JPWO2017099250A1 - 粉末粒子及びこれを用いたグリーン体の製造方法 - Google Patents
粉末粒子及びこれを用いたグリーン体の製造方法 Download PDFInfo
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Abstract
Description
母粒子として平均粒径3μmのアルミナ粒子(AA−3、住友化学社製)、添加粒子として平均粒径0.4μmの非架橋アクリル粒子(MP2701、綜研化学社製)を用いた複合粒子を作製した。具体的には、ポリアニオン(高分子電解質;アニオン性高分子)であるポリスチレンスルホン酸ナトリウム(PSS)を溶解させた水溶液を、pH7.0に調整した後、アルミナ粒子を分散させ、10分間攪拌することでアルミナ表面にPSSを吸着させた。その後、アルミナ粒子を沈殿させ、上澄み液を除去した後に脱イオン水にて洗浄し、未吸着のPSSを取り除いた。次いで、得られたPSS被覆アルミナ粒子を、ポリカチオン(高分子電解質;カチオン性高分子)であるポリジアチルジメチルアンモニウムクロリド(PDDA)を溶解した水溶液中に投入し10分間攪拌することでアルミナ粒子の最表面にPDDAを吸着させた。その後、上記と同様、洗浄、分別操作によってPDDA被覆アルミナ粒子を回収した。PSSおよびPDDAを被覆する操作は複数回繰り返して行い、PSSと、PDDAを交互に積層させ、最外層をPSSとすることで表面電荷を負とした。
母粒子として平均粒径3μmのアルミナ粒子(AA−3、住友化学社製)、子粒子して平均粒径0.1μmのアルミナ粒子(大明化学社製、タイミクロンTM−DAR)、添加粒子として平均粒径0.4μmの非架橋アクリル粒子(MP2701、綜研化学社製)とを用いた複合粒子を作製した。
平均粒径3μmのアルミナ粒子(AA−3、住友化学社製)の重量に対し、市販のバインダー(ポリビニルアルコール系、セレナWF−804、中京油脂株式会社製)が3wt%となる配合比で、アルミナ粒子とバインダーとをそれぞれ蒸留水に混合して懸濁液を作製した。その後、作製した懸濁液を、凍結乾燥機(EYELA社製、FDU−1200)により混凍結乾燥させて粉末粒子を得た。比較例1で用いたバインダーは液状であり、これにより、得られた粉末粒子は、アルミナ粒子がバインダーでコーティングされたものとなっている。
各実施例1、2および比較例1で得られた粉末粒子を用いたグリーン体について、インデンテーション法を用いて硬度を測定することで、強度の比較を行った。インデンテーション試験は、ビッカース硬度計(AVK−A、明石製作所製)を用い、最大圧入荷重1.5Nとし、最大荷重で形成した圧痕寸法から算出されるビッカース硬度を算出した。
母粒子の表面に樹脂粒子を担持させて複合化した粉末粒子を使用し、これによりグリーン体を形成したときの強度ムラについて実験を行った。その結果を以下に説明する。
(複合粒子による試料の作製)
実施例1と同様の方法により、樹脂粒子の添加量が異なる二種類の試料を作成した。母粒子としては平均粒径3μmのアルミナ粒子(AA−3、住友化学社製)を、添加粒子としては平均粒径0.4μmの非架橋アクリル粒子(MP2701、綜研化学社製)を用いて、母粒子に対する添加粒子の割合を1W%および3W%として、それぞれ複合粒子を作製した。
平均粒径3μmのアルミナ粒子(AA−3、住友化学社製)に、市販のバインダー(ポリビニルアルコール系、セレナWF−804、中京油脂株式会社製)を添加して二種類の比較試料を作製した。具体的には、アルミナ粒子の重量に対しバインダーが1W%および3wt%となる配合比で、アルミナ粒子とバインダーとをそれぞれ蒸留水に混合して二種類の懸濁液を作製した。その後、作製した二種類の懸濁液を、凍結乾燥機(EYELA社製、FDU−1200)により混凍結乾燥させて二種類の粉末粒子を得た。比較試料の作製に用いたバインダーは液状であり、これにより、得られた粉末粒子は、アルミナ粒子がバインダーでコーティングされたものとなっている。
四つの各試料(複合粒子による試料二種類および比較試料二種類)で得られた粉末粒子を用いたグリーン体について、インデンテーション法を用いて圧入荷重と圧入深さとの関係を各三点で測定した。具体的には、自作の圧入荷重と圧入深さを測定できる計装型インデンテーション装置を用いて、最大圧入荷重1.5Nとし、ビッカース圧子を用いた圧入荷重と圧入深さを測定した。これを異なる三点について行った。各測定結果をプロットし、グラフ化したものを図8および図9に示す。図は横軸が圧入深さ(検査針の圧入深度(μm))であり、縦軸が圧入荷重(荷重(N)の平方根)としている。なお、図8は、母粒子に対する樹脂粒子またはバインダーの割合を1W%としたものに関するグラフであり、図8(a)が複合粒子による試料、図8(b)が比較試料の結果である。また、図9は、母粒子に対する樹脂粒子またはバインダーの割合を3W%としたものに関するグラフであり、図9(a)が複合粒子による試料、図9(b)が比較試料の結果である。
2 樹脂粒子(熱可塑性樹脂粒子)
3 高分子電解質
4 子粒子
10,20 複合粒子(複合粒子、粉末粒子)
S2 子粒子複合化工程(前複合化工程)
S3 樹脂粒子複合化工程(複合化工程)
S5 成形工程(グリーン体成形工程の一部)
S7 熱処理工程(グリーン体成形工程の一部)
S10 母粒子電荷調整工程(第1表面電荷調整工程)
S20 樹脂粒子電荷調整工程(第2表面電荷調整工程)
S30 子粒子電荷調整工程(子粒子表面電荷調整工程)
Claims (15)
- 焼結体の主たる成分となる母粒子と、その母粒子よりも粒径が小さく、且つ、前記母粒子の表面上に担持された熱可塑性樹脂粒子とを備えた粉末粒子であって、前記熱可塑性樹脂粒子は前記母粒子に対し予め定めた体積比の範囲で前記母粒子の表面上に点在し、且つ、前記熱可塑性樹脂粒子が溶融した場合に隣接する母粒子間の接点周縁領域に樹脂溜まり部が形成されるような態様で前記母粒子に担持されていることを特徴とする粉末粒子。
- 前記熱可塑性樹脂粒子は、前記母粒子に対し体積比で2%以上5%以下の範囲にあることを特徴とする請求項1記載の粉末粒子。
- 前記母粒子に担持される前記熱可塑性樹脂粒子は、該母粒子の個々の表面上に4個以上120個以下であることを特徴とする請求項1記載の粉末粒子。
- 易焼結性または焼結助剤の機能を有し前記母粒子よりも粒径の小さな子粒子が前記母粒子の表面に付着しているものであることを特徴とする請求項1から3のいずれかに記載の粉末粒子。
- 前記子粒子の平均粒径は150nm以下であることを特徴とする請求項4記載の粉末粒子。
- 前記母粒子の平均粒径は500nm以上5μm以下であることを特徴とする請求項4または5に記載の粉末粒子。
- 前記母粒子の表面は、該母粒子の表面全体に対して40%以上100%以下の被覆率によって前記子粒子により被覆されていることを特徴とする請求項4から6のいずれかに記載の粉末粒子。
- 前記熱可塑性樹脂粒子は、その一部または全部が、前記母粒子の表面に付着する前記子粒子を介して前記母粒子上に担持されると共に、前記母粒子の表面上に点在する態様に配置されていることを特徴とする請求項4から7のいずれかに記載の粉末粒子。
- 前記母粒子、前記子粒子、前記熱可塑性樹脂粒子は、それぞれその表面に高分子電解質を有しており、その高分子電解質を介して他の粒子と接するものであることを特徴とする請求項4から8のいずれかに記載の粉末粒子。
- 前記各粒子が具有する前記高分子電解質の厚みは20nm以下であることを特徴とする請求項9記載の粉末粒子。
- 請求項1から10のいずれかに記載の粉末粒子を用いて、グリーン体を造形すると共に当該グリーン体に含まれる熱可塑性樹脂粒子が溶融する温度以上で加熱した後冷却してグリーン体を成形するグリーン体成形工程を備えたことを特徴とするグリーン体の製造方法。
- 焼結体の主たる成分となる母粒子の表面電荷を液体中において調整する第1表面電荷調整工程と、
その第1表面電荷調整工程で処理された前記母粒子に、当該母粒子よりも小さな粒径の熱可塑性樹脂粒子を静電引力の作用で付着させるため、液体中で前記熱可塑性樹脂粒子の表面電荷を調整する第2表面電荷調整工程と、
前記第1表面電荷調整工程での処理を経た前記母粒子と、前記第2表面電荷調整工程で処理された前記熱可塑性樹脂粒子とを、液体中で混合し静電引力によって複合化して複合粒子を作製する複合化工程と、
その複合化工程によって得られた前記複合粒子を用いてグリーン体を造形すると共に当該グリーン体に含まれる熱可塑性樹脂粒子が溶融する温度以上で加熱した後冷却してグリーン体を成形するグリーン体成形工程とを備えたことを特徴とするグリーン体の製造方法。 - 易焼結性または焼結助剤の機能を有し前記母粒子よりも粒径の小さな子粒子を、前記第1表面電荷調整工程で処理された前記母粒子が有する表面電荷と反対極性となるように、液体中で当該子粒子の表面電荷を調整する子粒子表面電荷調整工程と、
その子粒子表面電荷調整工程にて処理を行った前記子粒子と、前記第1表面電荷調整工程で処理された前記母粒子とを液体中で混合して静電引力によって複合化して母粒子と子粒子との複合粒子を作製する前複合化工程とを備え、
前記第2表面電荷調整工程は、前記前複合化工程で作製される複合粒子の表面電荷と反対極性となるように、液体中で前記熱可塑性樹脂粒子の表面電荷を調整するものであり、
前記複合化工程は、前記前複合化工程によって作製された母粒子と子粒子との複合粒子と、前記第2表面電荷調整工程にて処理を行った前記熱可塑性樹脂粒子とを更に複合化するものであることを特徴とする請求項12記載のグリーン体の製造方法。 - 易焼結性または焼結助剤の機能を有し前記母粒子よりも粒径の小さな子粒子を、前記第1表面電荷調整工程で処理された前記母粒子が有する表面電荷と反対極性となるように、液体中で当該子粒子の表面電荷を調整する子粒子表面電荷調整工程と、
その子粒子表面電荷調整工程にて処理を行った前記子粒子と、前記第1表面電荷調整工程で処理された前記母粒子とを液体中で混合して静電引力によって複合化して母粒子と子粒子との複合粒子を作製する前複合化工程と、
前記前複合化工程により作製された母粒子と子粒子との複合粒子について、該複合粒子の表面電荷を更に調整する表面電荷再調整工程を備え、
前記第2表面電荷調整工程は、前記表面電荷再調整工程で調整された複合粒子の表面電荷と反対極性となるように、液体中で前記熱可塑性樹脂粒子の表面電荷を調整するものであり、
前記複合化工程は、前記表面電荷再調整工程によって処理された複合粒子と、前記第2表面電荷調整工程にて処理を行った前記熱可塑性樹脂粒子とを更に複合化するものであることを特徴とする請求項12記載のグリーン体の製造方法。 - 前記グリーン体成形工程は、前記複合化工程で得られた前記複合粒子が分散されたスラリーを用いて前記グリーン体の造形を行った後に、乾燥を実施してから、熱可塑性樹脂粒子が溶融する温度以上で加熱することを特徴とする請求項12から14のいずれかに記載のグリーン体の製造方法。
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