JP2022084725A - 焼結体の製造方法、構造体および複合構造体 - Google Patents
焼結体の製造方法、構造体および複合構造体 Download PDFInfo
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- JP2022084725A JP2022084725A JP2022036068A JP2022036068A JP2022084725A JP 2022084725 A JP2022084725 A JP 2022084725A JP 2022036068 A JP2022036068 A JP 2022036068A JP 2022036068 A JP2022036068 A JP 2022036068A JP 2022084725 A JP2022084725 A JP 2022084725A
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- metal oxide
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- spinel
- sintered body
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- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
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Abstract
Description
スピネル型構造を有する金属酸化物の複数の粒子と金属アセチルアセトネートとを混合して混合物を作製する工程と、
前記混合物を、加圧下にて、前記金属アセチルアセトネートの融点以上かつ600℃以下の温度で加熱する工程と、を含む、
焼結体の製造方法が提供される。
前記アモルファス相は、1種以上の金属元素を含む、
構造体が提供される。
前記金属酸化物の複数の第2粒子の粒径は、前記金属酸化物の複数の第1粒子の粒径よりも小さく、
前記金属酸化物の複数の第2粒子が、前記金属酸化物の複数の第1粒子を粒子毎に囲うように存在し、
前記アモルファス相が、前記金属酸化物の複数の第1粒子と、前記金属酸化物の複数の第2粒子との間に介在し得る。
前記アモルファス相が、前記金属酸化物の複数の第1粒子と、前記金属材料、樹脂材料および炭素材料のうち少なくとも1つの材料の複数の粒子との間に介在し得る。
第2の要旨に記載の構造体と、
前記基材と前記構造体との間に位置する接合層と、を含み、
前記接合層は、前記金属酸化物の複数の第1粒子と、前記基材に含まれる1種以上の元素と同じ種類の元素と、前記金属酸化物の複数の第1粒子の間に介在するアモルファス相と、を含む、
複合構造体が提供される。
表2の実施例1-1を参照して、スピネル型構造を有する金属酸化物の複数の粒子としてZn0.5Ni0.5Fe2O4の組成を有する金属酸化物の粒子0.5gを乳鉢に入れ、金属アセチルアセトネートを当該粒子の全重量に対して1wt%(0.005g)で、更に水を当該粒子の全重量に対して10wt%(0.05g)で添加して、乳棒でよく混合した。金属アセチルアセトネートは、Zn(acac)2とNi(acac)2とFe(acac)3とを、Zn:Ni:Feのモル比が、当該粒子の金属酸化物中における化学量論比0.5:0.5:2に一致し、かつ、それら金属アセチルアセトネートの合計が当該粒子の全重量に対して1wt%となるように調製した。これにより、スピネル型構造を有する金属酸化物の複数の粒子と金属アセチルアセトネートと水とを含む原料混合物を調製した。得られた原料混合物を、一般的に加圧成型に用いられている直径7mmの金型に充填し、金型に充填された原料混合物をプレス機により上下の加熱板で挟んで500MPaまで加圧した。金型に充填された原料混合物を挟んでいる上下の加熱板の温度を300℃まで高めることにより原料混合物を加熱した。これら圧力および温度にて30分経過した後に加熱を終了し、自然空冷して、100℃以下になった焼結体を金型から取り出して評価を行った。
表3の比較例1-1を参照して、スピネル型構造を有する金属酸化物の複数の粒子としてZn0.5Ni0.5Fe2O4の組成を有する金属酸化物の粒子0.5gを、これに金属アセチルアセトネートおよび水を添加せずに、そのまま原料として用いたこと以外は、実施例1-1と同様の方法で焼結体(圧粉体)を得た。更に、表3の比較例1-2~1-5を参照して、スピネル型構造を有する金属酸化物の複数の粒子としてZn0.5Ni0.5Fe2O4の組成を有する金属酸化物の粒子0.5gを乳鉢に入れ、各種溶媒を当該粒子が粘土状になる程度(当該粒子の全重量に対して約10wt%(0.05g))で添加して、乳棒でよく混合した。比較例1-2~1-5では、溶媒としてそれぞれ1Mの酢酸水溶液、0.5MのEDTA水溶液、アセチルアセトンおよび0.4Mのゾルゲル水溶液を使用した。0.4Mのゾルゲル水溶液は、0.4MのNi(NO3)2水溶液と0.8MのFe(NO3)2水溶液と水とから調製した。比較例1-6では、溶媒として実施例1-2と同じ金属アセチルアセトネートと水とを使用した。これにより、スピネル型構造を有する金属酸化物の複数の粒子と溶媒とを含む原料混合物を調製した。得られた原料混合物を用いて、焼結温度を表3に示すように適宜変更した(溶媒の沸点以上または溶媒に含まれる成分の融点以上の温度とした)こと以外は、実施例1-1と同様の方法により焼結体を得た。得られた焼結体を上記と同様に評価した。結果を表3に示す。
表4の実施例2-1を参照して、スピネル型構造を有する金属酸化物の複数の粒子としてNiMn2O4(MNO)の組成を有する金属酸化物の粒子0.5gを乳鉢に入れ、金属アセチルアセトネートを当該粒子の全重量に対して10wt%(0.05g)で、更に水を当該粒子の全重量に対して10wt%(0.05g)で添加して、乳棒でよく混合した。金属アセチルアセトネートは、Ni(acac)2とMn(acac)3とを、Ni:Mnのモル比が、当該粒子の金属酸化物中における化学量論比1:2に一致し、かつ、それら金属アセチルアセトネートの合計が当該粒子の全重量に対して10wt%となるようにして添加した。これにより、スピネル型構造を有する金属酸化物の複数の粒子と金属アセチルアセトネートと水とを含む原料混合物を調製した。得られた原料混合物を用いて、実施例1-1と同様の方法により焼結体を得た。表4の比較例2-1を参照して、スピネル型構造を有する金属酸化物の複数の粒子としてNiMn2O4(MNO)の組成を有する金属酸化物の粒子0.5gを、これに金属アセチルアセトネートを添加せずに、そのまま原料として用いたこと以外は、実施例2-1と同様の方法で焼結体(圧粉体)を得た。
表5の実施例3-1を参照して、磁性材料である3%Si含有Fe0.9gとスピネル型構造を有する金属酸化物の複数の粒子としてZn0.5Ni0.5Fe2O4の組成を有する金属酸化物の粒子0.1gとを乳鉢に入れ、金属アセチルアセトネートを金属酸化物の粒子の全重量に対して10wt%(0.01g)で、更に水を金属酸化物の粒子の全重量に対して10wt%(0.01g)で添加して、乳棒でよく混合した。金属アセチルアセトネートは、Zn(acac)2とNi(acac)2とFe(acac)3とを、Zn:Ni:Feのモル比が、当該粒子の金属酸化物中における化学量論比0.5:0.5:2に一致し、かつ、それら金属アセチルアセトネートの合計が当該粒子の全重量に対して10重量%となるように調製した。これにより、スピネル型構造を有する金属酸化物の複数の粒子と金属アセチルアセトネートと水とを含む原料混合物を調製した。得られた原料混合物を用いて、実施例1-1と同様の方法により焼結体を得た。焼結体の理論密度の計算の課程において、LiNi0.5Mn1.5O4の理論密度は、文献値である5.2g/cm2を採用し、鉄の理論密度は純Feの文献値である7.874g/cm2を採用した。結果を表5に示す。
下記表6に示すように、実施例4-1では、実施例2-1と同様かつ同量の原料を用いて同様の条件下の手順による方法で、スピネル型構造を有する金属酸化物の複数の粒子(NiMn2O4(MNO)0.5g)と金属アセチルアセトネート(Ni(acac)2とMn(acac)310wt%(0.05g))を含む原料混合物を調製した。これに、適量の有機溶媒を添加してよく混合して、ペースト状の原料混合物を調製した。得られたペースト状の原料混合物を、厚さ10μmのポリイミドの基材上にスクリーン印刷した。ペースト状の原料混合物が印刷されたポリイミドの基材を、オーブンを用いて100℃で24時間乾燥させて有機溶媒を蒸発させ、その後加湿雰囲気下で30分間放置することによって水分を含ませた。これを、プレス機により300℃に設定された上下の加熱板で挟んで500MPaで加圧した。このようにして金属酸化物を含む構造体とポリイミドの基材とを含む複合構造体を得た。
実施例4-1で作製した複合構造体の薄片の試料を用いて、その電子線回折像に基づいて、アモルファス相とスピネル型構造を有する金属酸化物の粒子とを区別して観察した。図7A~図7Dに示す試料分析箇所のうち、C(図7B参照)や金属元素(Mn)(図7D参照)を含む部分の電子線回折像では、図11Aに示すように、回折スポット(ドット)は観測されなかった。そのため、このような部分は結晶構造を持たないアモルファス相であることがわかる。一方、原料混合物由来と考えられる金属酸化物の粒子の金属元素のみ(Mn)(図7D参照)を含む部分の電子回折像では、図11Bに示すように、スピネル型構造の結晶対称性に従った回折スポット(ドット)が得られた。そのため、このような部分は単結晶であることがわかる。より詳細には、ブラッグの法則より、回折スポット(ドット)の現れる位置は結晶構造によって決定する。結晶面間隔から透過光からの距離が決まり、各方位から透過光と各回折スポット(ドット)を結んだ直線がなす角が決まる。従って、電子線回折像の最も黒い部分と最も白い部分のちょうど中間を閾値として2値化して、結晶構造から考慮される位置に白い点が存在すれば単結晶と判別され(図11B参照)、原点を中心とする白い点のみが存在すればアモルファス相と判別される(図11A参照)。なお、スピネル型構造を有する金属酸化物の粒子の確認方法は、スピネル型構造については、例えばF. S. Galasso著「図解ファインセラミックスの結晶化学」(アグネ技術センター、1984年)において、結晶対称性については、例えば今野豊彦著「物質の対称性と群論」(共立出版、2001年)において、アモルファスの電子線回折像に関しては、例えば今野豊彦著「物質からの回折と結像」(共立出版、2003年)において各々説明されている当業者に公知の技術である。
2、2’ アモルファス相
11 大粒子
12 小粒子
13 基材含有元素
100 構造体
200 接合層
300 基材
Claims (16)
- スピネル型構造を有する金属酸化物を含む焼結体の製造方法であって、
スピネル型構造を有する金属酸化物の複数の粒子と金属アセチルアセトネートとを混合して混合物を作製する工程と、
前記混合物を、加圧下にて、前記金属アセチルアセトネートの融点以上かつ600℃以下の温度で加熱する工程と、を含む、
焼結体の製造方法。 - 前記混合物を流体の存在下で加熱する、請求項1に記載の方法。
- 前記流体が前記混合物に混合されている、請求項2に記載の方法。
- 前記金属アセチルアセトネートが、前記金属酸化物に含まれる1種以上の金属元素と同じ種類の金属元素を含む、請求項1~3のいずれか一項に記載の方法。
- 前記混合物が、金属材料、樹脂材料および炭素材料のうち少なくとも1つを更に含む、請求項1~4のいずれか一項に記載の方法。
- 前記金属酸化物がフェライトである、請求項1~5のいずれか一項に記載の方法。
- 前記金属酸化物がNiおよびMnを含む、請求項1~6のいずれか一項に記載の方法。
- スピネル型構造を有する金属酸化物の複数の第1粒子と、前記金属酸化物の複数の第1粒子の間に介在するアモルファス相と、を含み、
前記アモルファス相は、1種以上の金属元素を含む、
構造体。 - 前記1種以上の金属元素は、前記金属酸化物に含まれる1種以上の金属元素と同じ種類の金属元素である、請求項8に記載の構造体。
- スピネル型構造を有する金属酸化物の複数の第2粒子を更に含み、
前記金属酸化物の複数の第2粒子の粒径は、前記金属酸化物の複数の第1粒子の粒径よりも小さく、
前記金属酸化物の複数の第2粒子が、前記金属酸化物の複数の第1粒子を粒子毎に囲うように存在し、
前記アモルファス相が、前記金属酸化物の複数の第1粒子と、前記金属酸化物の複数の第2粒子との間に介在している、
請求項8または9に記載の構造体。 - 金属材料、樹脂材料および炭素材料のうち少なくとも1つの材料の複数の粒子を更に含み、
前記アモルファス相が、前記金属酸化物の複数の第1粒子と、前記金属材料、樹脂材料および炭素材料のうち少なくとも1つの材料の複数の粒子との間に介在している、
請求項8~10のいずれか一項に記載の構造体。 - 前記金属酸化物がフェライトである、請求項8~11のいずれか一項に記載の構造体。
- 前記金属酸化物がNiおよびMnを含む、請求項8~12のいずれか一項に記載の構造体。
- 金属材料、樹脂材料および炭素材料のうち少なくとも1つの材料を含む基材と、
請求項8~13のいずれか一項に記載の構造体と、
前記基材と前記構造体との間に位置する接合層と、を含み、
前記接合層は、前記金属酸化物の複数の第1粒子と、前記基材に含まれる1種以上の元素と同じ種類の元素と、前記金属酸化物の複数の第1粒子の間に介在するアモルファス相と、を含む、
複合構造体。 - 前記接合層の前記アモルファス相は、前記金属酸化物に含まれる1種以上の金属元素と同じ種類の金属元素を含む、請求項14に記載の複合構造体。
- 前記基材は、ポリイミドおよびポリエチレンテレフタラートの少なくとも1つを含む、請求項15に記載の複合構造体。
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EP3608298A1 (en) | 2020-02-12 |
EP3608298A4 (en) | 2020-12-30 |
US20200139442A1 (en) | 2020-05-07 |
CN110997594A (zh) | 2020-04-10 |
JP7318756B2 (ja) | 2023-08-01 |
JPWO2019009320A1 (ja) | 2020-04-23 |
CN110997594B (zh) | 2022-10-04 |
WO2019008711A1 (ja) | 2019-01-10 |
JP7040525B2 (ja) | 2022-03-23 |
WO2019009320A1 (ja) | 2019-01-10 |
US20200139441A1 (en) | 2020-05-07 |
US11607728B2 (en) | 2023-03-21 |
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