CN108793254A - 一种Na0.7ZnxMnyO2层状材料的制备方法 - Google Patents
一种Na0.7ZnxMnyO2层状材料的制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000011734 sodium Substances 0.000 claims abstract description 57
- 239000011572 manganese Substances 0.000 claims abstract description 56
- 239000011701 zinc Substances 0.000 claims abstract description 55
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 18
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 18
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 18
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910001415 sodium ion Inorganic materials 0.000 claims abstract description 16
- 238000000498 ball milling Methods 0.000 claims abstract description 12
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 9
- 239000011787 zinc oxide Substances 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 8
- 239000010431 corundum Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000007772 electrode material Substances 0.000 description 11
- 239000002243 precursor Substances 0.000 description 9
- 239000000843 powder Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 238000010532 solid phase synthesis reaction Methods 0.000 description 3
- 230000002441 reversible effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000005536 Jahn Teller effect Effects 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910014485 Na0.44MnO2 Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
本发明涉及一种Na0.7ZnxMnyO2层状材料的制备方法,属于新能源技术领域。一种Na0.7ZnxMnyO2层状材料的制备方法,将碳酸钠、氧化锌、二氧化锰按摩尔比0.35:0.1~0.2:0.775~0.725以无水乙醇为介质混合球磨,干燥,得前驱体材料;将前驱体材料置于刚玉坩埚中,将坩埚置于马弗炉中,升温速度为4~5℃/min,空气气氛800~900℃下煅烧8~12h;以2~3℃/min的速度冷却至室温,研磨后既得。本发明提供的制备方法简单易行;利用该方法制得层状材料可作为钠离子电池材料。当利用该层状材料作为钠离子电池的正极材料时,该电池前三圈的放电比容量有所提高、材料的粒径更加均匀。
Description
技术领域
本发明涉及一种Na0.7ZnxMnyO2层状材料的制备方法,属于新能源技术领域。
背景技术
与锂离子电池相比,钠离子电池具有更突出的优势,尤其是在成本方面,钠资源丰富,分布比较广泛;另外,钠离子电池选择电解质范围更大,具有相对稳定的电化学性能,使用更加安全。钠离子电池正极材料是影响钠离子电池发展非常重要的一部分,目前研究比较多的电极材料是Na0.44MnO2,但是Na+半径比较大,制备的材料在充放电过程中结构容易坍塌,循环性能不好;另外由于Jahn-Teller效应,这种效应会造成Mn的溶解,限制了锰基材料的实际应用,而目前对于钠离子电池电极材料的改性研究较少。
发明内容
为了提高钠离子电池的可逆容量,改善钠离子电池性能,本发明提供了一种钠离子电池正极材料Na0.7ZnxMnyO2的制备方法,利用该方法制得的电池正极材料Na0.7ZnxMnyO2为掺杂锌的层状材料,该材料在2~4.4V之间具有较高的可逆容量。
一种Na0.7ZnxMnyO2层状材料的制备方法,将碳酸钠、氧化锌、二氧化锰按摩尔比0.35:0.1~0.2:0.775~0.725以无水乙醇为介质混合球磨,400~500rad/min下球磨4~5h,干燥,得前驱体材料;将前驱体材料置于刚玉坩埚中,将坩埚置于马弗炉中,升温速度为4~5℃/min,空气气氛800~900℃下煅烧8~12h;以2~3℃/min的速度冷却至室温,研磨后既得Na0.7ZnxMnyO2层状材料,其中,x=0.1~0.2,y=0.775~0.725。
上述技术方案中,所述Na0.7ZnxMnyO2层状材料中,x,y满足在Na0.7ZnxMnyO2化学式中化合价代数和为零的准则。
上述技术方案中,所述干燥优选按下述方式操作:将球磨后的混合物放在恒温干燥箱中干燥4~6h得到前驱体材料。
本发明一个优选的技术方案为:将碳酸钠、氧化锌、二氧化锰按摩尔比0.35:0.1:0.775、0.35:0.15:0.75或0.35:0.2:0.725以无水乙醇为介质混合球磨,400~500rad/min下球磨4~5h,干燥,得前驱体材料;将前驱体材料置于刚玉坩埚中,将坩埚置于马弗炉中,升温速度为4~5℃/min,空气气氛800~900℃下煅烧8~12h;以2~3℃/min的速度冷却至室温,研磨后既得Na0.7ZnxMnyO2层状材料。
利用上述优选的制备方法所获得的Na0.7ZnxMnyO2层状材料,化学式Na0.7ZnxMnyO2中,x=0.1、y=0.775,或x=0.15、y=0.75,或x=0.2、y=0.725。
本发明的另一目的是提供由上述方法制得的Na0.7ZnxMnyO2层状材料,该Na0.7ZnxMnyO2层状材料按下述方法制得:将碳酸钠、氧化锌、二氧化锰按摩尔比0.35:0.1~0.2:0.775~0.725以无水乙醇为介质混合球磨,400~500rad/min下球磨4~5h,干燥,得前驱体材料;将前驱体材料置于刚玉坩埚中,将坩埚置于马弗炉中,升温速度为4~5℃/min,空气气氛800~900℃下煅烧8~12h;以2~3℃/min的速度冷却至室温,研磨后既得Na0.7ZnxMnyO2层状材料,其中,x=0.1~0.2,y=0.775~0.725。
本发明的又一目的提供上述Na0.7ZnxMnyO2层状材料作为钠离子电池正极材料的应用。
本发明的有益效果为:本发明提供的制备Na0.7ZnxMnyO的方法简单易行;利用该方法制得Na0.7ZnxMnyO2层状材料可作为钠离子电池材料。当利用Na0.7ZnxMnyO2层状材料作为钠离子电池的正极材料时,该电池前三圈的放电比容量有所提高、材料的粒径更加均匀。
附图说明
图1(a)和(b)分别为本发明Na0.7ZnxMnyO2(x=0.15、y=0.75)和Na0.7ZnxMnyO2(x=0.2、y=0.725)的XRD图谱;
图2(a)~(c)为本发明Na0.7ZnxMnyO2(x=0.1、y=0.775)、Na0.7ZnxMnyO2(x=0.15、y=0.75)和Na0.7ZnxMnyO2(x=0.2、y=0.725)的前三次充放电图谱;
图3为本发明Na0.7ZnxMnyO2(x=0.15、y=0.75)的循环性能图谱;
图4为本发明Na0.7ZnxMnyO2(x=0.15、y=0.75)的倍率性能图谱;
图5为本发明Na0.7ZnxMnyO2(x=0.15、y=0.75)的SEM图谱;
图6为本发明Na0.7ZnxMnyO2(x=0.15、y=0.75)的XPS图谱。
具体实施方式
下述非限制性实施例可以使本领域的普通技术人员更全面地理解本发明,但不以任何方式限制本发明。
下述实施例中所述试验方法,如无特殊说明,均为常规方法;所述试剂和材料,如无特殊说明,均可从商业途径获得。
实施例1
钠离子电池正极用电极材料Na0.7Zn0.1Mn0.775O2的制备方法,包括如下步骤:
步骤1,制备Na0.7Zn0.1Mn0.775O2前躯体:
(1)称取碳酸钠1.1463g、氧化锌0.2515g和二氧化锰2.0820g置于球磨罐中;
(2)加入分散剂无水乙醇10mL;
(3)将原料以400rad/min的转速球磨4h后取出,放在恒温干燥箱中干燥6h,得到的粉末即为Na0.7Zn0.1Mn0.775O2前躯体。
步骤2,制备Na0.7Zn0.1Mn0.775O2电极材料:
(1)将步骤1中所得的前驱体粉末放入刚玉坩埚并于马弗炉中,空气气氛下以800℃下煅烧10h,升温速度为5℃/min,以3℃/min的速度冷却至室温,最终得到电极材料Na0.7Zn0.1Mn0.775O2。
本发明通过固相法合成正极材料Na0.7Zn0.1Mn0.775O2,材料结构形态较好。将电池在0.1C下进行充放电测试,Na0.7Zn0.1Mn0.775O2的首次放电比容量高达(126.4mAh g-1)。
实施例2
钠离子电池正极用Na0.7Zn0.15Mn0.75O2电极材料的制备方法,包括如下步骤:
步骤1,制备Na0.7Zn0.15Mn0.75O2前躯体:
(1)称取碳酸钠1.1228g、氧化锌0.3695g和二氧化锰1.9735g置于球磨罐中;
(2)加入分散剂无水乙醇10mL;
(3)将原料以400rad/min的转速球磨4h后取出,放在恒温干燥箱中干燥6h,得到的粉末即为Na0.7Zn0.15Mn0.75O2前躯体。
步骤2,制备Na0.7Zn0.15Mn0.75O2电极材料:
(1)将步骤1中所得的前驱体粉末放入刚玉坩埚并于马弗炉中,空气气氛下以800℃下煅烧10h,升温速度为5℃/min,以3℃/min的速度冷却至室温,最终得到电极材料Na0.7Zn0.15Mn0.75O2。
本发明通过固相法合成正极材料Na0.7Zn0.15Mn0.75O2,材料结构形态较好,电池的循环性能好,衰减少,其电化学性能均得到不同程度的提高。将电池在0.1C下进行充放电测试,Na0.7Zn0.15Mn0.75O2的首次放电容量高达(158.1mAh g-1)。
实施例3
钠离子电池正极用Na0.7Zn0.2Mn0.725O2电极材料的制备方法,包括如下步骤:
步骤1,制备Na0.7Zn0.2Mn0.725O2前躯体:
(1)称取碳酸钠1.1018g、氧化锌0.4835g和二氧化锰1.8720g置于球磨罐中;
(2)加入分散剂无水乙醇10mL;
(3)将原料以400rad/min的转速球磨4h后取出,放在恒温干燥箱中干燥6h,得到的粉末即为Na0.7Zn0.2Mn0.725O2前躯体。
步骤2,制备Na0.7Zn0.2Mn0.725O2电极材料:
(1)将步骤1中所得的前驱体粉末放入刚玉坩埚并于马弗炉中,空气气氛下以800℃下煅烧10h,升温速度为5℃/min,以3℃/min的速度冷却至室温,最终得到电极材料Na0.7Zn0.2Mn0.725O2。
本发明通过固相法合成正极材料Na0.7Zn0.2Mn0.725O2,材料结构形态较好。将电池在0.1C下进行充放电测试,Na0.7Zn0.2Mn0.725O2的首次放电容量高达(171.7mAh g-1)。
Claims (4)
1.一种Na0.7ZnxMnyO2层状材料的制备方法,其特征在于:将碳酸钠、氧化锌、二氧化锰按摩尔比0.35:0.1~0.2:0.775~0.725以无水乙醇为介质混合球磨,400~500rad/min下球磨4~5h,干燥,得前驱体材料;将前驱体材料置于刚玉坩埚中,将坩埚置于马弗炉中,升温速度为4~5℃/min,空气气氛800~900℃下煅烧8~12h;以2~3℃/min的速度冷却至室温,研磨后既得Na0.7ZnxMnyO2层状材料,其中,x=0.1~0.2,y=0.775~0.725。
2.根据权利要求1所述的方法,其特征在于:所述碳酸钠、氧化锌、二氧化锰的摩尔比为0.35:0.1:0.775、0.35:0.15:0.75或0.35:0.2:0.725;所述Na0.7ZnxMnyO2式中x=0.1、y=0.775,或x=0.15、y=0.75,或x=0.2、y=0.725。
3.权利要求1所述方法制得的Na0.7ZnxMnyO2层状材料。
4.权利要求3所述Na0.7ZnxMnyO2层状材料作为钠离子电池正极材料的应用。
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KR20200083825A (ko) * | 2018-12-31 | 2020-07-09 | 동국대학교 산학협력단 | 나트륨 원자층에 아연이 치환된 양극활물질, 이의 제조방법 및 이를 포함하는 나트륨 이차전지 |
CN112830521A (zh) * | 2019-11-22 | 2021-05-25 | 南京理工大学 | 一种F掺杂P2-Na0.7MnO2电极材料及其制备方法 |
KR20220100261A (ko) * | 2021-01-08 | 2022-07-15 | 고려대학교 산학협력단 | 양극 활물질 |
CN115536072A (zh) * | 2022-10-24 | 2022-12-30 | 沈阳国科金能科技有限公司 | 一种锰铁基Na0.67Mn0.9Fe0.1O2钠离子电池正极材料的改性方法 |
CN117902631A (zh) * | 2024-03-14 | 2024-04-19 | 新乡学院 | 一种层状金属氧化物Na0.7MnO2.05及其制备方法 |
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KR20200083825A (ko) * | 2018-12-31 | 2020-07-09 | 동국대학교 산학협력단 | 나트륨 원자층에 아연이 치환된 양극활물질, 이의 제조방법 및 이를 포함하는 나트륨 이차전지 |
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CN112830521A (zh) * | 2019-11-22 | 2021-05-25 | 南京理工大学 | 一种F掺杂P2-Na0.7MnO2电极材料及其制备方法 |
CN112830521B (zh) * | 2019-11-22 | 2022-03-15 | 南京理工大学 | 一种F掺杂P2-Na0.7MnO2电极材料及其制备方法 |
KR20220100261A (ko) * | 2021-01-08 | 2022-07-15 | 고려대학교 산학협력단 | 양극 활물질 |
KR102586288B1 (ko) | 2021-01-08 | 2023-10-18 | 고려대학교 산학협력단 | 양극 활물질 |
CN115536072A (zh) * | 2022-10-24 | 2022-12-30 | 沈阳国科金能科技有限公司 | 一种锰铁基Na0.67Mn0.9Fe0.1O2钠离子电池正极材料的改性方法 |
CN115536072B (zh) * | 2022-10-24 | 2023-08-11 | 沈阳国科金能科技有限公司 | 一种锰铁基Na0.67Mn0.9Fe0.1O2钠离子电池正极材料的改性方法 |
CN117902631A (zh) * | 2024-03-14 | 2024-04-19 | 新乡学院 | 一种层状金属氧化物Na0.7MnO2.05及其制备方法 |
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