CN1684290A - 一种用于二次锂电池的正极材料和用途 - Google Patents
一种用于二次锂电池的正极材料和用途 Download PDFInfo
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Abstract
本发明涉及一种用于二次锂电池的正极材料。该材料为具有橄榄石结构的磷酸盐材料,化学式为LixAyMmNnTtPO4,其中,A为Na、K、Ca、Cu、Ag、Hg、Au或Li;M为Fe或Mn;N为Ni、Mg、Co、Cu、Zn、Ti、Fe或Mn;T为Li、Na、K、Cu、Ag、Hg、Au;且元素M,N,T不同时为一种元素;x,y,m,n,t代表摩尔百分比,0.8≤x≤1,0.001≤y≤0.2,0.7≤m≤1,0≤n≤0.3,0≤t≤0.2,且1≤x+y≤1.05。该正极材料用于二次锂电池的正极,与常规的负极、电解液组成二次锂电池。该正极材料使用半径大于锂离子的一些离子替换锂离子,或采用一价金属离子替换铁离子,得到的正极材料的电子电导率和离子电导率都有数量级的提高,其倍率性能也显著提高,并显示出较高的可逆储锂能量。
Description
技术领域
本发明涉及一种用于二次锂电池的正极材料,具体地说是涉及一种二次锂电池用的具有磷酸盐结构的正极材料及其用途。
背景技术
LiFePO4是一种新型二次锂电池的正极活性材料。在1997年,J.B.Goodenough等申请专利(5,910,382,USA)提出将它作为二次锂电池的正极材料。同年,Armand等将LiFePO4的铁位掺杂和磷位掺杂申请了专利(6,514,640,USA)。LiFePO4这类材料,其优点是原料便宜、不污染环境、安全性能好和理论容量较高(170mAhg-1),但是该材料的电导率很低,导致倍率性能差,限制了它的实际应用。目前,LiFePO4被认为电子电导率很低,改进的方法是表面进行碳包覆,包碳材料的倍率性能得到很大改善,但碳的加入会导致密度的降低,从而影响电池的能量密度。(Zhaohui Chen,and J.R.Dahn.Reducing Carbon in LiFePO4/C Composite Electrodes to Maximize Specific Energy,Volumetric Energy,and Tap Density.J.Electrochem.Soc.,149(9),A1184-A1189(2002))。另外,包碳这种方法仅仅提高了LiFePO4的表面电导,只能在一定程度上改善它的倍率性能。2002年,Chiang等提出了采用锂位掺杂高价金属离子的办法来提高LiFePO4的电导率(Sung-yoon chung,Jasont.Bloking and Yet-ming Chiang.Electronicallyconductive phospho-olivines as lithium storage electrodes.Nature material,2,123-128(2002))。Chiang认为在锂位掺杂半径小于锂离子的高价金属离子,会产生大量空位,因此大大提高LiFePO4的电子电导,继而改善了倍率性能。但是电池材料的倍率特性不仅仅与电子电导有关,而且与离子电导有关前述的对LiFePO4的包覆以及掺杂单纯提高电子电导,并不能满足高功率锂离子电池对倍率性能的要求。
发明内容
本发明的目的是为了克服现有LiFePO4作为二次锂电池的正极材料时,自身的电导率低,而碳包覆和前述位置的掺杂也只提高了电子电导的缺点,从而提供一种可以综合提高本体的电子电导率和离子电导率,从根本上改善材料的倍率性能的用于二次锂电池的正极材料。
本发明的目的是通过如下的技术方案实现的:
本发明提供一种用于二次锂电池的正极材料,其为具有橄榄石结构的磷酸盐材料,化学式为LixAyMmNnTtPO4
其中,A为Na、K、Ca、Cu、Ag、Hg、Au或Li;
M为Fe或Mn;
N为Ni、Mg、Co、Cu、Zn、Ti、Fe或Mn;
T为Li、Na、K、Cu、Ag、Hg、Au;
且元素M,N,T不同时为一种元素;
x,y,m,n,t代表摩尔百分比,0.8≤x≤1,0.001≤y≤0.2,0.7≤m≤1,0≤n≤0.3,0≤t≤0.2,且1≤x+y≤1.05。
使用本发明提供的用于二次锂电池的正极材料的优益之处在于:使用半径大于锂离子的一些离子替换锂离子,或采用一价金属离子替换铁离子,得到具有橄榄石结构的磷酸盐材料,这类正极材料的电子电导率和离子电导率都有数量级的提高,其倍率性能也显著提高,并显示出较高的可逆储锂能量。
本发明提供一种上述用于二次锂电池的正极材料的用途,可将此用于二次锂电池的正极材料制成二次锂电池的正极,与常规的负极、电解液组成二次锂电池。正极中使用的导电添加剂为碳、导电金属氧化物或金属;负极所使用的活性物质包括金属锂、锂合金、可脱嵌锂的碳材料、锂过渡金属氮化物或锂钛尖晶石;正极与负极之间充满电解液,正极和负极的一端分别焊上引线与相互绝缘的电池壳两端相连。
具体实施方式
实施例1、制备本发明的用于二次锂电池的正极材料Li0.99Na0.01FePO4。
磷酸盐正极活性材料Li0.99Na0.01FePO4可以通过以下步骤制备。首先,按照摩尔比称取Li2CO3、Na2CO3、FeC2O4·2H2O和NH4H2PO4,机械球磨后(转速为500转/分钟,3小时),将改混合物在Ar-H2混合气(Ar∶H2=92∶8,v/v)保护下热处理(热处理的步骤为:用1小时从室温升温至400℃,在400℃恒温8小时后,用两小时降到室温),再次球磨(转速为500转/分钟,1小时)后,混合物再次烧结(烧结步骤为:用2小时从室温升温至600℃,在600℃恒温24小时后,用3小时降到室温)。
将Li0.99Na0.01FePO4正极与乙炔黑和10%的环己烷溶液在常温常压下混合形成浆料(活性材料∶乙炔黑∶PVDF=75∶15∶10),均匀涂敷于铝箔衬底上,所得的薄膜厚度约2~20μm,作为模拟电池的正极。
模拟电池的负极使用锂片,电解液为1mol LiPF6溶于1L EC和DMC的混合溶剂中(体积比1∶1)。将正极、负极、电解液在氩气保护的手套箱内组装成模拟电池。
模拟电池的倍率测试步骤:首先以30mA/g充电至4.5V,然后倍率电流放电至2.0V,所放出的容量即为该倍率下的放电容量,放电结束后再以30mA/g放电至2.0V。然后进行下一倍率的测试。其中放电电流1C=150mA/g。该模拟电池的测试结果列于表1。
实施例2~59
按实施例1的方法制备各种组成的本发明的用于二次锂电池的正极材料,并制成模拟电池的正极。
模拟电池的负极(除实施例52~55以外)、电解液及电池组装同于实施例1,正极材料的组成及模拟电池的测试结果列于表1。
实施例52~59中模拟电池的负极使用MCMB作为负极活性材料,电极制备过程如下:将负极活性材料MCMB、乙炔黑和5%PVDF的环己烷溶液在常温常压下混合形成浆料(活性材料∶乙炔黑∶PVDF=90∶5∶5),均匀涂敷于铜箔衬底上,所得的薄膜厚度约2~20um,作为模拟电池的负极。
表1、正极材料的组成及模拟电池的测试结果
实施例 | 正极材料 | 放电容量 | 实施例 | 正极材料 | 放电容量 | ||||||
0.2C | 1C | 10C | 30C | 0.2C | 1C | 10C | 30C | ||||
1 | Li0.99Na0.01FePO4 | 133 | 125 | 100 | 71 | 31 | Li0.9Au0.1Fe0.8Co0.2PO4 | 128 | 112 | 88 | 62 |
2 | Li0.999Na0.001FePO4 | 153 | 121 | 84 | 47 | 32 | Li0.8Na0.2Fe0.7Co0.3PO4 | 108 | 95 | 73 | 48 |
3 | Li0.98Na0.02FePO4 | 129 | 120 | 99 | 73 | 33 | Li0.99Na0.01Fe0.99Ni0.01PO4 | 129 | 109 | 88 | 58 |
4 | Li1.05FePO4 | 145 | 133 | 106 | 81 | 34 | Li0.99Na0.01Fe0.8Ni0.1Mg0.1PO4 | 122 | 109 | 91 | 65 |
5 | Li0.9Na0.1FePO4 | 120 | 115 | 89 | 76 | 35 | Li1.02Fe0.7Ni0.2Co0.1PO4 | 109 | 98 | 85 | 62 |
6 | Li0.8Na0.2FePO4 | 115 | 87 | 71 | 56 | 36 | Li0.99K0.01Fe0.99Cu0.01PO4 | 132 | 118 | 96 | 64 |
7 | Li0.999K0.001FePO4 | 148 | 126 | 90 | 45 | 37 | Li0.99Ag0.01Fe0.9Au0.2PO4 | 122 | 109 | 91 | 65 |
8 | Li0.98K0.02FePO4 | 135 | 126 | 99 | 78 | 38 | LiFe0.98Ag0.04PO4 | 138 | 125 | 96 | 75 |
9 | Li0.8K0.2FePO4 | 113 | 87 | 69 | 61 | 39 | Li0.99Na0.01Fe0.99Zn0.01PO4 | 131 | 119 | 88 | 67 |
10 | Li0.998Ca0.002FePO4 | 145 | 126 | 76 | 55 | 40 | LiFe0.98Hg0.04PO4 | 139 | 120 | 103 | 78 |
11 | Li0.96Ca0.04FePO4 | 130 | 119 | 88 | 65 | 41 | Li0.8Au0.2Fe0.7Zn0.3PO4 | 98 | 87 | 65 | 51 |
12 | Li0.8Ca0.02FePO4 | 105 | 83 | 54 | 21 | 42 | Li0.999Na0.001Fe0.99Ti0.01PO4 | 139 | 122 | 95 | 76 |
13 | Li0.999Cu0.001FePO4 | 153 | 128 | 71 | 39 | 43 | Li0.9K0.1Fe0.9Ti0.1PO4 | 122 | 105 | 84 | 61 |
14 | Li0.98Cu0.02FePO4 | 137 | 116 | 68 | 59 | 44 | Li0.99Au0.01Fe0.7Ti0.3PO4 | 110 | 86 | 73 | 51 |
15 | Li0.8Cu0.2FePO4 | 118 | 89 | 73 | 58 | 45 | Li0.99Na0.01MnPO4 | 132 | 118 | 88 | 63 |
16 | Li0.999Ag0.001FePO4 | 147 | 118 | 65 | 47 | 46 | Li0.8Ca0.2Mn0.8Ti0.2PO4 | 95 | 72 | 58 | 32 |
17 | Li0.98Ag0.02FePO4 | 132 | 109 | 75 | 64 | 47 | Li0.99Cu0.01Mn0.99Ni0.01PO4 | 141 | 117 | 86 | 49 |
18 | Li0.8Ag0.2FePO4 | 108 | 86 | 61 | 44 | 48 | Li0.98Cu0.02MnPO4 | 131 | 111 | 91 | 62 |
19 | Li0.999Hg0.001FePO4 | 149 | 127 | 74 | 51 | 49 | Li0.999Na0.001Mn0.9Mg0.1PO4 | 136 | 114 | 78 | 54 |
20 | Li0.98Hg0.02FePO4 | 130 | 121 | 79 | 63 | 50 | Li0.99Au0.01Mn0.7Co0.3PO4 | 98 | 77 | 55 | 36 |
21 | Li0.8Hg0.2FePO4 | 105 | 88 | 57 | 46 | 51 | Li0.98K0.02Mn0.8Zn0.2PO4 | 115 | 91 | 72 | 59 |
22 | Li0.999Au0.001FePO4 | 152 | 121 | 78 | 41 | 52 | Li0.99Na0.01MnPO4 | 117 | 89 | 68 | 52 |
23 | Li0.98Au0.02FePO4 | 134 | 114 | 91 | 75 | 53 | Li0.99Na0.01FePO4 | 112 | 85 | 63 | 48 |
24 | Li0.8Au0.2FePO4 | 111 | 92 | 61 | 49 | 54 | Li0.99K0.01Fe0.9Co0.1PO4 | 103 | 74 | 57 | 45 |
25 | Li0.99Na0.01Fe0.99Mg0.01PO4 | 126 | 114 | 84 | 79 | 55 | Li0.99Na0.01Fe0.9Ni0.1PO4 | 97 | 72 | 60 | 51 |
26 | LiFe0.95Na0.1PO4 | 128 | 119 | 100 | 81 | 56 | Li0.99Na0.01Fe0.95Ni0.02Li0.06PO4 | 130 | 115 | 85 | 74 |
27 | LiFe0.93Ag0.14PO4 | 145 | 138 | 119 | 83 | 57 | Li0.99Na0.01Fe0.95Cu0.02Na0.06PO4 | 135 | 120 | 90 | 78 |
28 | Li0.99K0.01Fe0.7Mg0.3PO4 | 109 | 100 | 94 | 70 | 58 | Li0.99Na0.01Fe0.95Mg0.02Hg0.06PO4 | 145 | 130 | 100 | 75 |
29 | Li0.98Ca0.02Fe0.99Co0.01PO4 | 133 | 121 | 99 | 70 | 59 | Li0.99Na0.01Fe0.9Li0.2PO4 | 140 | 120 | 110 | 76 |
30 | Li0.999Au0.001Fe0.9Co0.1PO4 | 141 | 123 | 81 | 43 |
Claims (2)
1、一种用于二次锂电池的正极材料,其为具有橄榄石结构的磷酸盐材料,化学式为LixAyMmNnTtPO4
其中,A为Na、K、Ca、Cu、Ag、Hg、Au或Li;
M为Fe或Mn;
N为Ni、Mg、Co、Cu、Zn、Ti、Fe或Mn;
T为Li、Na、K、Cu、Ag、Hg、Au;
且元素M,N,T不同时为一种元素;
x,y,m,n,t代表摩尔百分比,0.8≤x≤1,0.001≤y≤0.2,0.7≤m≤1,0≤n≤0.3,0≤t≤0.2,且1≤x+y≤1.05。
2、一种权利要求1所述的用于二次锂电池的正极材料的用途。
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