JP5400602B2 - ナノ粉末、ナノインク、及びマイクロロッド、並びにこれらの製造方法 - Google Patents
ナノ粉末、ナノインク、及びマイクロロッド、並びにこれらの製造方法 Download PDFInfo
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- JP5400602B2 JP5400602B2 JP2009295702A JP2009295702A JP5400602B2 JP 5400602 B2 JP5400602 B2 JP 5400602B2 JP 2009295702 A JP2009295702 A JP 2009295702A JP 2009295702 A JP2009295702 A JP 2009295702A JP 5400602 B2 JP5400602 B2 JP 5400602B2
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- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/08—Metallic powder characterised by particles having an amorphous microstructure
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- B29C48/04—Particle-shaped
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- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/06—Rod-shaped
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Description
まず、溶媒に高分子を溶解させて高分子溶液を調製する。高分子は、熱硬化性樹脂と熱可塑性樹脂の両方が使用可能であり、溶液に粘度を与えて紡糸を効果的に行わせる役割を果たす。紡糸溶液に適切な粘度を与えるために添加される高分子としては、平均分子量が150,000〜1,500,000g/molの高分子が好ましい。例えば、ポリビニルアセテート、ポリウレタン、ポリウレタン共重合体、ポリエーテルウレタン、セルロースアセテートやセルロースアセテートブチレートやセルロースアセテートプロピオネートなどのセルロース誘導体、ポリメチルメタクリレート(PMMA)、ポリメチルアクリレート(PMA)、ポリアクリル共重合体、ポリビニルアセテート共重合体、ポリビニルアルコール(PVA)、ポリフルフリルアルコール(PPFA)、ポリスチレン(PS)、ポリスチレン共重合体、ポリエチレンオキシド(PEO)、ポリプロピレンオキシド(PPO)、ポリエチレンオキシド共重合体、ポリプロピレンオキシド共重合体、ポリカーボネート(PC)、ポリビニルクロライド(PVC)、ポリカプロラクトン、ポリビニルピロリドン(PVP)、ポリビニルフルオライド、ポリビニリデンフルオライド共重合体、ポリアクリロニトリル、ポリアミド、ピッチ(pitch)、及びフェノール樹脂からなる群から選択される少なくとも1つである。しかしながら、本発明の内容は、これらに限定されるものではなく、エレクトロスピニング法などの紡糸によりナノ繊維を形成できる高分子であれば、特に限定されない。
以上のようにして調製された紡糸溶液を紡糸して複合繊維ウェブを形成する。複合繊維ウェブとは、金属、非金属、金属酸化物、金属化合物、非金属化合物、又は複合金属酸化物と高分子が混在して繊維状に絡まっている状態をいう。
以上のようにして調製された複合繊維ウェブを高温熱処理する。これは、複合繊維ウェブ中の高分子を高温で分解して蒸発させるためである。高分子が蒸発されることによって、金属、非金属、金属酸化物、金属化合物、非金属化合物、又は複合金属酸化物のみのナノ粒子が凝集したナノ繊維が形成される。熱処理温度(300〜800℃)及び時間は、高分子の分解温度に応じて決定することができる。熱処理は、金属前駆体又は金属酸化物前駆体の種類によって、400〜900℃の温度範囲で行ってもよい。300〜400℃の熱処理の場合、結晶又は非晶質構造を有するナノ粒子が凝集したナノ繊維が得られる。また、このような熱処理は、空気、酸化雰囲気、還元雰囲気、又は真空中で行ってもよい。このようにして得られたナノ繊維は、超微細なナノ粒子から構成されており、比表面積が大きくて反応面積が極大化する。
前記ナノ繊維をビーズ粉砕して、ナノ粒子、ナノクラスター、又はこれらの混合物からなるナノ粉末を形成する。前記ナノクラスターは、幅が5〜100nmであり、前記幅に対する長さの比であるアスペクト比が1.5〜10.0であることが好ましい。また、前記ナノ粒子は、直径が5〜100nmであることが好ましい。
前記ナノ粉末を溶媒に分散させてナノインクを形成する。特に、ビーズ粉砕過程が溶媒中で行われた場合は、マイクロビーズミル時に溶媒中で粉砕が行われ、それ自体でナノインクを形成する。また、ナノインクに少量の添加剤(分散剤又は界面活性剤)を添加することにより、分散性を向上させ、粘度を調節してもよい。もちろん、添加剤を添加せず、溶媒にナノ粉末を分散させただけでもナノインクが形成される。
溶媒(ジメチルホルムアミド(DMF)2.583g)にチタンプロポキシド1mmol(0.284g)を入れ、さらに酢酸0.5gを入れて完全に溶解して、高分子を含有する溶液を調製する。この溶液に塩化ストロンチウム四水和物1mmol(0.266g)を入れ、さらに水(H2O)0.861gとエタノール0.861gを入れて完全に溶解した後、ポリビニルピロリドン(PVP、分子量:1,300,000)0.63gを入れて溶解することにより、紡糸溶液を製造した。
溶媒(DMF2.583g)にチタンプロポキシド1mmol(0.1847g)を入れ、さらに酢酸0.5gを入れて完全に溶解した。この溶液に塩化ストロンチウム四水和物1mmol(0.266g)を入れ、さらに水(H2O)0.861gとエタノール0.861gを入れて完全に溶解した後、さらにFeCl30.0567gを入れて完全に混合した。
Li4Ti5O12は、スピネル構造を有し、放電容量が160mAh/gである二次電池の陰極活物質である。特に、Liとの反応で構造が変化しないため、高出力、長寿命、安定性に優れた物質として注目されている。
LiMn2O4は、スピネル構造を有し、理論容量が148mAh/gであり、動作電圧が3.5Vの範囲を有する二次電池の陽極活物質である。特に、環境的な安定性が高く、他の陽極活物質に比べて安価であるため、ハイブリッド自動車用陽極活物質としても活用されている。
ポリビニルピロリドン(PVP)、ジメチルホルムアミド(DMF)、白金前駆体として塩化白金酸六水和物(H2PtCl6・6H2O)を利用して白金(Pt)ナノ粉末及びナノインクを製造した。
実施例4により製造されたLiMn2O4ナノ繊維を1〜10mmのジルコニアボールを利用して粉砕した場合、マイクロロッド状のクラスターを製造することができる。マイクロロッドは、平均サイズが5〜100nmのナノ粒子からなり、幅が50〜3000nmであり、前記幅に対する長さの比であるアスペクト比が1.5〜200の範囲であることを特徴とする。
実施例1で2時間のマイクロビーズミル過程を経て製造されたSrTiO3インクをエレクトロスプレーして薄膜を製造した。
11a ナノ粒子
11b ナノクラスター
12 溶媒
13 高分子
Claims (25)
- 高分子を含有する溶液に金属、非金属、金属酸化物、金属化合物、非金属化合物、及び複合金属酸化物からなる群から選択される1種以上を形成できる前駆体1種以上を添加して紡糸溶液を調製する段階と、
前記紡糸溶液を紡糸して高分子及び1種以上の前駆体を含む複合繊維ウェブを製造する段階と、
前記複合繊維ウェブを、空気、還元雰囲気、脱酸素雰囲気(N2/H2、CO、N2)、不活性ガス(Ar)雰囲気、又は真空雰囲気で300〜900℃の温度で熱処理して、前記高分子を分解し、そして前記紡糸された前駆体を結晶化又は非晶質化して、金属、非金属、金属酸化物、金属化合物、非金属化合物、及び複合金属酸化物からなる群から選択される1種以上のナノ粒子を含むナノ繊維を生成する段階と
前記ナノ繊維を粉砕して、直径が5〜100nmのナノ粒子、及び幅が5〜100nmであり、前記幅に対する長さの比であるアスペクト比が1.5〜10.0であるナノクラスターを含むナノ粉末を形成する段階と、
を含むことを特徴とするナノ粉末製造方法。 - 前記粉砕は、溶媒中で前記ナノ繊維に実施されるマイクロビーズ粉砕であることを特徴とする請求項1に記載のナノ粉末製造方法。
- 前記マイクロビーズ粉砕は、0.015〜0.1mmのジルコニアボールを利用して行うことを特徴とする請求項2に記載のナノ粉末製造方法。
- 前記溶媒は、水、エタノール、テトラヒドロフラン、N,N’−ジメチルホルムアミド、N,N’−ジメチルアセトアミド、N−メチルピロリドン、アセトニトリル、トルエン、クロロホルム、メチレンクロライド、ベンゼン、及びキシレンからなる群から1種以上選択されるものであることを特徴とする請求項2又は3に記載のナノインク製造方法。
- 前記金属は、Pt、Ni、Au、Fe、Co、Mo、In、Ir、Ag、Sn、Ti、Cu、Pd、及びRuからなる群から選択される少なくとも1つであることを特徴とする請求項1に記載のナノ粉末製造方法。
- 前記非金属はSiであり、前記金属化合物はSnPであり、前記非金属化合物はSiN及びSiOx(0<X<2)からなる群から選択される少なくとも1つであることを特徴とする請求項1に記載のナノ粉末製造方法。
- 前記金属酸化物は、SnO2、Al2O3、TiO2、Fe2O3、ZrO2、V2O5、CoO、Co3O4、CaO、MgO、CuO、ZnO、In2O3、NiO、MoO3、及びWO3からなる群から選択される2成分系金属酸化物、SnSiO3、Zn2SnO4、CoSnO3、Ca2SnO4、CaSnO3、ZnCo2O4、Co2SnO4、Mg2SnO4、Mn2SnO4、CuV2O6、NaMnO2、NaFeO2、LiCoO2、LiNiO2、SrTiO3、Li4Ti5O12、BaTiO3、及びLiMn2O4からなる群から選択される3成分系金属酸化物、LiFePO4、Li[Ni1/3Co1/3Mn1/3]O2、Li[Ni1/2Mn1/2]O2、LiNi1-xCoxO2、LiAl0.05Co0.85Ni0.15O2、La1-xSrxCoO3(0.1≦X≦0.9)、La0.8Sr0.2Fe0.8Co0.2O3、La1-xSrxMnO3(0.1≦X≦0.9)、及びLa1-xSrxFeO3(0.1≦X≦0.9)からなる群から選択される4成分系以上の金属酸化物であり、
前記複合金属酸化物は、Pt−RuO2、Au−RuO2、Pt-IrO2、Pt-TiO2、Pd-SnO2、Pd-TiO2、Ni−Y0.08Zr0.92O2、Ag−BaTiO3、Pt−LaNiO3、又はPt−Y0.08Zr0.92O2であることを特徴とする請求項1に記載のナノ粉末製造方法。 - 前記金属酸化物は、2種以上の金属酸化物を含み、2種以上の金属酸化物の固溶体、混合相、及び化合物から選択される少なくとも1つの微細構造を有することを特徴とする請求項1に記載のナノ粉末製造方法。
- 前記前駆体は、チタンプロポキシド、塩化ストロンチウム四水和物、硝酸リチウム、リチウムアセチルアセトネート、及び酢酸マンガン四水和物、シリコンテトラアセテート、塩化ルテニウム、酢酸スズ、塩化ニッケル、トリフェニルホスフィン、塩化ランタン七水和物、塩化白金酸六水和物(Chloroplatinic Acid Hexahydrate、H2PtCl6・6H2O)、塩化鉄、酢酸コバルト、酢酸アルミニウム、酢酸亜鉛、塩化バナジウム、塩化バリウム溶液、硫酸マグネシウム、及び酢酸銅からなる群から選択される1種以上であることを特徴とする請求項1に記載のナノ粉末製造方法。
- 前記紡糸は、エレクトロスピニング、メルトブローン紡糸、フラッシュ紡糸、又は静電メルトブローン紡糸を含むことを特徴とする請求項1に記載のナノ粉末製造方法。
- 前記ナノ繊維を粉砕した後、ナノ粒子及びナノクラスターを含む溶媒を常温又は高温で乾燥する段階をさらに含むことを特徴とする請求項2〜4のいずれか1項に記載のナノ粉末製造方法。
- 請求項1〜11のいずれか1項に記載の方法で製造されたナノ粉末を含むナノインクに、前記ナノ粉末の分散性又は粘度を調節するための添加剤を添加する段階を含むことを特徴とするナノインク製造方法。
- 前記添加剤は、ポリビニルアセテート、ポリウレタン、ポリエーテルウレタンを含むポリウレタン共重合体、セルロースアセテート、セルロース誘導体、ポリメチルメタクリレート(PMMA)、ポリメチルアクリレート(PMA)、ポリアクリル共重合体、ポリビニルアセテート共重合体、ポリビニルアルコール(PVA)、ポリフルフリルアルコール(PPFA)、ポリスチレン(PS)、ポリスチレン共重合体、ポリエチレンオキシド(PEO)、ポリプロピレンオキシド(PPO)、ポリエチレンオキシド共重合体、ポリプロピレンオキシド共重合体、ポリカーボネート(PC)、ポリビニルクロライド(PVC)、ポリカプロラクトン、ポリビニルピロリドン(PVP)、ポリビニルフルオライド、ポリビニリデンフルオライド共重合体、及びポリアミドからなる群から1種以上選択される分散剤であり、
前記セルロース誘導体は、セルロースアセテートブチレート又はセルロースアセテートプロピオネートであることを特徴とする請求項12に記載のナノインク製造方法。 - 前記分散剤は、前記ナノ粉末に対して0.1〜20重量%添加されることを特徴とする請求項13に記載のナノインク製造方法。
- 前記添加剤は、トリトンX−100、酢酸、セチルトリメチルアンモニウムブロマイド(CTAB)、イソプロピルトリスチタネート、及び3−アミノプロピルトリエトキシシランからなる群から1種以上選択される界面活性剤であることを特徴とする請求項12に記載のナノインク製造方法。
- 金属、非金属、金属酸化物、金属化合物、非金属化合物、及び複合金属酸化物からなる群から選択される1種以上のナノ粒子からなるナノ繊維から粉砕された、直径が5〜100nmのナノ粒子、及び幅が5〜100nmであり、前記幅に対する長さの比であるアスペクト比が1.5〜10.0であるナノクラスターを含むことを特徴とするナノ粉末。
- 前記ナノ繊維は、金属、非金属、金属酸化物、金属化合物、非金属化合物、及び複合金属酸化物からなる群から選択される1種以上を形成できる前駆体1種以上を結晶化又は非晶質化して形成されることを特徴とする請求項16に記載のナノ粉末。
- 前記ナノ繊維は、紡糸法により形成された前記1種以上の前駆体を熱処理して生成されることを特徴とする請求項16に記載のナノ粉末。
- 前記金属は、Pt、Ni、Au、Fe、Co、Mo、In、Ir、Ag、Sn、Ti、Cu、Pd、及びRuからなる群から選択される少なくとも1つであることを特徴とする請求項16に記載のナノ粉末。
- 前記非金属はSiであり、前記金属化合物はSnPであり、前記非金属化合物はSiN及びSiOx(0<X<2)からなる群から選択される少なくとも1つであることを特徴とする請求項16に記載のナノ粉末。
- 前記金属酸化物は、SnO2、Al2O3、TiO2、Fe2O3、ZrO2、V2O5、CoO、Co3O4、CaO、MgO、CuO、ZnO、In2O3、NiO、MoO3、及びWO3からなる群から選択される2成分系金属酸化物、SnSiO3、Zn2SnO4、CoSnO3、Ca2SnO4、CaSnO3、ZnCo2O4、Co2SnO4、Mg2SnO4、Mn2SnO4、CuV2O6、NaMnO2、NaFeO2、LiCoO2、LiNiO2、SrTiO3、Li4Ti5O12、BaTiO3、及びLiMn2O4からなる群から選択される3成分系金属酸化物、LiFePO4、Li[Ni1/3Co1/3Mn1/3]O2、Li[Ni1/2Mn1/2]O2、LiNi1-xCoxO2、LiAl0.05Co0.85Ni0.15O2、La1-xSrxCoO3(0.1≦X≦0.9)、La0.8Sr0.2Fe0.8Co0.2O3、La1-xSrxMnO3(0.1≦X≦0.9)、及びLa1-xSrxFeO3(0.1≦X≦0.9)からなる群から選択される4成分系以上の金属酸化物であり、
前記複合金属酸化物は、Pt−RuO2、Au−RuO2、Pt-IrO2、Pt-TiO2、Pd-SnO2、Pd-TiO2、Ni−Y0.08Zr0.92O2、Ag−BaTiO3、Pt−LaNiO3、又はPt−Y0.08Zr0.92O2であることを特徴とする請求項16に記載のナノ粉末。 - 請求項16〜21のいずれか1項に記載のナノ粉末と、
前記ナノ粉末の分散性又は粘度を調節するための添加剤と
を含むことを特徴とするナノインク。 - 前記添加剤は、ポリビニルアセテート、ポリウレタン、ポリエーテルウレタンを含むポリウレタン共重合体、セルロースアセテート、セルロース誘導体、ポリメチルメタクリレート(PMMA)、ポリメチルアクリレート(PMA)、ポリアクリル共重合体、ポリビニルアセテート共重合体、ポリビニルアルコール(PVA)、ポリフルフリルアルコール(PPFA)、ポリスチレン(PS)、ポリスチレン共重合体、ポリエチレンオキシド(PEO)、ポリプロピレンオキシド(PPO)、ポリエチレンオキシド共重合体、ポリプロピレンオキシド共重合体、ポリカーボネート(PC)、ポリビニルクロライド(PVC)、ポリカプロラクトン、ポリビニルピロリドン(PVP)、ポリビニルフルオライド、ポリビニリデンフルオライド共重合体、及びポリアミドからなる群から1種以上選択される分散剤であることを特徴とする請求項22に記載のナノインク。
- 前記分散剤は、前記ナノ粉末に対して0.1〜20重量%添加されることを特徴とする請求項23に記載のナノインク。
- 前記添加剤は、トリトンX−100、酢酸、セチルトリメチルアンモニウムブロマイド(CTAB)、イソプロピルトリスチタネート、及び3−アミノプロピルトリエトキシシランからなる群から1種以上選択される界面活性剤であることを特徴とする請求項22に記載のナノインク。
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