CN112366304A - 一种锂离子电池用纳米晶铁硅合金基正极材料及其制备方法 - Google Patents
一种锂离子电池用纳米晶铁硅合金基正极材料及其制备方法 Download PDFInfo
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910000676 Si alloy Inorganic materials 0.000 title claims abstract description 34
- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000010406 cathode material Substances 0.000 title claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 35
- 239000002243 precursor Substances 0.000 claims abstract description 21
- 239000010405 anode material Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000975 co-precipitation Methods 0.000 claims abstract description 9
- 239000008139 complexing agent Substances 0.000 claims abstract description 8
- 239000013078 crystal Substances 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 239000010941 cobalt Substances 0.000 claims abstract description 6
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 6
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 6
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 5
- 239000011572 manganese Substances 0.000 claims abstract description 5
- 238000007873 sieving Methods 0.000 claims abstract description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 4
- 238000001354 calcination Methods 0.000 claims abstract description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 12
- 239000000956 alloy Substances 0.000 claims description 12
- 239000007774 positive electrode material Substances 0.000 claims description 12
- 229910000519 Ferrosilicon Inorganic materials 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 230000009471 action Effects 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 229910005347 FeSi Inorganic materials 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 229910052493 LiFePO4 Inorganic materials 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910001021 Ferroalloy Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
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Abstract
本发明公开了一种锂离子电池用纳米晶铁硅合金基正极材料及其制备方法，其特征在于：以纳米晶铁硅合金粉末作为晶核，与络合剂、镍源、钴源、锰源、铝源用共沉淀法制备得锂离子电池前驱体，再将锂离子电池前驱体锻烧、研磨过筛而成，所述纳米晶铁硅合金粉末表面包覆一层正极材料。本发明提高了正极材料的高功率特性和快速充放电能力,而且提高了正极材料的电池容量，同时本发明制备工艺简单易控制,生产成本低。
Description
技术领域
本发明涉及锂离子电池正极材料领域，尤其涉及一种锂离子电池用铁硅合金基正极材料及其制备方法。
背景技术
随着新兴经济的快速发展,全球能源消耗量急剧增长。锂离子电池以其高电压、高能量密度、循环寿命长、安全性能好、无污染等优点成为现有市场上最为广泛使用的替代材料之一。近年来对电池正极材料的研究及改进是当前最为紧急的任务。
铁在地球上是占比最多的元素，自然资源非常丰富，LiFePO4材料具有原材料资源丰富、环境友好、循环寿命长和安全性能优异等优点，但是也存在放电电压低、大电流充放电性能差、低温充放电困难等问题，这限制了LiFePO4材料的广泛应用。
发明内容
本发明的目的是克服目前商业化铁基材料作为锂离子电池正极材料时放电电压低、大电流充放电性能差、低温充放电困难等缺点，提供一种锂离子电池用纳米晶铁硅合金基正极材料及制备方法，要求其提高比容量，快速充放电能力,同时该方法加工成本低、工艺简单易控制、周期短、高效节能。
本发明采用的的技术方案为：一种锂离子电池用纳米晶铁硅合金基正极材料以纳米晶铁硅合金粉末作为晶核，纳米晶铁硅合金粉末与络合剂和正极材料用共沉淀法制备得锂离子电池前驱体，再将锂离子电池前驱体锻烧、研磨过筛而成，所述纳米晶铁硅合金粉末表面包覆一层正极材料。
所述锂离子电池用纳米晶铁硅合金基正极材料的制备方法，其特征在于包括以下步骤：
步骤一：将纳米晶铁硅合金粉末作为晶核，将合金固体粉末放入反应釜中加入络合剂和正极材料在保护气体作用下用共沉淀法制备得锂离子电池前驱体；
步骤二：将所得的前驱体干燥后，放入管式炉中以1-2℃/min的速率升温至200-900℃并保温1-2小时，冷却至室温，研磨过筛得到锂离子电池用纳米晶铁硅合金基正极材料。
所述步骤一中纳米晶铁硅合金成分为Fe：85-92.7%；Si：2.3-6.6%；Al：5-10%。
所述正极材料为镍源、钴源、锰源、铝源的一种或多种。
所述步骤一中合金粉末粒径为0.2-44μm。
所述步骤二中管式炉中通入的气氛为空气、氧气。
本发明采用铁合金作为铁源通过共沉淀法制备了一种锂离子电池正极材料,其步骤包括纳米晶铁硅合金粉末的制备、高温烧结等制备复合材料具有较高的初始放电容量和循环稳定性，提高了正极材料的高功率特性。
由于采用了上述技术方案,本发明具有如下优点和效果：
1.本发明材料提高了正极材料的高功率特性和快速充放电能力,而且提高了正极材料的电池容量；
2.本发明制备工艺简单易控制,生产成本低。
具体实施方式
以下结合具体的实施例子对上述方案做进一步说明，本发明的优选实施例详述如下：
实施例1
纳米晶铁硅合金成分按Fe：90%；Si：5%；Al：5%，配成纳米晶铁硅合金粉末用作晶核，将合金固体粉末放入反应釜中加入络合剂、镍源、钴源、锰源在氮气气氛下用共沉淀法制备FeSi/NCM811锂离子电池前驱体；将所得的粉末用烘箱干燥后，放入管式炉中以1-2℃/min的速率升温至780℃并保温30min，冷却至室温，研磨过300目的筛得到锂离子电池用纳米晶铁硅合金基正极材料。
实施例2
纳米晶铁硅合金成分按Fe：90%；Si：6.5%；Al：3.5%，配成纳米晶铁硅合金粉末用作晶核，将合金固体粉末放入反应釜中加入络合剂、镍源、钴源、锰源在氮气气氛下用共沉淀法制备FeSi/NCM523锂离子电池前驱体；将所得的粉末用烘箱干燥后，放入管式炉中以1-2℃/min的速率升温至690℃并保温30min，冷却至室温，研磨过300目的筛得到锂离子电池用纳米晶铁硅合金基正极材料。
实施例3
纳米晶铁硅合金成分按Fe：87%；Si：6.5%；Al：6.5%，配成纳米晶铁硅合金粉末用作晶核，将合金固体粉末放入反应釜中加入络合剂、镍源、钴源、铝源在氮气气氛下用共沉淀法制备FeSi/NCA锂离子电池前驱体；将所得的粉末用烘箱干燥后，放入管式炉中以1-2℃/min的速率升温至730℃并保温30min，冷却至室温，研磨过300目的筛得到锂离子电池用纳米晶铁硅合金基正极材料。
本发明所述的实施例仅仅是对本发明的优选实施方式进行的描述，并非对本发明构思和范围进行限定，在不脱离本发明设计思想的前提下，本领域中工程技术人员对本发明的技术方案作出的各种变型和改进，均应落入本发明的保护范围，本发明请求保护的技术内容，已经全部记载在权利要求书中。
Claims (6)
1.一种锂离子电池用纳米晶铁硅合金基正极材料，其特征在于：以纳米晶铁硅合金粉末作为晶核，纳米晶铁硅合金粉末与络合剂和正极材料用共沉淀法制备得锂离子电池前驱体，再将锂离子电池前驱体锻烧、研磨过筛而成，所述纳米晶铁硅合金粉末表面包覆一层正极材料。
2.如权利要求1所述的一种锂离子电池用纳米晶铁硅合金基正极材料的制备方法，其特征在于包括以下步骤：
步骤一：将纳米晶铁硅合金粉末作为晶核，将合金固体粉末放入反应釜中加入络合剂和正极材料在保护气体作用下用共沉淀法制备得锂离子电池前驱体；
步骤二：将所得的前驱体干燥后，放入管式炉中以1-2℃/min的速率升温至200-900℃并保温1-2小时，冷却至室温，研磨过筛得到锂离子电池用纳米晶铁硅合金基正极材料。
3.根据权利要求2所述的一种锂离子电池用纳米晶铁硅合金基正极材料的制备方法，其特征在于，所述步骤一中纳米晶铁硅合金成分为Fe：85-92.7%；Si：2.3-6.6%；Al：5-10%。
4.根据权利要求1或2所述的一种锂离子电池用纳米晶铁硅合金基正极材料的制备方法，其特征在于，所述正极材料为镍源、钴源、锰源、铝源的一种或多种。
5.根据权利要求2所述的一种锂离子电池用纳米晶铁硅合金基正极材料的制备方法，其特征在于，所述步骤一中合金粉末粒径为0.2-44μm。
6.根据权利要求2所述的一种锂离子电池用纳米晶铁硅合金基正极材料的制备方法，其特征在于，所述步骤二中管式炉中通入的气氛为空气、氧气。
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| CN114214730A (zh) * | 2021-12-15 | 2022-03-22 | 中钢天源股份有限公司 | 一种高容量单晶正极电池材料的制备方法及产品 |
| CN114361423A (zh) * | 2022-01-12 | 2022-04-15 | 天能帅福得能源股份有限公司 | 一种纳米晶铁硅合金基正极材料及其制备方法 |
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