JP7004646B2 - Na3V2(PO4)2F3粒子状物質の製造方法 - Google Patents
Na3V2(PO4)2F3粒子状物質の製造方法 Download PDFInfo
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- C01B25/00—Phosphorus; Compounds thereof
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Description
a)元素態炭素の非存在下、1種以上のリン酸陰イオン前駆体の存在下で、酸化バナジウムV2O5を還元性雰囲気下で還元してリン酸バナジウムVPO4を形成する工程と、
b)工程a)で得られたVPO4と、有効量のフッ化ナトリウムNaF及び元素態炭素源としての1種以上の炭化水素系の含酸素化合物との混合物を、不活性雰囲気下で、該混合物を焼成するのに適した温度条件に暴露して、Na3V2(PO4)2F3物質を形成する工程と
を少なくとも含む方法に関する。
aは9.028~9.030であり、好ましくは実質的に9.029に等しく、
bは9.044~9.046であり、好ましくは実質的に9.045に等しく、
cは10.749以上であり、好ましくは実質的に10.751に等しい。
aは9.028~9.030、好ましくは実質的に9.029に等しく、
bは9.044~9.046、好ましくは実質的に9.045に等しく、
cは10.749以上、好ましくは実質的に10.751に等しい。
a)酸化バナジウムの還元
上述の通り、本方法の第1工程は、V2O5を還元性雰囲気下で還元することを必要とする。
還元工程の最後に得られたリン酸バナジウムは好適には連続的に処理されて所期の生成物を形成する。
本発明に係るこの物質は、以下の説明ではNVPF-HCという省略形で示すこともある。
aは9.028~9.030、好ましくは実質的に9.029に等しく、
bは9.044~9.046、好ましくは実質的に9.045に等しく、
cは10.749以上、好ましくは実質的に10.751に等しい。
前述の通り、本発明に係るNa3V2(PO4)2F3物質は電極活物質として特に有益である。
EPRスペクトルは、ER-4192-ST及びER-4131VTキャビティを備えるBruker EMXを用いて100Kで得た。
VPO4は、ミルで前駆体のV2O5(110g)とNH4H2PO4(140g)との予混合を実施することによって予め得ておく。得られた混合物を、2%H2を富化したアルゴン雰囲気下のオーブン内で10℃/分の加熱速度で800℃まで加熱し、この温度に3時間維持する。こうして得られた灰色の粉末をX線回折によって特性解析した。
実施例1に記載したプロトコルに従って、ただしここでは炭素熱還元を選択して、Na3V2(PO4)2F3物質を調製した。以下、この物質をNVPF-CBという。
これら2種類の物質の特性解析の結果、幾つかの構造上及び形態学的な相違点が明らかになったが、それらの最も顕著なものは、EPR分光法、XRD及びSEMによって検出できる。
Claims (7)
- Na3V2(PO4)2F3物質の製造方法であって、
a)元素態炭素の非存在下、1種以上のリン酸陰イオン前駆体の存在下で、酸化バナジウムV2O5を還元性雰囲気下で還元してリン酸バナジウムVPO4を形成する工程と、
b)工程a)で得られたVPO4と、有効量のフッ化ナトリウムNaF及び元素態炭素源としての1種以上の炭化水素系の含酸素化合物との混合物を、不活性雰囲気下で、該混合物を焼成するのに適した温度条件に暴露して、Na3V2(PO4)2F3物質を形成する工程と
を少なくとも含み、当該方法が、その工程a)と工程b)との間に機械的圧縮工程を含まない、上記方法。 - 前記還元性雰囲気が水素分子を還元剤として使用する、請求項1に記載の方法。
- 前記リン酸陰イオン前駆体が、H3PO4、H(NH4)2PO4及びH2NH4PO4から選択される、請求項1又は請求項2に記載の方法。
- 工程a)が、2%H2を富化されたアルゴンの雰囲気下で、約800℃の温度で実施される、請求項1乃至請求項3のいずれか1項に記載の方法。
- 工程b)の炭化水素系の含酸素化合物が、糖類及び炭水化物から選択される、請求項1乃至請求項4のいずれか1項に記載の方法。
- 工程b)の焼成が不活性雰囲気下800℃で実施される、請求項1乃至請求項5のいずれか1項に記載の方法。
- Na3V2(PO4)2F3物質が、平均粒径2μm未満の一次粒子の形態で存在し、該一次粒子が凝集体の構成粒子である、請求項1乃至請求項6のいずれか1項に記載の方法。
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FR3062384B1 (fr) * | 2017-02-01 | 2021-02-12 | Centre Nat Rech Scient | Procede de preparation d'un materiau composite phosphate de vanadium-carbone par voie liquide |
FR3067709B1 (fr) * | 2017-06-16 | 2020-06-19 | Rhodia Operations | Procede de preparation d'un phosphate de vanadium |
CN116598479A (zh) * | 2018-06-27 | 2023-08-15 | 宁德时代新能源科技股份有限公司 | 正极活性材料、正极极片及钠离子二次电池 |
CN112512966B (zh) * | 2018-07-30 | 2024-02-20 | 罗地亚经营管理公司 | 正极组合物 |
CN110092366B (zh) * | 2019-04-25 | 2023-03-31 | 西北工业大学 | 一种复相磷酸钒钠电极材料及其制备方法 |
CN112216823B (zh) * | 2019-07-10 | 2022-03-08 | 上海交通大学 | 氟磷酸钒钠包覆正极材料、钠离子电池及其制备方法和应用 |
CN112864358B (zh) * | 2019-11-27 | 2023-11-07 | 中国科学院大连化学物理研究所 | 一种一步法制备的钒基聚阴离子型化合物及应用 |
CN111606314B (zh) * | 2020-06-04 | 2023-05-26 | 哈尔滨工业大学 | 一种钠离子电池正极材料三氟磷酸钒钠的制备方法 |
CN111943161B (zh) * | 2020-08-24 | 2022-05-17 | 西北大学 | 一种氟磷酸钒钠和碳复合的二次电池正极材料的制备方法及其应用 |
CN114538400A (zh) * | 2020-11-24 | 2022-05-27 | 天津理工大学 | 多元阳离子取代磷酸盐电极材料及其制备方法 |
CN113293459A (zh) * | 2021-05-24 | 2021-08-24 | 中南大学 | 一种介孔纳米纤维氟磷酸钒钠正极材料及其制备方法 |
CN113764662A (zh) * | 2021-07-29 | 2021-12-07 | 武汉理工大学 | 一种碳包覆磷酸钒钛锰钠微米球及其制备方法与应用 |
CN114572957B (zh) * | 2022-02-22 | 2023-03-28 | 鞍钢集团北京研究院有限公司 | 一种磷酸钒钠材料的制备方法 |
CN114572958B (zh) * | 2022-03-04 | 2023-03-21 | 湖南大学 | 一种含氟聚阴离子型正极材料的制备方法及含氟聚阴离子型正极材料 |
CN114933293B (zh) * | 2022-04-29 | 2024-06-14 | 广州鹏辉能源科技股份有限公司 | 氟磷酸钒钠的制备和在钠离子电池中的应用 |
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SG171958A1 (en) * | 2008-12-19 | 2011-07-28 | Conocophillips Co | Process for making fluorinated lithium vanadium polyanion powders for batteries |
CN102306771A (zh) * | 2011-08-17 | 2012-01-04 | 中南大学 | 一种混合离子电池氟磷酸钒钠正极材料的制备方法 |
JP2013089391A (ja) | 2011-10-14 | 2013-05-13 | Kyushu Univ | ナトリウムイオン二次電池用の電極活物質 |
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US9564656B1 (en) * | 2015-09-14 | 2017-02-07 | Nanotek Instruments, Inc. | Process for producing alkali metal or alkali-ion batteries having high volumetric and gravimetric energy densities |
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CN108349738A (zh) | 2018-07-31 |
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WO2017064189A1 (fr) | 2017-04-20 |
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US20180297847A1 (en) | 2018-10-18 |
JP7301101B2 (ja) | 2023-06-30 |
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