JP2827586B2 - Method for producing tin dioxide whiskers - Google Patents
Method for producing tin dioxide whiskersInfo
- Publication number
- JP2827586B2 JP2827586B2 JP3164292A JP16429291A JP2827586B2 JP 2827586 B2 JP2827586 B2 JP 2827586B2 JP 3164292 A JP3164292 A JP 3164292A JP 16429291 A JP16429291 A JP 16429291A JP 2827586 B2 JP2827586 B2 JP 2827586B2
- Authority
- JP
- Japan
- Prior art keywords
- tin
- gas
- tin dioxide
- furnace
- whiskers
- 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 - Lifetime
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、高純度二酸化錫（Ｓｎ
Ｏ2）ウィスカーの製造方法に関する。The present invention relates to high purity tin dioxide (Sn).
O 2 ) whiskers.
【０００２】[0002]
【従来の技術】高純度二酸化錫単結晶の育成法として、
反応管の前半部に金属錫を配置して９００〜１２００℃
の温度に保持し、これに水蒸気と不活性ガスを同時に連
続送入して気体状一酸化錫を生成させて反応管の後半部
に送り、後半部に酸素を送入して二酸化錫単結晶を得る
方法、または原料に金属錫粉末と二酸化錫粉末を用い、
管状炉において一方より酸素，窒素ガスを同時に連続送
入し、原料を入れたるつぼ内もしくはその付近において
生成させる方法が報告されている。2. Description of the Related Art As a method for growing a high purity tin dioxide single crystal,
900-1200 ° C by placing metal tin in the first half of the reaction tube
, And steam and inert gas are continuously fed into it at the same time to generate gaseous tin monoxide, which is sent to the latter half of the reaction tube, and oxygen is sent into the latter half to produce tin dioxide single crystal. Or using metal tin powder and tin dioxide powder as raw materials,
There has been reported a method in which oxygen and nitrogen gas are continuously and simultaneously supplied from one side in a tubular furnace, and are generated in or near a crucible in which raw materials are stored.
【０００３】また、酸化錫繊維の製造法として二酸化錫
を原料として、銅を溶媒とするフラックス法による方法
などがある。[0003] As a method for producing tin oxide fibers, there is a flux method using tin dioxide as a raw material and copper as a solvent.
【０００４】[0004]
【発明が解決しようとする課題】しかし、上記のような
方法では金属錫からの蒸発速度が遅く極めて少ない錫蒸
気しか得られないため、少量で、かつ小さな寸法のウィ
スカーしか生成させることができなかった。この対応策
として、原料に二酸化錫を用いることが行われていた。
この方法によれば二酸化錫が熱分解して一酸化錫が得ら
れるため、金属錫を用いた場合より二酸化錫ウィスカー
の成長が速められる。However, in the above-mentioned method, the evaporation rate from metallic tin is so slow that only a very small amount of tin vapor can be obtained, so that only a small amount of small whiskers can be produced. Was. As a countermeasure, tin dioxide has been used as a raw material.
According to this method, tin dioxide is thermally decomposed to obtain tin monoxide, so that the growth of tin dioxide whiskers is faster than when metal tin is used.
【０００５】また、反応炉の構造として反応管を用い、
原料供給部とウィスカー生成部が分離されていること
は、製造技術的に見れば合理的であるが、キャリアーガ
スを用いるため錫蒸気濃度が薄められ、結晶が成長する
ウィスカー生成部において、大寸法の結晶を成長させる
のに長時間を要するという問題がある。Further, a reaction tube is used as a structure of the reaction furnace,
Although it is reasonable from the viewpoint of manufacturing technology that the raw material supply unit and the whisker generation unit are separated from each other, the whisker generation unit where the tin vapor concentration is reduced due to the use of the carrier gas and the crystal grows is large. There is a problem that it takes a long time to grow the crystal.
【０００６】原料に二酸化錫粉末と金属錫粉末を用い、
管状炉において一端から酸素と窒素ガスを連続送入する
方法は、原料付近での成長速度が速い二酸化錫ウィスカ
ーの生成方法であるとされているが、酸化反応による結
晶成長が持続せず、高い製造能率を期待できない。Using tin dioxide powder and metal tin powder as raw materials,
The method of continuously feeding oxygen and nitrogen gas from one end in a tubular furnace is said to be a method of producing tin dioxide whiskers with a high growth rate near the raw material, but the crystal growth by the oxidation reaction is not sustained and high. Production efficiency cannot be expected.
【０００７】さらに、フラックス法においては、生成物
と溶媒との分離工程が必要で工程が複雑となり、また生
成されたウィスカーに溶媒金属である銅の混入があり純
度の問題が残る。Further, in the flux method, a step of separating a product and a solvent is required, which complicates the process. In addition, copper, which is a solvent metal, is mixed in the generated whiskers, and the problem of purity remains.
【０００８】本発明は上記問題を解決しようとするもの
で、高純度で大型、かつ形状が均一な二酸化錫ウィスカ
ーを高能率で製造する方法を提供することを目的とす
る。An object of the present invention is to solve the above-mentioned problem, and an object of the present invention is to provide a method for efficiently producing tin dioxide whiskers of high purity, large size and uniform shape.
【０００９】[0009]
【課題を解決するための手段】上記の目的を達成するた
めに、本発明の二酸化錫ウィスカーの製造方法は、酸素
を含むガスが自然流入または強制送給によって系外から
供給される反応炉において、反応炉内に金属錫または金
属錫と錫酸化物の混合物である原料を蒸発させるための
るつぼを配設し、そのるつぼに原料を供給しておいて反
応炉内を錫蒸気が発生する１０００℃〜１３５０℃の温
度範囲に保ちながら、錫蒸気が存在する雰囲気中に不活
性ガスを原料の近傍に断続的に送入するようにしたもの
である。In order to achieve the above object, the present invention provides a method for producing a tin dioxide whisker in a reactor in which a gas containing oxygen is supplied from outside the system by natural inflow or forced supply. A crucible for evaporating a raw material which is metal tin or a mixture of metal tin and tin oxide is provided in the reaction furnace, and the raw material is supplied to the crucible to generate tin vapor in the reaction furnace. The inert gas is intermittently fed into the vicinity of the raw material in the atmosphere where the tin vapor is present, while maintaining the temperature in the range of 1 ° C to 1350 ° C.
【００１０】[0010]
【作用】上記した手段によれば、断続的に送入される不
活性ガスは反応炉内の酸素濃度を制御する働きをする。
反応炉内の酸素濃度が高過ぎるとウィスカーではなく粉
末状酸化錫を生成し、さらに高酸素濃度状態が続くと溶
融金属錫表面に酸化錫膜を形成し、酸化錫膜が錫蒸気発
生を妨げるようになる。本発明のＳｎＯ2ウィスカーの
製造方法によれば、炉内の酸素濃度が、交互に流入また
は供給される酸素を含むガスと不活性ガスの量により制
御されるため、最適の酸素濃度で二酸化錫ウィスカーの
生成が可能となる。According to the above-mentioned means, the inert gas fed intermittently serves to control the oxygen concentration in the reactor.
If the oxygen concentration in the reactor is too high, tin oxide is generated instead of whiskers, and if the oxygen concentration continues, a tin oxide film is formed on the surface of molten metal tin, and the tin oxide film prevents tin vapor generation Become like According to the method for producing a SnO 2 whisker of the present invention, the oxygen concentration in the furnace is controlled by the amounts of the oxygen-containing gas and the inert gas alternately supplied or supplied. Whiskers can be generated.
【００１１】一方、反応炉内の錫蒸気濃度が高くなると
酸化錫は多く多結晶体となる。また従来例において、金
属錫を蒸発源とする蒸発では、錫の溶融物表面に錫特有
の錫蒸気濃度の高い拡散層が形成されるため、上部空間
への錫蒸気の蒸発が妨げられる。この時不活性ガスを金
属錫の近傍に送入すると、高濃度錫蒸気を散乱し錫蒸気
濃度を減少させ、錫蒸気の拡散層が散乱することにより
錫の蒸発が促される。On the other hand, when the tin vapor concentration in the reaction furnace increases, the amount of tin oxide increases and becomes polycrystalline. Further, in the conventional example, in the evaporation using metal tin as an evaporation source, a diffusion layer having a high tin vapor concentration specific to tin is formed on the surface of the tin melt, so that evaporation of tin vapor into the upper space is prevented. Gold this time inert gas
When it is sent to the vicinity of the tin, the high-concentration tin vapor is scattered to reduce the tin vapor concentration, and the tin vapor diffusion layer is scattered to promote the evaporation of tin.
【００１２】高濃度錫蒸気の拡散層が発生したとき、酸
素を含むガスを流入させると、拡散層は十分に散乱する
ことなく、酸化反応が先行して膜状または粉末状酸化錫
を形成し、目的とする二酸化錫ウィスカーは成長しな
い。When a gas containing oxygen is caused to flow when a diffusion layer of high-concentration tin vapor is generated, the diffusion layer is not sufficiently scattered, and the oxidation reaction precedes and forms a film-like or powdery tin oxide. However, the intended tin dioxide whiskers do not grow.
【００１３】このように、酸素を含むガスと不活性ガス
を交互に反応炉に流入または供給することにより、二酸
化錫ウィスカーは二次的な結晶成長が抑制され、その断
面が正方形のものと長方形のものの混合物として高収率
で生成させることができる。As described above, by alternately flowing or supplying the gas containing oxygen and the inert gas into the reactor, the secondary crystal growth of the tin dioxide whiskers is suppressed, and the cross sections of the tin whiskers are square and rectangular. Can be produced in high yield as a mixture of
【００１４】また、この反応系（反応炉）でキャリアー
ガスを使わないという特殊性から、錫の蒸発源の近傍に
二酸化錫ウィスカーが生成するように送入ガス量を調整
すれば、二酸化錫ウィスカーの生成範囲での高濃度錫蒸
気を保つことができるため、他の箇所で生成する二酸化
錫ウィスカーより大寸法で形状が均一な二酸化錫ウィス
カーが得られる。In addition, because of the specialty of not using a carrier gas in this reaction system (reactor), if the amount of gas supplied is adjusted so that tin dioxide whiskers are generated near the tin evaporation source, tin dioxide whiskers can be obtained. Can maintain high-concentration tin vapor in the production range, so that tin dioxide whiskers having larger dimensions and a uniform shape than tin dioxide whiskers produced in other places can be obtained.
【００１５】[0015]
【実施例】本発明の二酸化錫ウィスカーの製造方法に用
いる反応炉の一例を図１に示す。FIG. 1 shows an example of a reaction furnace used in the method for producing tin dioxide whiskers of the present invention.
【００１６】図１において、１はムライトを材料とした
反応炉の炉芯管、２は反応炉を加熱する電気式ヒータ、
３はガスを通過させない材料を用いた管端栓Ａ、４は多
孔質材料を材料としガスを通過させる管端栓Ｂ、５は不
活性ガス供給口、６は金属錫または金属錫と錫酸化物の
混合物である原料７を溶解するためのるつぼである。In FIG. 1, reference numeral 1 denotes a furnace core tube of a reactor made of mullite, 2 denotes an electric heater for heating the reactor,
3 is a pipe end plug A made of a material that does not allow gas to pass through, 4 is a pipe end plug made of a porous material and B is made to pass a gas, 5 is an inert gas supply port, 6 is metal tin or metal tin and tin oxide. This is a crucible for dissolving the raw material 7 which is a mixture of materials.
【００１７】図１に示す反応炉の炉芯管１の中のるつぼ
６の中に金属錫または金属と錫酸化物の混合物である原
料（以下単に原料という）７を供給後、炉の中（以下炉
内という）に不活性ガスを不活性ガス供給口５から供給
しておいて、ヒータ２によって炉芯管１とともに炉内を
加熱する。炉内の不活性ガスと原料７が原料７の溶融温
度に達し十分な錫蒸気の発生後、不活性ガスの送入を停
止する。不活性ガスの送給を停止すると、酸素を含むガ
スを炉内に供給することにより錫蒸気が酸化され二酸化
錫ウィスカーが生成する。図１に示す本発明の二酸化錫
ウィスカーの製造方法に用いた反応炉の場合には管端栓
Ｂに多孔質材料を使用しているので、不活性ガスの炉内
への供給を停止すると管端栓Ｂを通過して酸素を含むガ
スが自然に流入し蒸気化した錫を酸化する。蒸気化した
錫がほぼ全部酸化された後、不活性ガスを炉内に供給す
ると酸素を含むガスの炉内への流入が停止し、炉内は不
活性ガス雰囲気となり、再び錫蒸気が発生するので、再
び不活性ガスの送給を停止し、酸素を含むガスを流入さ
せ錫蒸気を酸化させる。このように不活性ガスの送給・
停止と酸素を含むガスの停止・送給を交互に行い、るつ
ぼ６内の原料７が全て蒸発し二酸化錫ウィスカーに転化
するまで、両ガスの送給と停止を交互に繰り返す。A raw material (hereinafter simply referred to as a raw material) 7 which is metal tin or a mixture of metal and tin oxide is supplied into a crucible 6 in a furnace core tube 1 of the reaction furnace shown in FIG. In the furnace, the inert gas is supplied from the inert gas supply port 5 and the furnace is heated together with the furnace core 1 by the heater 2. After the inert gas and the raw material 7 in the furnace reach the melting temperature of the raw material 7 and sufficient tin vapor is generated, the supply of the inert gas is stopped. When the supply of the inert gas is stopped, tin vapor is oxidized by supplying a gas containing oxygen into the furnace, and tin dioxide whiskers are generated. In the case of the reactor used in the method for producing tin dioxide whiskers of the present invention shown in FIG. 1, a porous material is used for the pipe end plug B. The gas containing oxygen naturally flows through the end plug B and oxidizes the vaporized tin. When almost all of the vaporized tin is oxidized, when an inert gas is supplied into the furnace, the flow of oxygen-containing gas into the furnace stops, the furnace becomes an inert gas atmosphere, and tin vapor is generated again. Therefore, the supply of the inert gas is stopped again, and a gas containing oxygen is introduced to oxidize the tin vapor. In this way, the supply of inert gas
The stoppage and the supply and the supply of the gas containing oxygen are alternately performed, and the supply and the stoppage of the two gases are alternately repeated until all the raw materials 7 in the crucible 6 evaporate and are converted into tin dioxide whiskers.
【００１８】本発明に用いる不活性ガスとは、ヘリウム
やアルゴンのような不活性原素のガスの他、原料を蒸発
させるのに必要な１０００℃〜１３５０℃の温度で熱解
離しないＮ2などのガスを用いてもよい。また、酸素を
含むガスとは空気，酸素・窒素の混合調整ガス，酸素等
が利用できる。さらに、原料としては金属錫の塊状物，
インゴット，粉末等が、錫酸化物としては一酸化錫，二
酸化錫が使用でき、また金属錫と錫酸化物の混合物を用
いてもよい。The inert gas used in the present invention is, for example, an inert element gas such as helium or argon, or N 2 which is not thermally dissociated at a temperature of 1000 ° C. to 1350 ° C. necessary for evaporating the raw material. May be used. The oxygen-containing gas may be air, mixed gas of oxygen and nitrogen, oxygen, or the like. In addition, the raw material is a lump of metallic tin,
Ingots, powders and the like can be used as tin oxide, and tin monoxide and tin dioxide can be used, or a mixture of metal tin and tin oxide can be used.
【００１９】以上の述べたように不活性ガス雰囲気中で
行われる錫の蒸気化、酸素を含むガスの雰囲気中におけ
る錫蒸気の酸化と結晶成長の過程には、使用するガスと
原料の種類，不活性ガスと酸素を含む気体の炉内への供
給の時間割合，炉内温度等、種々の要素が関わってい
る。As described above, in the process of vaporizing tin in an inert gas atmosphere, oxidizing tin vapor in an atmosphere of a gas containing oxygen, and growing a crystal, the types of gas and raw materials used, Various factors are involved, such as the time ratio of the supply of the gas containing the inert gas and oxygen into the furnace, the furnace temperature, and the like.
【００２０】以下、４つ実施例と２つの比較例について
説明する。 （実施例１）図１に示す反応炉を用い、原料７として金
属錫１５ｇをるつぼ６に入れ炉芯管１の中央部にるつぼ
６を置き、不活性ガスとして窒素ガスを用い０.２５ｌ
／ｍｉｎの流量で不活性ガス供給口５から炉内に供給
し、炉内温度は１２００℃に設定する。Hereinafter, four examples and two comparative examples will be described. (Example 1) Using the reaction furnace shown in FIG. 1, 15 g of metallic tin as a raw material 7 was put in a crucible 6, and the crucible 6 was placed at the center of the furnace core tube 1, and 0.25 l of nitrogen gas was used as an inert gas.
The gas is supplied into the furnace from the inert gas supply port 5 at a flow rate of / min, and the furnace temperature is set to 1200 ° C.
【００２１】上記の条件下で、全焼成時間を１.５時間
とし、焼成開始後３０分で窒素ガスの供給を停止し、そ
の１０分後に再び窒素ガスを供給、以後１０分ごとに窒
素の供給と停止を繰り返した。Under the above conditions, the total calcination time was 1.5 hours, the supply of nitrogen gas was stopped 30 minutes after the start of calcination, the nitrogen gas was supplied again 10 minutes after that, and the nitrogen gas was supplied every 10 minutes thereafter. Supply and stop were repeated.
【００２２】その結果、るつぼ内には直径が約１０μ
ｍ、長さが１０ｍｍまでの二酸化錫ウィスカーが生成
し、るつぼ６内には金属錫は残存せず、全て二酸化錫ウ
ィスカーだけであった。As a result, the diameter in the crucible is about 10 μm.
m, tin dioxide whiskers having a length of up to 10 mm were formed, no metallic tin remained in the crucible 6, and all were only tin dioxide whiskers.
【００２３】（実施例２）実施例１における諸条件の
内、炉内温度だけを１１５０℃とし、他は全て実施例１
と同様に焼成を行った。(Embodiment 2) Of the various conditions in Embodiment 1, only the furnace temperature was set at 1150 ° C.
Calcination was performed in the same manner as described above.
【００２４】その結果は、二酸化錫ウィスカーの直径お
よび長さが若干小さくなったが、実施例１とほぼ同様の
結果が得られた。As a result, although the diameter and length of the tin dioxide whiskers were slightly reduced, substantially the same results as in Example 1 were obtained.
【００２５】（実施例３）実施例１と同様の条件のもと
に窒素ガスの送給と停止の時間だけを変えて焼成を行っ
た。窒素ガスを０.２５ｌ／ｍｉｎの流量で３０分間炉
内に供給し、１０分間供給を停止した後、１分間流量１
ｌ／ｍｉｎで窒素ガスを送給し、再び１０分間停止す
る。この窒素ガスの送給と停止を１.５時間繰り返して
焼成を行った。(Example 3) The sintering was performed under the same conditions as in Example 1 except for changing the supply and stop times of the nitrogen gas. Nitrogen gas is supplied into the furnace at a flow rate of 0.25 l / min for 30 minutes, the supply is stopped for 10 minutes, and then the flow rate is reduced to 1 for 1 minute.
Nitrogen gas is supplied at 1 / min and stopped again for 10 minutes. The feeding and stopping of the nitrogen gas were repeated for 1.5 hours to perform firing.
【００２６】その結果は、実施例１と同様の結果が得ら
れた。 （実施例４）実施例１とほとんど同様の条件下におい
て、不活性ガスとしてヘリウムガスを用い、流量を０.
２５ｌ／ｍｉｎを３０分供給し、１０分間停止する。そ
の後は１ｌ／ｍｉｎの流量でヘリウムガスを送給し１分
後に停止し、このヘリウムガスの送給と停止を１.５時
間繰り返した。As a result, a result similar to that of Example 1 was obtained. (Example 4) Under almost the same conditions as in Example 1, helium gas was used as the inert gas, and the flow rate was set at 0.5.
Supply 25 l / min for 30 minutes and stop for 10 minutes. Thereafter, helium gas was supplied at a flow rate of 1 l / min, and stopped after 1 minute. This supply and stop of helium gas were repeated for 1.5 hours.
【００２７】その結果は、実施例１と同様の結果が得ら
れた。さらに不活性ガスとしてアルゴンガスを用いた
が、全く同様の結果が得られた。As a result, the same result as in Example 1 was obtained. Further, although argon gas was used as an inert gas, exactly the same results were obtained.
【００２８】（比較例１）実施例１と同様の反応炉を用
い、窒素ガスと空気を各１ｌ／ｍｉｎの流量で同時に炉
内に供給し、炉内温度を１２００℃、焼成時間を１.５
時間とした。(Comparative Example 1) Using the same reactor as in Example 1, nitrogen gas and air were simultaneously supplied into the furnace at a flow rate of 1 l / min, the furnace temperature was 1200 ° C., and the firing time was 1. 5
Time.
【００２９】その結果、るつぼ６の縁に極少量の二酸化
錫ウィスカーが生成したが、るつぼ６内には表面に酸化
錫膜を形成した金属錫が残った。As a result, a very small amount of tin dioxide whiskers was formed on the edge of the crucible 6, but metal tin having a tin oxide film formed on the surface remained in the crucible 6.
【００３０】（比較例２）実施例１と同様の反応炉を用
い、窒素ガスを０.２５ｌ／ｍｉｎとして炉内に供給
し、炉内温度を１２００℃とした。焼成温度は１.５時
間とし、途中１時間経過時に窒素ガスの供給を停止し、
酸素を含むガスを流入させた。Comparative Example 2 Using the same reactor as in Example 1, nitrogen gas was supplied into the furnace at 0.25 l / min, and the furnace temperature was set to 1200 ° C. The firing temperature was 1.5 hours, and the supply of nitrogen gas was stopped when 1 hour had elapsed on the way,
A gas containing oxygen was allowed to flow.
【００３１】その結果、るつぼ６内に直径１０μｍ、長
さ数ｍｍの二酸化錫ウィスカーが生成したが、極少量で
あり、るつぼ６内には表面に酸化錫膜を形成した金属錫
が残った。As a result, tin dioxide whiskers having a diameter of 10 μm and a length of several mm were formed in the crucible 6, but the amount was extremely small, and the tin metal having a tin oxide film formed on the surface remained in the crucible 6.
【００３２】[0032]
【発明の効果】以上の説明からも明らかなように本発明
の二酸化錫ウィスカーの製造方法によれば、金属錫の近
傍に不活性ガスを断続的に送入して、酸素濃度を制御す
ると共に錫蒸気の蒸発を促進するので、短時間で大型で
形状が均一な二酸化錫ウィスカーが得られる。また、導
電性に優れ１０-2Ωｃｍの値のものが得られ、さらに高
純度であるから、産業界における用途は極めて大であ
る。As is clear from the above description, according to the method for producing tin dioxide whiskers of the present invention, the vicinity of metallic tin is improved.
Control the oxygen concentration by intermittently feeding an inert gas
In addition, since tin vaporization is promoted , tin dioxide whiskers having a large size and a uniform shape can be obtained in a short time. In addition, since it has excellent conductivity and a value of 10 −2 Ωcm, and has high purity, it is very large in industrial use.
【図１】本発明の二酸化錫ウィスカーの製造方法に用い
た反応炉の一例を示す縦断面図FIG. 1 is a longitudinal sectional view showing an example of a reactor used in a method for producing a tin dioxide whisker of the present invention.
６ るつぼ ７ 原料 6 Crucible 7 Raw material
───────────────────────────────────────────────────── フロントページの続き (72)発明者 佐藤 隆重 大阪府門真市大字門真1006番地 松下電 器産業株式会社内 (56)参考文献 特開 昭61−17421（ＪＰ，Ａ) 特公 昭39−205（ＪＰ，Ｂ１) (58)調査した分野(Int.Cl.6，ＤＢ名) C01G 1/00 - 57/00──────────────────────────────────────────────────続 き Continuation of front page (72) Inventor Takashige Sato 1006 Kazuma Kadoma, Kadoma City, Osaka Prefecture Matsushita Electric Industrial Co., Ltd. 205 (JP, B1) (58) Field surveyed (Int. Cl. 6 , DB name) C01G 1/00-57/00
Claims (3)
給によって系外から供給される反応炉において、反応炉
内に金属錫または金属錫と錫酸化物の混合物である原料
を蒸発させるためのるつぼを配設し、そのるつぼに原料
を供給しておいて反応炉内を錫蒸気が発生する１０００
℃〜１３５０℃の温度範囲に保ちながら、錫蒸気が存在
する雰囲気中に不活性ガスを原料の近傍に断続的に送入
する二酸化錫ウィスカーの製造方法。In a reactor in which a gas containing oxygen is supplied from outside the system by spontaneous inflow or forced supply, a raw material which is metal tin or a mixture of metal tin and tin oxide is evaporated in the reactor. A crucible is provided, and the raw material is supplied to the crucible.
A method for producing a tin dioxide whisker in which an inert gas is intermittently fed into the vicinity of a raw material in an atmosphere in which tin vapor is present, while maintaining the temperature in a temperature range of from 1C to 1350C.
１０００℃〜１３５０℃の温度下で、熱解離しないＮ2
等のガスである請求項１記載の二酸化錫ウィスカーの製
造方法。Wherein N 2 inert gas, at a temperature of gas or 1000 ° C. to 1350 ° C. in inert element, which is not thermally dissociated
The method for producing tin dioxide whiskers according to claim 1, which is a gas such as the above.
載の二酸化錫ウィスカーの製造方法。3. The method for producing tin dioxide whiskers according to claim 1, wherein the gas containing oxygen is air.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3164292A JP2827586B2 (en) | 1991-07-04 | 1991-07-04 | Method for producing tin dioxide whiskers |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3164292A JP2827586B2 (en) | 1991-07-04 | 1991-07-04 | Method for producing tin dioxide whiskers |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0517145A JPH0517145A (en) | 1993-01-26 |
| JP2827586B2 true JP2827586B2 (en) | 1998-11-25 |
Family
ID=15790340
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3164292A Expired - Lifetime JP2827586B2 (en) | 1991-07-04 | 1991-07-04 | Method for producing tin dioxide whiskers |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2827586B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103059846A (en) * | 2013-01-10 | 2013-04-24 | 郑水姣 | Sn/SnO2 composite luminescent material and preparation method thereof |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5837209A (en) * | 1995-04-10 | 1998-11-17 | Sumitomo Chemical Company, Limited | Tin oxide whisker |
| JP2013170092A (en) * | 2012-02-20 | 2013-09-02 | National Institute For Materials Science | Single crystal tin oxide wire |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6117421A (en) * | 1984-07-04 | 1986-01-25 | Natl Inst For Res In Inorg Mater | Preparation of fibrous electrically-conductive stannic oxide |
-
1991
- 1991-07-04 JP JP3164292A patent/JP2827586B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103059846A (en) * | 2013-01-10 | 2013-04-24 | 郑水姣 | Sn/SnO2 composite luminescent material and preparation method thereof |
| CN103059846B (en) * | 2013-01-10 | 2015-04-22 | 张香丽 | Sn/SnO2 composite luminescent material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0517145A (en) | 1993-01-26 |
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