Metalorganic Deposition Research Articles

Single-coated thick superconducting films for metal–organic deposition using trifluoroacetates

Metal-organic deposition using trifluoroacetates (TFA-MOD) is known to yield uniform superconducting wires by a liquid growth mode. However, it has been difficult to prepare thick films because of drying stress during the calcining process. To avoid the drying stress, conventional crack-preventing chemicals such as H(CH2)8COOH are applied in conventional metal–organic deposition. However, large amounts of hydrogen atoms react with fluorine atoms during calcining process in TFA-MOD, and the consequent increased harmful carbon residue decreases superconductivity of the resulting films. To avoid the chemical reaction, new crack-preventing chemicals such as H(CF2)8COOH were applied to prepare single-coated thick films. A low ratio of hydrogen atoms decreases the chemical reaction and generates hydrogen fluorine gas, consequently suppressing the carbon residue. Above the calcining temperature, the crack-preventing chemical is decomposed into low-boiling-point chemicals such as CF2CF2 or CF3CF3. Consequently, single-coated thick film having low carbon residue and sufficient superconducting current per width was realized. For a long time, the authors have studied other possible candidate crack-preventing chemicals. Newly introduced fluorine ion measurement of decomposed materials during the calcining process revealed the nature of the crack-preventing chemicals. Based on the accumulated results, we have concluded that among over one million chemicals there are only two groups suitable for preparing single-coated thick superconducting films by TFA-MOD. One group is hydrogenated perfluoro-carboxylic acids such as H(CF2)8COOH and the other group is perfluoro di-carboxylic acids. With H(CF2)8COOH, using a single-coating process we were able to achieve a 560 nm-thick YBa2Cu3O6.93 film having Jc of 4.70 MA/cm2 (77 K,0T). Compared with a standard 150 nm-thick YBa2Cu3O6.93 film having Jc of 7.70 MA/cm2 (77 K,0T), the critical current per width is improved to about 227 %.

Lateral NiO/AlN Heterojunction Rectifiers with Breakdown Voltage >11 kV

Lateral NiO/AIN heterojunction diodes (HJDs) with breakdown voltage up to 11.6 kV and Ni/Au/AlN Schottky barrier diodes (SBDs) with VB of 8.6 kV were fabricated on layers grown on sapphire substrates by metalorganic chemical vapor phase deposition. The power figure-of-merits VB 2/RON where RON is the on-resistance were 0.31 MW·cm−2 for HJD and 0.16 MW·cm−2 for SBD. The lowest turn-on voltages were ∼2.03 and 1.91 V for HJDs and SBDs, respectively, with ON/OFF ratios up to 102. The maximum field before breakdown was 0.45 MV·cm−1 in HJDs and 0.31 MV·cm−1 in SBDs. These correspond to <3% of the critical field in AlN of ∼15 MV·cm−1. This work demonstrates there is still significant optimization to be done in the overall quality of the AlN, including purity, crystal perfection, and defect density to realize the potential of this material as an ultra-wide bandgap semiconductor for efficient multi-kV power switching applications. Our results also demonstrate the promise of NiO as a p-type conducting oxide for forming heterojunctions with AlN.

The flux pinning effect of different doping element combinations on metal-organic deposition-derived YBa2Cu3O7−δ nanocomposite films

Elemental doping has been proven effective in improving the flux pinning of yttrium barium copper oxide (YBa2Cu3O7−δ, YBCO) nanocomposite thin films. In the present work, we increased the number of doping elements to five to investigate the flux pinning effect of YBCO. The Zr-doped, Zr, Hf and Sn co-doped, Zr, Hf, Sn and Ta co-doped, and Zr, Hf, Sn, Ta and Mn co-doped YBCO films deposited on LaMnO3/MgO/Y2O3/Al2O3/ Hastelloy substrate were systematically studied. The samples were prepared by low-fluorine metal-organic deposition method, with a total dopant of 8 mol%. All films exhibit good c-axis growth and the multi-doping helps refining the surface particles, resulting in a smoother surface. The in-field properties of the films increase with the increase of co-doped element numbers, especially at a low temperature of 30 K. The pinning force density (Fp) and critical current density (Jc) are significantly improved by five-element Zr, Hf, Sn, Ta and Mn co-doped, which is about 3 times and 1.6 times higher, respectively, than that of the undoped film at 30 K and 1 T.

Study on rapid growth and improved performance of superconducting YBa2Cu3O7-δ coated conductors assisted by transient liquid phase

This study employs a fluorine-free metal organic deposition method (FF-MOD), with transient liquid phase assistance, to expedite the growth (TLAG) of superconducting YBa2Cu3O7-δ (YBCO) thin films on LaMnO3 metal substrates. The research evaluates the phase formation and performance of YBCO films with varying proportions of preformed BaZrO3 (BZO) nanocrystals. The experimental results indicate that the optimal proportion for incorporating BZO nanocrystals is 5 %, leading to the YBCO film displaying critical current density at 77 K under zero-field conditions. This achievement marks a significant advancement in the rapid growth of YBCO films on metal substrates with enhanced current-carrying capacity. Additionally, the research assesses the changes in overall uniformity and microstrain of YBCO films after the addition of BZO nanocrystals, shedding light on the key factors contributing to performance enhancement and offering insights for future improvements. This investigation offers valuable insights for attaining high-speed, high-performance growth of superconducting YBCO coating conductors.

Flexible LaNiO3 film with both high electrical conductivity and mechanical robustness

Lanthanum nickel oxide (LaNiO3, LNO) films exhibit excellent electrical conductivity but poor mechanical properties, considerably limiting their further development in the field of flexible electronics. In this study, flexible LNO thin films of different thicknesses were fabricated on a unique two-dimensional (2D) mica platform using a simple metal organic deposition technique. The obtained LNO films exhibited a pseudocubic phase without impurities. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) characterisations proved that the films were well-crystallised, dense, and flat, with controllable thickness. In addition, the flexible LNO/mica element possesses low resistivity (5 × 10−4 Ω cm), translucency, and good bending resistance. The electrical resistivity can remain stable under various bending radii (r = 10∼2 mm), thousands of bending cycles, and a wide temperature range (28–200 °C), demonstrating good durability, mechanical stability and temperature resistance. Furthermore, a ferroelectric BiFeO3 film was constructed based on the obtained conductive LNO electrode, which exhibited typical ferroelectric characteristics. This excellent performance suggests that the flexible LNO electrode is promising for flexible electronic applications.

Introduction of BaMO3 artificial pins into high mixing entropy FF-MOD REBCO thin films

Abstract We have synthesized middle-entropy type REBCO (ME-REBCO) and high-entropy type REBCO (HE-REBCO) superconducting thin films with BaCeO3 artificial pins by fluorine-free metal organic deposition (FF-MOD) method and evaluated their crystallinity and superconducting properties. The c-axis orientation of crystals was confirmed by XRD analysis for all thin films. The superconducting transition temperatures in all films were over 90 K. STEM observation revealed that the crystal lattice of HE-REBCO was slightly distorted compared to a normal GdBCO film. This distortion is expected to be a “backlash” in the crystal and contribute to an increase in the allowable amounts of artificial pins. The critical current densities and flux pinning force densities at 77.3 K were enhanced by Ce doping, indicating that BaCeO3 artificial pins were introduced into the FF-MOD ME-REBCO and HE-REBCO films.

Synthesis and characterization of BaIrO3-doped YBCO superconducting thin films via TFA-MOD technique

High-temperature superconducting materials (HTS) are characterized by remarkably high critical current density (Jc) values when exposed to low temperatures and magnetic fields. In the realm of such investigations, various crystalline imperfections, including finely dispersed non-superconducting phases, dislocations, vacancies, grain boundaries, twin boundaries, antiphase boundaries, and insulating regions within grain boundaries, have been recognized as potential sources of pinning centers. However, it is essential to acknowledge that Jc values experience a rapid decline as the temperature rises in the presence of a magnetic field. The primary contributing factors to this decline are attributed to the intrinsic crystalline anisotropy of HTS materials and the thermal fluctuations that prevail at elevated temperatures. Nevertheless, a noteworthy factor in the diminishment of Jc values is the scarcity of efficacious pinning centers. In response to these challenges, a pioneering technology has emerged, revolving around nanostructure engineering for the deliberate creation of artificial pinning centers within HTS materials. In alignment with this approach, the present study endeavors to augment the critical current density and enhance the flux pinning properties of YBa2Cu3O6.56 (YBCO) superconducting films. This augmentation is achieved through the integration of BaIrO3 (BIO) perovskite nanodots, nanorods, or nanoparticles as strategically positioned pinning centers. The films are deposited on a SrTiO3 (STO) substrate employing the Trifluoroacetate Metal–Organic Deposition (TFA-MOD) technique. This research initiative seeks to contribute to the advancement of knowledge regarding the controlled manipulation of artificial pinning centers in HTS materials, particularly focusing on YBCO thin films, with the ultimate goal of enhancing their performance under the influence of elevated magnetic fields.

Reductive Segregation During the Synthesis of Sb−SnO2-Supported Iridium Electrocatalysts for the Oxygen Evolution Reaction

A metal-organic chemical deposition approach using an Ir(acac)3 precursor was employed to synthesise oxide−supported iridium-based electrocatalysts for the oxygen evolution reaction (OER) in acidic media. Inert and oxidising deposition conditions were explored in two temperature regimes, and the influence of these parameters on the physicochemical and electrochemical properties of catalysts consisting of IrOx supported on Sb–SnO2 (ATO) were studied. Surprisingly, it was found that increasing the deposition temperature up to 620 °C favoured the formation of reduced iridium phases even in the presence of an oxidising reaction environment. This was explained by a thermodynamic preference for reduced phases at high temperatures, as well as the presence of acetylacetonate ligand decomposition products serving as reducing agents. Similarly, the reductive segregation of Sb from the ATO support at high temperatures leads to the loss of conductivity of the support, and the formation of Ir–Sb–Sn alloyed nanoparticles. These processes resulted in a loss of OER performance for the materials prepared under high-temperature conditions. Our findings highlight the importance of carefully selecting the temperature range during the synthesis of oxidic support materials and electrocatalysts for the OER.

Elastic and inelastic strain in submicron-thick ZnO epilayers grown on r-sapphire substrates by metal-organic vapour phase deposition.

A significant part of the present and future of optoelectronic devices lies on thin multilayer heterostructures. Their optical properties depend strongly on strain, being essential to the knowledge of the stress level to optimize the growth process. Here the structural and microstructural characteristics of sub-micron a-ZnO epilayers (12 to 770 nm) grown on r-sapphire by metal-organic chemical vapour deposition are studied. Morphological and structural studies have been made using scanning electron microscopy and high-resolution X-ray diffraction. Plastic unit-cell distortion and corresponding strain have been determined as a function of film thickness. A critical thickness has been observed as separating the non-elastic/elastic states with an experimental value of 150-200 nm. This behaviour has been confirmed from ultraviolet photoelectron spectroscopy, X-ray photoelectron spectroscopy and high-resolution transmission electron microscopy measurements. An equation that gives the balance of strains is proposed as an interesting method to experimentally determine this critical thickness. It is concluded that in the thinnest films an elongation of the Zn-O bond takes place and that the plastic strained ZnO films relax through nucleation of misfit dislocations, which is a consequence of three-dimensional surface morphology.

High-voltage AlN Schottky barrier diodes on bulk AlN substrates by MOCVD

This letter reports the demonstration of Aluminum nitride (AIN) Schottky barrier diodes on bulk AlN substrates by metalorganic chemical vapor phase deposition with breakdown voltages exceeding 3 kV. The devices exhibited good rectifying characteristics with ON/OFF ratios of 106–108 and excellent thermal stability from 298 to 623 K. The device Schottky barrier height increased from 0.89 to 1.85 eV, and the ideality factor decreased from 4.29 to 1.95 with increasing temperature, ascribed to the inhomogeneous metal/AlN interface. This work demonstrates the potential of AlN as an ultra-wide bandgap semiconductor for developing multi-kV AlN high-voltage and high-power devices.

Property Tuning through Fine Size Control and Hierarchical Nanostructuring of Metal Oxide Nanoparticles Supported in Porous Matrices: a Review

In the nanoscale, matter presents different properties compared to its bulk counterparts, owing to the considerable increase of the surface/bulk ratio, as well as the occurrence of quantum confinement effects. One method to fine control the growth of nanoparticles, their size and nanostructure is to use metalorganic deposition combined with a porous matrix as host, where pores act as nanoreactors for nanoparticle growth, resulting in chemically integrated systems. In this review, we look at the history and achievements of the chemical method of impregnation-decomposition cycles for the precise size control, property tuning and tailored synthesis of metal oxide nanoparticles. We give an overview of the various oxide nanoparticles and nanomaterials developed over the years, and how the method of impregnation-decomposition cycles allowed the synthesis of pure, doped and core-shell oxide nanoparticles, as well as the tuning of their properties through the combined fine control of nanoparticle size, nanostructure, and composition.

Selector-less crossbar array resistive RAM based on TiO2 fabricated by photochemical metal-organic deposition

In this study, we demonstrated a TiO2-based 32 × 32 crossbar array resistive RAM (ReRAM), a promising candidate for next-generation non-volatile memory (NVM), by utilizing a photochemical metal-organic deposition (PMOD) process. We achieved an interface-type resistive switching device with rectifying characteristics by controlling the oxidation state of directly patterned TiOx films through post-heat treatment. The photochemical reaction induced by UV in the PMOD process and the anatase phase formation during the post-heat treatment were analyzed using Fourier-transform infrared spectroscopy, X-ray diffraction, and X-ray photoelectron spectroscopy (XPS). XPS analysis revealed the immediate formation of Ti peroxide post-PMOD process, underscoring the efficacy of post-heat treatments in controlling oxidation states. Employing 350 °C annealed TiOX as the active material, we successfully fabricated a high-yield (93%), selectorless 32 × 32 crossbar array architecture for ReRAM. Our findings highlight the PMOD process as a viable, cost-effective alternative for memory devices, offering optimized oxidation states crucial for the performance of redox-based ReRAM.

Competitive nucleation and growth control of a- and c-axis YBCO films by metal organic deposition

This paper utilizes the TFA-MOD (Trifluoroacetate Metal-Organic Decomposition) method to prepare YB2C3O7-δ (YBCO) superconducting films on a LaMnO3 metal substrate. Using a self-made process curve, we investigate the nucleation and growth orientation of crystals at various temperatures under specific oxygen partial pressures (PO2). We successfully obtain an oxygen partial pressure-temperature phase diagram at a fixed time. This diagram provides critical insight into the trends that guide our regulation of parameters to ultimately achieve a relatively pure a-axis oriented YBCO film. Temperature and nucleation rate are important parameters that influence crystal nucleation orientation. The key conditions for producing a-axis-oriented YBCO films include low temperature, high Δμ, and extended crystallization time.

Magnetism and Thermal Transport of Exchange-Spring-Coupled La2/3Sr1/3MnO3/La2MnCoO6 Superlattices with Perpendicular Magnetic Anisotropy.

Superlattices (SLs) comprising layers of a soft ferromagnetic metal La2/3Sr1/3MnO3 (LSMO) with in-plane (IP) magnetic easy axis and a hard ferromagnetic insulator La2MnCoO6 (LMCO, out-of-plane anisotropy) were grown on SrTiO3 (100)(STO) substrates by a metalorganic aerosol deposition technique. Exchange spring magnetic (ESM) behavior between LSMO and LMCO, manifested by a spin reorientation transition of the LSMO layers towards perpendicular magnetic anisotropy below TSR = 260 K, was observed. Further, 3ω measurements of the [(LMCO)9/(LSMO)9]11/STO(100) superlattices revealed extremely low values of the cross-plane thermal conductivity κ(300 K) = 0.32 Wm-1K-1. Additionally, the thermal conductivity shows a peculiar dependence on the applied IP magnetic field, either decreasing or increasing in accordance with the magnetic disorder induced by ESM. Furthermore, both positive and negative magnetoresistance were observed in the SL in the respective temperature regions due to the formation of 90°-Néel domain walls within the ESM, when applying IP magnetic fields. The results are discussed in the framework of electronic contribution to thermal conductivity originating from the LSMO layers.

Monodisperse BaZrO3 nanocrystals and flux pinning effect on upscaling MOD-derived (Y,Dy)Ba2Cu3O7− δ superconducting tapes

In the present work, monodisperse BaZrO3 (BZO) nanocrystals with controllable sizes are successfully introduced into trifluoroacetate metal–organic deposition derived (Y,Dy)Ba2Cu3O7−δ ((Y,Dy)BCO)-coated superconducting tapes to act as effective pinning centers. The BZO nanocrystal addition strategy is extended to upscaling coated conductors as long as hundreds of meters, and as thick as 3.4 μm, of (Y,Dy)BCO layers. The corresponding superconducting performances of BZO-added (Y,Dy)BCO-coated conductors are systematically investigated under various applied magnetic fields and temperatures. It is revealed that the I c (77 K, self-field) of BZO-added tapes decreases linearly with BZO concentration, while the corresponding in-field lift-factors increase for all studied BZO additions. In-field J c values under various fields at low temperatures show that the (Y,Dy)BCO tape with 5%-BZO addition exhibits a better performance than that of other concentrations. Besides, this benefit of BZO addition appears identical for both thin and thick samples, as well as for tapes that are hundreds of meters long. The angular dependence of in-field I c also shows that significant improvement occurs in all the studied angular ranges after nanocrystal BZO additions, demonstrating that the nanocrystal addition strategy is of great value for upscaling commercial (Y,Dy)BCO tape for in-field applications.

(Invited) Dilute Anion Alloyed III-Nitride Nanowires for Photoelectrochemical Water Splitting

The record efficiencies in photovoltaic devices and hydrogen production via photoelectrochemical water splitting have been achieved in both cases by employing complex architectures of III-V alloys 1, which has been enabled by the outstanding charge carrier transport properties, band gap and band edge engineering flexibility, as well as highly mismatch growth that can be achieved in III-V alloys by controlling their chemical composition.It has been extensively demonstrated that Molecular Beam Epitaxy (MBE) and Metal-Organic Physical Vapor Deposition (MOPVD) techniques can produce III-V multinary alloys with compositions beyond miscibility gaps due to their “far from equilibrium” nature. And although great progress has been made towards improving the growth rate in these techniques, III-V device synthesis cost is still significantly higher (one order of magnitude) than Si solar cells manufacturing technologies 2. In this context, it is necessary to develop novel synthesis methods that yield high crystalline quality III-V alloys, higher throughput, and lower operational cost. For instance, Hydride/Halide Vapor Phase Epitaxy HVPE-grown GaAs top cell incorporated in a GaAs/Si tandem cell is an example of an optimized photovoltaic device with 31.4% efficiency, showcasing the uttermost potential of this growth method 2.More recently, Halide Vapor Phase Epitaxy growth of GaSbzP1-z polycrystalline free-standing films with up to 6.7% antimony incorporation and growth rates around 500 µm/h has been reported3. Linear sweep voltammetry measurements in 1M H2SO4 using GaSbzP1-z photoanodes showed lower onset potentials and higher fill factors compared to single crystal GaP. These results have been attributed to the visible light absorbing capabilities (direct band gaps between 2.2 and 2.5 eV), and lower charge transfer resistance at the semiconductor/electrolyte interface.On the other hand, a novel method for gallium nitridation involving plasma-activated nitrogen species dissolution into molten gallium has enabled the growth of single crystal GaN4. Furthermore, dilute anion Ga-Nitride alloys have been synthesized with the same technique but including other V-group species ions, i.e., Sb+ and Bi+, that can substitute nitrogen forming ternary GaSbxN1-x and GaBiyN1-y.In this presentation, we show the progress with dilute anion alloyed III-Nitride nanowires, GaSbxN1-x and GaBiyN1-y, synthesized by dissolving gallium, antimony or bismuth and plasma-activated nitrogen species into copper or gold droplets. Antimony and bismuth incorporation levels determined through x-ray diffraction c-plane peak shift, x and y, reached levels as high as 5.6 and 8.8 at%, respectively, resulting in direct band gap energies around 2.0 eV, determined through diffuse reflectance and photocurrent spectroscopy measurements. The visible light absorbing nanowire films exhibited photocurrent onset potentials around 0.0 V vs RHE when tested in 1 M sulfuric acid solution and 3-electrode setup with Ag/AgCl reference and Pt counter electrodes. 2-electrode chronoamperometry measurements with p-Si and n-type dilute alloys showed stable photocurrent densities up to 8.5 mA*cm-2 in 30 h. These results show the promising potential of dilute anion alloyed III-Nitrides as stable photoanodes for water splitting applications, and demonstrate the advantage of this novel synthesis technique over MOCVD that in previous studies has enabled the obtention of 0-D or 1-D GaSbxN1-x structures with up to 7% anion incorporation, while compromising crystalline quality.5

Cleaning deteriorated elements of ammunition: Development of a procedure applied to cartridge cases from the Second World War

Deteriorated elements of ammunition can be found while investigating different types of events. Exposure to adverse environmental conditions may lead to metal alteration (corrosion) or organic material deposition (contaminations) on the exposed elements of ammunition. From a forensic perspective, both types of deterioration pose challenges when observing marks left by the firearms used to discharge the corresponding ammunition (e.g. firing pin, extractor). The longer the time of exposure to the adverse environmental conditions, the more challenging the observation of such marks. A literature review highlighted three previously published restorative methods used to clean deteriorated elements of ammunition. The aim of this research is to develop a cleaning procedure applicable to cartridge cases exposed to adverse environmental conditions, while avoiding the degradation of marks left by the firearms used to discharge the corresponding ammunition. A first batch of 21 brass cartridge cases dating back to the Second World War (WWII) was used to develop a cleaning sequence involving the three methods. The efficiency of each restorative method was qualitatively assessed using optical macroscopy and the Evofinder® ballistic identification system. The developed sequence relies on successive applications of Tickopur® TR 7 (a diluted soft metal cleaner), sulfuric acid and finally Aqua Regia (HCl 37% and HNO3 75%), all of them involving ultrasonic baths. The resulting cleaning sequence was subsequently applied to three batches of Second World War cartridge cases discovered in France and Russia. This sequential procedure allows the effective cleaning of WWII brass cartridge cases while highlighting different marks left by firing pins, extractors, ejectors, and breech faces. Applying a forensic analysis and comparison process to the marks highlighted on these elements of ammunition can support the verification of historical facts when reconstructing events which took place more than seventy years ago.

Superconducting Properties of High-Entropy Type RE123 Thin Films by Fluorine-Free MOD Method

We have fabricated a high-entropy type RE123 (HE-RE123) superconducting thin film that RE site is replaced multiple Gd, Sm, Nd, Eu, Y elements, by fluorine-free metal organic deposition (FF-MOD) method for the first time and evaluated their superconducting properties. The crystal structure evaluated by XRD indicated the c-axis oriented RE123 crystal, and elemental analysis confirmed a homogeneous distribution of the five elements at the RE site. The critical temperature of HE-RE123 was 90.4 K, exceeding 90 K. The critical current density of 2.4 MA/cm <sup xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">2</sup> was obtained at 77.3 K, 0 T, which is higher than that of Gd123 films prepared by the same method. The maximum pinning force of HE-RE123 at 77.3 K was 1.2 times higher than that of Gd123.

Rapid preparation of cobalt doped GdBa2Cu3O7-δ films by non-fluorine chemical solution deposition method

The efficient preparation of superconducting layer is significant for large-scale applications of REBa2Cu3O7-δ coated conductors. In this work, a series of GdBa2Cu3-xCoxO7-δ films were prepared on LaAlO3 (00 l) substrates by non-fluorine metal organic deposition method. The influence of polymers on the pyrolysis process of the gel film was investigated, and the effect of cobalt doping on the epitaxial growth of the precursor film was analyzed. It was found that smooth and dense precursor film was obtained after decomposition at a high rate of 15 ℃/min. The rapid c-axis textured growth of the precursor film was achieved by optimizing the cobalt doping level for only ten minutes of firing. The optimal film possesses better texture, denser microstructure and larger critical current density (77 K, self-field) up to 1.3 MA/cm2.

Toluene combustion over Co3O4-CNTs/PSSF catalysts and investigation of the effects of acid treatment on catalytic activity

BackgroundCo3O4 shows potential as a cost-effective alternative to precious metal catalysts for VOCs catalytic combustion. However, its catalytic activity requires further enhancement. MethodsA new type of paper-like carbon nanotube membrane composite (CNTs/PSSF) was used as a support to prepare Co3O4-CNTs/PSSF catalysts by metal-organic vapor deposition (MOCVD) and impregnation method (IM) respectively for toluene combustion. Besides, the effects of acid treatment to support on the catalytic activity were investigated. Various characterization techniques, including X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), electron paramagnetic resonance (EPR), and oxygen temperature-programmed desorption (O2-TPD), were employed to evaluate the effects of different preparation methods and acid treatment on the structure and catalytic performance mechanism of Co3O4-CNTs/PSSF. Significant findingsThe preparation method significantly affects the catalyst's properties and catalytic activity. Compared with IM, the MOCVD-prepared catalysts show stronger coordination of carbon nanotubes, resulting in more oxygen vacancies and surface active oxygen. Additionally, oxygenous groups introduced by HNO3 form Co-O-C linkage between Co and CNTs, promoting oxygen vacancies and enhancing surface active oxygen content, thereby dramatically improving the catalyst's catalytic activity, especially for HIM-10 whose T90 is reduced by 140 °C. This work provides insights for enhancing the catalytic combustion activity of cobalt oxide.