JP2021523253A - 組成物を形成する方法及びそれから形成される組成物 - Google Patents
組成物を形成する方法及びそれから形成される組成物 Download PDFInfo
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Abstract
Description
一態様では、組成物を作製する方法であって、この方法は、ポリマー及び溶媒を含有する溶媒混合物を形成する工程と、非溶媒によって溶媒混合物を沈殿させて、フィブリル化ポリマーマトリクス中にフィラーを含む組成物を形成する工程であって、組成物は粒子の形態にあり、溶媒及び非溶媒の少なくとも1つはフィラーを含む、組成物を形成する工程と、組成物を溶媒及び非溶媒から分離して、組成物を単離する工程とを備える。
以下の図は例示的な態様であり、本開示を説明するために提供されている。これらの図は、本発明に従って製造されたデバイスを、本明細書に記載の材料、条件、又はプロセスパラメータに限定することを意図していない実施例を例示するものである。
理論に束縛されることを意図せずに、組成物を形成するときに、ポリマー分子が、他の隣接するポリマー分子との伸長、絡み合い、又は相互侵入がほとんどなく、リコイル又は崩壊して高密度のコイル状構造に戻ることができる場合、ポリマーは活性物質を含むさまざまなフィラーの結合効果が低く、構造的完全性が十分でない可能性がある。理想的な状況は、粒子状物質(例えば、不活性フィラー又は活性バッテリー電極材料)及び隣接する伸長ポリマー鎖の両方とより完全に伸長及び絡み合っているポリマーを含む組成物又は他のフィルムを作成することであることが見出された。理論に拘束されることなく、隣接するポリマー鎖と、また粒子状物質(粉末、繊維、フレーク、凝集体など)の塊全体に伸びて絡み合う単一の「糸」として本質的に展開される単一のポリマー鎖は、粒子を捉え、粒子を露出させ、互いに密接に接触させ続けるための最大の捕捉(すなわち、構造安定性)を提供すると考えられている(それぞれ、イオン速度及び電子速度の能力が向上している)。
沈殿物は、液相から単離されたものとして、例えば、粒子形態で使用することができ、又は分離された沈殿物は、その後、層に形成することができる。層は、沈殿物を基板(例えば、平坦な基板)上に堆積させ、沈殿物を乾燥させて、残っている溶媒及び非溶媒を除去することによって形成することができる。層を形成することは、熱成形、カレンダー加工、積層、ロールコーティング、又は他の方法のうちの少なくとも1つを含むことができる。複数の層は、析出物を順次堆積して複数の層を一度に成形することによって、又は各堆積後に成形することによって形成することができる。
ポリマーは、フルオロポリマー(例えば、ポリフッ化ビニリデン(PVDF))、アクリルポリマー、ポリオレフィン、ポリアクリロニトリル、ナイロン、ポリエステル、ポリアミド、ポリエーテル、ゴム、ポリ(塩化ビニル)、ポリ(酢酸ビニル)、ポリ(ビニルアルコール)、ポリ(ビニルピロリドン)、又はシランのうちの少なくとも1つを含むことができる。 ポリマーが疎水性ポリマー(例えば、フルオロポリマー)を含む場合、溶媒は、アセトンなどの疎水性溶媒を含むことができ、非溶媒は、水などの親水性非溶媒を含むことができる。ポリマーが親水性ポリマー(例えば、ポリ(ビニルアルコール))を含む場合、溶媒は、水などのプロトン性又は極性溶媒を含むことができ、非溶媒は、アセトンなどの非極性非溶媒を含むことができる。
実施例1:相反転技術を使用したアノードの作製
非溶媒として水を使用する相反転技術を使用して多孔質カーボンブラック−PVDFアノード(C−PVDF)を作製した。1グラムのPVDFを42.5グラムのアセトンに溶解した。19グラムのカーボンブラックをPVDF混合物に添加し、シルバーソンミキサーを用いて毎分10回転で混合して溶媒混合物を形成した。溶媒混合物の一部を、ピペットを介して溶媒混合物を水中に迅速に噴出させ、すべての溶媒混合物が沈殿するまで沈殿物を濾過することにより、25ミリリットルの水に注入した。注入している間、攪拌棒を用いて活発に水を攪拌した。PVDFはカーボンブラックの存在下でフィブリル化し、組成物を形成した。コーヒーフィルターに注ぐことにより濾過を行った。沈殿物を摂氏90度(℃)で乾燥させてアセトンと水を除去し、沈殿物を圧縮して厚さ2ミリメートルの自立マットを形成した。次にマットを130℃で再度乾燥させた。
米国特許第8,147,732号に従って異なる相反転プロセスによって非充填ポリマー膜及び充填ポリマー膜を調製した。走査型電子顕微鏡画像が撮影され、それぞれ図4,5に示されている。図4は、多孔質材料の形成を示している。図5は、フィラーがポリマーで完全に覆われていること、つまり、フィラーの表面積が露出していないことを示している。
実施例1の相反転後の、溶媒及び非溶媒中に存在する沈殿物のある組成物の写真を撮影した。ここで、フィラー対PVDF重量比は95:5であり、水対アセトンの重量比は90:10であった。上面図と側面図をそれぞれ図6A1と図6A2に示す。図6A1は、皿の端又は溶液の表面にフィラーがないことを示している。図6A2は、皿中央にある溶媒/非溶媒の透明な層によって示されるように、フィラーが沈殿物中にあることを示している。これらの2つの図は、カーボンフィラーが実際にPVDFポリマーに結合していることを示している。
1グラムのPVDFを42.5グラムのアセトンに溶解し、19gの塩化ナトリウムを加えて、周囲温度(約23℃)で混合することにより溶媒混合物を形成した。溶媒混合物の一部を、ピペットを介して溶媒混合物を水中に迅速に噴出させ、すべての溶媒混合物が沈殿するまで沈殿物を濾過することにより、25ミリリットルの水に注入した。PVDFは塩の結晶の存在下でフィブリル化し、組成物を形成した。コーヒーフィルターに注ぐことにより濾過を行った。塩を洗い流して、塩を含まないフィブリル化PVDFを得た。フィブリル化されたPVDFを90℃で乾燥させてアセトン及び水を除去し、フィブリル化されたPDVFを圧縮して自立マットを形成した。次にマットを130℃で再度乾燥させた。塩の存在なしに同じプロセスを実行し、フィブリルを形成することなく溶液からPVDFを沈殿させた。
実施例5:ポリ(ビニルアルコール)組成物の形成
0.5グラムのポリ(ビニルアルコール)を20グラムの水に溶解し、4.25グラムの二酸化チタンと0.25グラムの二酸化ケイ素をフィラーとして追加し、溶媒組成物を、非溶媒としての3グラムのアセトンに加えたことを除いて、実施例1に従ってポリ(ビニルアルコール)組成物を調製した。 相反転組成物が形成された。
0.25グラムのポリ(ビニルアルコール−ヘキサフルオロプロピレン)を20グラムのアセトンに溶解し、4.75グラムのカーボンブラックをフィラーとして追加し、溶媒組成物を、非溶媒としての3グラムのイソプロパノールに加えたことを除いて、実施例1に従ってPVDF−HPF組成物を調製した。 ポリマー:カーボンブラックの重量比を0.25:4.75から、0.5:4.5及び0.75:4.25グラムまで変化させて、このプロセスを繰り返した。相反転組成物が形成された。
0.5グラムのポリスチレンを20グラムのキシレンに溶解し、5グラムの活性炭をフィラーとして追加し、溶媒組成物を非溶媒としての3グラムの水に加えたことを除いて、実施例1に従ってポリスチレン組成物を調製した。 相反転組成物が形成された。
0.75グラムのポリ(アミド−イミド)を20グラムのDMACに溶解し、5グラムの六方晶窒化ホウ素をフィラーとして添加し、溶媒組成物を、非溶媒としてのエチレングリコール3グラムに加えたことを除いて、実施例1に従ってポリ(アミド−イミド)組成物を調製した。相反転組成物が形成された。
態様1: 一態様では、組成物を作製する方法であって、この方法は、ポリマー及び溶媒を含有する溶媒混合物を形成する工程と、非溶媒によって溶媒混合物を沈殿させて、フィブリル化ポリマーマトリクス中にフィラーを含む組成物を形成する工程であって、組成物は粒子の形態にあり、溶媒及び非溶媒の少なくとも1つはフィラーを含む、組成物を形成する工程と、組成物を溶媒及び非溶媒から分離して、組成物を単離する工程とを備えることを要旨とする。
態様12: 組成物がフィラーのタップ密度以上の多孔性の少なくとも1つを有し、組成物が0.05〜10ミリメートル、又は2.5〜5ミリメートルの厚さを有する層の形態であり、又は組成物が自立型である、態様11の組成物を要旨とする。
態様14: 態様1〜10のいずれか1つ以上の方法によって製造される多孔質材料であって、溶媒及び非溶媒を除去した後、フィラー粒子がポリマーによって機械的に一緒に結合され、フィラメントがフィラー粒子に付着し、フィラー粒子間の隙間空間を横切ってフィラー粒子を結合するようにポリマーが存在し、それぞれのフィラー粒子は1つ以上の他の粒子とのフィラメントで結合するように結合している、多孔質材料を要旨とする。
「上記の少なくとも1つを含む組み合わせ」又は「少なくとも1つの」との用語は、リストに各要素が個別に含まれること、及びリストの2つ以上の要素の組み合わせや、リストの少なくとも1つの要素とリストに記載されない同様の要素の組み合わせが含まれることを意味する。また、「組み合わせ」という用語は、ブレンド、混合物、合金、反応生成物などを含む。
引用されたすべての特許、特許出願、及びその他の参考文献は、参照によりその全体が本明細書に組み込まれる。しかしながら、本出願における用語が、組み込まれた参考文献における用語と矛盾又は矛盾する場合、本出願からの用語は、組み込まれた参考文献からの矛盾する用語よりも優先される。
Claims (20)
- 組成物を作製する方法であって、
ポリマーと溶媒とを含んでなる溶媒混合物を形成する工程と、
非溶媒によって前記溶媒混合物を沈殿させて、フィブリル化ポリマーマトリクス中にフィラーを含む組成物を形成する工程であって、前記組成物は粒子の形態にあり、前記溶媒及び前記非溶媒の少なくとも1つはフィラーを含む、組成物を形成する工程と、
前記組成物を前記溶媒及び前記非溶媒から分離して、組成物を単離する工程とを備える、方法。 - 前記組成物は、
75重量パーセント以上のフィラーと、
1〜25重量パーセントのフィブリル化ポリマーマトリクスとを含み、
重量は、前記組成物の総重量からあらゆる溶媒を差し引いたものに基づき、あるいは、前記溶媒混合物が、前記溶媒混合物の総重量に対して、50〜95重量パーセント以上の溶媒を含む、請求項1に記載の方法。 - 溶媒及び非溶媒の少なくとも一方が、アセトン、シクロヘキサノン、ジメチルアセトアミド、メチルエチルケトン、N,N−ジメチルホルムアミド、ジメチルスルホキシド、N−メチルピロリドン、テトラヒドロフラン、テトラメチル尿素、又はリン酸トリメチルのうちの少なくとも1つを含み、
溶媒及び非溶媒の他方は、酸性溶液、アルコール、脂肪族炭化水素、芳香族炭化水素、塩基性溶液、ブチロラクトン、酢酸N−ブチル、酢酸カルビトール、ジイソブチルケトン、ジメチルフタレート、エチルアセトアセテート、グリコールエーテル、グリコールエーテルエステル、トリアセテートグリセリル、ハロゲン化溶媒、イソホロン、イソブチルケトンメチル、炭酸プロピレン、リン酸トリエチル、又は水のうちの少なくとも1つを含む、請求項1又は2に記載の方法。 - 前記溶媒混合物を前記非溶媒と混合する工程が、前記溶媒混合物を前記非溶媒に注ぎ、又は注入することからなり、混合は能動的に攪拌することを含む、請求項1〜3のいずれか一項に記載の方法。
- 沈殿物を分離する工程は、
工程には95重量パーセント以上、又は99重量パーセント以上の溶媒及び非溶媒を沈殿物から、15秒以下又は1秒以下の速度で、沈殿物を排出、スクリーニング、又は濾過する工程のうちの少なくとも1つと、
組成物を乾燥させる工程とを含んでなる、請求項1〜4のいずれか一項に記載の方法。 - 層を形成する工程をさらに備え、任意選択で複数の層が前記組成物を形成し、前記組成物を形成する工程は、押し出し、貼り付け、成形、トロール、熱成形、カレンダー加工、積層、ロールコーティング、又は層を形成する他の方法を含んでなる、請求項1〜5のいずれか1つ以上の方法。
- 前記フィラーが、塩、金属酸化物、シリカ、ガラス、二酸化ケイ素ガラス、炭素質材料、有機材料、非金属酸化物、粘土、石英、炭酸カルシウム、粒子状ゴム、ガラス繊維、又は木材パルプのうちの少なくとも1つを含む、請求項1〜6のいずれか一項に記載の方法。
- 前記フィラーが溶解性フィラーを含み、前記方法が前記組成物から前記溶解性フィラーを溶解する工程をさらに備え、ここで、前記組成物は、組成物の総重量から溶媒を差し引いた量に基づいて、0〜15重量%、又は0〜1重量%の溶解性フィラーを含む、請求項1〜7のいずれか一項に記載の方法。
- 前記組成物から層を形成する工程をさらに備え、層を形成する工程は、前記組成物を熱成形、カレンダー加工、積層、又はロールコーティングのうちの少なくとも1つを含む、請求項1〜8のいずれか一項に記載の方法。
- 前記ポリマーが、フルオロポリマー、アクリルポリマー、ポリオレフィン、ポリアクリロニトリル、ナイロン、ポリエステル、ポリアミド、ポリエーテル、ゴム、ポリ(塩化ビニル)、ポリ(酢酸ビニル)、ポリ(ビニルアルコール)、ポリ(ビニルピロリドン)、シラン、又はエポキシのうちの少なくとも1つを含む、請求項1〜9のいずれか一項に記載の方法。
- 請求項1〜10のいずれか一項の方法によって形成された組成物。
- 組成物がフィラーのタップ密度以上の多孔性の少なくとも1つを有し、組成物が0.05〜10ミリメートル、又は2.5〜5ミリメートルの厚さを有する層の形態であり、又は組成物が自立型である、請求項11に記載の組成物。
- 前記物品が、フィルター、絶縁体、コンデンサ、電極、バッテリー、又はセパレータである、請求項11又は12に記載の組成物を含んでなる物品。
- 請求項1〜10のいずれか1つ以上に記載の方法によって製造される多孔質材料であって、前記溶媒及び前記非溶媒を除去した後、フィラー粒子が前記ポリマーによって機械的に一緒に結合され、フィラメントが前記フィラー粒子に付着し、前記ポリマーが前記フィラー粒子間の隙間空間を横切ってフィラー粒子を結合するように存在し、それぞれのフィラー粒子は1つ以上の他の粒子とのフィラメントで結合するように結合している、多孔質材料。
- 前記フィラメントが前記フィラー粒子間の隙間空間に配置され、前記フィラーの充填密度がポリマーなしのフィラー粒子から不変であり、前記ポリマーによって置き換えられた空隙の体積に比例する場合を除いて、前記多孔質材料の空隙体積が大部分がフィラーを含まない粒子の場合から不変である、請求項14に記載の多孔質材料。
- 40〜99体積パーセント、又は50〜95体積パーセントのボイド含有量を有する、請求項14又は15に記載の多孔質材料であって、
平均フィラー粒子直径はマイクロメートル又はサブマイクロメートルであり、かつ、前記ポリマーのフィラメントは、0.5マイクロメートル以下の平均直径及び2マイクロメートル以下の長さを有し、あるいは、
平均フィラー粒子直径が100マイクロメートル以下又は10マイクロメートル以下であり、かつ、前記ポリマーのフィラメントの平均直径がフィラー直径の5〜50%であり、
ここで、隣接する粒子を結合する公称フィラメント長は、平均フィラー直径の1〜500%である、多孔質材料。 - 前記フィラーと前記ポリマーの両方が、フィラーの凝集又は塊成化、又はポリマーの凝固又は層化なしに均一な分布で配置され、
細孔に対する露出しているフィラーの表面積が50面積パーセント以上、又は95面積パーセント以上である、請求項14、15、又は16のいずれか1つ以上に記載の多孔質材料。 - 前記多孔質材料が多孔質材料全体にわたって均一な多孔性を有し、気泡点が最小細孔直径の10倍未満、好適には2倍未満である細孔対称性を有する請求項14、15、16、又は17のいずれか1つ以上に記載の多孔質材料。
- 相反転によって生成されたポリマー溶液から沈殿した多孔質材料であって、溶媒と非溶媒を含む液体の大部分である、通常は90%以上が、例えば、ろ過、沈下、デカンテーション、遠心分離、スプレーアップ、又はフィルターケーキ圧縮の少なくとも1つによって機械的に除去される多孔質材料であって、機械的除去は、乾燥、蒸発、液浴急冷、液体抽出、又は前記多孔質材料から液体を除去するための同様の方法に依存する典型的な相反転プロセスによって達成される方法よりも経済的かつ迅速な方法である、多孔質材料。
- 最初の液体除去後に生成され、散在するポリマーとフィラーの多孔質構造を維持し、液体がすべて又は一部の細孔を満たすように安定化されたポリマーフィラー構造を有する多孔質材料は、従来のスラリー処理装置、例えば、抄紙機、フィルタープレスなどによって物品を製造するための前駆体の役割を果たし、液体含有量は、乾燥、蒸発、圧縮などの少なくとも1つによってさらに低減されて、液体を含まない多孔質材料の結合した塊を生成する、請求項19に記載の方法によって作製された多孔質材料。
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WO2019217381A1 (en) | 2019-11-14 |
GB202015988D0 (en) | 2020-11-25 |
DE112019001856T5 (de) | 2020-12-31 |
US20190341604A1 (en) | 2019-11-07 |
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