锌镍电池正极材料镍铝层状双氢氧化物的制备、结构与性能
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摘要
镍铝层状双氢氧化物（Ni-Al LDHs）又称作Al掺杂稳定的α-Ni(OH)_2，充放电时发生α(II)/γ(III)循环，晶格不会出现明显的膨胀或收缩，放电比容量和电压平台较高，可望代替β-Ni(OH)_2用作锌镍电池的正极活性材料，从而明显提高电池的比能量和循环寿命。Ni-Al LDHs常用化学共沉淀法制备，得到的样品往往比表面积较小，粒度分布较宽，电化学性能有待提高。另外，Ni-Al LDHs的电子导电性很差，大倍率放电性能不理想，用作锌镍电池正极材料时与碱性复合电解液和Zn负极的匹配性也有待研究。针对上述问题，本文采用正交试验研究了化学共沉淀法制备Ni-Al LDHs的过程中主要因素对产物电性能的影响，应用喷涂技术对中间产物凝胶状沉淀进行了喷涂处理以改善产物的物理性能和电化学性能，制备出了Co、La共掺杂的Ni-Al LDHs样品，并研究了Ni-Al LDHs正极锌镍电池的电性能，得出的主要结果和结论如下：
1.通过正交试验研究了化学共沉淀法制备Ni-Al LDHs过程中主要因素条件对产物放电比容量的影响。结果表明，在给定因素水平下影响从大到小的顺序依次是原料配比nNi~(2+): nAl~(3+)、凝胶状沉淀的干燥处理温度、粉末研磨尺寸、体系反应温度、pH值和母液陈化时间，较佳的制备条件是原料配比nNi~(2+): nAl~(3+)为85:15，反应温度为45℃，pH值为10.5，陈化时间为36h，干燥处理温度为140℃，粉末研磨尺寸为600目。进一步的研究结果表明，原料配比影响产物的晶型结构和结晶度，降低原料配比可提高产物的结晶度和放电电压平台。干燥处理温度影响产物的结晶度和层板间H2O分子的嵌入量，升高干燥处理温度可提高产物的电化学活性、放电比容量和电极放电电压平台。粉末研磨尺寸影响产物的粒度分布和平均粒径，降低研磨尺寸可提高产物的电化学活性和放电比容量。
2.在化学共沉淀法制备Ni-Al LDHs的过程中，采用喷涂技术对中间产物凝胶状沉淀进行处理。与常规方法相比，得到的粉末样品有较窄的粒度分布和较高的结晶度，比表面积由6.8m~2/g提高到14.1m~2/g，电极反应可逆性较好，有更高的电化学活性、放电比容量和电极循环稳定性。以0.5C倍率进行充放电时，样品的最高放电比容量和平均放电比容量分别达到347.5mAh/g和337.9mAh/g，循环100次后容量保持率为95.4%。
3.采用化学共沉淀法制备出了Co、La共掺杂的Ni-Al LDHs。样品颗粒呈松散的球形或类球形，平均粒径在5μm以下，比表面积高达132.5m~2/g。层板间嵌入有较多的H_2O分子和CO_3~(2-)、NO_3~-杂质阴离子，并与金属阳离子或OH~-形成较强的配位作用，从而提高了层状结构的稳定性，充放电循环100周后材料的晶型结构仍为α相。循环伏安测试结果表明，样品电极反应的可逆性好，质子扩散系数D0达到5.7×10~(-9)cm~2/s。充放电结果表明，样品电化学活性高，1C倍率充放电时平均比容量达到311.5mAh/g，电极循环稳定性好，有较低的充电电压和较高的放电电压平台，高放电倍率下表现更突出。按相同方法制备的Co掺杂样品颗粒呈不规则角块状，比表面积仅为5.4m~2/g，而且粒度分布宽，电化学活性低，电极反应可逆性差，放电电压平台和循环稳定性均不理想。La掺杂样品的物理性能和电化学活性等与Co、La共掺杂样品接近，但放电比容量明显偏低。
4.将喷涂处理制备的Ni-Al LDHs样品用作正极活性材料制备锌镍实验电池，并研究了其充放电循环性能。结果表明，实验电池的平均放电比容量达到308.6mAh/g（以正极活性物质的质量计算），明显高于球形β-Ni(OH)_2正极锌镍实验电池，而且1C倍率下电池的放电中值电压比后者约高出57mV。实验电池放电倍率增大至5C后电压平台下降较明显，但中值电压仍可达1.60V以上。实验电池的循环性能受电解液的影响较大，采用7mol/L KOH电解液时循环40次后放电容量呈快速下降趋势且波动明显，采用3.2mol/L KOH~+1.8mol/L K2CO3~+1.8mol/L KF复合电解液时电池循环性能得到显著改善，120次循环容量保持率在90%以上。但采用复合电解液时实验电池的充放电性能略有下降，其原因是电荷转移步骤的阻抗增大，阳极氧化和阴极还原时更容易极化，电极可逆性变差。进一步的研究结果表明，负极活性物质ZnO的溶解对实验电池的放电容量、循环寿命以及充放电性能影响均较明显，采用复合电解液时ZnO的溶解得到了有效抑制，因而电池的循环寿命得到显著提高。
Ni-Al layered double hydroxides (Ni-Al LDHs), also known as stable α-Ni(OH)_2dopedwith Al, follows the α(II)/γ(III) cycle and the crystal lattice doesn’t obviously expand orshrink during charge-discharge process. It also has higher specific discharge capacity anddischarge voltage plateau than β-Ni(OH)_2. Those advantages make it a promising substitute ascathode active material for Zn/Ni batteries. The specific energy and cycle life of the batteriesshould be enhanced markedly. Ni-Al LDHs is often synthesized by chemical co-precipitationmethod. However, the samples obtained normally have small specific surface areas, wideparticle distribution ranges and not ideal electrochemical performances. Moreover, lowelectronic conductivity of Ni-Al LDHs results in poor discharge performance at high rates. Onthe other hand, the matching properties of Ni-Al LDHs electrode with alkaline compoundelectrolyte and Zn anode need to be researched also. Aiming at those problems, thedissertation used orthogonal experiments to study the influence of main factors in thesynthesis process on the electrochemical performances of Ni-Al LDHs. Spray technique wasapplied to treat the gel precipitate intermediate to improve the physical properties andelectrochemical performances of the product. Ni-Al LDHs sample doped with Co and La wasprepared also. Finally, the performances of Zn/Ni battery with Ni-Al LDHs cathode materialwere studied. The main results and conclusions obtained were as follows:
1. The influence of main factors in the synthesis process with chemical co-precipitationmethod on the specific discharge capacity of Ni-Al LDHs product was studied by orthogonalexperiments. The experimental results showed that the influence order from great to smallwas raw material ratio nNi~(2+): nAl~(3+), drying temperature of gel precipitate, grinding size of thepowder, reaction temperature, pH value and aging temperature of mother solution. Thepreferable synthesis condition was that the raw material ratio nNi~(2+): nAl~(3+)was85:15, reactiontemperature was45℃, pH value was10.5, aging time was36h, drying temperature was140℃, and grinding size was600mesh. Further research results showed that the raw materialratio affected the crystal structure and crystallinity of the product. Reducing the material ratiocould enhance the crystallinity of the product and the discharge voltage plateau of electrode.Drying temperature affected the crystallinity and intercalation content of water molecular between the layer plates. Elevating the drying temperature could enhance the electrochemicalactivity, discharge specific capacity of the product and discharge voltage plateau of theelectrode. Grinding size of the powder influenced the particle size distribution and averageparticle size. Reducing the grinding size could enhance the electrochemical activity anddischarge specific capacity of the final sample.
2. Spray technique was used to treat the gel-like intermediate in the synthesis process ofNi-Al LDHs with chemical co-precipitation method. Comparing with that obtained by normalmethod, the powder sample had more narrow particle distribution range and highercrystallinity, and the specific surface area increased from6.8m~2/g to14.1m~2/g.Electrochemical testing results showed that the sample had higher electrochemical activityand discharge specific capacity. The electrode reaction was more reversible and showed bettercycle stability. The highest and average specific discharge capacity of the sample reached347.5mAh/g and337.9mAh/g at0.5C rate, respectively. Meanwhile, the capacity retentionrate was95.4%after100cycles.
3. Ni-Al LDHs doped with both Co and La was synthesized by chemicalco-precipitation method. The sample obtained consisted of loose spherical particles with sizebelow5μm, while its specific surface area reached132.5m~2/g. The crystal structure retained αphase well after charge-discharged for100cycles. CV testing results showed that theelectrode had better reversibility and the proton diffusion coefficient reached5.7×10~(-9)cm~2/s.Charged-discharge testing results showed that the sample had higher electrochemical activityand its average discharge capacity attained311.5mAh/g at1C rate. The electrode had bettercycle stability, lower charge but higher discharge voltage plateau, which was moreoutstanding at higher rate. The sample doped with Co only synthesized with the same methodhad irregular particle shape, a much small specific surface area of5.4m~2/g and wider particledistribution range. Meanwhile, the electrochemical activity was lower, and the reversibility ofthe electrode reaction was poorer. Neither the discharge voltage plateau nor the cycle stabilitywas ideal. As for the sample doped with La only, though it had quite similar physicalproperties and electrochemical activity to that of the sample doped with both Co and La, butits specific discharge capacity was obviously lower.
4. Zn/Ni experimental battery was manufactured with Ni-Al LDHs sample synthesized by spray technique as cathode active material, and the charge-discharge cycling performancewas studied. Experimental results showed that the average discharge capacity of the batteryreached308.6mAh/g (calculated with the mass of cathode active material), which wasobviously higher than that with β-Ni(OH)_2. And, the middle discharge voltage was about57mV higher than that of the latter. Although the discharge voltage plateau reduced remarkablyat5C rate, the middle voltage was still above1.60V. Further experimental results showed thatthe cycle performance of the battery was affected by the electrolyte used greatly. With7mol/L KOH electrolyte, the discharge capacity reduced quickly and fluctuated obviously after40cycles. While with3.2mol/L KOH~+1.8mol/L K_2CO_3~+1.8mol/L KF compoundelectrolyte, the cycle performance was improved markedly and the capacity retention rateexceeded90%after120cycles. Slight decrease of the charge and discharge performances wasfound with the compound electrolyte, because the impedance of charge transfer step and thepolarization of anodic oxidation and cathodic reduction increased. Further experimentalresults showed that the dissolution of anode active material ZnO affected the dischargecapacity, cycle life and charge-discharge performance distinctly. Using the compoundelectrolyte inhibited the dissolving of ZnO and enhanced the cycle life of battery significantly.
1.通过正交试验研究了化学共沉淀法制备Ni-Al LDHs过程中主要因素条件对产物放电比容量的影响。结果表明，在给定因素水平下影响从大到小的顺序依次是原料配比nNi~(2+): nAl~(3+)、凝胶状沉淀的干燥处理温度、粉末研磨尺寸、体系反应温度、pH值和母液陈化时间，较佳的制备条件是原料配比nNi~(2+): nAl~(3+)为85:15，反应温度为45℃，pH值为10.5，陈化时间为36h，干燥处理温度为140℃，粉末研磨尺寸为600目。进一步的研究结果表明，原料配比影响产物的晶型结构和结晶度，降低原料配比可提高产物的结晶度和放电电压平台。干燥处理温度影响产物的结晶度和层板间H2O分子的嵌入量，升高干燥处理温度可提高产物的电化学活性、放电比容量和电极放电电压平台。粉末研磨尺寸影响产物的粒度分布和平均粒径，降低研磨尺寸可提高产物的电化学活性和放电比容量。
2.在化学共沉淀法制备Ni-Al LDHs的过程中，采用喷涂技术对中间产物凝胶状沉淀进行处理。与常规方法相比，得到的粉末样品有较窄的粒度分布和较高的结晶度，比表面积由6.8m~2/g提高到14.1m~2/g，电极反应可逆性较好，有更高的电化学活性、放电比容量和电极循环稳定性。以0.5C倍率进行充放电时，样品的最高放电比容量和平均放电比容量分别达到347.5mAh/g和337.9mAh/g，循环100次后容量保持率为95.4%。
3.采用化学共沉淀法制备出了Co、La共掺杂的Ni-Al LDHs。样品颗粒呈松散的球形或类球形，平均粒径在5μm以下，比表面积高达132.5m~2/g。层板间嵌入有较多的H_2O分子和CO_3~(2-)、NO_3~-杂质阴离子，并与金属阳离子或OH~-形成较强的配位作用，从而提高了层状结构的稳定性，充放电循环100周后材料的晶型结构仍为α相。循环伏安测试结果表明，样品电极反应的可逆性好，质子扩散系数D0达到5.7×10~(-9)cm~2/s。充放电结果表明，样品电化学活性高，1C倍率充放电时平均比容量达到311.5mAh/g，电极循环稳定性好，有较低的充电电压和较高的放电电压平台，高放电倍率下表现更突出。按相同方法制备的Co掺杂样品颗粒呈不规则角块状，比表面积仅为5.4m~2/g，而且粒度分布宽，电化学活性低，电极反应可逆性差，放电电压平台和循环稳定性均不理想。La掺杂样品的物理性能和电化学活性等与Co、La共掺杂样品接近，但放电比容量明显偏低。
4.将喷涂处理制备的Ni-Al LDHs样品用作正极活性材料制备锌镍实验电池，并研究了其充放电循环性能。结果表明，实验电池的平均放电比容量达到308.6mAh/g（以正极活性物质的质量计算），明显高于球形β-Ni(OH)_2正极锌镍实验电池，而且1C倍率下电池的放电中值电压比后者约高出57mV。实验电池放电倍率增大至5C后电压平台下降较明显，但中值电压仍可达1.60V以上。实验电池的循环性能受电解液的影响较大，采用7mol/L KOH电解液时循环40次后放电容量呈快速下降趋势且波动明显，采用3.2mol/L KOH~+1.8mol/L K2CO3~+1.8mol/L KF复合电解液时电池循环性能得到显著改善，120次循环容量保持率在90%以上。但采用复合电解液时实验电池的充放电性能略有下降，其原因是电荷转移步骤的阻抗增大，阳极氧化和阴极还原时更容易极化，电极可逆性变差。进一步的研究结果表明，负极活性物质ZnO的溶解对实验电池的放电容量、循环寿命以及充放电性能影响均较明显，采用复合电解液时ZnO的溶解得到了有效抑制，因而电池的循环寿命得到显著提高。
Ni-Al layered double hydroxides (Ni-Al LDHs), also known as stable α-Ni(OH)_2dopedwith Al, follows the α(II)/γ(III) cycle and the crystal lattice doesn’t obviously expand orshrink during charge-discharge process. It also has higher specific discharge capacity anddischarge voltage plateau than β-Ni(OH)_2. Those advantages make it a promising substitute ascathode active material for Zn/Ni batteries. The specific energy and cycle life of the batteriesshould be enhanced markedly. Ni-Al LDHs is often synthesized by chemical co-precipitationmethod. However, the samples obtained normally have small specific surface areas, wideparticle distribution ranges and not ideal electrochemical performances. Moreover, lowelectronic conductivity of Ni-Al LDHs results in poor discharge performance at high rates. Onthe other hand, the matching properties of Ni-Al LDHs electrode with alkaline compoundelectrolyte and Zn anode need to be researched also. Aiming at those problems, thedissertation used orthogonal experiments to study the influence of main factors in thesynthesis process on the electrochemical performances of Ni-Al LDHs. Spray technique wasapplied to treat the gel precipitate intermediate to improve the physical properties andelectrochemical performances of the product. Ni-Al LDHs sample doped with Co and La wasprepared also. Finally, the performances of Zn/Ni battery with Ni-Al LDHs cathode materialwere studied. The main results and conclusions obtained were as follows:
1. The influence of main factors in the synthesis process with chemical co-precipitationmethod on the specific discharge capacity of Ni-Al LDHs product was studied by orthogonalexperiments. The experimental results showed that the influence order from great to smallwas raw material ratio nNi~(2+): nAl~(3+), drying temperature of gel precipitate, grinding size of thepowder, reaction temperature, pH value and aging temperature of mother solution. Thepreferable synthesis condition was that the raw material ratio nNi~(2+): nAl~(3+)was85:15, reactiontemperature was45℃, pH value was10.5, aging time was36h, drying temperature was140℃, and grinding size was600mesh. Further research results showed that the raw materialratio affected the crystal structure and crystallinity of the product. Reducing the material ratiocould enhance the crystallinity of the product and the discharge voltage plateau of electrode.Drying temperature affected the crystallinity and intercalation content of water molecular between the layer plates. Elevating the drying temperature could enhance the electrochemicalactivity, discharge specific capacity of the product and discharge voltage plateau of theelectrode. Grinding size of the powder influenced the particle size distribution and averageparticle size. Reducing the grinding size could enhance the electrochemical activity anddischarge specific capacity of the final sample.
2. Spray technique was used to treat the gel-like intermediate in the synthesis process ofNi-Al LDHs with chemical co-precipitation method. Comparing with that obtained by normalmethod, the powder sample had more narrow particle distribution range and highercrystallinity, and the specific surface area increased from6.8m~2/g to14.1m~2/g.Electrochemical testing results showed that the sample had higher electrochemical activityand discharge specific capacity. The electrode reaction was more reversible and showed bettercycle stability. The highest and average specific discharge capacity of the sample reached347.5mAh/g and337.9mAh/g at0.5C rate, respectively. Meanwhile, the capacity retentionrate was95.4%after100cycles.
3. Ni-Al LDHs doped with both Co and La was synthesized by chemicalco-precipitation method. The sample obtained consisted of loose spherical particles with sizebelow5μm, while its specific surface area reached132.5m~2/g. The crystal structure retained αphase well after charge-discharged for100cycles. CV testing results showed that theelectrode had better reversibility and the proton diffusion coefficient reached5.7×10~(-9)cm~2/s.Charged-discharge testing results showed that the sample had higher electrochemical activityand its average discharge capacity attained311.5mAh/g at1C rate. The electrode had bettercycle stability, lower charge but higher discharge voltage plateau, which was moreoutstanding at higher rate. The sample doped with Co only synthesized with the same methodhad irregular particle shape, a much small specific surface area of5.4m~2/g and wider particledistribution range. Meanwhile, the electrochemical activity was lower, and the reversibility ofthe electrode reaction was poorer. Neither the discharge voltage plateau nor the cycle stabilitywas ideal. As for the sample doped with La only, though it had quite similar physicalproperties and electrochemical activity to that of the sample doped with both Co and La, butits specific discharge capacity was obviously lower.
4. Zn/Ni experimental battery was manufactured with Ni-Al LDHs sample synthesized by spray technique as cathode active material, and the charge-discharge cycling performancewas studied. Experimental results showed that the average discharge capacity of the batteryreached308.6mAh/g (calculated with the mass of cathode active material), which wasobviously higher than that with β-Ni(OH)_2. And, the middle discharge voltage was about57mV higher than that of the latter. Although the discharge voltage plateau reduced remarkablyat5C rate, the middle voltage was still above1.60V. Further experimental results showed thatthe cycle performance of the battery was affected by the electrolyte used greatly. With7mol/L KOH electrolyte, the discharge capacity reduced quickly and fluctuated obviously after40cycles. While with3.2mol/L KOH~+1.8mol/L K_2CO_3~+1.8mol/L KF compoundelectrolyte, the cycle performance was improved markedly and the capacity retention rateexceeded90%after120cycles. Slight decrease of the charge and discharge performances wasfound with the compound electrolyte, because the impedance of charge transfer step and thepolarization of anodic oxidation and cathodic reduction increased. Further experimentalresults showed that the dissolution of anode active material ZnO affected the dischargecapacity, cycle life and charge-discharge performance distinctly. Using the compoundelectrolyte inhibited the dissolving of ZnO and enhanced the cycle life of battery significantly.
引文
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