JP4496353B2 - Silicon nanoparticles coated with zinc selenide film and method for producing the same - Google Patents
Silicon nanoparticles coated with zinc selenide film and method for producing the same Download PDFInfo
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- PFNQVRZLDWYSCW-UHFFFAOYSA-N (fluoren-9-ylideneamino) n-naphthalen-1-ylcarbamate Chemical compound C12=CC=CC=C2C2=CC=CC=C2C1=NOC(=O)NC1=CC=CC2=CC=CC=C12 PFNQVRZLDWYSCW-UHFFFAOYSA-N 0.000 title claims description 68
- 239000005543 nano-size silicon particle Substances 0.000 title claims description 57
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 35
- 239000000843 powder Substances 0.000 claims description 23
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims description 20
- 239000011261 inert gas Substances 0.000 claims description 12
- 239000012528 membrane Substances 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 238000005259 measurement Methods 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 6
- 239000010949 copper Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000002070 nanowire Substances 0.000 description 4
- 239000011669 selenium Substances 0.000 description 4
- 230000007704 transition Effects 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000005693 optoelectronics Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 2
- 238000002083 X-ray spectrum Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 229910052711 selenium Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 2
- OBUADXGKBSZKJY-UHFFFAOYSA-N [Se-2].[Zn+2].[Si+4].[Se-2].[Se-2] Chemical compound [Se-2].[Zn+2].[Si+4].[Se-2].[Se-2] OBUADXGKBSZKJY-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Description
本発明は、ナノサイズの電子デバイスや光電子デバイスの分野に利用可能な、セレン化亜鉛膜で被覆された珪素ナノ粒子及びその製造方法に関する。 The present invention relates to silicon nanoparticles coated with a zinc selenide film and a method for producing the same, which can be used in the field of nano-sized electronic devices and optoelectronic devices.
珪素は、約１．２ｅＶのバンドギャップエネルギーを有する間接遷移型半導体であって、現代の半導体工業を支える重要な材料となっている。一方、セレン化亜鉛は、約２．７ｅＶのバンドギャップエネルギーを有する直接遷移型半導体であって、青色または緑色の発光ダイオードやエレクトロルミネッセンスデバイス用に検討されている（例えば、非特許文献１，２参照）
本発明者らは、セレン化亜鉛と一酸化ケイ素とを１２００℃より高温で加熱することにより、珪素ナノワイヤーとセレン化亜鉛ナノワイヤーが軸方向に接合した珪素−セレン化亜鉛複合ナノワイヤーが製造できることをすでに報告している（例えば、非特許文献３参照）。
しかしながら、珪素ナノ粒子をセレン化亜鉛膜で被覆したものやその製造方法については知られていなかった。
The present inventors manufactured a silicon-zinc selenide composite nanowire in which silicon nanowire and zinc selenide nanowire are joined in the axial direction by heating zinc selenide and silicon monoxide at a temperature higher than 1200 ° C. It has already been reported that it can be performed (for example, see Non-Patent Document 3).
However, nothing has been known about the coating of silicon nanoparticles with a zinc selenide film or a method for producing the same.
そこで、本発明は、上記の現状に鑑み、新規なナノサイズの電子デバイスへの応用が可能なセレン化亜鉛膜で被覆された珪素ナノ粒子を提供することを第一の目的とする。
また、本発明は、簡単に効率よく合成することができる、セレン化亜鉛膜で被覆された珪素ナノ粒子の製造方法を提供することを第二の目的とする。
Therefore, in view of the above-described present situation, the first object of the present invention is to provide silicon nanoparticles coated with a zinc selenide film that can be applied to novel nano-sized electronic devices.
A second object of the present invention is to provide a method for producing silicon nanoparticles coated with a zinc selenide film, which can be easily and efficiently synthesized.
上記第一の目的を達成するために、本発明のセレン化亜鉛膜で被覆された珪素ナノ粒子は、珪素ナノ粒子内層と、この内層を被覆したセレン化亜鉛外層と、から成ることを特徴とする。この構成において、好ましくは、外層の厚みが３０ｎｍであり、全体の外径が１２０ｎｍ〜２００ｎｍである。
上記構成によれば、珪素ナノ粒子がセレン化亜鉛膜で被覆されているので、間接遷移型の珪素ナノ粒子を直接遷移型のセレン化亜鉛膜で被覆し、珪素とセレン化亜鉛のエネルギーギャップの差が大きいことから、新規なナノサイズの電子デバイスや光電子デバイスを提供することが可能となる。
In order to achieve the first object, silicon nanoparticles coated with the zinc selenide film of the present invention are characterized by comprising a silicon nanoparticle inner layer and a zinc selenide outer layer covering the inner layer. To do. In this configuration, preferably, the thickness of the outer layer is 30 nm and the entire outer diameter is 120 nm to 200 nm.
According to the above configuration, since the silicon nanoparticles are coated with the zinc selenide film, the indirect transition type silicon nanoparticles are coated with the direct transition type zinc selenide film, and the energy gap between silicon and zinc selenide is reduced. Since the difference is large, it is possible to provide a novel nano-sized electronic device or optoelectronic device.
上記第二の目的を達成するために、本発明のセレン化亜鉛膜で被覆された珪素ナノ粒子の製造方法は、加熱炉に、一酸化ケイ素粉末とセレン化亜鉛粉末とを入れた坩堝を配置し、不活性ガスを流しながら、上記坩堝を９００℃〜１１００℃の温度範囲で加熱することにより珪素ナノ粒子を生成し、次に、上記坩堝を１０５０℃〜１１５０℃の温度範囲で加熱することにより、上記珪素ナノ粒子をセレン化亜鉛膜で被覆することを特徴とする。
この構成において、珪素ナノ粒子を生成する際に加熱する時間は、好ましくは、０．８時間〜１．５時間の加熱時間の範囲とする。また、珪素ナノ粒子をセレン化亜鉛膜で被覆
する際に加熱する時間は、好ましくは、１時間〜２時間の加熱時間の範囲とする。また、一酸化ケイ素粉末とセレン化亜鉛粉末との質量比は、好ましくは、１：１〜１：２の範囲とする。また、不活性ガスとして、好ましくは、窒素ガスを使用する。不活性ガスの流量は、好ましくは、０．８ｌｔｒ（リットル、以下、本出願ではｌｔｒと表記する。）／分〜１．５ｌｔｒ／分の範囲とする。
この方法により、珪素ナノ粒子を生成し、この表面にセレン化亜鉛膜が被覆する。このセレン化亜鉛膜で被覆された珪素ナノ粒子は、上記の好ましい条件の下で、外層としてのセレン化亜鉛膜の厚みが３０ｎｍであり、セレン化亜鉛膜が被覆された状態で、全体の外径が１２０ｎｍ〜２００ｎｍのものが得られる。
In order to achieve the second object described above, the method for producing silicon nanoparticles coated with a zinc selenide film of the present invention includes arranging a crucible containing silicon monoxide powder and zinc selenide powder in a heating furnace. And heating the crucible in a temperature range of 900 ° C. to 1100 ° C. while flowing an inert gas, and then heating the crucible in a temperature range of 1050 ° C. to 1150 ° C. Thus, the silicon nanoparticles are coated with a zinc selenide film.
In this configuration, the time for heating when producing the silicon nanoparticles is preferably in the range of 0.8 to 1.5 hours. Further, the heating time when the silicon nanoparticles are coated with the zinc selenide film is preferably in the range of 1 to 2 hours. The mass ratio of the silicon monoxide powder and the zinc selenide powder is preferably in the range of 1: 1 to 1: 2. Further, nitrogen gas is preferably used as the inert gas. The flow rate of the inert gas is preferably in a range of 0.8 ltr (liter, hereinafter referred to as ltr in the present application) / min to 1.5 ltr / min.
By this method, silicon nanoparticles are generated, and the surface thereof is covered with a zinc selenide film. The silicon nanoparticles coated with this zinc selenide film have the thickness of the zinc selenide film as the outer layer of 30 nm under the above preferred conditions, and the entire outer surface of the silicon nanoparticle coated with the zinc selenide film is coated with the zinc selenide film. A diameter of 120 nm to 200 nm is obtained.
本発明のセレン化亜鉛膜で被覆された珪素ナノ粒子及びその製造方法によれば、加熱炉にセレン化亜鉛粉末及び一酸化ケイ素粉末の混合物を加熱して温度制御を行うことで、珪素ナノ粒子上にセレン化亜鉛膜を被覆することができ、新しいナノメートルサイズの電子デバイスや光電子デバイスなどに利用することができる。
また、この方法は、先ず第１段階として珪素ナノ粒子を生成し、次に第２段階として珪素ナノ粒子上にセレン化亜鉛膜を堆積させるという、二段階に分けて合成を行うので、第１段階や第２段階の温度や時間調整を行うことで、容易に、効率よく、セレン化亜鉛膜で被覆された珪素ナノ粒子を合成することができる。
According to the silicon nanoparticles coated with the zinc selenide film of the present invention and the method for producing the same, the temperature of the silicon nanoparticles is controlled by heating a mixture of zinc selenide powder and silicon monoxide powder in a heating furnace. A zinc selenide film can be coated thereon, and can be used for new nanometer-sized electronic devices and optoelectronic devices.
In addition, this method performs the synthesis in two steps, firstly forming silicon nanoparticles as the first step and then depositing a zinc selenide film on the silicon nanoparticles as the second step. By adjusting the temperature and time of the stage and the second stage, it is possible to synthesize silicon nanoparticles coated with a zinc selenide film easily and efficiently.
以下、本発明を実施するための最良の形態を図面に基づき詳細に説明する。
図１は、本発明のセレン化亜鉛膜で被覆された珪素ナノ粒子を製造する装置の一例を示す模式図である。この装置を例に製造方法を説明する。図において、加熱装置１は、反応管２の周囲に、抵抗加熱炉３を有している。そして、一酸化ケイ素粉末およびセレン化亜鉛粉末の混合物４を入れた坩堝５を、反応管２内に配置している。抵抗加熱炉３で坩堝５が加熱される。矢印６は反応管２に供給される不活性ガスを示している。
ここで、加熱装置１には、抵抗加熱法による横型の加熱炉を用いているが、この場合、加熱炉は横型に限らず縦型でもよい。また、加熱装置は、抵抗加熱に限らず、坩堝５を加熱することができるランプ加熱や高周波誘導加熱による加熱装置でもよい。
Hereinafter, the best mode for carrying out the present invention will be described in detail with reference to the drawings.
FIG. 1 is a schematic view showing an example of an apparatus for producing silicon nanoparticles coated with a zinc selenide film of the present invention. A manufacturing method will be described using this apparatus as an example. In the figure, the heating device 1 has a resistance heating furnace 3 around a reaction tube 2. A crucible 5 containing a mixture 4 of silicon monoxide powder and zinc selenide powder is disposed in the reaction tube 2. The crucible 5 is heated in the resistance heating furnace 3. An arrow 6 indicates an inert gas supplied to the reaction tube 2.
Here, although the horizontal heating furnace by the resistance heating method is used for the heating apparatus 1, in this case, the heating furnace is not limited to the horizontal type and may be a vertical type. The heating device is not limited to resistance heating, and may be a heating device that can heat the crucible 5 by lamp heating or high-frequency induction heating.
図１の装置を用いて、セレン化亜鉛で被覆された珪素ナノ粒子を製造する方法を説明する。
セレン化亜鉛粉末と一酸化ケイ素粉末の混合物４を坩堝５に入れて、反応管２内に配置し、窒素ガスなどの不活性ガス６を流す。
そして、坩堝５を抵抗加熱炉３で加熱して昇温する。坩堝５中の混合物４が所定の温度に達したら、この状態を一定時間保持する。この温度で、坩堝５中に入れた混合物４から珪素の蒸気が生じ、この蒸気が不活性ガス６の流れに乗って反応管２で温度の低い領域に流れ、反応管２の内壁に凝縮し、珪素ナノ粒子を生成する。
この後、坩堝５を抵抗加熱炉３で珪素ナノ粒子生成時より高い温度状態となるようにし、坩堝５が所定の温度に達したら、この状態を一定時間保持する。この温度で、坩堝５中のセレン化亜鉛粉末を蒸気にして珪素ナノ粒子上にセレン化亜鉛膜を堆積させる。以上の操作により、セレン化亜鉛で被覆された珪素ナノ粒子を製造することができる。
A method for producing silicon nanoparticles coated with zinc selenide using the apparatus of FIG. 1 will be described.
A mixture 4 of zinc selenide powder and silicon monoxide powder is placed in a crucible 5 and placed in the reaction tube 2, and an inert gas 6 such as nitrogen gas is allowed to flow.
And the crucible 5 is heated with the resistance heating furnace 3, and it heats up. When the mixture 4 in the crucible 5 reaches a predetermined temperature, this state is maintained for a certain time. At this temperature, silicon vapor is generated from the mixture 4 placed in the crucible 5, and this vapor rides on the flow of the inert gas 6 and flows to a low temperature region in the reaction tube 2 and is condensed on the inner wall of the reaction tube 2. To produce silicon nanoparticles.
Thereafter, the temperature of the crucible 5 is set to a higher temperature than when the silicon nanoparticles are generated in the resistance heating furnace 3, and when the temperature of the crucible 5 reaches a predetermined temperature, this state is maintained for a predetermined time. At this temperature, the zinc selenide powder in the crucible 5 is vaporized to deposit a zinc selenide film on the silicon nanoparticles. By the above operation, silicon nanoparticles coated with zinc selenide can be produced.
ここで、坩堝５に入れる一酸化ケイ素粉末とセレン化亜鉛粉末の質量比は、１：１〜１：２の範囲が好ましい。この範囲よりもセレン化亜鉛粉末の量が多いと、珪素ナノ粒子の中にセレン化亜鉛が不純物として混入するので好ましくない。逆に、この範囲よりもセレン化亜鉛粉末の量が少ないと収量が低下するので好ましくない。 Here, the mass ratio of the silicon monoxide powder and the zinc selenide powder placed in the crucible 5 is preferably in the range of 1: 1 to 1: 2. When the amount of zinc selenide powder is larger than this range, zinc selenide is mixed as an impurity in the silicon nanoparticles, which is not preferable. Conversely, if the amount of zinc selenide powder is less than this range, the yield is unfavorable.
また、珪素ナノ粒子を生成する際の温度は、９００℃〜１１００℃の範囲が好ましい。
これ以上の温度では珪素ナノワイヤーが生成されるから好ましくない。逆に、９００℃未満では、珪素ナノ粒子が生成しないから好ましくない。
このときの加熱時間は、０．８時間〜１．５時間の範囲が好ましい。これ以上の時間では珪素ナノ粒子の表面が酸化物で覆われるから好ましくない。逆に、０．８時間未満では珪素ナノ粒子の収量が低下するから好ましくない。
Moreover, the temperature at the time of producing | generating a silicon nanoparticle has the preferable range of 900 to 1100 degreeC.
A temperature higher than this is not preferable because silicon nanowires are generated. Conversely, if it is less than 900 ° C., silicon nanoparticles are not generated, which is not preferable.
The heating time at this time is preferably in the range of 0.8 hours to 1.5 hours. A time longer than this is not preferable because the surface of the silicon nanoparticles is covered with an oxide. On the other hand, when the time is less than 0.8 hours, the yield of silicon nanoparticles decreases, which is not preferable.
また、珪素ナノ粒子にセレン化亜鉛膜を堆積させる際の温度は、１０５０℃〜１１５０℃の範囲が好ましい。１１５０℃でセレン化亜鉛の蒸気が十分発生するので、これ以上の温度にする必要がない。逆に、１０５０℃未満では、セレン化亜鉛膜が得られないから好ましくない。
このときの加熱時間は、１時間〜２時間の範囲が好ましい。これ以上の時間では珪素ナノ粒子の中に若干のセレン化亜鉛が不純物として混入するから好ましくない。逆に、１時間未満では収量が低下するから好ましくない。
Moreover, the temperature at the time of depositing a zinc selenide film | membrane on a silicon nanoparticle has the preferable range of 1050 to 1150 degreeC. Since sufficient vapor of zinc selenide is generated at 1150 ° C., it is not necessary to set the temperature higher than this. Conversely, if it is less than 1050 ° C., a zinc selenide film cannot be obtained, which is not preferable.
The heating time at this time is preferably in the range of 1 hour to 2 hours. The time longer than this is not preferable because some zinc selenide is mixed as an impurity in the silicon nanoparticles. On the other hand, if it is less than 1 hour, the yield decreases, which is not preferable.
不活性ガスの流量は、０．８ｌｔｒ／分〜１．５ｌｔｒ／分の範囲が好ましい。１．５ｌｔｒ／分の流量でその目的を十分達成するので、これ以上の流量にする必要はない。逆に、０．８ｌｔｒ／分未満にすると収量が低下する。 The flow rate of the inert gas is preferably in the range of 0.8 ltr / min to 1.5 ltr / min. The flow rate of 1.5 ltr / min sufficiently achieves its purpose, so there is no need for a flow rate higher than this. On the other hand, when it is less than 0.8 ltr / min, the yield decreases.
このような操作を施すことにより、先ず、珪素ナノ粒子が内層（コア）として形成され、次に、珪素ナノ粒子の表面に外層（シェル）としてセレン化亜鉛膜が堆積する。すなわち、全体の直径が１２０ｎｍ〜２００ｎｍで、外層のセレン化亜鉛膜の厚さが約３０ｎｍの、セレン化亜鉛膜で被覆された珪素ナノ粒子を得ることができる。
このセレン化亜鉛膜で被覆された珪素ナノ粒子は、加熱装置１の反応管２の内壁に黄色の粉末として堆積する。
By performing such an operation, first, silicon nanoparticles are formed as an inner layer (core), and then a zinc selenide film is deposited as an outer layer (shell) on the surface of the silicon nanoparticles. That is, silicon nanoparticles covered with a zinc selenide film having an overall diameter of 120 nm to 200 nm and an outer zinc selenide film thickness of about 30 nm can be obtained.
The silicon nanoparticles coated with the zinc selenide film are deposited as a yellow powder on the inner wall of the reaction tube 2 of the heating apparatus 1.
次に、実施例に基づき詳細に説明する。
先ず、一酸化ケイ素粉末（シグマ・アルドリッチ社製、３２５メッシュ）１．０ｇとセレン化亜鉛粉末（シグマ・アルドリッチ社製、純度９９．９９％) １．５ｇとの混合物４を、グラファイト製の坩堝５に入れて、この坩堝５を加熱装置１の反応管２としての石英管内に配置し、不活性ガスとして窒素ガスを１ｌｔｒ／分の流量で流した。そして、１０℃／分の昇温速度で、混合物４を９５０℃に加熱した。この温度に到達したとき、混合物４を９５０℃で１時間保持した。その後、坩堝５の温度をさらに上げ、１１００℃で１．５時間加熱した。
その結果、反応管２としての石英管の内壁で７００℃〜８００℃に保たれていた部分に黄色の粉末が数ｍｇ堆積した。
Next, it demonstrates in detail based on an Example.
First, a mixture 4 of 1.0 g of silicon monoxide powder (manufactured by Sigma-Aldrich, 325 mesh) and 1.5 g of zinc selenide powder (manufactured by Sigma-Aldrich, purity 99.99%) was converted into a graphite crucible. 5, the crucible 5 was placed in a quartz tube as the reaction tube 2 of the heating apparatus 1, and nitrogen gas was flowed as an inert gas at a flow rate of 1 ltr / min. And the mixture 4 was heated to 950 degreeC with the temperature increase rate of 10 degreeC / min. When this temperature was reached, Mixture 4 was held at 950 ° C. for 1 hour. Thereafter, the temperature of the crucible 5 was further raised and heated at 1100 ° C. for 1.5 hours.
As a result, several mg of yellow powder was deposited on the inner wall of the quartz tube as the reaction tube 2 which was kept at 700 ° C. to 800 ° C.
図２は、実施例で合成した堆積物の透過型電子顕微鏡像を示す図である。図２から明らかなように、直径約１２０〜２００ｎｍの球状または楕円体状粒子が生成していることが分かる。また、各ナノ粒子には、明瞭な明暗が写っていることから、同心状の二重構造のナノ粒子であることが分かる。外層の厚さは約３０ｎｍであることが分かる。 FIG. 2 is a view showing a transmission electron microscope image of the deposit synthesized in the example. As can be seen from FIG. 2, spherical or ellipsoidal particles having a diameter of about 120 to 200 nm are generated. In addition, each nanoparticle has clear light and darkness, which indicates that the nanoparticle has a concentric double structure. It can be seen that the thickness of the outer layer is about 30 nm.
図３は、本発明の実施例で合成した堆積物の外層のエネルギー分散型Ｘ線分析（ＥＤＸ：Ｅｎｅｒｇｙ−Ｄｉｓｐｅｒｓｉｖｅ Ｘ−ｒａｙ Ａｎａｌｙｓｉｓ）による測定結果を示す図である。図の縦軸はＸ線強度（任意目盛り）を示し、横軸はＸ線のエネルギー（ｋｅＶ）を示している。
図３のＸ線スペクトルから、亜鉛（Ｚｎ）、セレン（Ｓｅ）の各シグナルが現れており、外層が化学量論組成のセレン化亜鉛からなることが分かる。
なお、図３のＸ線スペクトルには、銅（Ｃｕ）、炭素（Ｃ）、酸素（Ｏ）のシグナルが現れているが、これらのシグナルのうち、銅のシグナルは、観察用試料を作製する際に用
いた銅グリッドから発生し、炭素のシグナルは、銅グリッドにコートされているカーボン膜から発生したものである。酸素のシグナルは、測定用の試料が作製中に酸化され、発生したものである。
FIG. 3 is a diagram showing a measurement result by energy-dispersive X-ray analysis (EDX) of the outer layer of the deposit synthesized in the example of the present invention. In the figure, the vertical axis represents the X-ray intensity (arbitrary scale), and the horizontal axis represents the X-ray energy (keV).
From the X-ray spectrum of FIG. 3, it can be seen that signals of zinc (Zn) and selenium (Se) appear, and the outer layer is made of zinc selenide having a stoichiometric composition.
Note that copper (Cu), carbon (C), and oxygen (O) signals appear in the X-ray spectrum of FIG. 3. Of these signals, the copper signal produces an observation sample. The carbon signal generated from the copper grid used at the time was generated from the carbon film coated on the copper grid. The oxygen signal is generated when a measurement sample is oxidized during production.
図４は、本発明の実施例で合成した堆積物全体のエネルギー分散型Ｘ線分析による測定結果を示す図である。図の縦軸はＸ線強度（任意目盛り）を示し、横軸はＸ線のエネルギー（ｋｅＶ）を示している。図４のスペクトルから、図３で観測された亜鉛（Ｚｎ）とセレン（Ｓｅ）の各シグナルの他に、珪素（Ｓｉ）のシグナルが現れていることが分かる。よって、図３の測定結果とから、二重構造のナノ粒子の内側の層は珪素から成る組成であることが分かる。 FIG. 4 is a diagram showing a measurement result by energy dispersive X-ray analysis of the entire sediment synthesized in the example of the present invention. In the figure, the vertical axis represents the X-ray intensity (arbitrary scale), and the horizontal axis represents the X-ray energy (keV). From the spectrum of FIG. 4, it can be seen that in addition to the signals of zinc (Zn) and selenium (Se) observed in FIG. 3, a signal of silicon (Si) appears. Therefore, it can be seen from the measurement results of FIG. 3 that the inner layer of the double-structured nanoparticles has a composition composed of silicon.
上記結果から、内層として珪素ナノ粒子が形成され、珪素ナノ粒子上外層としてセレン化亜鉛膜が堆積していることが分かる。また、全体の直径が１２０ｎｍ〜２００ｎｍで、外層のセレン化亜鉛膜の厚さが約３０ｎｍの、セレン化亜鉛膜で被覆された珪素ナノ粒子を製造できることが分かる。 From the above results, it can be seen that silicon nanoparticles are formed as the inner layer, and a zinc selenide film is deposited as the upper and outer layers of the silicon nanoparticles. Moreover, it turns out that the silicon nanoparticle coat | covered with the zinc selenide film | membrane whose whole diameter is 120 nm-200 nm and whose thickness of the outer layer zinc selenide film | membrane is about 30 nm can be manufactured.
本発明によれば、セレン化亜鉛膜で被覆された珪素ナノ粒子を、加熱温度を調整することで容易に製造することができる。また、セレン化亜鉛膜を被覆された珪素ナノ粒子は、ナノ電子デバイスやナノ光電子デバイスなど各種デバイスへ利用可能である。 According to the present invention, silicon nanoparticles coated with a zinc selenide film can be easily produced by adjusting the heating temperature. Silicon nanoparticles coated with a zinc selenide film can be used for various devices such as nanoelectronic devices and nanophotoelectronic devices.
１ 加熱装置
２ 反応管
３ 抵抗加熱炉
４ 混合物
５ 坩堝
６ 不活性ガス
DESCRIPTION OF SYMBOLS 1 Heating device 2 Reaction tube 3 Resistance heating furnace 4 Mixture 5 Crucible 6 Inert gas
Claims (8)
上記坩堝を９００℃〜１１００℃の温度範囲で加熱することにより、珪素ナノ粒子を生成し、
次に、上記坩堝を１０５０℃〜１１５０℃の温度範囲で加熱することにより、上記珪素ナノ粒子をセレン化亜鉛膜で被覆することを特徴とする、セレン化亜鉛膜で被覆された珪素ナノ粒子の製造方法。 In a heating furnace, a crucible containing silicon monoxide powder and zinc selenide powder is placed, and while flowing an inert gas,
By heating the crucible in a temperature range of 900 ° C. to 1100 ° C., silicon nanoparticles are generated,
Next, by heating the crucible in a temperature range of 1050 ° C. to 1150 ° C., the silicon nanoparticles are coated with the zinc selenide film, and the silicon nanoparticles coated with the zinc selenide film Production method.
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