CN115010186A - 一种高容量氧变价钠离子电池正极材料及其制备方法 - Google Patents
一种高容量氧变价钠离子电池正极材料及其制备方法 Download PDFInfo
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- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910001415 sodium ion Inorganic materials 0.000 title claims abstract description 27
- 239000007774 positive electrode material Substances 0.000 title claims abstract description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 239000001301 oxygen Substances 0.000 title claims abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000011734 sodium Substances 0.000 claims abstract description 51
- 239000011572 manganese Substances 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 6
- 229910052802 copper Inorganic materials 0.000 claims abstract description 4
- 229910052742 iron Inorganic materials 0.000 claims abstract description 4
- KLARSDUHONHPRF-UHFFFAOYSA-N [Li].[Mn] Chemical compound [Li].[Mn] KLARSDUHONHPRF-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 12
- 229910052708 sodium Inorganic materials 0.000 claims description 11
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 10
- 229910052744 lithium Inorganic materials 0.000 claims description 8
- 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 claims description 6
- 229910052748 manganese Inorganic materials 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052723 transition metal Inorganic materials 0.000 claims description 4
- 150000003624 transition metals Chemical class 0.000 claims description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000003746 solid phase reaction Methods 0.000 claims description 3
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- 239000011363 dried mixture Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 150000004706 metal oxides Chemical class 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 230000002441 reversible effect Effects 0.000 abstract description 7
- 239000010405 anode material Substances 0.000 abstract description 3
- 238000010277 constant-current charging Methods 0.000 abstract 1
- 230000001351 cycling effect Effects 0.000 abstract 1
- 238000007599 discharging Methods 0.000 abstract 1
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract 1
- 239000011888 foil Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 239000002033 PVDF binder Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 4
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 230000033116 oxidation-reduction process Effects 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
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- C01G51/44—Cobaltates containing alkali metals, e.g. LiCoO2 containing manganese
- C01G51/50—Cobaltates containing alkali metals, e.g. LiCoO2 containing manganese of the type [MnO2]n-, e.g. Li(CoxMn1-x)O2, Li(MyCoxMn1-x-y)O2
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- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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Abstract
本发明属于钠离子电池技术领域,具体为一种高容量氧变价的锂锰基钠离子电池正极材料及其制备方法。本发明的钠离子电池正极材料化学式为Na0.75Li0.2Mn0.7Me0.1O2,Me=Cu,Fe,Co。该正极材料采用固相合成法制备,本发明的正极材料在1.5‑4.5 V电位窗口的可逆质量比容量约为190.9‑213.8mAhg‑1,且在恒电流充放电过程中表现出优异的循环稳定性和倍率性能。该层状正极材料比能量高,循环和倍率性能好,制备方法简单,是一种优良的钠离子电池正极材料。
Description
技术领域
本发明属于钠离子电池技术领域,具体涉及一种钠离子电池正极材料及其制备方法。
背景技术
钠离子电池由于其原材料丰富和成本低廉,在大规模储能领域应用潜力巨大,近年来得到越来越多的关注。开发高性能的正极材料是钠离子电池发展和应用的关键。在锂离子电池中,激发层状正极材料中氧的氧化还原可以提高电池的能量密度,得益于非键合O-2p能级的存在,具有氧变价特征的富锂材料其容量可以达到300 mAh g-1,突破了传统正极材料的容量瓶颈。类似富锂材料,在锰基钠离子电池层状氧化物正极材料中引入弱电负性的Li、Mg等元素,或者直接引入过渡金属空位,同样可以引发氧的氧化还原,进一步提高钠离子电池的能量密度。然而此类材料中阴离子氧化还原的可逆性以及动力学性能有待进一步提高,因此设计合理的材料组分和结构以实现高容量高稳定性钠离子电池至关重要。
本发明利用固相反应法制备了高容量氧变价钠离子电池正极材料Na0.75Li0.2Mn0.7Me0.1O2,是一种新型层状正极材料,是一种具有较高充放电容量、良好循环稳定性和优越倍率性能的钠离子电池正极材料。
发明内容
本发明的目的在于提出了一种由过渡金属调节的高稳定性高容量氧变价钠离子电池层状正极材料及其制备方法。
本发明提供的高容量氧变价钠离子电池正极材料,是锂锰基三元金属氧化物,其化学式为Na0.75Li0.2Mn0.7Me0.1O2 ;其中,Me选自Cu、Fe、Co;锂、锰、Me摩尔比例为2:7:1。
本发明提供的高容量氧变价钠离子电池层状正极材料Na0.75Li0.2Mn0.7Me0.1O2,Me金属位于过渡金属层,Li部分位于碱金属钠层。
本发明提供的高容量氧变价钠离子电池层状正极材料Na0.75Li0.2Mn0.7Me0.1O2,为固体粉末,其颗粒尺寸为3-5 μm。
本发明提供的高容量氧变价钠离子电池层状正极材料Na0.75Li0.2Mn0.7Me0.1O2的制备方法,采用固相反应法,具体步骤如下:
将Na2CO3、MnO2、LiOH和CuO(或Fe2O3、CoO)按照Na0.75Li0.2Mn0.7Me0.1O2的化学计量比混合,在无水乙醇中用球磨机球磨5-6h,将球磨后的混合物烘干并置于管式炉中,在700-900℃加热10-15h ,冷却到室温,即获得Na0.75Li0.2Mn0.7Me0.1O2产品。
本发明中,Na0.75Li0.2Mn0.7Me0.1O2的晶体结构由X射线衍射(XRD)确定。衍射结果表明该方法制备的Na0.75Li0.2Mn0.7Me0.1O2产品为单相,属于P型结构层状材料。
本发明中,将Na0.75Li0.2Mn0.7Me0.1O2材料、Super P和PVDF以7: 2: 1的比例混合均匀,加入适量NMP溶液,均匀涂覆于铝箔上,经过干燥后,冲裁成直径为14 mm的圆形电极片,作为钠离子电池的正极。
本发明中,Na0.75Li0.2Mn0.7Me0.1O2电化学性能测试采用三电极体系。以Na0.75Li0.2Mn0.7Me0.1O2极片作为工作电极,金属钠箔作为对电极和参比电极。电解液为1MNaClO4+EC/PC+5% vol. FEC(VEC:VPC=1:1),电池在氩气氛围的手套箱内进行组装。该钠离子电池的电化学性能在Land电池测试系统上进行。
本发明中,Na0.75Li0.2Mn0.7Me0.1O2具有优秀的电化学性能,在1.5-4.5 V电压范围(vs. Na+/Na),具有较高的比容量和良好的倍率性能。可逆容量约为190.9-213.8 mAhg-1,在600mAg-1电流密度下仍有超过100mAhg-1的可逆比容量,在氧变价的钠离子电池正极材料中十分优异。该层状正极材料比能量高,循环和倍率性能好,制备方法简单,是一种优良的钠离子电池正极材料。
附图说明
图1为Na0.75Li0.2Mn0.7Me0.1O2的XRD图谱。
图2为Na0.75Li0.2Mn0.7Me0.1O2在12mAg-1的电流密度下首圈循环曲线图谱。
图3为Na0.75Li0.2Mn0.7Cu0.1O2电极在1.5-4.5 V电位窗口、不同电流密度的倍率性能。
具体实施方式
实施例1
以Na2CO3、MnO2、LiOH和CuO作为前驱物,按照Na : Li : Mn : Cu为0.75: 0.2:0.7:0.1的比例在无水乙醇中球磨混合5 h后烘干,将获得的混合物粉末置于管式炉中,于700 ℃烧结12 h,降温后即可获得Na0.75Li0.2Mn0.7Cu0.1O2样品。
XRD表明(见附图1),合成的Na0.75Li0.2Mn0.7Cu0.1O2是单相,属于斜方晶系,空间群为R3m。将样品、Super P和PVDF以7: 2: 1的比例混合均匀,溶于适量NMP溶液中调制成浆液。均匀涂覆在铝箔上,经过干燥后,冲裁成直径为14 mm的圆形电极片。以极片作为工作电极,金属钠箔作为对电极和参比电极在充满氩气的手套箱中组装成纽扣电池。其电解液为1MNaClO4+EC/PC+5% vol. FEC (VEC: VPC =1: 1)。电池的恒电流充放电测试在蓝电电池测试系统上进行。Na0.75Li0.2Mn0.7Cu0.1O2在1.5-4.5 V(vs. Na+/Na)的电化学窗口内,充放电可逆容量为213.8 mAhg-1(见附图2),电流密度增加至600 mAg-1时,可逆比容量仍能保持110.9mAhg-1(见附图3)。
实施例2
以Na2CO3、MnO2、LiOH和Fe2O3作为前驱物,按照Na:Li:Mn: Fe为0.75: 0.2:0.7:0.1的比例在无水乙醇中球磨混合5 h后烘干,将获得的混合物粉末置于管式炉中,于900 ℃烧结12h,降温后即可获得Na0.75Li0.2Mn0.7Fe0.1O2样品。
XRD表明(见附图1),合成的Na0.75Li0.2Mn0.7Fe0.1O2是单相,属于六方晶系,空间群为P63/mmc。将样品、Super P和PVDF以7: 2: 1的比例混合均匀,溶于适量NMP溶液中调制成浆液。均匀涂覆在铝箔上,经过干燥后,冲裁成直径为14 mm的圆形电极片。以极片作为工作电极,金属钠箔作为对电极和参比电极在充满氩气的手套箱中组装成纽扣电池。其电解液为1M NaClO4+EC/PC+5% vol. FEC (VEC: VPC =1: 1)。电池的恒电流充放电测试在蓝电电池测试系统上进行。Na0.75Li0.2Mn0.7Fe0.1O2在1.5-4.5 V(vs. Na+/Na)的电化学窗口内,充放电可逆容量为194.9mAhg-1(见附图2)。
实施例3
以Na2CO3、MnO2、LiOH和CoO作为前驱物,按照Na : Li : Mn : Co为0.75: 0.2:0.7:0.1的比例在无水乙醇中球磨混合5 h后烘干,将获得的混合物粉末置于管式炉中,于800 ℃烧结12 h,降温后即可获得Na0.75Li0.2Mn0.7Co0.1O2样品。
XRD表明(见附图1),合成的Na0.75Li0.2Mn0.7Co0.1O2是单相,属于六方晶系,空间群为P63/mmc。将样品、Super P和PVDF以7: 2: 1的比例混合均匀,溶于适量NMP溶液中调制成浆液。均匀涂覆在铝箔上,经过干燥后,冲裁成直径为14 mm的圆形电极片。以极片作为工作电极,金属钠箔作为对电极和参比电极在充满氩气的手套箱中组装成纽扣电池。其电解液为1M NaClO4+EC/PC+5% vol. FEC (VEC: VPC =1: 1)。电池的恒电流充放电测试在蓝电电池测试系统上进行。Na0.75Li0.2Mn0.7Co0.1O2在1.5-4.5 V(vs. Na+/Na)的电化学窗口内,充放电可逆容量为190.9 mAhg-1(见附图2)。
Claims (3)
1.一种高容量氧变价钠离子电池正极材料,其特征在于,是锂锰基三元金属氧化物,其化学式为Na0.75Li0.2Mn0.7Me0.1O2 ;其中,Me选自Cu、Fe、Co;锂、锰、Me摩尔比例为2:7:1;
Me金属位于过渡金属层,Li部分位于碱金属钠层。
2. 根据权利要求1所述的高容量氧变价钠离子电池正极材料,其特征在于,形态为固体粉末,其颗粒尺寸为3-5 μm。
3.如权利要求1所述的高容量氧变价钠离子电池正极材料的制备方法,其特征在于,采用固相反应法,具体步骤如下:
将Na2CO3、MnO2、LiOH,以及CuO、Fe2O3或CoO,按照化学计量比混合,在无水乙醇中用球磨机球磨5-6h,将球磨后的混合物烘干并置于管式炉中,在700-900℃加热10-15h,冷却到室温,即获得Na0.75Li0.2Mn0.7Me0.1O2产品。
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