Zinc sulfide Substances 0.000 claims abstract description 28
- 229910052984 zinc sulfide Inorganic materials 0.000 claims abstract description 28
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002070 nanowire Substances 0.000 claims abstract description 26
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims abstract description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims description 28
- 230000006698 induction Effects 0.000 claims description 10
- 239000011261 inert gas Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 13
- 229910052710 silicon Inorganic materials 0.000 abstract description 10
- 239000010703 silicon Substances 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 5
- 229910021430 silicon nanotube Inorganic materials 0.000 abstract description 5
- 239000000243 solution Substances 0.000 abstract description 4
- 239000007864 aqueous solution Substances 0.000 abstract description 3
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 229910002804 graphite Inorganic materials 0.000 description 10
- 239000010439 graphite Substances 0.000 description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 239000002071 nanotube Substances 0.000 description 6
- 229920000049 Carbon (fiber) Polymers 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 239000004917 carbon fiber Substances 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 1
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 description 1
- 229940005991 chloric acid Drugs 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- VDCSGNNYCFPWFK-UHFFFAOYSA-N diphenylsilane Chemical compound C=1C=CC=CC=1[SiH2]C1=CC=CC=C1 VDCSGNNYCFPWFK-UHFFFAOYSA-N 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000004093 laser heating Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
Description
この出願の発明は、単結晶の珪素ナノチューブとその製造方法に関するもので、さらに詳しくは、ナノスケールの半導体デバイス等に有用な単結晶の珪素ナノチューブの製造方法に関する。 The invention of this application relates to a single crystal silicon nanotube and a method for manufacturing the same, and more particularly to a method for manufacturing a single crystal silicon nanotube useful for a nanoscale semiconductor device or the like.
従来より、珪素ナノワイヤーは、金属触媒を用いたレーザー加熱法（非特許文献１参照）や、珪素と珪素酸化物の加熱による方法（非特許文献２参照）、ジフェニルシランの高温熱分解による方法（非特許文献３参照）などによって製造されることが知られている。
上記のように、珪素ナノワイヤーは、すでにその製造方法が知られているが、珪素ナノチューブについては、そのバンド構造等が計算により予測されているものの、いまだ実際に製造されたことはない。そこで、この出願の発明は、単結晶の珪素ナノチューブとその製造方法を提供することを課題としている。 As described above, the manufacturing method of silicon nanowires is already known, but the silicon nanotube has not been actually manufactured, although the band structure and the like thereof are predicted by calculation. Accordingly, an object of the invention of this application is to provide a single crystal silicon nanotube and a manufacturing method thereof.
この出願の発明は上記の課題を解決するものとして、第１には、外径が１２０〜１８０ナノメートル、チューブ壁の厚さが４０〜６０ナノメートルである単結晶珪素ナノチューブを提供する。 In order to solve the above problems, the invention of this application first provides a single crystal silicon nanotube having an outer diameter of 120 to 180 nanometers and a tube wall thickness of 40 to 60 nanometers.
また、この出願の発明は、第２には、硫化亜鉛粉末を不活性雰囲気で１１５０〜１２５０℃に加熱して硫化亜鉛ナノワイヤーを生成させ、この硫化亜鉛ナノワイヤーを不活性雰囲気で一酸化珪素と１２００〜１４００℃で加熱反応させることを特徴とする単結晶珪素ナノチューブの製造方法を提供する。 In addition, the invention of this application is, secondly, zinc sulfide powder is heated to 1150 to 1250 ° C. in an inert atmosphere to produce zinc sulfide nanowires, and the zinc sulfide nanowires are silicon monoxide in an inert atmosphere. And a method for producing a single crystal silicon nanotube, wherein the reaction is performed at 1200 to 1400 ° C.
さらに具体的には、この出願の発明は、第３には、たとえばグラファイト製るつぼ中に硫化亜鉛粉末を入れ、このるつぼを縦型高周波誘導加熱炉中のグラファイト製加熱円筒管の中央部に設置し、不活性気体を流しながら、１１５０〜１２５０℃に１〜２時間加熱して、硫化亜鉛ナノワイヤーを生成させ、次に、グラファイト製るつぼの中に、一酸化ケイ素粉末を入れ、このるつぼを上記の加熱炉中のグライファイト製円筒管の中央部に設置し、不活性気体を流しながら、１２００〜１４００℃に、１〜２時間加熱し、加熱炉を室温に冷却した後、生成物を加熱炉から取り出し、塩酸で処理することにより、単結晶の珪素ナノチューブを製造する方法を提供する。 More specifically, according to the invention of this application, thirdly, for example, zinc sulfide powder is placed in a graphite crucible, and this crucible is installed at the center of a graphite heated cylindrical tube in a vertical high frequency induction heating furnace. Then, while flowing an inert gas, it is heated to 1150 to 1250 ° C. for 1 to 2 hours to form zinc sulfide nanowires. Next, silicon monoxide powder is put into a graphite crucible, and the crucible is placed in the crucible. Installed in the center of the griffite cylindrical tube in the heating furnace, heated to 1200-1400 ° C for 1-2 hours while flowing an inert gas, cooled the heating furnace to room temperature, Provided is a method for producing single-crystal silicon nanotubes by removing them from a heating furnace and treating with hydrochloric acid.
上記のとおりのこの出願の発明によって、マイクロエレクトロニクス、オプトエレクトロニクス分野において、その応用が期待されている単結晶珪素ナノチューブが提供され、また硫化亜鉛、一酸化ケイ素を原料として加熱することにより単結晶珪素ナノチューブの製造が可能とされている。 According to the invention of this application as described above, single crystal silicon nanotubes that are expected to be applied in the microelectronics and optoelectronic fields are provided, and single crystal silicon is heated by heating using zinc sulfide and silicon monoxide as raw materials. Nanotubes can be manufactured.
この出願の発明は上記のとおりの特徴をもつものであるが、以下にその実施の形態について説明する。 The invention of this application has the features as described above, and an embodiment thereof will be described below.
より具体的な好適な形態について説明すると、この出願の発明の単結晶珪素ナノチューブの製造方法では、まず、加熱装置として、好適には石英管の内側に断熱材のカーボン繊維で覆われたグラファイト製の誘導加熱円筒管を有する縦型高周波誘導加熱炉を用いて、たとえば好ましくはグラファイト製るつぼの中に、硫化亜鉛粉末を入れ、このるつぼをグラファイト製の誘導加熱円筒管の中央部に設置する。アルゴンガスなどの不活性気体を流しながら、１１５０〜１２５０℃に、１〜２時間加熱して硫化亜鉛ナノワイヤーを生成させる。この際、加熱温度は上記の範囲が好ましく、１２５０℃よりも加熱温度を高くすると、硫化亜鉛ナノワイヤーの直径が太くなり、１１５０℃よりも低いと、硫化亜鉛ナノワイヤーの収率が低下する。加熱時間は１〜２時間が好ましく、２時間で十分に原料の蒸発が終了する。１時間未満の場合には硫化亜鉛ナノワイヤーの生成量が減少する。 A more specific preferred embodiment will be described. In the method for producing single-crystal silicon nanotubes of the invention of this application, first, as a heating device, preferably made of graphite covered with a carbon fiber of a heat insulating material inside a quartz tube. Using a vertical high-frequency induction heating furnace having an induction heating cylindrical tube, for example, zinc sulfide powder is preferably placed in a graphite crucible, and this crucible is placed at the center of the graphite induction heating cylindrical tube. While flowing an inert gas such as argon gas, it is heated to 1150 to 1250 ° C. for 1 to 2 hours to generate zinc sulfide nanowires. In this case, the heating temperature is preferably within the above range, and if the heating temperature is higher than 1250 ° C., the diameter of the zinc sulfide nanowire becomes thicker, and if it is lower than 1150 ° C., the yield of the zinc sulfide nanowire decreases. The heating time is preferably 1 to 2 hours, and the evaporation of the raw material is completed in 2 hours. In the case of less than 1 hour, the amount of zinc sulfide nanowires produced decreases.
次に、グライファイト製るつぼの中に、一酸化ケイ素粉末を入れ、このるつぼをグラファイト製の誘導加熱円筒管の中央部に取り付け、不活性気体を流しながら、１２００〜１４００℃に、１〜２時間加熱した後、加熱炉を室温に冷却する。これによりナノワイヤー生成物が得られることになる。このナノワイヤー生成物は、硫化亜鉛・珪素のコア・シェル構造を有するものである。この生成したナノワイヤーを酸水溶液、たとえば塩酸、硫酸、塩素酸等の酸の水溶液、より好適には塩酸水溶液で処理することにより、単結晶の珪素ナノチューブを得ることができる。塩酸水溶液の場合には、その濃度を５〜２０％程度、より好適には１０％前後とすることが考慮される。 Next, silicon monoxide powder is put into a griffet crucible, this crucible is attached to the center of a graphite induction heating cylindrical tube, and an inert gas is allowed to flow to 1200-1400 ° C. at 1-2. After heating for an hour, the furnace is cooled to room temperature. This will result in a nanowire product. This nanowire product has a core-shell structure of zinc sulfide / silicon. By treating the produced nanowire with an acid aqueous solution, for example, an aqueous solution of an acid such as hydrochloric acid, sulfuric acid, or chloric acid, more preferably an aqueous hydrochloric acid solution, single crystal silicon nanotubes can be obtained. In the case of an aqueous hydrochloric acid solution, the concentration is considered to be about 5 to 20%, more preferably about 10%.
硫化亜鉛ナノワイヤーと一酸化珪素との加熱においては、硫化亜鉛粉末と一酸化ケイ素粉末の重量比は１：１〜２：１が好ましく、これよりも一酸化ケイ素の量が多いと、最終生成物の中に、珪素ナノワイヤーが混入する。加熱温度は、１２００〜１４００℃が好ましく、これ以上の温度に上げても収量の向上は望めない。また、１２００℃よりも加熱温度が低いと、珪素の蒸気の発生が十分でなく、硫化亜鉛・珪素のコア・シェル構造のナノワイヤーが生成しない。加熱時間は１〜２時間が好ましく、２時間以上加熱しても収量の向上は望めないし、さらに長時間加熱すると、硫化亜鉛・珪素コア・シェルナノワイヤーの表面に珪素ナノ粒子が付着してしまう。１時間未満だと硫化亜鉛・珪素コア・シェルナノワイヤーの収量が低下する。不活性ガスの流量は１００〜２００ｓｃｃｍが好ましく、２００ｓｃｃｍ以上流す必要はない。１００ｓｃｃｍ未満だと最終生成物の収量が低下する。 In the heating of zinc sulfide nanowires and silicon monoxide, the weight ratio of zinc sulfide powder to silicon monoxide powder is preferably 1: 1 to 2: 1. If the amount of silicon monoxide is larger than this, the final product Silicon nanowires are mixed in the object. The heating temperature is preferably 1200 to 1400 ° C. Even if the heating temperature is raised beyond this, no improvement in yield can be expected. On the other hand, if the heating temperature is lower than 1200 ° C., the generation of silicon vapor is not sufficient, and nanowires having a core / shell structure of zinc sulfide / silicon are not generated. The heating time is preferably 1 to 2 hours, and improvement in yield cannot be expected even when heated for 2 hours or longer, and when heated for a longer time, silicon nanoparticles adhere to the surface of zinc sulfide / silicon core / shell nanowires . If it is less than 1 hour, the yield of zinc sulfide, silicon core, and shell nanowires will decrease. The flow rate of the inert gas is preferably 100 to 200 sccm, and it is not necessary to flow 200 sccm or more. If it is less than 100 sccm, the yield of the final product decreases.
なお、上記いずれの場合の不活性気流については、アルゴン、ヘリウム等の不活性ガスの流通下であってよい。 Note that the inert airflow in any of the above cases may be under the flow of an inert gas such as argon or helium.
そこで以下に実施例を説明する。もちろん以下の例によって発明が限定されることはない。 Accordingly, examples will be described below. Of course, the invention is not limited by the following examples.
石英管の内側に断熱材のカーボン繊維で覆われたグラファイト製の誘導加熱円筒管を有する縦型高周波誘導加熱炉を反応装置として用い、グラファイト製るつぼの中に、シグマアルドリッチ社製の硫化亜鉛粉末（純度９９．９９％）１．５ｇを入れ、このるつぼを前記の誘導加熱円筒管の中央部に設置した。流量１２０ｓｃｃｍのアルゴンガスを流しながら、１２００℃に１．５時間加熱した。加熱炉を室温に冷却すると、カーボン繊維の表面に直径約５０ナノメートルの硫化亜鉛ナノワイヤーが成長した。 Zinc sulfide powder made by Sigma-Aldrich Co., Ltd. is used in a graphite crucible using a vertical high frequency induction heating furnace having a graphite induction heating cylindrical tube covered with carbon fiber as a heat insulating material inside the quartz tube. (Purity 99.99%) 1.5 g was added, and this crucible was placed in the center of the induction heating cylindrical tube. While flowing argon gas at a flow rate of 120 sccm, the mixture was heated to 1200 ° C. for 1.5 hours. When the heating furnace was cooled to room temperature, zinc sulfide nanowires having a diameter of about 50 nanometers grew on the surface of the carbon fiber.
次に、グラファイト製るつぼの中に、シグマアルドリッチ社製の一酸化ケイ素粉末（３
２５メッシュ）１．０ｇを入れ、このるつぼを前記の誘導加熱円筒管の中央部に取り付けた。流量１２０ｓｃｃｍのアルゴンガスを流しながら、１３５０℃に１時間加熱した。加熱終了後、加熱炉を室温に冷却すると、カーボン繊維の表面に硫化亜鉛・ケイ素のコア・シェル構造のナノワイヤーが生成した。この生成したナノワイヤーを１０％塩酸水溶液で処理した後、蒸留水、エタノールで洗浄した。
Next, in a graphite crucible, a silicon monoxide powder (3
(25 mesh) 1.0 g was put, and this crucible was attached to the central portion of the induction heating cylindrical tube. While flowing argon gas at a flow rate of 120 sccm, the mixture was heated to 1350 ° C. for 1 hour. After heating, when the heating furnace was cooled to room temperature, nanowires with a zinc sulfide / silicon core / shell structure formed on the surface of the carbon fiber. The produced nanowire was treated with a 10% aqueous hydrochloric acid solution, and then washed with distilled water and ethanol.
図１に、得られた生成物のＸ線回折のパターンを示した。この回折図から格子定数ａ＝５．４２８Åを有する立方晶系の珪素であることが確認された。図２には、このナノチューブの透過型電子顕微鏡像の写真を示した。この写真から、ナノチューブの外径は１２０〜１８０ナノメートル、チューブ壁の厚さは４０〜６０ナノメートルで、ナノチューブの先端は開口していることがわかる。図３は、このナノチューブのＸ線エネルギー拡散スペクトルを示したものであるが、その化学組成は珪素からなることがわかる。この図３には、少量の酸素と銅のピークが見られるが、酸素は試料を作製するときに酸素に触れたために現れたもので、銅のピークは試料を作製するときに用いた銅グリッドから由来するものである。先のＸ線回折のパターンと合わせて考えると、このナノチューブは単結晶の珪素で構成されていることが理解される。 FIG. 1 shows an X-ray diffraction pattern of the obtained product. From this diffraction pattern, it was confirmed to be cubic silicon having a lattice constant a = 5.428Å. FIG. 2 shows a photograph of a transmission electron microscope image of the nanotube. From this photograph, it can be seen that the outer diameter of the nanotube is 120 to 180 nm, the thickness of the tube wall is 40 to 60 nm, and the tip of the nanotube is open. FIG. 3 shows the X-ray energy diffusion spectrum of this nanotube, and it can be seen that its chemical composition is made of silicon. In FIG. 3, a small amount of oxygen and copper peaks can be seen. Oxygen appeared because the oxygen was touched when preparing the sample, and the copper peak was the copper grid used when preparing the sample. Is derived from Considering the above X-ray diffraction pattern, it is understood that the nanotube is composed of single crystal silicon.
この出願の発明により、単結晶の珪素ナノチューブの製造が可能となり、ナノスケール領域における半導体デバイスへの応用が期待される。 The invention of this application enables the production of single-crystal silicon nanotubes, and is expected to be applied to semiconductor devices in the nanoscale region.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006117443A (en) * | 2004-10-19 | 2006-05-11 | National Institute For Materials Science | Crystalline silicon microtube and its manufacturing method |
| WO2006057464A2 (en) * | 2004-11-29 | 2006-06-01 | Univ Tokyo Nat Univ Corp | Process for producing silicon nanofilamentous form |
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