JP4604248B2 - Indium germanate submicron tube and manufacturing method thereof - Google Patents
Indium germanate submicron tube and manufacturing method thereof Download PDFInfo
- Publication number
- JP4604248B2 JP4604248B2 JP2006047763A JP2006047763A JP4604248B2 JP 4604248 B2 JP4604248 B2 JP 4604248B2 JP 2006047763 A JP2006047763 A JP 2006047763A JP 2006047763 A JP2006047763 A JP 2006047763A JP 4604248 B2 JP4604248 B2 JP 4604248B2
- Authority
- JP
- Japan
- Prior art keywords
- indium
- germanate
- submicron
- oxide powder
- submicron tube
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Catalysts (AREA)
Description
本発明は、インジウム、ゲルマニウム及び酸素からなる三元素系のサブミクロンの直径を有する、ゲルマニウム酸インジウムサブミクロンチューブとその製造方法に関する。 The present invention relates to an indium germanate submicron tube having a three-element submicron diameter composed of indium, germanium, and oxygen, and a method of manufacturing the same.
ゲルマニウム酸塩は、重油や薬品類中の大きな分子の分離（例えば、非特許文献１参照）や湿度センサー（例えば、非特許文献２参照）として注目されている。また、ゲルマニウム酸インジウムは、特殊な層状構造を有する化合物であることも既に知られている（例えば、非特許文献３参照）。 Germanate is attracting attention as a separation of large molecules in heavy oil and chemicals (for example, see Non-Patent Document 1) and a humidity sensor (for example, see Non-Patent Document 2). Further, it is already known that indium germanate is a compound having a special layered structure (see, for example, Non-Patent Document 3).
しかしながら、単斜晶系の単結晶構造から成る、ゲルマニウム酸インジウムのサブミクロンチューブは現在まで実現されておらず、そのため、触媒、大分子の分離、湿度センサーなどへの優れた応用が制限されていた。また、上記ゲルマニウム酸インジウムから成るサブミクロンチューブを効率良く製造する方法も未だ実現されていない。 However, indium germanate submicron tubes composed of a monoclinic single crystal structure have not been realized so far, which limits their excellent application to catalysts, separation of large molecules, humidity sensors, etc. It was. Moreover, a method for efficiently producing a submicron tube made of indium germanate has not yet been realized.
本発明は、単斜晶系の単結晶構造から成る、ゲルマニウム酸インジウムサブミクロンチューブ及びその製造方法を提供することを目的とする。 An object of the present invention is to provide an indium germanate submicron tube having a monoclinic single crystal structure and a method for producing the same.
上記目的を達成するため、本発明のゲルマニウム酸インジウムサブミクロンチューブは、単斜晶系の単結晶構造から成ることを特徴とする。
上記構成において、好ましくは、ゲルマニウム酸インジウムサブミクロンチューブの長さは数百μｍであり、その外径はおおよそ６００ｎｍである。
上記構成によれば、チューブの中空部の断面形状が六角形又は円形で、単結晶から成るゲルマニウム酸インジウムサブミクロンチューブを提供することができる。
In order to achieve the above object, the indium germanate submicron tube of the present invention is characterized by comprising a monoclinic single crystal structure.
In the above configuration, the length of the indium germanate submicron tube is preferably several hundred μm and the outer diameter is approximately 600 nm.
According to the said structure, the cross-sectional shape of the hollow part of a tube is a hexagon or a circle, and the indium germanate submicron tube which consists of a single crystal can be provided.
本発明のゲルマニウム酸インジウムサブミクロンチューブの製造方法は、酸化インジウム粉末、酸化ゲルマニウム粉末及び活性炭粉末の混合物を、不活性ガス気流中で、所定温度において所定時間加熱し、ゲルマニウム酸インジウムサブミクロンチューブを合成することを特徴とする。
上記構成において、好ましくは、酸化インジウム粉末、酸化ゲルマニウム粉末及び活性炭粉末のモル比は、０．５〜１．５：１〜３：２〜６の範囲である。加熱温度は、好ましくは、８００〜１２００℃の範囲であり、加熱時間は０．５〜３時間の範囲とすることが好ましい。
不活性ガスは、好ましくはアルゴンガスであり、この不活性ガスの流量は、好ましくは５０〜１０００ｃｍ3 ／分の範囲である。
上記構成によれば、長さが数百μｍで、外径がおおよそ６００ｎｍの寸法を有する単斜晶系の、新規な単結晶のゲルマニウム酸インジウムサブミクロンチューブを製造することができる。
According to the method for producing an indium germanate submicron tube of the present invention, a mixture of indium oxide powder, germanium oxide powder and activated carbon powder is heated in an inert gas stream at a predetermined temperature for a predetermined time. It is characterized by combining.
In the above configuration, the molar ratio of the indium oxide powder, the germanium oxide powder, and the activated carbon powder is preferably in the range of 0.5 to 1.5: 1 to 3: 2 to 6. The heating temperature is preferably in the range of 800 to 1200 ° C., and the heating time is preferably in the range of 0.5 to 3 hours.
The inert gas is preferably argon gas, and the flow rate of the inert gas is preferably in the range of 50 to 1000 cm 3 / min.
According to the above configuration, a novel monoclinic indium germanate submicron tube having a length of several hundred μm and an outer diameter of approximately 600 nm can be manufactured.
本発明により、長さが数百μｍで、外径がおおよそ６００ｎｍの寸法を有する単結晶のゲルマニウム酸インジウムサブミクロンチューブ及びその製造方法を提供することができる。 According to the present invention, it is possible to provide a single crystal indium germanate submicron tube having a length of several hundreds μm and an outer diameter of approximately 600 nm and a method for manufacturing the same.
以下、本発明を実施するための好ましい実施の形態を詳細に説明する。
本発明のゲルマニウム酸インジウムサブミクロンチューブは、その長さが数百μｍで、外径がおおよそ６００ｎｍの寸法を有する、新規な単斜晶系の単結晶構造のゲルマニウム酸インジウムから成り、サブミクロンチューブの中空部の断面形状は、六角形あるいは円形をなしている。
Hereinafter, preferred embodiments for carrying out the present invention will be described in detail.
The indium germanate submicron tube of the present invention is composed of a novel monoclinic single crystal structure indium germanate having a length of several hundreds μm and an outer diameter of approximately 600 nm. The cross-sectional shape of the hollow portion is hexagonal or circular.
このゲルマニウム酸インジウムサブミクロンチューブは、次のようにして製造することができる。
酸化インジウム（Ｉｎ2 Ｏ3 ）粉末、酸化ゲルマニウム（ＧｅＯ2 ）粉末及び活性炭粉末の混合物を反応容器に入れ、この容器を加熱炉に配置する。
次に、加熱炉の中に不活性ガスを流し、この不活性ガス気流中において、上記混合物を、所定温度で所定時間加熱することで、ゲルマニウム酸インジウム（Ｉｎ2 Ｇｅ2 Ｏ7 ）サブミクロンチューブを合成することができる。
This indium germanate submicron tube can be manufactured as follows.
A mixture of indium oxide (In 2 O 3 ) powder, germanium oxide (GeO 2 ) powder and activated carbon powder is placed in a reaction vessel, and this vessel is placed in a heating furnace.
Next, an inert gas is allowed to flow through the heating furnace, and the mixture is heated at a predetermined temperature for a predetermined time in the inert gas stream, thereby allowing an indium germanate (In 2 Ge 2 O 7 ) submicron tube to be heated. Can be synthesized.
上記の原料粉末のモル比は、酸化インジウム粉末：酸化ゲルマニウム粉末：活性炭粉末＝０．５〜１．５：１〜３：２〜６の範囲が好ましい。酸化インジウム粉末の量は、上記範囲の上限値で十分であるので、これ以上の量を使用する必要はない。逆に、酸化インジウム粉末の量が上記範囲の下限値未満の場合は、ゲルマニウム酸インジウムサブミクロンチューブの収量が低下するので好ましくない。 The molar ratio of the raw material powder is preferably in the range of indium oxide powder: germanium oxide powder: activated carbon powder = 0.5-1.5: 1-3: 2-6. Since the upper limit of the above range is sufficient for the amount of the indium oxide powder, it is not necessary to use an amount larger than this. Conversely, when the amount of the indium oxide powder is less than the lower limit of the above range, the yield of the indium germanate submicron tube is lowered, which is not preferable.
酸化ゲルマニウム粉末の量は、上記範囲の上限値で十分であるので、これ以上の量を使用する必要はない。逆に、酸化ゲルマニウム粉末の量が上記範囲の下限値未満の場合は、収量が低下するので好ましくない。 Since the upper limit of the above range is sufficient for the amount of germanium oxide powder, it is not necessary to use an amount larger than this. Conversely, if the amount of germanium oxide powder is less than the lower limit of the above range, the yield is unfavorable.
活性炭粉末の量が上記範囲の上限値よりも多い場合は、金属インジウムや金属ゲルマニウムが生成するので好ましくない。逆に、活性炭粉末の量が上記範囲の下限値よりも少ない場合は、収量が低下するので好ましくない。 When the amount of the activated carbon powder is larger than the upper limit of the above range, metal indium or metal germanium is generated, which is not preferable. Conversely, when the amount of the activated carbon powder is less than the lower limit of the above range, the yield decreases, which is not preferable.
上記加熱温度は、８００〜１２００℃の範囲が好ましい。この加熱温度が１２００℃を超えると収量が低下するので、好ましくない。逆に、加熱温度が８００℃未満では、中空部の存在しないウィスカーが生成するので好ましくない。 The heating temperature is preferably in the range of 800 to 1200 ° C. If the heating temperature exceeds 1200 ° C., the yield decreases, which is not preferable. On the other hand, if the heating temperature is less than 800 ° C., whiskers having no hollow portion are generated, which is not preferable.
上記加熱時間は０．５〜３時間の範囲が好ましい。この加熱時間は３時間で十分に反応が進行するので、これ以上の時間をかける必要はない。逆に、加熱時間が０．５時間未満では反応が完結しないため、収量が低下するので好ましくない。 The heating time is preferably in the range of 0.5 to 3 hours. Since the reaction proceeds sufficiently in 3 hours, it is not necessary to spend more time. On the other hand, if the heating time is less than 0.5 hours, the reaction is not completed, and therefore the yield is unfavorable.
上記不活性ガスとしては、アルゴンガスを使用することができ、その流量は、５０〜１０００ｃｍ3 ／分の範囲が好ましい。不活性ガスの流量が１０００ｃｍ3 ／分よりも供給が多いと、生成物が飛散し収量が低下するので好ましくない。逆に、不活性ガスの流量が５０ｃｍ3 ／分よりも少ないと、ウィスカーが生成するので好ましくない。 Argon gas can be used as the inert gas, and the flow rate is preferably in the range of 50 to 1000 cm 3 / min. When the flow rate of the inert gas is more than 1000 cm 3 / min, the product is scattered and the yield is lowered, which is not preferable. Conversely, if the flow rate of the inert gas is less than 50 cm 3 / min, whiskers are generated, which is not preferable.
上記のような操作を施すことにより、加熱炉の内壁に白色の粉末が堆積する。この白色の粉末を分析することにより、ゲルマニウム酸インジウムサブミクロンチューブであることが確認できる。 By performing the operation as described above, white powder is deposited on the inner wall of the heating furnace. By analyzing this white powder, it can be confirmed that it is an indium germanate submicron tube.
次に、実施例を示してさらに具体的に本発明を説明する。
最初に、酸化インジウム粉末（高純度化学研究所製、純度９９．９９％）１．１１ｇと、酸化ゲルマニウム粉末（高純度化学研究所製、純度９９．９９５％）０．８４ｇと、活性炭粉末（アルドリッチ社製、純度９９．９５％）０．２ｇと、の混合物を石英坩堝に入れた。この石英坩堝を横型抵抗加熱炉中に配置した石英製の反応管の中央部に設置した。次に、反応管に流量２００ｃｍ3 ／分のアルゴンガスを供給しながら、２０Ｋ／分の昇温速度で１０００℃まで温度を上げ、この温度に２時間保った。
最後に、加熱炉の温度を自然冷却により室温まで下げた。加熱中に、おおよそ６００℃を示していた反応管の内壁に白色の粉末０．１ｇが堆積した。
Next, the present invention will be described more specifically with reference to examples.
First, 1.11 g of indium oxide powder (manufactured by High Purity Chemical Laboratory, purity 99.99%), 0.84 g of germanium oxide powder (manufactured by High Purity Chemical Laboratory, purity 99.995%), activated carbon powder ( A mixture of Aldrich (purity 99.95%) 0.2 g was put in a quartz crucible. This quartz crucible was placed in the center of a quartz reaction tube placed in a horizontal resistance heating furnace. Next, while supplying argon gas to the reaction tube at a flow rate of 200 cm 3 / min, the temperature was increased to 1000 ° C. at a temperature increase rate of 20 K / min, and this temperature was maintained for 2 hours.
Finally, the temperature of the heating furnace was lowered to room temperature by natural cooling. During the heating, 0.1 g of white powder was deposited on the inner wall of the reaction tube, which had been approximately 600 ° C.
次に、実施例で合成した白色の粉末について、さらに詳しく説明する。
図１は上記実施例で合成した白色粉末のＸ線回折像を示す図である。図１において、縦軸はＸ線回折強度（任意目盛）を示し、横軸は角度（°）、即ち、Ｘ線の原子面への入射角θの２倍に相当する角度を示している。図１から明らかなように、実施例で合成した白色粉末は、単斜晶系のゲルマニウム酸インジウムであることが分かった。そして、Ｉｎ2 Ｏ3 、ＧｅＯ2 、Ｉｎ、Ｇｅのような不純物のピークは観測されなかった。
Next, the white powder synthesized in the examples will be described in more detail.
FIG. 1 is an X-ray diffraction image of the white powder synthesized in the above example. In FIG. 1, the vertical axis represents the X-ray diffraction intensity (arbitrary scale), and the horizontal axis represents the angle (°), that is, an angle corresponding to twice the incident angle θ of the X-ray to the atomic plane. As is clear from FIG. 1, the white powder synthesized in the example was found to be monoclinic indium germanate. No impurity peaks such as In 2 O 3 , GeO 2 , In and Ge were observed.
図２は、実施例で合成した白色粉末の一部の走査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、実施例で得た白色粉末は、細長い繊維状の形状をしており、その長さは数百μｍに達している。 FIG. 2 is a diagram showing a scanning electron microscope image of a part of the white powder synthesized in the example. As is apparent from FIG. 2, the white powder obtained in the example has an elongated fibrous shape, and its length reaches several hundred μm.
図３は上記実施例で合成した白色粉末の一部の高倍率走査型電子顕微鏡像を示す図である。図３から明らかなように、実施例で合成したゲルマニウム酸インジウムは、先端部が開口したチューブ状構造であることが分かった。その外径はおおよそ６００ｎｍであり、１μｍ以下のサブミクロンの寸法を有するチューブである。このチューブ壁の厚さはおおよそ２００ｎｍであり、内径はおおよそ２００ｎｍであることが確認できた。 FIG. 3 is a diagram showing a high-magnification scanning electron microscope image of a part of the white powder synthesized in the above example. As apparent from FIG. 3, it was found that the indium germanate synthesized in the example has a tube-like structure with an open end. Its outer diameter is approximately 600 nm and is a tube having a submicron dimension of 1 μm or less. It was confirmed that the thickness of the tube wall was approximately 200 nm and the inner diameter was approximately 200 nm.
図４は、ゲルマニウム酸インジウムサブミクロンチューブの先端部分の高倍率走査型電子顕微鏡像を示す図である。図４から明らかなように、チューブ穴の断面形状は六角形あるいは円形であることが判明した。 FIG. 4 is a diagram showing a high-magnification scanning electron microscope image of the tip portion of the indium germanate submicron tube. As is apparent from FIG. 4, the cross-sectional shape of the tube hole was found to be hexagonal or circular.
本発明は、上記実施例に限定されることなく、特許請求の範囲に記載した発明の範囲内で種々の変形が可能であり、ゲルマニウム酸インジウムサブミクロンチューブの寸法については、所望の値が得られるように合成条件を適宜選択すればよいことは勿論である。 The present invention is not limited to the above-described embodiments, and various modifications can be made within the scope of the invention described in the claims, and a desired value can be obtained for the dimensions of the indium germanate submicron tube. Needless to say, the synthesis conditions may be selected as appropriate.
本発明により、ゲルマニウム酸インジウムサブミクロンチューブの製造が可能となったので、触媒、大分子の分離、湿度センサーなどへの応用が期待される。 Since the present invention makes it possible to produce indium germanate submicron tubes, it is expected to be applied to catalysts, separation of large molecules, humidity sensors, and the like.
Claims (8)
Characterized in that said supplying an inert gas at a range of flow rates 50～1000Cm 3 / min, the production method of the germanium acid indium submicron tube according to claim 3 or 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2006047763A JP4604248B2 (en) | 2006-02-24 | 2006-02-24 | Indium germanate submicron tube and manufacturing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2006047763A JP4604248B2 (en) | 2006-02-24 | 2006-02-24 | Indium germanate submicron tube and manufacturing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2007223851A JP2007223851A (en) | 2007-09-06 |
| JP4604248B2 true JP4604248B2 (en) | 2011-01-05 |
Family
ID=38546003
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2006047763A Expired - Fee Related JP4604248B2 (en) | 2006-02-24 | 2006-02-24 | Indium germanate submicron tube and manufacturing method thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP4604248B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102225782B (en) * | 2011-04-14 | 2013-03-20 | 南京大学 | A method for preparing ultrafine In2Ge2O7(En) hybrid nanowires and nanowires prepared by the method |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3873124B2 (en) * | 2002-12-10 | 2007-01-24 | 独立行政法人物質・材料研究機構 | Single crystal indium oxide nanotubes containing metal indium and method for producing the same |
| JP4336249B2 (en) * | 2004-05-27 | 2009-09-30 | ソタジャパン有限会社 | Semiconductor fine particle manufacturing method, manufacturing apparatus, and jewelry, fiber, fabric, clothing using semiconductor fine particles |
-
2006
- 2006-02-24 JP JP2006047763A patent/JP4604248B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JP2007223851A (en) | 2007-09-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Dai et al. | Synthesis and growth mechanism of SiC nanofibres on carbon fabrics | |
| JP4534016B2 (en) | Method for producing high purity boron nitride nanotubes | |
| JP2008266101A (en) | Boron nitride nanotube and method for producing the same | |
| JP4604248B2 (en) | Indium germanate submicron tube and manufacturing method thereof | |
| JP3985044B2 (en) | Single crystal silicon nanotube and method for producing the same | |
| JP5448067B2 (en) | Method for producing boron nitride nanotubes | |
| JP3571287B2 (en) | Method for producing silicon oxide nanowires | |
| CN113979427B (en) | Method for preparing single-walled carbon nanotube by using rhenium as catalyst | |
| CN100384725C (en) | Method for preparing silicon carbide nano line | |
| Peng et al. | Growth and mechanism of network‐like branched Si3N4 nanostructures | |
| JP5382673B2 (en) | Cerium oxide nanotube and method for producing the same | |
| Du et al. | Effects of growth parameters on the yield and morphology of Si3N4 microcoils prepared by chemical vapor deposition | |
| Zhong et al. | Preparation and ultraviolet− visible luminescence property of novel BN whiskers with a cap-stacked structure | |
| Wang et al. | Synthesis and carbothermal nitridation mechanism of ultra-long single crystal α-Si3N4 nanobelts | |
| Wang et al. | Large-scale synthesis of SrCrO4 nanowires and PbCrO4 nanorods by a solution-phase method at room temperature | |
| TWI555720B (en) | Method of manufacturing nano ceramic material | |
| JP4576607B2 (en) | Single crystal zinc sulfide nanotube and method for producing the same | |
| Chu et al. | Screw dislocation assisted spontaneous growth of single-crystalline α-Al2O3 microrods | |
| Kim et al. | Facile fabrication of silicon and aluminum oxide nanotubes using antimony telluride nanowires as templates | |
| JP2006298684A (en) | Carbon-based one-dimensional material and synthesis method thereof, catalyst for synthesizing carbon-based one-dimensional material, synthesis method thereof, electronic device, and production method thereof | |
| JP3834661B2 (en) | Method for producing silicon carbide-silicon dioxide-carbon coaxial nanocable and nanochain in which silicon carbide nanorods and carbon nanotubes are alternately joined at the tips | |
| JP3918059B2 (en) | Single crystal magnesium oxide nanotubes containing gallium, method for producing the same, and temperature sensing element using the same | |
| Park et al. | Controlling the size of nanograins in TiO2 nanofibers | |
| JP4452813B2 (en) | Method for producing hexagonal zinc sulfide nanotubes | |
| JP2005306663A (en) | Silica nanotube production method and nano-sized micro thermometer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20090219 |
|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20100909 |
|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20100914 |
|
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20100915 |
|
| R150 | Certificate of patent or registration of utility model |
Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20131015 Year of fee payment: 3 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20131015 Year of fee payment: 3 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| S533 | Written request for registration of change of name |
Free format text: JAPANESE INTERMEDIATE CODE: R313533 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| LAPS | Cancellation because of no payment of annual fees |