JPWO2021040932A5 - - Google Patents

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JPWO2021040932A5
JPWO2021040932A5 JP2022510172A JP2022510172A JPWO2021040932A5 JP WO2021040932 A5 JPWO2021040932 A5 JP WO2021040932A5 JP 2022510172 A JP2022510172 A JP 2022510172A JP 2022510172 A JP2022510172 A JP 2022510172A JP WO2021040932 A5 JPWO2021040932 A5 JP WO2021040932A5
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precursor particles
particles
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Priority claimed from PCT/US2020/043621 external-priority patent/WO2021040932A1/en
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１０００μｍ未満の平均粒径を有する、ある量の前駆体粒子を得ることと、
５００μｍ未満の平均粒径及び前記前駆体粒子の硬度より高い硬度を有する、ある量の鋳型媒体を得ることと、
前記量の前駆体粒子及び鋳型媒体を含む混合物を調製することと、
前記混合物に高剪断及び高圧力場を受けさせ、前記前駆体粒子を製品粒子へと凝集させることと、
前記前駆体粒子を製品粒子へと凝集させた後、前記製品粒子を前記前駆体粒子から分離することと、
を含み、
前記混合物に高剪断及び高圧力場を受けさせることが、前記混合物を乾式メカノフュージョンに供することを含む、前駆体粒子を凝集させるミクロ粒状化法。 obtaining a quantity of precursor particles having an average particle size of less than 1000 μm;
obtaining a quantity of template media having an average particle size of less than 500 μm and a hardness greater than that of said precursor particles;
preparing a mixture comprising the amount of precursor particles and templating medium;
subjecting the mixture to a high shear and high pressure field to agglomerate the precursor particles into product particles ;
After aggregating the precursor particles into product particles, separating the product particles from the precursor particles;
including
A method of microparticulation to agglomerate precursor particles, wherein subjecting the mixture to a high shear and high pressure field comprises subjecting the mixture to dry mechanofusion. 前記混合物に高剪断及び高圧力場を受けさせるステップが、前記混合物をメカノフュージョンすることを含む、請求項１に記載の方法。 2. The method of claim 1, wherein subjecting the mixture to high shear and high pressure fields comprises mechanofusion of the mixture. 前記前駆体粒子の平均粒径が５０μｍ未満である、請求項１に記載の方法。 2. The method of claim 1, wherein the precursor particles have an average particle size of less than 50 [mu]m. 前記前駆体粒子の平均粒径が１０μｍ未満である、請求項３に記載の方法。 4. The method of claim 3, wherein the precursor particles have an average particle size of less than 10 [mu]m. 前記前駆体粒子が、バッテリー電極、肥料、医薬品、トナー、顔料、充填剤又は触媒での使用のための粉末である、請求項１に記載の方法。 2. The method of claim 1, wherein the precursor particles are powders for use in battery electrodes, fertilizers, pharmaceuticals, toners, pigments, fillers or catalysts. 前記前駆体粒子が、炭素質粉末、又は混合金属酸化物粉末、又は金属炭酸塩粉末である、請求項５に記載の方法。 6. The method of claim 5, wherein the precursor particles are carbonaceous powders, or mixed metal oxide powders, or metal carbonate powders. 前記前駆体粒子がカーボン又はグラファイト化可能なカーボンを含む、請求項６に記載の方法。 7. The method of claim 6, wherein the precursor particles comprise carbon or graphitizable carbon . 前記前駆体粒子が、グラファイトフレーク又はＬｉＮｉ１／３Ｍｎ１／３Ｃｏ１／３Ｏ２粉末である、請求項６に記載の方法。 7. The method of claim 6, wherein the precursor particles are graphite flakes or LiNi1 / 3Mn1 / 3Co1/ 3O2 powder. 前記前駆体粒子が混合金属酸化物粉末であり、前記量の前駆体粒子を得るステップが、
金属酸化物原材料粉末を得ることと、
前記金属酸化物原材料粉末をボールミル加工し、前記前駆体粒子を製造することと
を含む、請求項６に記載の方法。 said precursor particles being a mixed metal oxide powder and obtaining said amount of precursor particles comprising:
obtaining a metal oxide raw material powder;
7. The method of claim 6, comprising ball milling the metal oxide raw material powder to produce the precursor particles. 前記混合物を調製する前に、前記量の前駆体粒子の少なくとも一部分をボールミル加工することを含む、請求項１に記載の方法。 2. The method of claim 1, comprising ball milling at least a portion of said quantity of precursor particles prior to preparing said mixture. 前記混合物を調製する前に、前記量の前駆体粒子の少なくとも一部分を加熱することを含む、請求項１に記載の方法。 2. The method of claim 1, comprising heating at least a portion of said quantity of precursor particles prior to preparing said mixture. 前記前駆体粒子が不規則に成形された粉末である、請求項１に記載の方法。 2. The method of claim 1, wherein the precursor particles are irregularly shaped powders. 前記鋳型媒体の平均粒径が１００μｍ以下である、請求項１に記載の方法。 2. The method of claim 1, wherein the templating medium has an average grain size of 100 [mu]m or less. 前記鋳型媒体が、酸化ジルコニウム、炭化タングステン、タングステン、酸化ケイ素、酸化アルミニウム、窒化ケイ素、硬化鋼、ステンレス鋼及びメノウからなる群から選択される、請求項１に記載の方法。 2. The method of claim 1, wherein the mold medium is selected from the group consisting of zirconium oxide, tungsten carbide, tungsten, silicon oxide, aluminum oxide, silicon nitride, hardened steel, stainless steel and agate. 前記鋳型媒体の表面が平滑である、請求項１に記載の方法。 2. The method of claim 1, wherein the surface of said template medium is smooth. 前記鋳型媒体が球状である、請求項１５に記載の方法。 16. The method of claim 15, wherein the templating medium is spherical. 前記鋳型媒体の径分布が（Ｄ９０－Ｄ１０）／Ｄ５０＜２のように均一である、請求項１に記載の方法。 The method of claim 1, wherein the templating medium has a uniform diameter distribution such that (D90-D10)/D50<2. 前記量の鋳型媒体の容積体積が、前記量の前駆体粒子の容積体積よりも大きい、請求項１に記載の方法。 2. The method of claim 1, wherein the volumetric volume of said quantity of templating medium is greater than the volumetric volume of said quantity of precursor particles. 前記量の鋳型媒体の容積体積が、前記量の前駆体粒子の容積体積の１０％よりも大きい、請求項１に記載の方法。 2. The method of claim 1, wherein the volumetric volume of said quantity of templating medium is greater than 10% of the volumetric volume of said quantity of precursor particles. 前記量の鋳型媒体の容積体積が、前記量の前駆体粒子の容積体積の約３倍以上である、請求項１９に記載の方法。 20. The method of claim 19, wherein the volumetric volume of said quantity of templating medium is at least about three times the volumetric volume of said quantity of precursor particles. 前記メカノフュージョンが、チャンバー、前記チャンバー内の回転壁部、前記回転壁部内のスクレーパー及び前記回転壁部内のプレスヘッドを含むメカノフュージョンシステム中で実行される、請求項２に記載の方法。 3. The method of claim 2, wherein said mechanofusion is performed in a mechanofusion system comprising a chamber, a rotating wall within said chamber, a scraper within said rotating wall and a press head within said rotating wall. 前記メカノフュージョンが、
前記スクレーパー及び前記回転壁部の間で約０．５ｍｍの間隔を設定することと、
前記プレスヘッド及び前記回転壁部の間で約１．４ｍｍの間隔を設定することと、
壁部表面速度が約８ｍ／秒以上であるように回転させることと
を含む、請求項２１に記載の方法。 The mechanofusion is
setting a distance of about 0.5 mm between the scraper and the rotating wall;
setting a distance of about 1.4 mm between the press head and the rotating wall;
and rotating such that the wall surface velocity is greater than or equal to about 8 m/s. 前記製品粒子の平均粒径が１０～１００μｍである、請求項１に記載の方法。 The method according to claim 1, wherein the product particles have an average particle size of 10 to 100 µm. 前記製品粒子の径分布が（Ｄ９０－Ｄ１０）／Ｄ５０＜２のように均一である、請求項１に記載の方法。 The method according to claim 1, wherein the product particles have a uniform size distribution such that (D90-D10)/D50<2. 前記製品粒子の表面が平滑である、請求項２に記載の方法。 3. The method of claim 2, wherein the surface of the product particles is smooth. 前記製品粒子の表面がキャビティを含有しない、請求項２に記載の方法。 3. The method of claim 2, wherein the surface of said product particles does not contain cavities. 前記製品粒子が変異係数０．０２未満の粗さを有する、請求項２に記載の方法。 3. The method of claim 2, wherein the product particles have a roughness with a coefficient of variation of less than 0.02. 前記製品粒子が球形である、請求項２５に記載の方法。 26. The method of claim 25, wherein said product particles are spherical. 前記製品粒子が四面体形である、請求項２５に記載の方法。 26. The method of claim 25, wherein the product particles are tetrahedral in shape. 高温で前記製品粒子を焼き戻しすることを追加的に含む、請求項２に記載の方法。 3. The method of claim 2, additionally comprising tempering the product particles at an elevated temperature. 前記鋳型媒体が、前記前駆体粒子の存在下で破壊されないように、前記前駆体粒子の硬度よりも高い硬度を有する、請求項１に記載の方法。 2. The method of claim 1, wherein the templating medium has a hardness greater than that of the precursor particles so as not to fracture in the presence of the precursor particles. バッテリー電極、肥料、医薬品、トナー、顔料、充填剤又は触媒のための製品粒子の製造方法であって、
１０００μｍ未満の平均粒径を有する、ある量の前駆体粒子を得ることと、
５００μｍ未満の平均粒径及び前記前駆体粒子の硬度より高い硬度を有する、ある量の鋳型媒体を得ることと、
前記量の前駆体粒子及び鋳型媒体を含む混合物を調製することと、
前記混合物に高剪断及び高圧力場を受けさせ、前記前駆体粒子を製品粒子へと凝集させることと、
前記前駆体粒子を製品粒子へと凝集させた後、前記製品粒子を前記前駆体粒子から分離することと、
を含み、
前記混合物に高剪断及び高圧力場を受けさせることが、前記混合物を乾式メカノフュージョンに供することを含む、方法。 A method for producing product particles for battery electrodes, fertilizers, pharmaceuticals, toners, pigments, fillers or catalysts, comprising:
obtaining a quantity of precursor particles having an average particle size of less than 1000 μm;
obtaining a quantity of template media having an average particle size of less than 500 μm and a hardness greater than that of said precursor particles;
preparing a mixture comprising the amount of precursor particles and templating medium;
subjecting the mixture to a high shear and high pressure field to agglomerate the precursor particles into product particles;
After aggregating the precursor particles into product particles, separating the product particles from the precursor particles;
including
A method wherein subjecting the mixture to a high shear and high pressure field comprises subjecting the mixture to dry mechanofusion . アノード電極及びカソード電極を含む充電式バッテリーであって、前記アノード及びカソード電極の少なくとも１つが、請求項１に記載の方法に従って製造される製品粒子を含む、充電式バッテリー。 A rechargeable battery comprising an anode electrode and a cathode electrode, wherein at least one of said anode and cathode electrodes comprises product particles produced according to the method of claim 1. 前記量の前駆体粒子が第１の組成の第１の粒子及び第２の組成の第２の粒子の混合物を含み、前記第１及び第２の組成が異なる、請求項１に記載の方法。 2. The method of claim 1, wherein said quantity of precursor particles comprises a mixture of first particles of a first composition and second particles of a second composition, said first and second compositions being different. 第１の前駆体粒子の平均結晶子径が、第２の前駆体粒子の平均結晶子径と少なくとも１０％異なる、請求項３４に記載の方法。 35. The method of claim 34 , wherein the average crystallite size of the first precursor particles differs from the average crystallite size of the second precursor particles by at least 10%.
JP2022510172A 2019-08-29 2020-07-24 Improved microgranulation process and its product particles Pending JP2022546264A (en)

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US62/946,938 2019-12-11
US202063020526P 2020-05-05 2020-05-05
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