CN103715420B - 高压实密度锂镍钴铝氧三元正极材料的制备方法 - Google Patents
高压实密度锂镍钴铝氧三元正极材料的制备方法 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000010405 anode material Substances 0.000 title claims abstract description 9
- NDPGDHBNXZOBJS-UHFFFAOYSA-N aluminum lithium cobalt(2+) nickel(2+) oxygen(2-) Chemical compound [Li+].[O--].[O--].[O--].[O--].[Al+3].[Co++].[Ni++] NDPGDHBNXZOBJS-UHFFFAOYSA-N 0.000 title claims abstract description 7
- 238000005056 compaction Methods 0.000 title claims abstract description 7
- 239000000243 solution Substances 0.000 claims abstract description 58
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- IWTZGPIJFJBSBX-UHFFFAOYSA-G aluminum;cobalt(2+);nickel(2+);heptahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Al+3].[Co+2].[Ni+2] IWTZGPIJFJBSBX-UHFFFAOYSA-G 0.000 claims abstract description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 8
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 8
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000000536 complexating effect Effects 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- PFYQFCKUASLJLL-UHFFFAOYSA-N [Co].[Ni].[Li] Chemical compound [Co].[Ni].[Li] PFYQFCKUASLJLL-UHFFFAOYSA-N 0.000 claims abstract description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000000498 ball milling Methods 0.000 claims abstract description 5
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 4
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 4
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000005245 sintering Methods 0.000 claims abstract description 4
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 4
- 229910013716 LiNi Inorganic materials 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 150000001768 cations Chemical class 0.000 claims description 3
- 238000013467 fragmentation Methods 0.000 claims description 3
- 238000006062 fragmentation reaction Methods 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052744 lithium Inorganic materials 0.000 abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract 6
- 229910017906 NH3H2O Inorganic materials 0.000 abstract 2
- 238000012360 testing method Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
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Abstract
本发明涉及锂电极正极材料的制备方法,具体是一种高压实密度锂镍钴铝氧三元正极材料的制备方法。该方法包括以下步骤:a.配置硝酸钴溶液,用氨水络合,编号溶液1;配置NaOH溶液,并加入NH3·H2O溶液,编号溶液2;配置硝酸钴、硝酸镍和硝酸铝混合溶液,用氨水络合,编号溶液3;配置NaOH溶液,并加入NH3·H2O溶液,编号溶液4;b.将溶液1和溶液2混合反应,获得钴氧前躯体;c.将钴氧前躯体与溶液3和溶液4反应,得氢氧化镍钴铝前躯体;d.将碳酸锂和氢氧化镍钴铝前躯体球磨混合;e.马弗炉烧结;f.得锂镍钴铝氧正极三元材料。本发明提高了三元材料的压实密度,其材料的电池容量和循环性能均显著提高。
Description
技术领域
本发明涉及锂电极正极材料的制备方法,具体是一种高压实密度锂镍钴铝氧三元正极材料的制备方法。
背景技术
锂镍钴铝氧三元材料已经被广泛用于锂电池的正极材料,但现有三元正极材料压实密度难以提高,限制了三元正极材料电池容量和循环性等性能的进一步提高。
发明内容
本发明所要解决的技术问题是,提供一种具有较高的材料压实密度,同时材料的电池容量和循环性能优良的高压实密度锂镍钴铝氧三元正极材料的制备方法。
本发明的高压实密度锂镍钴铝氧三元正极材料的制备方法包括以下步骤:
a.配置2.0mol/L硝酸钴溶液,用氨水络合至pH为6.6,编号溶液1;
配置6.0mol/LNaOH溶液,并加入0.4mol/LNH3·H2O溶液,二者体积比为10:1,编号溶液2;
配置阳离子总浓度为2.0mol/L的硝酸钴、硝酸镍和硝酸铝混合溶液,其中镍钴铝摩尔比为0.8:0.15:0.05,用氨水络合至pH为8.6,编号溶液3;
配置3.0mol/LNaOH溶液,并加入0.8mol/LNH3·H2O溶液,二者体积比为7:1,编号溶液4;
b.将配置好的溶液1和溶液2混合反应,并控制溶液2使混合溶液pH为13,反应温度28-30℃,反应过程中通入N2保护;待反应分离出沉淀颗粒,用去离子水洗涤后烘干;在380-390℃煅烧6-8h,获得钴氧前躯体;
c.将制备的钴氧前躯体加入反应釜中,并将配置好的溶液3和溶液4同时泵入反应釜,并控制溶液4使混合溶液pH为10.5,搅拌并保持恒温55-60℃,反应过程中通入N2保护;待反应分离出沉淀颗粒,用去离子水洗涤后烘干,得氢氧化镍钴铝前躯体;
d.将碳酸锂和氢氧化镍钴铝前躯体按摩尔比Li/M=1.06球磨混合;其中M是镍钴铝三种元素的摩尔数之和;
e.马弗炉烧结:室温-450℃,升温速率3-4℃/min,450℃时不保温;450-740℃,升温速率1-1.5℃/min,740℃保温18-20h;740-350℃,降温速率1.5-2.5℃/min,后随炉温自然冷却,整个过程中气氛为空气,气流量为8-10L/min;
f.破碎后,得锂镍钴铝氧正极三元材料LiNi0.78Co0.17Al0.05O2。
本发明通过特殊的工艺参数和原料选择,能够有效改善材料颗粒的形貌,提高了三元材料的压实密度,进而改善了正极材料的性能,经检测和试验,其材料的电池容量和循环性能均显著提高。
具体实施方式
本发明实施例的方法包括以下步骤:
a.配置2.0mol/L硝酸钴溶液,用氨水络合至pH为6.6,编号溶液1;
配置6.0mol/LNaOH溶液,并加入0.4mol/LNH3·H2O溶液,二者体积比为10:1,编号溶液2;
配置阳离子总浓度为2.0mol/L的硝酸钴、硝酸镍和硝酸铝混合溶液,其中镍钴铝摩尔比为0.8:0.15:0.05,用氨水络合至pH为8.6,编号溶液3;
配置3.0mol/LNaOH溶液,并加入0.8mol/LNH3·H2O溶液,二者体积比为7:1,编号溶液4;
b.将配置好的溶液1和溶液2同时泵入10L的反应釜中,混合溶液流速为200mL/min,0.5h后结束加料,并控制溶液2使混合溶液pH为13,搅拌并保持恒温30℃,反应过程中通入N2保护;待反应进行5h后分离出沉淀颗粒,用去离子水洗涤后烘干;在390℃煅烧8h,获得钴氧前躯体,平均粒径2.3μm;
c.将制备的钴氧前躯体加入反应釜中,并将配置好的溶液3和溶液4同时泵入反应釜,混合溶液流速为40mL/min,并控制溶液4使混合溶液pH为10.5,搅拌并保持恒温55℃,反应过程中通入N2保护;待反应进行15h后分离出沉淀颗粒,用去离子水洗涤后烘干,得氢氧化镍钴铝前躯体,平均粒径8.7μm,化学组成为Ni:Co:Al=0.777:0.171:0.048;
d.将碳酸锂和氢氧化镍钴铝前躯体按摩尔比Li/M=1.06球磨混合,球磨时间为4h;其中M是镍钴铝三种元素的摩尔数之和;
e.马弗炉烧结:室温-450℃,升温速率3-4℃/min,450℃时不保温;450-740℃,升温速率1-1.5℃/min,740℃保温19h;740-350℃,降温速率1.5-2.5℃/min,后随炉温自然冷却,整个过程中气氛为空气,气流量为10L/min;
f.万能破碎后过200目筛网,得锂镍钴铝氧正极三元材料LiNi0.78Co0.17Al0.05O2。
本发明实施例制备的正极材料,经检测和试验,结果如下:
1、振实密度:用BT-300振实密度测试仪测试该材料振实密度为2.35g/cm3;
2、压实密度:30Mpa下测得该材料的压实密度为3.96g/cm3;
2、SEM观察该材料二次颗粒形貌近似球形;
3、液氮吸附法测得该材料比表面积为0.71m2/g;
4、常温下电池测试:3.0~4.4V,1C下,该材料首次放电比容量为198.3mAh/g,效率为90.2%;1C循环100次后容量保持率≥88.6%。
Claims (1)
1.一种高压实密度锂镍钴铝氧三元正极材料的制备方法,其特征是:该方法包括以下步骤,
a.配置2.0mol/L硝酸钴溶液,用氨水络合至pH为6.6,编号溶液1;
配置6.0mol/LNaOH溶液,并加入0.4mol/LNH3·H2O溶液,二者体积比为10:1,编号溶液2;
配置阳离子总浓度为2.0mol/L的硝酸钴、硝酸镍和硝酸铝混合溶液,其中镍钴铝摩尔比为0.8:0.15:0.05,用氨水络合至pH为8.6,编号溶液3;
配置3.0mol/LNaOH溶液,并加入0.8mol/LNH3·H2O溶液,二者体积比为7:1,编号溶液4;
b.将配置好的溶液1和溶液2混合反应,并控制溶液2使混合溶液pH为13,反应温度28-30℃,反应过程中通入N2保护;待反应分离出沉淀颗粒,用去离子水洗涤后烘干;在380-390℃煅烧6-8h,获得钴氧前躯体;
c.将制备的钴氧前躯体加入反应釜中,并将配置好的溶液3和溶液4同时泵入反应釜,并控制溶液4使混合溶液pH为10.5,搅拌并保持恒温55-60℃,反应过程中通入N2保护;待反应分离出沉淀颗粒,用去离子水洗涤后烘干,得氢氧化镍钴铝前躯体;
d.将碳酸锂和氢氧化镍钴铝前躯体按摩尔比Li/M=1.06球磨混合;其中M是镍钴铝三种元素的摩尔数之和;
e.马弗炉烧结:室温-450℃,升温速率3-4℃/min,450℃时不保温;450-740℃,升温速率1-1.5℃/min,740℃保温18-20h;740-350℃,降温速率1.5-2.5℃/min,后随炉温自然冷却,整个过程中气氛为空气,气流量为8-10L/min;
f.破碎后,得锂镍钴铝氧正极三元材料LiNi0.78Co0.17Al0.05O2。
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Synthesis and electrochemical properties of LiNi0.8Co0.15Al0.05O2 prepared from the precursor Ni0.8Co0.15Al0.05OOH;Guorong Hu et al;《Journal of Power Sources》;20111005;第198卷(第2012期);全文 * |
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