Article(id=1320107552248016950, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320107530261479891, articleNumber=null, orderNo=null, doi=10.14062/j.issn.0454-5648.20250553, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1752422400000, receivedDateStr=2025-07-14, revisedDate=1757347200000, revisedDateStr=2025-09-09, acceptedDate=null, acceptedDateStr=null, onlineDate=1792667766868, onlineDateStr=2026-10-22, pubDate=1777305600000, pubDateStr=2026-04-28, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1792667766868, onlineIssueDateStr=2026-10-22, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1792667766868, creator=13701087609, updateTime=1792667766868, updator=13701087609, issue=Issue{id=1320107530261479891, tenantId=1146029695717560320, journalId=1263187385517883426, year='2026', volume='54', issue='7', pageStart='2171', pageEnd='2576', issueExtLink='null', onlineDate='null', pubDate='1784476800000', pubDateStr='2026-07-20', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1792667761625, creator='13701087609', updateTime=1792720444956, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1320328500238725499, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320107530261479891, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1320328500238725500, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320107530261479891, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=2445, endPage=2457, ext={EN=ArticleExt(id=1320107552440954935, articleId=1320107552248016950, tenantId=1146029695717560320, journalId=1263187385517883426, language=EN, title=Oxygen Vacancy-Engineered Co
3Zn
1Mn
0.5O
5 Nanoflowers for Supercapacitor Applications, columnId=1263922769897599102, journalTitle=Journal of the Chinese Ceramic Society, columnName=Research Articles, runingTitle=null, highlight=null, articleAbstract=
Introduction Achieving the "carbon peaking and carbon neutrality" targets requires efficient energy storage technologies. Supercapacitors with the high power density, rapid charge-discharge, and long cycle life show a great potential in renewable energy, electric vehicles, and smart grids. However, their low energy density limits wider applications. Transition metal oxides such as RuO2 and MnO2 are promising electrode materials due to their reversible faradaic reactions and high theoretical capacitance. Single-component oxides suffer from insufficient active sites and structural degradation, impairing rate capability and stability. Multi-metal oxide strategies leverage synergistic effects to optimize lattice, charge distribution, morphology, and performance. Cobalt-based oxides provide abundant Co2+/Co3+ redox pairs, manganese adds multiple valence states and structural buffering, while zinc enhances conductivity and stability. Nevertheless, low conductivity and poor kinetics persist. Oxygen vacancies improve conductivity, tune band structure, and create active sites via reducing bandgap and accelerating kinetics. In this work, oxygen-vacancy-rich Ov-Co3Zn1Mn0.5O5 nanoflowers were synthesized via hydrothermal-annealing-NaBH4 reduction and multi-metal synergy and defect engineering to optimize morphology and electronic structure. This approach could validate the synergistic benefits and offer a strategy for high-performance transition metal oxide supercapacitor electrodes.
Methods All chemicals were of analytical grade and used as received. Nickel foam substrates (2 cm × 3 cm) were pretreated in HCl solution of 3 mol/L under ultrasonication for 5 min to remove surface oxides and thoroughly rinsed with deionized water. For the synthesis of Co3Zn1Mn0.5O5, stoichiometric amounts of Co(CH3COO)2·6H2O (3 mmol), Zn(CH3COO)2·H2O (1 mmol), MnC4H6O4·4H2O (0.5 mmol), and urea (0.2 g) were dissolved in deionized water of 60 mL to form a homogeneous precursor solution. The solution together with the pretreated nickel foam was sealed in a 100 mL Teflon-lined autoclave and maintained at 120 ℃ for 6 h. After natural cooling, the nickel foam-supported precursor was washed, dried, and subsequently annealed in air at 400 ℃ for 2 h, yielding Co3Zn1Mn0.5O5 with a mass loading of 1.12 mg·cm-2. For comparison, binary and other ternary oxides (i.e., Co3Zn1O4, Co3Mn0.5O4, Zn1Mn0.5O2, Co2Zn1Mn0.5O4, and Co4Zn1Mn0.5O6) were prepared under the same conditions above. Oxygen vacancies were introduced via immersing the annealed Co3Zn1Mn0.5O5 in NaBH4 solution for 12 min, followed by vacuum drying at 80 ℃ for 2 h to obtain Ov-Co3Zn1Mn0.5O5 (a mass loading of 1.02 mg·cm-2). Comparative samples Ov-Co2Zn1Mn0.5O4 and Ov-Co4Zn1Mn0.5O6 were also prepared.
The morphology was determined by field-emission scanning electron microscopy (S-4800, Hitachi Co., Japan) and transmission electron microscopy (JEM-2100F, JEOL Co., Japan). The rystal structure was identified by X-ray diffraction (D/MAX-2500, Rigaku Co., Japan, Cu Kα, λ = 0.154156 nm). The surface chemical states and valence distributions were analyzed by X-ray photoelectron spectroscopy (K-Alpha, Thermo Co., USA). The oxygen vacancy concentration was quantified by electron paramagnetic resonance (EMXplus, Bruker Co., Germany) and thermogravimetric analysis (TG 209 F3 Netzsch Co., Germany). The electrochemical measurements were conducted in a three-electrode configuration with 6 mol/L KOH electrolyte using a CHI760e workstation. The cyclic voltammetry and galvanostatic charge-discharge within 0-0.5 V at different scan rates of 10-100 mV·s-1 and various current densities were detremined. The electrochemical impedance spectroscopy was performed on a BioLogic SP-150 workstation. The density functional theory calculations were carried out by a software named Materials Studio package using the projector-augmented wave method.
Results and discussion The three-step hydrothermal-annealing-NaBH4 reduction process yields uniform flower-like Ov-Co3Zn1Mn0.5O5 nanoflowers directly grown on nickel foam. The SEM images reveal that the binary oxides display irregular nanosheets or nanowires, whereas the ternary Co3Zn1Mn0.5O5 forms large-sized nanosheets assembled into a loose porous flower-like morphology that provides abundant redox active sites. After NaBH4 treatment, the overall morphology is preserved, while porosity is markedly increased. The TEM images confirm the porous nanosheet structure in the both samples, with Co3Zn1Mn0.5O5 exhibiting more mesopores and atomic-level defects evidenced by disordered lattice fringes. The HRTEM images display lattice spacings of 0.202 nm and 0.156 nm, corresponding to the plane (400) of MnCo2O4.5 and the plane (511) of ZnCo2O4. The EDS mapping shows a homogeneous distribution of elements Co, Zn, Mn and O, and Mn content is lower than the nominal ratio. The XRD patterns confirm the coexistence of cubic spinel MnCo2O4.5 and ZnCo2O4 phases in all the samples, and Ov-Co3Zn1Mn0.5O5 shows a higher crystallinity. The TGA and EPR unambiguously verify abundant oxygen vacancies. The XPS analysis reveals positive shifts in Co 2p, Mn 2p, Zn 2p, and O 1s binding energies after reduction, accompanied by increased proportions of low-valence Co2+, Mn3+, and a larger OV peak area, confirming mixed-valence states and defect formation. The results of electrochemical tests demonstrate clear synergistic effects. The CV curves at 10 mV·s-1 exhibit the largest integrated area for the ternary composition. The oxygen-vacancy introduction further enlarges the area due to more active sites and lowered OH- intercalation barrier. The b-values of 0.70 and 0.77 indicate combined diffusion and pseudocapacitive contributions. The GCD measurements deliver an ultrahigh specific capacitance of 1509.8 F·g-1 at 2 A·g-1 and retain 809.1 F·g-1 at 20 A·g-1, demonstrating an excellent rate capability. The assembled Ov-Co3Zn1Mn0.5O5//AC asymmetric supercapacitor maintains stable CV shapes up to 100 mV·s-1 within a 1.6 V window, achieves a high energy density of 53.8 W·h·kg-1 at 750 W·kg-1, and retains 76.4% capacitance after 5000 cycles with the Coulombic efficiency of 99%. The DFT calculations reveal that oxygen vacancies eliminate the original 0.098 eV bandgap, introduce mid-gap defect states, increase carrier concentration and facilitate electron hopping between low-valence Co2+and Mn3+ sites, thereby significantly enhancing conductivity and redox kinetics.
Conclusions The flower-like Ov-Co3Zn1Mn0.5O5 with rich oxygen vacancies was successfully synthesized by a facile hydrothermal-annealing-NaBH4 reduction method. The unique nanosheets-assembled nanoflower structure could expose abundant active sites and enhance redox kinetics. The introduction of oxygen vacancies regulated the electronic structure, improved conductivity, and induced low-valence Co2+ and intermediate Mn3+ to promote redox reactions. The Ov-Co3Zn1Mn0.5O5 electrode delivered a high specific capacitance of 1509.8 F·g-1 at 2 A·g-1 with the excellent rate performance. The assembled asymmetric supercapacitor achieved 53.8 W·h·kg-1 energy density at 750 W·kg-1 and retained 76.4% of its initial capacitance after 5000 cycles with the Coulombic efficiency of 99%. This work could demonstrate the synergistic optimization of multi-metal composition and oxygen vacancy engineering for advanced transition metal oxide electrodes in supercapacitors.
, authors=Xiaohua ZHANG, Kangjie HAN, Xinyu GAN, Changwei GONG, Xinxin ZHAO, Xiaoyan YAN, authorsList=Xiaohua ZHANG, Kangjie HAN, Xinyu GAN, Changwei GONG, Xinxin ZHAO, Xiaoyan YAN, authorCompany=null, correspAuthors=null, authorNote=
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3Zn
1Mn
0.5O
5超级电容器电极材料的制备及性能, columnId=1263922770220560512, journalTitle=硅酸盐学报, columnName=研究论文, runingTitle=null, highlight=null, articleAbstract=
针对过渡金属氧化物导电性能差和电化学利用率低的问题，优化设计了具有氧空位（Ov）的三元金属氧化物Ov-Co3Zn1Mn0.5O5电极材料。通过多金属协同调控和NaBH4还原处理，成功实现了材料形貌与电子结构的双重优化：1）独特的花状纳米片组装结构提供了丰富的电化学活性位点；2）引入的氧空位有效调节电子结构，促进多价态金属离子的形成，显著提升材料的导电性和电荷传输动力学。得益于这种协同优化，Ov-Co3Zn1Mn0.5O5电极展现出优异的储能性能，比电容高达1509.8 F·g-1。组装的非对称超级电容器（Ov-Co3Zn1Mn0.5O5//活性炭）在750.0 W·kg-1的功率密度下实现53.8 W·h·kg-1的高能量密度，并且经过5000次循环后仍能保持809.1 F·g-1的比电容和99%的库伦效率。该研究为通过形貌设计和缺陷工程协同优化过渡金属氧化物储能性能提供了新思路。
, authors=张晓华, 韩康杰, 甘欣雨, 宫长伟, 赵新新, 闫晓燕, authorsList=张晓华, 韩康杰, 甘欣雨, 宫长伟, 赵新新, 闫晓燕, authorCompany=null, correspAuthors=null, authorNote=
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张晓华（1992—），女，博士，副教授。
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