JP6320533B2 - 均一な金属酸化物ナノ粒子を再現性高く製造する方法 - Google Patents
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Description
前記反応器の内部温度が200乃至400℃になるように昇温させて前記混合溶液を反応させることによって金属酸化物ナノ粒子を形成する段階と、を含み、前記混合溶液を反応させる段階で発生する水を除去することを特徴とする。
前記反応器の内部温度が200乃至400℃になるように昇温させて前記混合溶液を反応させることによって金属酸化物ナノ粒子を形成する段階と、を含み、前記混合溶液を反応させる段階で発生する水を除去することを特徴とする。
水酸化鉄(FeOOH)は、Sigma社と、Alfa Aesar社で購入して使用した。Sigma社の水酸化鉄は、無定形グラニュールタイプであり、アルミナ乳棒と乳鉢を用いて粉砕して140μmの大きさの篩を通過した粉末を実験に使用した。Alfa Aesar社の水酸化鉄は、α相のゲータイトで針状の結晶である粉末であり、これをそのまま実験に使用した。オレイン酸とオクタデセンはSigma社から購入して使用した。
水酸化鉄(Sigma社)7.1g、オレイン酸90.3g、オクタデセン100gを1Lの丸底3口フラスコに入れて磁石攪拌が可能なマントルに設置した。フラスコに攪拌用磁石を入れてフラスコ上端にトラップを設置し、その上に冷却器を設置した。一側入口には窒素注入および真空ポンプ連結ラインを設置し、一側には温度調節用温度計を設置した。真空ポンプを用いてフラスコ内部を真空に作り、60℃まで2℃/minの速度で昇温させた後、60℃で2時間維持した。
水酸化鉄(Alfa Aesar社)7.1g、オレイン酸90.3g、オクタデセン100gを1Lの丸底3口フラスコに入れて磁石攪拌が可能なマントルに設置した。フラスコに攪拌用磁石を入れてフラスコ上端にトラップを設置し、その上に冷却器を設置した。一側入口には窒素注入および真空ポンプ連結ラインを設置し、一側には温度調節用温度計を設置した。真空ポンプを用いてフラスコ内部を真空に作り、60℃まで2℃/minの速度で昇温させた後、60℃で2時間維持した。
FeOOH(Sigma社)7.1g、オレイン酸90.3g、オクタデセン100gを1Lの丸底3口フラスコに入れて磁石攪拌が可能なマントルに設置した。フラスコに攪拌用磁石を入れてフラスコ上端に冷却器を設置した。一側入口には窒素注入および真空ポンプ連結ラインを設置し、一側には温度調節用温度計を設置した。真空ポンプを用いてフラスコ内部を真空に作り、60℃まで2℃/minの速度で昇温させた後、60℃で2時間維持した。
〔ナノ粒子の観察〕
前記実施例1、2および比較例1で得られたナノ粒子を透過電子顕微鏡(TEM)を用いて観察した。比較例1では、ナノ粒子が良好に形成されず、上澄み液をサンプリングして観察した。
実施例1で各反復実験(batch)別にナノ粒子粒径の最大値、最小値、平均、標準偏差、分散係数(Cv、標準偏差/平均×100)を下記表1に示した。
実施例1でナノ粒子の形成過程中、温度調節器を通じて設定した温度と反応器内部の温度を測定して比較したグラフを図4に示した。また、比較例1でナノ粒子の形成過程中、温度調節器を通じて設定した温度と反応器内部の温度を測定して比較したグラフを図5に示した。
20…還流装置
30…冷却器
40…トラップ
50…気化物
60…水
Claims (5)
- 反応器に金属前駆体化合物、カルボン酸、および沸点200℃以上の溶媒を投入して混合溶液を形成する段階と、
前記反応器の内部温度が200乃至400℃になるように昇温させて前記混合溶液を反応させることによって金属酸化物ナノ粒子を形成する段階と、を含み、前記混合溶液を反応させる段階で発生する水を除去する方法であって、
前記混合溶液を反応させることによって金属酸化物ナノ粒子を形成する段階は、前記反応段階で発生する気化物を還流し、前記還流工程で冷却された水をトラップ(trap)を利用して除去して再流入を防止しながら行われ、
前記金属前駆体化合物は、水酸化鉄(FeOOH)である、金属酸化物ナノ粒子の製造方法。 - 前記反応器の内部温度を昇温させた後、前記設定された温度で5分以上維持する、請求項1に記載の金属酸化物ナノ粒子の製造方法。
- 前記反応器内部の温度を昇温させた後、前記反応器内部の温度(T’)が前記設定された温度(T)に対して、T−5℃≦T’≦T+5℃に維持される、請求項1に記載の金属酸化物ナノ粒子の製造方法。
- 前記カルボン酸は、オレイン酸(oleic acid)、ステアリン酸(stearic acid)、ラウリン酸(lauric acid)、パルミチン酸(palmitic acid)、オクタン酸(octanoic acid)およびデカン酸(decanoic acid)からなる群より選択される1種以上を含む、請求項1に記載の金属酸化物ナノ粒子の製造方法。
- 反応器に水酸化鉄(FeOOH)100重量部、オレイン酸を1,000乃至1,400重量部、およびオクタデセン1,200乃至1,500重量部を投入して混合溶液を形成する段階と、
前記反応器の内部温度を310±5℃になるように昇温させて前記混合溶液を反応させることによって酸化鉄ナノ粒子を形成する段階と、を含み、前記混合溶液を反応させる段階で発生する水をトラップ(trap)を利用して除去する、酸化鉄ナノ粒子の製造方法。
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KR1020130151760A KR101508281B1 (ko) | 2013-12-06 | 2013-12-06 | 균일한 금속 산화물 나노 입자를 재현성 높게 제조하는 방법 |
KR10-2013-0151760 | 2013-12-06 | ||
PCT/KR2014/011140 WO2015083960A1 (ko) | 2013-12-06 | 2014-11-19 | 균일한 금속 산화물 나노 입자를 재현성 높게 제조하는 방법 |
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US20160297687A1 (en) | 2016-10-13 |
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CN105793189A (zh) | 2016-07-20 |
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