CN102969499A - 一种单分散镍钴铝球形前驱体的制备方法 - Google Patents
一种单分散镍钴铝球形前驱体的制备方法 Download PDFInfo
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 29
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title abstract description 15
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- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 claims description 22
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- 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 description 5
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 5
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 5
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
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- 239000007921 spray Substances 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 2
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 claims description 2
- 239000003570 air Substances 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 2
- 229940009827 aluminum acetate Drugs 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 229940011182 cobalt acetate Drugs 0.000 claims description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 2
- MULYSYXKGICWJF-UHFFFAOYSA-L cobalt(2+);oxalate Chemical compound [Co+2].[O-]C(=O)C([O-])=O MULYSYXKGICWJF-UHFFFAOYSA-L 0.000 claims description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- 229910052754 neon Inorganic materials 0.000 claims description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 2
- 229940078494 nickel acetate Drugs 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- DOLZKNFSRCEOFV-UHFFFAOYSA-L nickel(2+);oxalate Chemical compound [Ni+2].[O-]C(=O)C([O-])=O DOLZKNFSRCEOFV-UHFFFAOYSA-L 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims 1
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- 239000002184 metal Substances 0.000 claims 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims 1
- 229910001220 stainless steel Inorganic materials 0.000 claims 1
- 239000010935 stainless steel Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 6
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 6
- 239000010405 anode material Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 4
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- 229910004424 Li(Ni0.8Co0.15Al0.05)O2 Inorganic materials 0.000 abstract 3
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- 239000008367 deionised water Substances 0.000 description 4
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- 229910012820 LiCoO Inorganic materials 0.000 description 1
- 229910013292 LiNiO Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
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- 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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Abstract
本发明涉及一种合成单分散镍钴铝前驱体的制备方法,用作锂离子二次电池正极材料Li(Ni0.8Co0.15Al0.05)O2。本发明通过对镍化合物、钴化合物和铝化合物的混合溶液通过超声雾化,低温干燥得到用于合成粒径可调,范围1nm~2μm,单分散的球形镍钴铝前驱体颗粒,是后期制备锂离子二次电池正极材料Li(Ni0.8Co0.15Al0.05)O2的关键技术,此种方法合成的镍钴铝球形前驱体的粒径均一,保证后期制备锂离子二次电池正极材料的均一性,提高振实密度,提高锂离子二次电池用Li(Ni0.8Co0.15Al0.05)O2的电性能。
Description
技术领域
本发明涉及电池制造技术领域,特别是锂离子二次电池用正极材料—镍钴铝前驱体的合成方法。
背景技术
目前商品化锂离子二次电池主要选用LiCoO2为正极材料,但钴元素相对贫乏导致原料成本高,LiNiO2和LiCoO2具有相同的层状结构并且资源丰富、成本低,无环境污染,是一种理想的替代LiCoO2后选材料,但是LiNiO2在合成过程中不易准确控制化学计量比,充放电过程中Ni3+已转化成Ni4+将严重影响其循环寿命,热稳定性差,甚至氧化分解电解质带来安全隐患。研究表明,掺入Co元素可以改善LiNiO2结构的稳定性,且20%左右的Ni被Co取代制得的正极材料电性能良好。而掺入Al元素后,可以抑制充放电过程中晶体结构的变化,改善其热稳定性和耐过充性,大大提高其循环性能。若同时引入Co和Al元素制备双掺杂的LiNiO2正极材料,则可以制备出具有良好的电性能的正极材料Li(Ni0.08Co0.15Al0.05)O2。
现有制备镍钴铝正极材料主要是采用控制结晶共沉淀法和固相烧结法。其中控制结晶共沉淀法先在反应釜中制备出球形的氢氧化物前驱体,后按配比与锂盐混合,再经高温下烧结固相反应而成,然而共沉淀法所需制备周期长,工序繁多,产品电性能均一性较差;固相烧结法是将锂化合物,镍化合物,钴化合物和铝化合物的固体混合物在高温下直接以固体形式反应,其工艺操作简单,但是各固体接触面积远比其表面积小,难以控制合成元素的分布均匀,且形貌不均匀,影响该正极材料电性能。
发明内容
本发明目的在于通过超声雾化的方法合成一种具有实用价值且热稳定性好,电性能优异的镍钴铝球形前驱体。用该方法可快速制备粒径在1nm~2μm可调,单分散实心球形镍钴铝前驱体粉末。
本发明提出的技术方案包括以下步骤:
1)将镍化合物、钴化合物和铝化合物在溶剂中溶解得到混合溶液;所述镍化合物为硝酸镍、氯化镍、醋酸镍、草酸镍或硫酸镍中的至少一种;所述钴化合物为硝酸钴、氯化钴、醋酸钴、草酸钴或硫酸钴中的至少一种;所述铝化合物为硝酸铝、氯化铝、醋酸铝、草酸铝或硫酸铝中的至少一种;所述溶剂为水、烷烃、醇、醚、酮、酯或芳香烃中的一种或几种组合;2)将所述混合溶液在超声雾化器中雾化,用载料气体把料雾液滴送入高温干燥室以一定温度干燥,制成粒径1nm~2μm的球形前驱体;所述载料气体为空气、氮气、氩气、氧气或氖气中的至少一种。
本发明所述溶解时,镍化合物、钴化合物和铝化合物的投料摩尔比为0.70~0.90︰0.10~0.20 ︰0.00~0.10。镍化合物、钴化合物和铝化合物的混合溶液浓度为0.01~2mol/L。
本发明所使用的仪器为超声雾化器,操作过程安全,实验成本低,操作步骤简单,生产周期短且可实现工业化大生产,在目前锂离子二次电池正极材料的制备和工业生产工程中具备很高的实用价值。超声雾化器的雾化频率为1.7MHz±0.17 MHz,在雾化成雾滴同时可使溶液由于超声波的作用混合均匀。雾化蒸发温度为镍化合物、钴化合物和铝化合物的分解温度以上:150℃~600℃,进料时间为2~10小时左右,通过调控超声雾化雾量大小来控制合成粒径1nm~2μm,单分散的镍钴铝前驱体,使得后续制备的正极材料—Li(Ni0.08Co0.15Al0.05)O2中各种离子的扩散程相当,达到具有良好均一稳定的充放电性能的目的。
步骤2)中的高温干燥气流为150~650℃,进料时间为2~10h。
本发明使用镍化合物、钴化合物和铝化合物混合溶液通过超声雾化法制备用于合成镍钴铝的球形前驱体,通过控制反应时超声雾化的雾量大小,使得镍钴铝溶质随水溶液蒸发,干燥形成粒径大小均一、实心球形颗粒前驱体,使得各种物质的扩散路径相当,使得后续制备的Li(Ni0.08Co0.15Al0.05)O2具有良好均一稳定的充放电性能。该方法的优点是通过控制镍钴铝球形前驱体的直径大小尺寸提高了后续制备正极材料—Li(Ni0.08Co0.15Al0.05)O2性能的一致性。
附图说明
图1为本发明的装置示意图。
图2为400℃高温干燥气流下进料2h所得单分散镍钴铝球形前驱体的SEM照片。
图3为450℃高温干燥气流下进料2h所得单分散镍钴铝球形前驱体的SEM照片。
图4为500℃高温干燥气流下进料2h所得单分散镍钴铝球形前驱体的SEM照片。
图5为400℃高温干燥气流下进料2h所得单分散镍钴铝球形前驱体的XRD图谱。
图6为400℃高温干燥气流下进料2h后所得单分散镍钴铝球形前驱体的TEM照片。
具体实施方式
本发明通过对镍化合物、钴化合物和铝化合物以固定比例配比,在去离子水中溶解,把混合溶液通过超声雾化器中雾化,用载料气体把料雾液滴送入高温干燥室以一定温度干燥,制成直径1nm~2μm,单分散的球形前驱体颗粒。
实施例一
1、配置反应溶液:分别称取35 g硝酸镍、6g硝酸钴、3g硝酸铝在烧杯中加入去离子水搅拌均匀,转移到100mL容量瓶中定容,配置成1.5moL/L的反应溶液。
2、料雾形成:把反应溶液加入超声雾化器中的进料杯,控制超声雾化的频率在1.7M Hz左右,形成雾滴。
3、干燥过程:通过载料气体把雾滴送到高温干燥室中,高温干燥室的温度控制在400℃,通过控制载料气体的流量,持续在高温干燥室中干燥2小时,得到用于合成粒径1.4μm,单分散的镍钴铝球形前驱体颗粒,扫描电镜(SEM)照片如图2所示,X射线衍射图谱(XRD)如图5所示,透射电镜(TEM)照片如图6所示。
实施例二
1、配置反应溶液:分别称取35 g硝酸镍、6g硝酸钴、3g硝酸铝在烧杯中加入去离子水搅拌均匀,转移到100mL容量瓶中定容,配置成1.5moL/L的反应溶液。
2、料雾形成:把反应溶液加入超声雾化器中的进料杯,控制超声雾化的频率在1.7MHz左右,形成雾滴。
3、干燥过程:通通过载料气体把雾滴送到高温干燥室中,高温干燥室的温度控制在450℃,通过控制载料气体的流量,持续在高温干燥室中干燥2小时,得到用于合成粒径1.6μm,单分散的镍钴铝球形前驱体颗粒,扫描电镜(SEM)照片如图3所示。
实施例三
1、配置反应溶液:分别称取35 g硝酸镍、6g硝酸钴、3g硝酸铝在烧杯中加入去离子水搅拌均匀,转移到100mL容量瓶中定容,配置成1.5moL/L的反应溶液。
2、料雾形成:把反应溶液加入超声雾化器中的进料杯,控制超声雾化的频率在1.7M Hz左右,形成雾滴。
3、干燥过程:通过载料气体把雾滴送到高温干燥室中,高温干燥室的温度控制在500℃,通过控制载料气体的流量,持续在高温干燥室中干燥2小时,得到用于合成粒径1.8μm,单分散的镍钴铝球形前驱体颗粒,扫描电镜(SEM)照片如图4所示。
Claims (6)
1.一种单分散镍钴铝球形前驱体的制备方法,其特征在于包括以下步骤:
1)将镍化合物、钴化合物和铝化合物在溶剂中溶解得到混合溶液;所述镍化合物为硝酸镍、氯化镍、醋酸镍、草酸镍或硫酸镍中的至少一种;所述钴化合物为硝酸钴、氯化钴、醋酸钴、草酸钴或硫酸钴中的至少一种;所述铝化合物为硝酸铝、氯化铝、醋酸铝、草酸铝或硫酸铝中的至少一种;所述溶剂为水、烷烃、醇、醚、酮、酯或芳香烃中的一种或几种组合;2)将所述混合溶液在超声雾化器中雾化,用载料气体把料雾液滴送入高温干燥室以一定温度干燥,制成粒径1nm~2μm的球形前驱体;所述载料气体为空气、氮气、氩气、氧气或氖气中的至少一种。
2.根据权利要求1所述的一种单分散镍钴铝球形前驱体的制备方法,其特征在于所述镍化合物、钴化合物和铝化合物的投料摩尔比为0.70~0.90︰0.10~0.20 ︰0.00~0.10。
3.根据权利要求2所述的一种单分散镍钴铝球形前驱体的制备方法,其特征在于所述步骤1)中所述在溶剂溶解时,镍化合物、钴化合物和铝化合物的混合溶液浓度为1~2mol/L。
4.根据权利要求1所述的一种单分散镍钴铝球形前驱体的制备方法,其特征在于所述步骤2)中,超声雾化雾化器的频率为1.7MHz±0.17MHz,雾化蒸发温度为150℃~600℃。
5.根据权利要求1所述的一种单分散镍钴铝球形前驱体的制备方法,其特征在于所述步骤2)中,高温干燥时,在高温干燥室中金属箔材作为集料体,所用箔材为铂箔、金箔、银箔、铝箔、铜箔或不锈钢箔中的至少一种。
6.根据权利要求1所述的一种单分散镍钴铝球形前驱体的制备方法,其特征在于,所述步骤2)中,高温干燥室的温度为150~650℃,干燥时间为2~10h。
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