JP2007238402A - Powder production apparatus and powder production method - Google Patents
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本発明は、粉体製造装置および粉体製造方法、特に、ナノ粉体の製造に適する粉体製造装置および粉体製造方法に関する。 The present invention relates to a powder manufacturing apparatus and a powder manufacturing method, and more particularly to a powder manufacturing apparatus and a powder manufacturing method suitable for manufacturing nanopowder.
例えば２次電池や半導体などの材料となる粉体の製造に適用される従来の粉体製造装置として、特許文献１に、プラズマ放電を行う電極を有する粉体生成塔内に、原料水溶液を噴霧し、プラズマ放電によって形成する超高温のプラズマ空間で、原料水溶液を乾燥、熱分解して融合させるものが開示されている。 For example, as a conventional powder production apparatus applied to the production of powder used as a material for secondary batteries and semiconductors, Patent Document 1 discloses that a raw material aqueous solution is sprayed into a powder production tower having an electrode for performing plasma discharge. However, there is disclosed a method in which an aqueous raw material solution is dried, thermally decomposed and fused in an ultra-high temperature plasma space formed by plasma discharge.
図６に、例として、従来の粉体製造装置で製造したＬａＧａＯ３系酸化物粉体の電子顕微鏡写真を示す。従来の粉体製造装置で製造した粉体粒子は、形状がいびつで、不均一である。これは、原料水溶液の液滴が超高温のプラズマ空間で瞬間的に加熱され、粒子内の水分が一瞬のうちに気化膨張することで、粒子が水蒸気爆発して破壊されるためである。
前記問題点に鑑みて、本発明は、粒子形状の均一な粉体を製造できる粉体製造装置および粉体製造方法を提供することを課題とする。 In view of the above problems, an object of the present invention is to provide a powder manufacturing apparatus and a powder manufacturing method capable of manufacturing a powder having a uniform particle shape.
前記課題を解決するために、本発明による粉体製造装置は、原料液のミストを生成するミスト発生手段と、前記ミストを乾燥させて原料粉体を生成する乾燥装置と、超高温のプラズマ空間を形成するプラズマ発生手段を備え、前記プラズマ空間において前記原料粉体を熱分解して融合させるプラズマ加熱装置とを有するものとする。 In order to solve the above problems, a powder manufacturing apparatus according to the present invention includes a mist generating means for generating a mist of a raw material liquid, a drying device for generating a raw material powder by drying the mist, and an ultra-high temperature plasma space. And a plasma heating device that thermally decomposes and fuses the raw material powder in the plasma space.
この構成によれば、原料液のミストを乾燥装置で乾燥して粉体にしてから、乾燥した粉体をプラズマ空間で熱変成させる。これによって、原料の水蒸気爆発を防止して、原料液のミスト形状を破壊せずに所定の粉体に変性させることができ、粒子形状の均一な粉体を製造することができる。 According to this configuration, the mist of the raw material liquid is dried with a drying device to form a powder, and then the dried powder is thermally transformed in the plasma space. As a result, the steam explosion of the raw material can be prevented, and the mist shape of the raw material liquid can be modified into a predetermined powder without destroying it, and a powder having a uniform particle shape can be produced.
前記乾燥装置の乾燥温度は、１００℃以上２００℃以下であるのがよい。 The drying temperature of the drying device may be 100 ° C. or higher and 200 ° C. or lower.
この構成によれば、原料液のミスト形状を破壊せずに水分を蒸発させて、形状の均一な乾燥した原料粉体を生成できる。これによって、プラズマ空間において水蒸気爆発が防止される。 According to this configuration, moisture can be evaporated without destroying the mist shape of the raw material liquid, and a dry raw material powder having a uniform shape can be generated. This prevents water vapor explosion in the plasma space.
また、本発明による粉体の製造方法は、原料液のミストを生成し、前記ミストを気流によって搬送し、前記気流を加熱することで前記ミストを乾燥して原料粉体を生成し、前記原料粉体を超高温のプラズマ空間で熱分解して融合させる方法とする。 In addition, the method for producing a powder according to the present invention generates a mist of a raw material liquid, conveys the mist by an air flow, heats the air flow to dry the mist, and generates a raw material powder. The powder is thermally decomposed and fused in an ultra-high temperature plasma space.
この方法によれば、原料液のミストを搬送する気流を加熱してミストを乾燥するので、略球形の乾燥した原料粉体が得られ、乾燥した原料粉体を高温のプラズマ空間で熱変性させるので水蒸気爆発することなく、略球形の均一な粉体を生成できる。 According to this method, since the mist is dried by heating the air current carrying the mist of the raw material liquid, a substantially spherical dry raw material powder is obtained, and the dried raw material powder is thermally denatured in a high-temperature plasma space. Therefore, a substantially spherical uniform powder can be generated without causing a steam explosion.
また、本発明による粉体の製造方法において、前記原料液をモル比に換算してＬａ：Ｓｒ：Ｇａ：Ｍｇが８：２：８：２の水溶液にすれば、前記プラズマ空間でＬａＧａＯ３系酸化物の粉体を生成することができる。 In the method for producing powder according to the present invention, if the raw material liquid is converted to a molar ratio to make an aqueous solution of La: Sr: Ga: Mg of 8: 2: 8: 2, the LaGaO 3 system in the plasma space. Oxide powder can be produced.
また、本発明による粉体の製造方法において、前記原料液をモル比に換算してＬｉ：Ｎｉ：Ｃｏ：Ｍｎが３：１：１：１の水溶液にすれば、前記プラズマ空間でＬｉ（Ｃｏ１／３Ｎｉ１／３Ｍｎ１／３）Ｏ２の粉体を生成することができる。 In the method for producing a powder according to the present invention, if the raw material liquid is converted into a molar ratio to make an aqueous solution of Li: Ni: Co: Mn of 3: 1: 1: 1, Li (Co 1/3 Ni 1/3 Mn 1/3 ) O 2 powder can be produced.
また、本発明による粉体の製造方法において、モル比に換算してＢａ：Ｔｉが１：１の酢酸またはクエン酸の水溶液にすれば、前記プラズマ空間でＢａＴｉＯ３の粉体を生成することができる。 Further, in the method for producing a powder according to the present invention, if an aqueous solution of acetic acid or citric acid in which Ba: Ti is 1: 1 in terms of molar ratio, BaTiO 3 powder can be produced in the plasma space. it can.
以上のように、本発明によれば、原料液のミストを乾燥してからプラズマ空間で熱変成させるので、ミストの粒子を破壊せずに乾燥、熱変性して球形の粉体を生成できる。 As described above, according to the present invention, since the mist of the raw material liquid is dried and then thermally transformed in the plasma space, a spherical powder can be generated by drying and heat denaturation without destroying the mist particles.
これより、本発明の実施形態について、図面を参照しながら説明する。
図１は、本発明の第１実施形態の粉体製造装置１を示す。粉体製造装置１は、乾燥塔（乾燥装置）２、プラズマ加熱炉（プラズマ加熱装置）３およびバグフィルタ４を直列に接続し、排気ファン５で空気を引き抜くことで、乾燥塔２からプラズマ加熱炉３を経てバグフィルタ４を通過する気流を発生させるものである。
Embodiments of the present invention will now be described with reference to the drawings.
FIG. 1 shows a powder production apparatus 1 according to a first embodiment of the present invention. The powder manufacturing apparatus 1 connects a drying tower (drying apparatus) 2, a plasma heating furnace (plasma heating apparatus) 3, and a bag filter 4 in series, and draws air with an exhaust fan 5, thereby plasma heating from the drying tower 2. An airflow passing through the bag filter 4 through the furnace 3 is generated.
乾燥塔２は、直立筒状をしており、頂部にミスト発生手段であるスプレーノズル６が配置され、胴部を外側から加熱する電熱ヒータ７を有している。スプレーノズル６は、乾燥塔２内に原料液を噴霧して原料液のミスト（液滴）を生成することができる。また、電熱ヒータ７は、乾燥塔２内の気流を設定した温度に加熱するようにコントロールされる。 The drying tower 2 has an upright cylindrical shape, and has a spray nozzle 6 as a mist generating means at the top and an electric heater 7 that heats the body from the outside. The spray nozzle 6 can generate a mist (droplet) of the raw material liquid by spraying the raw material liquid into the drying tower 2. The electric heater 7 is controlled so as to heat the airflow in the drying tower 2 to a set temperature.
プラズマ加熱炉３は、直立筒状に形成され、乾燥塔２の直下に設置されており、胴部に複数のプラズマ電極８が配置されている。プラズマ電極８は、それぞれの間でプラズマ放電をすることによって、プラズマ加熱炉３内に２０００℃を超える超高温のプラズマ空間を形成する。 The plasma heating furnace 3 is formed in an upright cylindrical shape, is installed immediately below the drying tower 2, and a plurality of plasma electrodes 8 are arranged on the body. The plasma electrodes 8 form a super-high temperature plasma space exceeding 2000 ° C. in the plasma heating furnace 3 by performing plasma discharge between them.
バグフィルタ４は、濾布９によってプラズマ加熱炉３の下部から流出する気流から粉体を分離する。 The bag filter 4 separates the powder from the airflow flowing out from the lower part of the plasma heating furnace 3 by the filter cloth 9.
続いて、粉体製造装置１における粉体製造について説明する。
スプレーノズル６で生成された原料液のミストは、排気ファン５による気流に乗って乾燥塔２内を下方に搬送される。電気ヒータ７は、原料液のミストを搬送する気流の温度を１００℃から２００℃に加熱する。これによって、原料液のミストは、各液滴の形状を維持したまま水分が蒸発し、略球形の乾燥した微粒子からなる原料粉体になる。気流の温度が１００℃より低いと乾燥が不十分になるおそれがあり、２００℃を超えると水分が爆発的に気化して液滴を分裂させるおそれがある。
Subsequently, powder production in the powder production apparatus 1 will be described.
The mist of the raw material liquid generated by the spray nozzle 6 is transported downward in the drying tower 2 on the air current by the exhaust fan 5. The electric heater 7 heats the temperature of the airflow carrying the raw material mist from 100 ° C. to 200 ° C. Thus, the mist of the raw material liquid evaporates while maintaining the shape of each droplet, and becomes a raw material powder composed of substantially spherical dried fine particles. If the temperature of the airflow is lower than 100 ° C., drying may be insufficient, and if it exceeds 200 ° C., water may explosively vaporize and break the droplets.
乾燥塔２内で乾燥された原料粉体は、気流に乗ってプラズマ加熱炉３内に搬送され、プラズマ電極８が形成する超高温のプラズマ空間に到達する。原料微粒子は、プラズマ空間において瞬間的に加熱され、熱分解して融合することで、目的の粉体に変性される。この工程においては、乾燥した原料粉体をさらに加熱するので、原料粉体に瞬間的に大きな熱を与えても水蒸気爆発によって粒子が破壊される心配がない。このため、原料粉体を破壊することなく変性して、略球形の微粒子からなる粉体を得ることができる。また、スプレーノズル６が生成したミストの液滴を分裂させることなくそのまま熱変性するので、得られる粉体の粒度のバラツキが小さくなる。 The raw material powder dried in the drying tower 2 is carried in an air current and transported into the plasma heating furnace 3 and reaches an ultra-high temperature plasma space formed by the plasma electrode 8. The raw material fine particles are instantaneously heated in the plasma space, and thermally decomposed and fused to be modified into the target powder. In this step, since the dried raw material powder is further heated, there is no concern that the particles are destroyed by the steam explosion even if the raw material powder is momentarily heated. For this reason, the raw material powder can be modified without breaking to obtain a powder composed of substantially spherical fine particles. Further, since the mist droplets generated by the spray nozzle 6 are thermally denatured as they are without being disrupted, variations in the particle size of the obtained powder are reduced.
さらに、図２に、本発明の第２実施形態の粉体製造装置１’を示す。本実施形態において、前記第１実施形態と同じ構成要素には同じ符号を付して説明を省略する。
粉体製造装置１’は、スプレーノズル６に換えて、ミスト発生手段として、ミストボックス１０と挿気ファン１１とが設けられている。
Further, FIG. 2 shows a powder production apparatus 1 ′ according to the second embodiment of the present invention. In the present embodiment, the same components as those in the first embodiment are denoted by the same reference numerals and description thereof is omitted.
The powder production apparatus 1 ′ is provided with a mist box 10 and an air insertion fan 11 as mist generating means instead of the spray nozzle 6.
ミストボックス１０は、底部に超音波振動子１２を備える水槽であり、所定量の原料液を貯留するようになっている。超音波振動子１２によって振動させられた原料液からは、挿気ファン１１が送り込んだ気流中に微細な液滴が飛び出してミストを生成し、原料液のミストは、そのまま気流に乗って乾燥塔２内に搬送される。 The mist box 10 is a water tank having an ultrasonic transducer 12 at the bottom, and stores a predetermined amount of raw material liquid. From the raw material liquid oscillated by the ultrasonic vibrator 12, fine droplets are ejected into the air stream sent by the air intake fan 11 to generate mist. 2 is conveyed.
本実施形態では、超音波振動によって液径数μｍの微細なミストを生成でき、形状が均一で微細な粉体を製造することができる。なお、第１実施形態においても、スプレーノズル６を超音波振動子を有する超音波スプレーノズルにすれば、数十μｍ以下の微細なミストを発生させることができる。 In the present embodiment, a fine mist having a liquid diameter of several μm can be generated by ultrasonic vibration, and a fine powder having a uniform shape can be produced. In the first embodiment as well, if the spray nozzle 6 is an ultrasonic spray nozzle having an ultrasonic vibrator, a fine mist of several tens of μm or less can be generated.
続いて、本発明の実施例を説明する。
実施例１として、第２実施形態の粉体製造装置１’により、燃料電池の固体電解質材料に用いられるＬａＧａＯ３系酸化物（Ｌａ０．８Ｓｒ０．２Ｇａ０．８Ｍｇ０．２Ｏ３）を製造した。
Next, examples of the present invention will be described.
As Example 1, a LaGaO 3 -based oxide (La 0.8 Sr 0.2 Ga 0.8 Mg 0.2 O) used for a solid electrolyte material of a fuel cell by the powder manufacturing apparatus 1 ′ of the second embodiment. 3 ) was produced.
原料として、硝酸ランタン、硝酸ストロンチウム、硝酸ガリウムおよび硝酸マグネシウムの各硝酸塩を用い、モル比に換算してＬａ：Ｓｒ：Ｇａ：Ｍｇが８：２：８：２になるように各硝酸塩を秤量し、各硝酸塩のモル比が等しくなるように秤量して０．１ｍｏｌ／ｄｍ３の濃度になるように蒸留水に溶解したものを原料液とした。 Using each nitrate of lanthanum nitrate, strontium nitrate, gallium nitrate and magnesium nitrate as raw materials, each nitrate was weighed so that La: Sr: Ga: Mg was 8: 2: 8: 2 in terms of molar ratio. A raw material solution was prepared by weighing so that the molar ratios of the nitrates were equal and dissolving in distilled water to a concentration of 0.1 mol / dm 3 .
ミストボックス１０において液滴径２〜３μｍのミストを発生させ、乾燥塔２において２００℃で乾燥し、プラズマ加熱炉３において７０００℃で熱分解して融合した。こうして得られたＬＳＣＭの粉体は、ＬａＳｒＧａ３Ｏ７およびＬａＳｒＧａＯ４を含んでいたが、さらにこの粉体を１３００℃で１０時間２次焼成することで、純度の高いＬａＧａＯ３系酸化物を得ることができた。 Mist having a droplet diameter of 2 to 3 μm was generated in the mist box 10, dried at 200 ° C. in the drying tower 2, and thermally decomposed at 7000 ° C. in the plasma heating furnace 3 to be fused. The LSCM powder thus obtained contained LaSrGa 3 O 7 and LaSrGaO 4 , and this powder was further subjected to secondary firing at 1300 ° C. for 10 hours to obtain a highly pure LaGaO 3 -based oxide. I was able to.
図３に、本実施例で得られた粉体粒子の電子顕微鏡写真を示す。本実施例では、平均粒子径が９３０ｎｍで幾何標準偏差が１．３６の粉体を得ることができた。図６に示す従来の製造方法によって得られた粉体と比較すると、本実施例の粉体は、粒子形状が均一な球形で、粒度の均一性も高いことが分かる。 FIG. 3 shows an electron micrograph of the powder particles obtained in this example. In this example, a powder having an average particle size of 930 nm and a geometric standard deviation of 1.36 could be obtained. Compared with the powder obtained by the conventional manufacturing method shown in FIG. 6, it can be seen that the powder of this example has a uniform spherical particle shape and high uniformity of particle size.
さらに、実施例２として、第２実施形態の粉体製造装置１’により、リチウムイオン２次電池の正極材料に用いられるＬｉ（Ｃｏ１／３Ｎｉ１／３Ｍｎ１／３）Ｏ２を製造した。 Furthermore, as Example 2, Li (Co 1/3 Ni 1/3 Mn 1/3 ) O 2 used for the positive electrode material of the lithium ion secondary battery is manufactured by the powder manufacturing apparatus 1 ′ of the second embodiment. did.
原料として、硝酸リチウム、硝酸ニッケル、硝酸コバルトおよび硝酸マンガンの各硝酸塩を用い、モル比に換算してＬｉ：Ｎｉ：Ｃｏ：Ｍｎが３：１：１：１になるように各硝酸塩を秤量し、０．５ｍｏｌ／ｄｍ３の濃度になるように蒸留水に溶解したものを原料液とした。 Using each nitrate of lithium nitrate, nickel nitrate, cobalt nitrate and manganese nitrate as raw materials, each nitrate was weighed so that the molar ratio of Li: Ni: Co: Mn was 3: 1: 1: 1. The raw material solution was dissolved in distilled water to a concentration of 0.5 mol / dm 3 .
ミストボックス１０において液滴径２〜３μｍのミストを発生させ、乾燥塔２において２００℃で乾燥し、プラズマ加熱炉３において７０００℃で熱分解して融合した。 Mist having a droplet diameter of 2 to 3 μm was generated in the mist box 10, dried at 200 ° C. in the drying tower 2, and thermally decomposed at 7000 ° C. in the plasma heating furnace 3 to be fused.
図４に、こうして得られた粉体粒子の電子顕微鏡写真を示す。本実施例では、平均粒子径が２０ｎｍで幾何標準偏差が１．２の微細で粒度のバラツキの少ない、形状の均一な粉体を得ることができた。 FIG. 4 shows an electron micrograph of the powder particles thus obtained. In this example, it was possible to obtain a fine powder having an average particle diameter of 20 nm, a geometric standard deviation of 1.2, and a uniform shape with little variation in particle size.
さらに、実施例３として、第２実施形態の粉体製造装置１’により、セラミック積層コンデンサなどの誘電体材料やＰＴＣＲサーミスタに用いられるＢａＴｉＯ３を製造した。 Furthermore, as Example 3, BaTiO 3 used for a dielectric material such as a ceramic multilayer capacitor and a PTCR thermistor was manufactured by the powder manufacturing apparatus 1 ′ of the second embodiment.
原料として、酢酸バリウムおよびチタンテトライソプロピルモノマーを用い、モル比に換算してＢａ：Ｔｉが１：１になるように酢酸の水溶液に０．１ｍｏｌ／ｄｍ３の濃度になるように溶解したものを原料液とした。 As raw materials, barium acetate and titanium tetraisopropyl monomer were used and dissolved in an aqueous solution of acetic acid to a concentration of 0.1 mol / dm 3 so that Ba: Ti was 1: 1 in terms of molar ratio. A raw material liquid was used.
ミストボックス１０において液滴径２〜３μｍのミストを発生させ、乾燥塔２において２００℃で乾燥し、プラズマ加熱炉３において７０００℃で熱分解して融合した。 Mist having a droplet diameter of 2 to 3 μm was generated in the mist box 10, dried at 200 ° C. in the drying tower 2, and thermally decomposed at 7000 ° C. in the plasma heating furnace 3 to be fused.
図５に、こうして得られた粉体粒子の電子顕微鏡写真を示す。本実施例では、平均粒子径が５０ｎｍで幾何標準偏差が１．２の微細で粒度のバラツキの少ない、形状の均一な粉体を得ることができた。 FIG. 5 shows an electron micrograph of the powder particles thus obtained. In this example, it was possible to obtain a fine powder having an average particle diameter of 50 nm, a geometric standard deviation of 1.2, and having a uniform shape and a small variation in particle size.
本実施例の酢酸バリウムに代えて塩化バリウムまたは硝酸バリウムを用いてもよく、酢酸に代えてクエン酸の水溶液を用いても、形状の均一なＢａＴｉＯ３の微細な粉体が得られる。 Barium chloride or barium nitrate may be used in place of barium acetate in this example, and a fine powder of BaTiO 3 having a uniform shape can be obtained by using an aqueous solution of citric acid instead of acetic acid.
本発明は、各実施例の粉体のみならず、多様な粉体、特にナノサイズの粉体を製造するのに適用できる。 The present invention can be applied not only to the powder of each example but also to manufacture various powders, particularly nano-sized powders.
１，１’ 粉体製造装置
２ 乾燥塔（乾燥装置）
３ プラズマ加熱炉（プラズマ加熱装置）
６ スプレーノズル（ミスト発生手段）
７ 電熱ヒータ
８ プラズマ電極（プラズマ発生手段）
１０ ミストボックス（ミスト発生手段）
１２ 超音波振動子
1,1 'Powder production equipment 2 Drying tower (drying equipment)
3 Plasma heating furnace (plasma heating device)
6 Spray nozzle (mist generating means)
7 Electric heater 8 Plasma electrode (plasma generating means)
10 Mist box (Mist generating means)
12 Ultrasonic transducer
Claims (7)
前記ミストを乾燥させて原料粉体を生成する乾燥装置と、
超高温のプラズマ空間を形成するプラズマ発生手段を備え、前記プラズマ空間において前記原料粉体を熱分解して融合させるプラズマ加熱装置とを有することを特徴とする粉体製造装置。 Mist generating means for generating a mist of the raw material liquid;
A drying apparatus for drying the mist to produce a raw material powder;
A powder manufacturing apparatus comprising: a plasma generating unit that forms an ultra-high temperature plasma space; and a plasma heating device that thermally decomposes and fuses the raw material powder in the plasma space.
前記ミストを気流によって搬送し、
前記気流を加熱することで前記ミストを乾燥して原料粉体を生成し、
前記原料粉体を超高温のプラズマ空間で熱分解して融合させることを特徴とする粉体製造方法。 Generate mist of raw material liquid,
Transport the mist by airflow,
The mist is dried by heating the airflow to produce a raw material powder,
A powder manufacturing method, characterized in that the raw material powder is thermally decomposed and fused in an ultra-high temperature plasma space.
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