JP2003267728A - Method for producing fine particle of niobium oxide - Google Patents
Method for producing fine particle of niobium oxideInfo
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- JP2003267728A JP2003267728A JP2002072382A JP2002072382A JP2003267728A JP 2003267728 A JP2003267728 A JP 2003267728A JP 2002072382 A JP2002072382 A JP 2002072382A JP 2002072382 A JP2002072382 A JP 2002072382A JP 2003267728 A JP2003267728 A JP 2003267728A
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- Prior art keywords
- niobium
- niobium oxide
- fine particles
- raw material
- particle size
- Prior art date
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、酸化ニオブ微粒子
の製造方法に関し、特に、キャパシタ用電極材料として
好適なニオブ粉末原料を作製するのに好適な酸化ニオブ
微粒子を、塩化ニオブ蒸気の加水分解により製造する方
法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing niobium oxide fine particles, and in particular, niobium oxide fine particles suitable for producing a niobium powder raw material suitable as an electrode material for capacitors are hydrolyzed with niobium chloride vapor. It relates to a method of manufacturing.
【０００２】[0002]
【従来の技術】キャパシタ用電極材料として使用するニ
オブ粉末原料を作製する酸化ニオブ粉末は、通常、以下
に述べる方法で作製する。ニオブを含む鉱石やスクラッ
プをフッ化水素（ＨＦ）にて溶解し、これを溶媒抽出剤
（ＭＩＢＫ）で他成分と分離し、Ｎｂを有機相に抽出す
る。次に、希硫酸によりＮｂＯＦ5 2-の形態で水相へ逆
抽出する。これにＮＨ4ＯＨ水溶液を加えて水酸化物を
沈殿させ、ろ過、乾燥、か焼して酸化ニオブを得る。2. Description of the Related Art Niobium oxide powder for producing a niobium powder raw material used as a capacitor electrode material is usually produced by the method described below. Ore or scrap containing niobium is dissolved with hydrogen fluoride (HF), and this is separated from other components with a solvent extractant (MIBK), and Nb is extracted into an organic phase. Then, back-extracted into the aqueous phase at NbOF 5 2- embodiment with dilute sulfuric acid. NH 4 OH aqueous solution is added to this to precipitate the hydroxide, which is filtered, dried and calcined to obtain niobium oxide.
【０００３】このような方法で得られた平均粒径４μｍ
程度の酸化ニオブ粉末を、約１４００℃で大気焼成し、
これを粉砕・分級することにより二次粒子径を所定の粒
径（例えば、５０〜２００μｍ）とし、さらに還元する
ことによりキャパシタ用電極材料のニオブ粉末原料を製
造するプロセスが知られている。二次粒子を構成する一
次粒子の平均粒径は出発原料の粒径よりわずかに成長
し、５〜６μｍ程度となる。Average particle size 4 μm obtained by such a method
Niobium oxide powder is baked in the air at about 1400 ° C,
A process is known in which the secondary particle size is adjusted to a predetermined particle size (for example, 50 to 200 μm) by crushing and classifying this, and further reduction is performed to manufacture a niobium powder raw material for a capacitor electrode material. The average particle diameter of the primary particles constituting the secondary particles grows slightly from the particle diameter of the starting material and becomes about 5 to 6 μm.
【０００４】しかしながら、還元工程における出発原料
の酸化ニオブ粉末の平均粒径が、上記のように５〜６μ
ｍ程度であるために、還元により得られるニオブ粉末原
料の粒子間の空隙もμｍオーダーとなる。この内部の空
隙の存在により、得られるニオブ粉末原料の単位質量あ
たりの比表面積は小さくなり（例えば０．１ｍ2／
ｇ）、出発原料の酸化ニオブ粉末の大きい粒径（４μｍ
程度）が、結果として、キャパシタの電気容量を制限す
る一因になっていた。However, the average particle size of the starting niobium oxide powder in the reduction step is 5 to 6 μm as described above.
Since it is about m, the voids between particles of the niobium powder raw material obtained by the reduction are also in the μm order. Due to the presence of the voids inside, the specific surface area of the obtained niobium powder raw material per unit mass becomes small (for example, 0.1 m 2 /
g), large particle size of starting niobium oxide powder (4 μm)
However, as a result, it has been a cause of limiting the capacitance of the capacitor.
【０００５】[0005]
【発明が解決しようとする課題】本発明は、単位質量あ
たりの比表面積がより大きい（２ｍ2／ｇ程度）酸化ニ
オブ粉末を焼結で得るのに好適で、微細な粒径の酸化ニ
オブ微粒子の製造方法を提供することを課題とする。The present invention is suitable for obtaining a niobium oxide powder having a larger specific surface area per unit mass (about 2 m 2 / g) by sintering, and niobium oxide fine particles having a fine particle size. It is an object to provide a manufacturing method of
【０００６】[0006]
【課題を解決するための手段】本発明者らは、従来の酸
化ニオブ粉末に比べて、より微細な粒径の酸化ニオブ粉
末を得るための検討を進めた結果、１．０μｍ以下の粒
径（単位質量あたりの比表面積が１．５〜２．５ｍ2／
ｇ）を有する酸化ニオブ微粒子を得るに至った。Means for Solving the Problems As a result of investigations by the present inventors for obtaining a niobium oxide powder having a finer particle size than the conventional niobium oxide powder, a particle size of 1.0 μm or less was obtained. (Specific surface area per unit mass is 1.5 to 2.5 m 2 /
Thus, niobium oxide fine particles having g) are obtained.
【０００７】すなわち、本発明の酸化ニオブ微粒子は、
塩化ニオブを不活性ガス気流中で揮発させ、この塩化ニ
オブ蒸気に水蒸気を反応させて気流中で加水分解するこ
とにより得られ、１．０μｍ以下の微細な粒径を有す
る。That is, the niobium oxide fine particles of the present invention are
It is obtained by volatilizing niobium chloride in an inert gas stream, reacting this niobium chloride vapor with water vapor, and hydrolyzing it in the stream, and has a fine particle size of 1.0 μm or less.
【０００８】本発明の酸化ニオブ微粒子の製造方法は、
塩化ニオブを１７０〜２４０℃の温度において揮発さ
せ、得られた塩化ニオブ蒸気からなる原料気流中に、水
蒸気を添加して加水分解し、気流中において粒径１．０
μｍ以下の酸化ニオブ微粒子を製造する方法である。The method for producing fine particles of niobium oxide of the present invention comprises:
Niobium chloride is volatilized at a temperature of 170 to 240 ° C., and steam is added to the raw material air stream of the obtained niobium chloride vapor to hydrolyze it, and the particle size is 1.0 in the air stream.
It is a method for producing niobium oxide fine particles having a size of μm or less.
【０００９】あるいは、オキシ塩化ニオブを３００〜４
００℃の温度において揮発させ、得られたオキシ塩化ニ
オブ蒸気からなる原料気流中に、水蒸気を添加して加水
分解し、気流中において粒径１．０μｍ以下の酸化ニオ
ブ微粒子を製造する方法である。Alternatively, 300 to 4 niobium oxychloride is added.
It is a method of producing niobium oxide fine particles having a particle size of 1.0 μm or less in an air stream by volatilizing at a temperature of 00 ° C. and adding water vapor to a raw material air stream made of the obtained niobium oxychloride to hydrolyze. .
【００１０】前記の揮発および加水分解を、縦型反応器
内で行い、加水分解する部分の温度が４００℃以上であ
ることが望ましい。The above-mentioned volatilization and hydrolysis are carried out in a vertical reactor, and the temperature of the portion to be hydrolyzed is preferably 400 ° C. or higher.
【００１１】また、縦型反応器内で上昇する前記原料気
流内を、前記水蒸気が下方から上方に向かって流れ、得
られる酸化ニオブ微粒子を縦型反応器の上方より吸引し
て回収することが望ましい。Further, in the raw material air stream rising in the vertical reactor, the water vapor flows from the lower side to the upper side, and the obtained niobium oxide fine particles are sucked and collected from the upper side of the vertical reactor. desirable.
【００１２】[0012]
【発明の実施の形態】キャパシタ用電極材料の原料とし
て、酸化ニオブを選んだ場合、酸化ニオブ粉末を焼結
後、アルカリ金属やアルカリ土類金属で還元する。この
とき、酸化ニオブ粉末の単位質量当りの比表面積を大き
くすることにより、換言すれば、酸化ニオブ粉末の平均
粒径を小さくすることにより、ニオブ粉末原料の単位質
量当りの比表面積を大きくすることができる。なお、平
均粒径と、単位質量あたりの比表面積とは、図４に示す
ようような関係がある。すなわち、酸化ニオブ粉末の平
均粒径を１．０μｍ以下にすれば、ニオブ粉末原料の単
位質量当たりの比表面積を１．５〜２．５ｍ2／ｇにす
ることができる。BEST MODE FOR CARRYING OUT THE INVENTION When niobium oxide is selected as a raw material for a capacitor electrode material, niobium oxide powder is sintered and then reduced with an alkali metal or an alkaline earth metal. At this time, by increasing the specific surface area of the niobium oxide powder per unit mass, in other words, by decreasing the average particle size of the niobium oxide powder, increasing the specific surface area of the niobium powder raw material per unit mass. You can The average particle size and the specific surface area per unit mass have a relationship as shown in FIG. That is, if the average particle size of the niobium oxide powder is 1.0 μm or less, the specific surface area per unit mass of the niobium powder raw material can be 1.5 to 2.5 m 2 / g.
【００１３】本発明の製造方法は、上記の目的で、平均
粒径が小さい微細な粒径の酸化ニオブ粉末（酸化ニオブ
微粒子）を得る方法であって、不活性ガス気流中で塩化
ニオブを１７０〜２４０℃で、あるいはオキシ塩化ニオ
ブを３００〜４００℃で、加熱することにより揮発さ
せ、４００℃以上の高温である気流中に、水蒸気を添加
して加水分解し、気流中で酸化ニオブ微粒子を得る。For the above-mentioned purpose, the production method of the present invention is a method for obtaining a niobium oxide powder (fine particles of niobium oxide) having a small average particle diameter and fine particles of niobium chloride in an inert gas stream. To 240 ° C. or niobium oxychloride is heated to 300 to 400 ° C. to volatilize, and steam is added to the air stream having a high temperature of 400 ° C. or higher to hydrolyze the niobium oxide fine particles in the air stream. obtain.
【００１４】気流中の塩化ニオブ濃度を制御することに
より、加水分解により得られる酸化ニオブ微粒子の平均
粒径を制御することができる。すなわち、図５に示すよ
うに、加水分解気流中の塩化ニオブ濃度と、生成した酸
化ニオブ粒子の平均粒径の関係が得られる。すなわち、
塩化ニオブ濃度が、各々１．５％、１．０％、０．５％
のとき、酸化ニオブ粉末の平均粒径は、各々０．３μ
ｍ、０．２μｍ、０．１μｍのようになる。By controlling the niobium chloride concentration in the air stream, the average particle size of the niobium oxide fine particles obtained by hydrolysis can be controlled. That is, as shown in FIG. 5, the relationship between the niobium chloride concentration in the hydrolysis gas stream and the average particle size of the generated niobium oxide particles is obtained. That is,
Niobium chloride concentration is 1.5%, 1.0%, 0.5%
, The average particle size of the niobium oxide powder is 0.3 μm
m, 0.2 μm, 0.1 μm.
【００１５】また、本発明の方法において、原料の塩化
ニオブを揮発させる温度の上限である２４０℃と、原料
のオキシ塩化ニオブを揮発させる温度の上限である４０
０℃は、それぞれの沸点であり、この上限以上に温度を
上昇させることの効果はない。In the method of the present invention, the upper limit of the temperature at which the raw material niobium chloride is volatilized is 240 ° C. and the upper limit of the temperature at which the raw material niobium oxychloride is volatilized is 40.
0 ° C. is each boiling point, and there is no effect of raising the temperature above this upper limit.
【００１６】また、本発明の方法において、原料の塩化
ニオブを揮発させる温度の下限である１７０℃と、原料
のオキシ塩化ニオブを揮発させる温度の下限である３０
０℃は、工業的に実用的な温度であり、この下限以下に
温度を低下させると、蒸気圧が低下し、反応が進まなく
なる。In the method of the present invention, the lower limit of the temperature at which the raw material niobium chloride is volatilized is 170 ° C. and the lower limit of the temperature at which the raw material niobium oxychloride is volatilized is 30.
0 ° C. is an industrially practical temperature, and if the temperature is lowered below this lower limit, the vapor pressure will drop and the reaction will not proceed.
【００１７】また、加水分解温度を４００℃以上とする
のは、塩化ニオブ（ＮｂＣｌ5）が、ＮｂＯＣｌ3へ、さ
らにＮｂ2Ｏ5へと、順次変化するので、固体のオキシ塩
化ニオブ（ＮｂＯＣｌ3）が存在しない様に、その沸点
以上としておくためである。Further, the hydrolysis temperature is set to 400 ° C. or higher because the niobium chloride (NbCl 5 ) is sequentially changed to NbOCl 3 and then to Nb 2 O 5 , so that solid niobium oxychloride (NbOCl 3) is used. This is because it is kept above its boiling point so that no) exists.
【００１８】さらに、工業的には加水分解温度は６００
℃から１０００℃程度が好ましい。６００℃以下である
と反応が進みにくく、１０００℃を超えると、設備の選
定、保守またはエネルギー効率の面からも経済的でな
い。Further, industrially, the hydrolysis temperature is 600.
C. to 1000.degree. C. are preferable. If it is 600 ° C or lower, the reaction is difficult to proceed, and if it exceeds 1000 ° C, it is not economical from the viewpoint of equipment selection, maintenance or energy efficiency.
【００１９】本発明の方法を行なう装置として、前記塩
化ニオブまたはオキシ塩化ニオブの揮発、および下流で
の水蒸気による加水分解を図３に断面図を示すような縦
型反応器内で行い、塩化ニオブまたはオキシ塩化ニオブ
の蒸気からなる原料気流は、縦型反応器内を上昇させ、
水蒸気を、縦型反応器の下方から上方に向かって流して
加水分解を生じさせ、これにより得られる酸化ニオブ微
粒子を縦型反応器の上方より吸引して回収できる装置を
選択した。このような構成とすることは、水蒸気の逆流
を極力防止するためである。水蒸気が逆流すると、塩化
ニオブがオキシ塩化ニオブに変化し、得られる酸化ニオ
ブ微粒子の収率が低下したり、オキシ塩化ニオブが酸化
ニオブ微粒子中に混入することとなる。As an apparatus for carrying out the method of the present invention, the niobium chloride or niobium oxychloride is volatilized, and the downstream hydrolysis is carried out in a vertical reactor as shown in the sectional view of FIG. Alternatively, a raw material air stream made of niobium oxychloride vapor rises in the vertical reactor,
A device was selected in which water vapor was caused to flow upward from below the vertical reactor to cause hydrolysis, and the niobium oxide fine particles thus obtained could be sucked and collected from above the vertical reactor. This structure is for preventing the reverse flow of water vapor as much as possible. When the water vapor flows backward, niobium chloride is changed to niobium oxychloride, the yield of the obtained niobium oxide fine particles is reduced, and niobium oxychloride is mixed in the niobium oxide fine particles.
【００２０】また、本発明の方法において、生産効率を
上昇させるため、加水分解用の水蒸気を多段で吹き込む
方法や、水蒸気を予熱する方法も効果的である。Further, in the method of the present invention, in order to increase the production efficiency, a method of blowing steam for hydrolysis in multiple stages and a method of preheating the steam are also effective.
【００２１】[0021]
【実施例】（実施例１）塩化ニオブ３０ｇを坩堝に入
れ、該坩堝を、縦型に配置した内径７０ｍｍ×１７００
ｍｍの石英管に入れ、内部をアルゴンガスで置換した。Example 1 Niobium chloride (30 g) was placed in a crucible, and the crucible was arranged in a vertical shape and an inner diameter of 70 mm × 1700.
It was put in a quartz tube of mm and the inside was replaced with argon gas.
【００２２】さらに、加水分解を行う加水分解部の温度
を１０００℃に昇温した。Further, the temperature of the hydrolysis part for performing hydrolysis was raised to 1000.degree.
【００２３】その後、５Ｌ／分のアルゴンガス気流中に
て前記塩化ニオブを１８５℃に加熱し、前記加水分解部
に、窒素を８０℃の水に潜らせて得られた窒素中水蒸気
を２００ｍＬ／分で流し、窒素中水蒸気と揮発した塩化
ニオブガスとを作用させて加水分解し、生成した微粒子
をフィルターで補集した。Thereafter, the niobium chloride was heated to 185 ° C. in an argon gas stream of 5 L / min, and 200 mL of water vapor in nitrogen obtained by dipping nitrogen into water at 80 ° C. was added to the hydrolysis part. The mixture was allowed to flow for a minute, hydrolyzed by the action of water vapor and volatilized niobium chloride gas in nitrogen, and the produced fine particles were collected by a filter.
【００２４】得られた微粒子は、Ｘ線回折の結果、Ｎｂ
2Ｏ5であることが確認された。The obtained fine particles were confirmed to be Nb as a result of X-ray diffraction.
It was confirmed to be 2 O 5 .
【００２５】また、表１に示すようにＥＰＭＡによる半
定量分析においても、塩素は検出されず、オキシ塩化ニ
オブの存在は確認されなかった。なお、Ｓｉが不可避的
に混入していた。Further, as shown in Table 1, chlorine was not detected and the presence of niobium oxychloride was not confirmed in the semi-quantitative analysis by EPMA. In addition, Si was inevitably mixed.
【００２６】[0026]
【表１】 [Table 1]
【００２７】得られた微粒子をＳＥＭで観察したとこ
ろ、図１に示すように、粒径０．１μｍ程度の超微細粒
子が、多数得られたことが確認された。The SEM observation of the obtained fine particles confirmed that a large number of ultrafine particles having a particle size of about 0.1 μm were obtained as shown in FIG.
【００２８】（実施例２）塩化ニオブを加熱する温度
を、２００℃とした以外は、実施例１と同様にして、微
粒子を得た。(Example 2) Fine particles were obtained in the same manner as in Example 1 except that the temperature at which niobium chloride was heated was 200 ° C.
【００２９】得られた微粒子は、Ｘ線回折の結果、Ｎｂ
2Ｏ5であることが確認された。The obtained fine particles were confirmed to be Nb as a result of X-ray diffraction.
It was confirmed to be 2 O 5 .
【００３０】また、表２に示すようにＥＰＭＡによる半
定量分析においても、塩素は検出されず、オキシ塩化ニ
オブの存在は確認されなかった。Also, as shown in Table 2, chlorine was not detected and the presence of niobium oxychloride was not confirmed in the semi-quantitative analysis by EPMA.
【００３１】[0031]
【表２】 [Table 2]
【００３２】得られた微粒子をＳＥＭで観察したとこ
ろ、図２に示すように、粒径０．１μｍ以下の超微細粒
子も得られたが、粒径０．１〜１μｍの比較的大きな微
粒子も、多数得られた。When the obtained fine particles were observed by SEM, ultrafine particles having a particle size of 0.1 μm or less were obtained as shown in FIG. 2, but relatively large fine particles having a particle size of 0.1 to 1 μm were also obtained. , Obtained many.
【００３３】（実施例３）酸化ニオブ（Ｎｂ2Ｏ5）原料
５０ｇに、活性炭を加え、これに塩素ガスを通過させつ
つ、６００℃に加熱して塩化した。Example 3 Activated carbon was added to 50 g of a niobium oxide (Nb 2 O 5 ) raw material, and chlorine gas was passed through the activated carbon to heat it to 600 ° C. for chlorination.
【００３４】その結果、得られた混合物には、塩化ニオ
ブＮｂＣｌ5とオキシ塩化ニオブＮｂＯＣｌ3が混在して
いた。As a result, the obtained mixture contained niobium chloride NbCl 5 and niobium oxychloride NbOCl 3 .
【００３５】得られた混合物約６０ｇを坩堝に入れ、該
坩堝を、縦型に配置した内径７０ｍｍ×１７００ｍｍの
石英管に入れ、内部をアルゴンガスで置換した。About 60 g of the obtained mixture was placed in a crucible, and the crucible was placed in a quartz tube having an inner diameter of 70 mm × 1700 mm arranged vertically, and the inside was replaced with argon gas.
【００３６】さらに、加水分解を行う加水分解部の温度
を１０００℃に昇温した。Further, the temperature of the hydrolysis part for performing hydrolysis was raised to 1000.degree.
【００３７】その後、５Ｌ／分のアルゴンガス気流中に
て前記混合物を２００℃に加熱し、前記加水分解部に、
窒素を８０℃の水に潜らせて得られた窒素中水蒸気を２
００ｍＬ／分で流し、窒素中水蒸気と揮発したガスとを
作用させて加水分解し、生成した微粒子をフィルターで
補集した。得られた微粒子は、Ｎｂ2Ｏ5であることが確
認された。Thereafter, the mixture was heated to 200 ° C. in an argon gas stream of 5 L / min, and the hydrolysis section was heated to
Water vapor in nitrogen obtained by dipping nitrogen in water at 80 ° C
The mixture was flown at a rate of 00 mL / min, hydrolyzed by allowing water vapor and volatilized gas in nitrogen to act, and the generated fine particles were collected by a filter. It was confirmed that the obtained fine particles were Nb 2 O 5 .
【００３８】坩堝内に残留物があり、オキシ塩化ニオブ
ＮｂＯＣｌ3であった。これは、２００℃の加熱では揮
発しないので、加水分解部に到達しないで残ったものと
思われる。There was a residue in the crucible, which was niobium oxychloride NbOCl 3 . This does not volatilize by heating at 200 ° C., so it is considered that the residue did not reach the hydrolysis part.
【００３９】引き続き、微粒子回収部を切り替えた後、
坩堝内の温度を３５０℃に加熱し、５Ｌ／分のアルゴン
ガス気流中にて揮発させ、加水分解部に、窒素を８０℃
の水に潜らせて得られた窒素中水蒸気を２００ｍＬ／分
で流し、窒素中水蒸気と揮発したガスを作用させて加水
分解した。Subsequently, after switching the fine particle collecting section,
The temperature in the crucible is heated to 350 ° C, and the mixture is volatilized in an argon gas stream of 5 L / min, and nitrogen is added to the hydrolysis portion at 80 ° C.
The water vapor in nitrogen obtained by dipping in the water was flowed at 200 mL / min, and the water vapor in nitrogen and the vaporized gas were caused to act on each other for hydrolysis.
【００４０】その結果、粒径０．１μｍ以下を多く含む
粒径１μｍ以下の酸化ニオブ微粒子が得られた。As a result, niobium oxide fine particles having a particle size of 1 μm or less, which contained a large amount of 0.1 μm or less, were obtained.
【００４１】[0041]
【発明の効果】以上、説明したように、本発明の方法に
よれば、従来より単位質量あたりの比表面積が大きい粒
径１．０μｍ以下の酸化ニオブ微粒子を、容易に得るこ
とができる。As described above, according to the method of the present invention, it is possible to easily obtain niobium oxide fine particles having a particle size of 1.0 μm or less, which has a larger specific surface area per unit mass than before.
【図１】 実施例１で得られた微粒子のＳＥＭ観察写真
である。FIG. 1 is a SEM observation photograph of fine particles obtained in Example 1.
【図２】 実施例２で得られた微粒子のＳＥＭ観察写真
である。FIG. 2 is an SEM observation photograph of fine particles obtained in Example 2.
【図３】 塩化ニオブの加熱部と、加水分解部との関係
を示す断面図である。FIG. 3 is a cross-sectional view showing the relationship between a niobium chloride heating part and a hydrolysis part.
【図４】 酸化ニオブ粉末の平均粒径と単位質量あたり
の比表面積との関係を示すグラフである。FIG. 4 is a graph showing the relationship between the average particle size of niobium oxide powder and the specific surface area per unit mass.
【図５】 加水分解気流中の塩化ニオブ濃度と、生成し
た酸化ニオブ粒子の平均粒径の関係を示すグラフであ
る。FIG. 5 is a graph showing the relationship between the concentration of niobium chloride in the hydrolysis stream and the average particle size of the generated niobium oxide particles.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 金坂 淳 愛媛県新居浜市磯浦町17−５ 住友金属鉱 山株式会社新居浜研究所内 (72)発明者 高橋 洋孝 愛媛県新居浜市西原町３−５−３ 住友金 属鉱山株式会社別子事業所内 Ｆターム(参考） 4G048 AA02 AB02 AC08 AD03 AE06 ─────────────────────────────────────────────────── ─── Continued front page (72) Inventor Atsushi Kanasaka 17-5 Isoura-cho, Niihama-shi, Ehime Sumitomo Metal Ore Niihama Research Center, Yama Co., Ltd. (72) Inventor Hirotaka Takahashi 3-5-3 Nishihara-cho, Niihama-shi, Ehime Sumitomo Kin Besshi Works, Inc. F-term (reference) 4G048 AA02 AB02 AC08 AD03 AE06
Claims (4)
おいて揮発させ、得られた塩化ニオブ蒸気からなる原料
気流中に、水蒸気を添加して加水分解し、気流中におい
て粒径１．０μｍ以下の酸化ニオブ微粒子を得ることを
特徴とする酸化ニオブ微粒子の製造方法。1. Niobium chloride is volatilized at a temperature of 170 to 240 ° C., and steam is added to the raw material stream of the obtained niobium chloride vapor to hydrolyze it. A method for producing fine particles of niobium oxide, which comprises obtaining fine particles of niobium oxide.
温度において揮発させ、得られたオキシ塩化ニオブ蒸気
からなる原料気流中に、水蒸気を添加して加水分解し、
気流中において粒径１．０μｍ以下の酸化ニオブ微粒子
を得ることを特徴とする酸化ニオブ微粒子の製造方法。2. Niobium oxychloride is volatilized at a temperature of 300 to 400.degree. C., and steam is added to the raw material stream of the obtained niobium oxychloride vapor for hydrolysis.
A method for producing fine niobium oxide particles, which comprises obtaining fine niobium oxide particles having a particle size of 1.0 μm or less in an air stream.
器内で行い、加水分解する部分の温度が４００℃以上で
あることを特徴とする請求項１または２に記載の酸化ニ
オブ微粒子の製造方法。3. The niobium oxide fine particles according to claim 1 or 2, wherein the volatilization and hydrolysis are carried out in a vertical reactor, and the temperature of the portion to be hydrolyzed is 400 ° C. or higher. Production method.
内を、前記水蒸気が下方から上方に向かって流れ、加水
分解を生じさせ、これにより得られる酸化ニオブ微粒子
を縦型反応器の上方より吸引して回収することを特徴と
する請求項３に記載の酸化ニオブ微粒子の製造方法。4. In the vertical reactor, the water vapor flows upward from the lower stream in the ascending raw material stream to cause hydrolysis, and the niobium oxide fine particles obtained by the hydrolysis are generated in the vertical reactor. The method for producing niobium oxide fine particles according to claim 3, wherein the fine particles are suctioned and collected from above.
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|---|---|---|---|
| JP2002072382A JP2003267728A (en) | 2002-03-15 | 2002-03-15 | Method for producing fine particle of niobium oxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002072382A JP2003267728A (en) | 2002-03-15 | 2002-03-15 | Method for producing fine particle of niobium oxide |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009073675A (en) * | 2007-09-18 | 2009-04-09 | Mitsui Mining & Smelting Co Ltd | Metal oxide powder and method for producing the same |
| CN116443927A (en) * | 2023-02-24 | 2023-07-18 | 浙江农林大学 | Method for synthesizing mesoporous niobium pentoxide with high specific surface area by one-pot method |
| CN116514169A (en) * | 2023-05-05 | 2023-08-01 | 南京工业大学 | Niobium oxychloride-based composite positive electrode material for chloride ion battery and preparation method thereof |
| KR20230116777A (en) | 2020-12-08 | 2023-08-04 | 디아이씨 가부시끼가이샤 | Niobium oxide particles and method for producing niobium oxide particles |
-
2002
- 2002-03-15 JP JP2002072382A patent/JP2003267728A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009073675A (en) * | 2007-09-18 | 2009-04-09 | Mitsui Mining & Smelting Co Ltd | Metal oxide powder and method for producing the same |
| KR20230116777A (en) | 2020-12-08 | 2023-08-04 | 디아이씨 가부시끼가이샤 | Niobium oxide particles and method for producing niobium oxide particles |
| DE112020007825T5 (en) | 2020-12-08 | 2023-09-28 | Dic Corporation | NIOBOXIDE PARTICLES AND METHOD FOR PRODUCING NIOBOXIDE PARTICLES |
| CN116443927A (en) * | 2023-02-24 | 2023-07-18 | 浙江农林大学 | Method for synthesizing mesoporous niobium pentoxide with high specific surface area by one-pot method |
| CN116514169A (en) * | 2023-05-05 | 2023-08-01 | 南京工业大学 | Niobium oxychloride-based composite positive electrode material for chloride ion battery and preparation method thereof |
| CN116514169B (en) * | 2023-05-05 | 2024-04-05 | 南京工业大学 | Niobium oxychloride-based composite positive electrode material for chloride ion battery and preparation method thereof |
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