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Facile synthesis of lanthanum carbonate octahydrate and lanthanum oxide nanoparticles by sonochemical method: systematic characterizations 利用声化学方法轻松合成八水合碳酸镧和纳米氧化镧:系统表征
Pub Date : 2024-03-19 DOI: 10.1515/zpch-2023-0396
Sentienla Imsong, Punazungba Imsong, Swapnali Hazarika, M. Indira Devi
This study could present the size and morphology of two synthesized nanoparticles (NPs) by observing their smallest possible dimensions. Lanthanum carbonate nanoparticles were synthesized by sonochemical method through the interaction of lanthanum acetate hydrate and sodium carbonate in an aqueous medium with a probe sonicator. After rigorous washing followed by drying, the La2(CO3)3·8H2O(S1) NPs were calcined at a temperature of 600 °C to obtain lanthanum oxide nanoparticles (S2). Both NPs were characterised through various instrumental techniques. PXRD study showed orthorhombic with space group of Pccn (56) and hexagonal phases with space group of P 3 m 1 $Poverline{3}m1$ (164) for S1 and S2 respectively whose morphology and elemental analysis were studied through FESEM and EDX. High resolution TEM image of La2(CO3)3·8H2O and La2O3 showed spherical shapes of the nanoparticles. Further study of XPS and FTIR conveyed detailed information of both nanoparticles whose TGA-DSC showed three step decomposition curves. The size and morphology of the synthesized nanoparticles have been found to have a distinct morphology and are found comparatively smaller in size than those observed in the earlier reported works (Table 1 Table 1: Comparative study of synthesized lanthanum carbonate and lanthanum oxide NPs with various techniques applied by other researchers.
本研究通过观察两种合成纳米粒子(NPs)的最小尺寸,展示了它们的尺寸和形态。碳酸镧纳米粒子是通过声化学法,在水介质中用探针声波仪使水合醋酸镧和碳酸钠相互作用而合成的。La2(CO3)3-8H2O(S1) 纳米粒子经过严格的洗涤和干燥后,在 600 °C 的温度下煅烧,得到氧化镧纳米粒子(S2)。通过各种仪器技术对这两种 NPs 进行了表征。PXRD 研究显示,S1 和 S2 分别为空间群为 Pccn 的正方晶相(56)和空间群为 P 3 ‾ m 1 $Poverline{3}m1$ 的六方晶相(164),并通过 FESEM 和 EDX 对其形貌和元素分析进行了研究。La2(CO3)3-8H2O 和 La2O3 的高分辨率 TEM 图像显示纳米颗粒呈球形。对 XPS 和傅立叶变换红外光谱的进一步研究提供了这两种纳米粒子的详细信息,其 TGA-DSC 显示了三步分解曲线。合成纳米粒子的尺寸和形态具有明显的形态特征,其尺寸相对小于早期报告的作品(表 1 表 1:合成的碳酸镧和氧化镧 NPs 与其他研究人员应用的各种技术的比较研究。 序号 NPs 名称 方法 条件 NP 尺寸 参考 1 La2(CO3)3-8H2O 声化学法 时间:25 分钟 XRD:Pccn (56) a = 8.9840 Å b = 9.5800 Å c = 17.0000 Å 本作品 温度:301 K 尺寸:24.102 nm 起始材料:(a) La(CH3COO)2:0.050 M(b) Na2CO3:0.050 M TEM:尺寸:4-30 nm La2(CO3)3 反胶束 时间:1 h XRD:尺寸:无纳米颗粒 [20] 温度:303 K 起始材料:(a) La(CH3COO)2:0.050 M(b) Na2CO3:0.050 M303 K 起始材料:(a) Triton X-100(b)环己烷(c) 正丁醇(d) La(NO3)3(aq) e) NaCO3(aq) La2(CO3)3-8H2O 水热时间:2-5 天 XRD:Pccn a = 8.984 Å b = 9.580 Å c = 17.00 Å [21] 温度:773 K 尺寸:无纳米颗粒 通过缓慢水解 La(CCl3COO)3 La2(CO3)3-1.
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引用次数: 0
Oxygen doped g-C3N4/LDH composite as highly efficient photocatalyst for wastewater treatment 掺氧 g-C3N4/LDH 复合材料作为高效光催化剂用于废水处理
Pub Date : 2024-03-18 DOI: 10.1515/zpch-2023-0468
Sadaf Mutahir, Muhammad Asim Khan, Wishma Noor, Rimsha Butt, S. Elkholi, Mohamed Bououdina, A. Alsuhaibani, K. Munawar, Muhammad Humayun
Herein, we fabricated a highly efficient oxygen-doped graphitic carbon nitride (O–CN) and layered double hydroxide (LDH) nanocomposite photocatalyst and utilized it in the degradation of organic dyes in wastewater. The composite’s structure, morphology, and different optical features were examined using different techniques such as FT-IR spectroscopy, UV-visible spectroscopy, scanning electron microscopy (SEM), SEM-EDX, energy dispersive X-ray (EDX), and X-ray diffraction (XRD). The composite has shown a crystalline structure, in contrast to the amorphous nature of oxygen-doped g-C3N4. Using a wide range of experimental parameters, including dye concentration, visible light, irradiation time, catalyst dose, contact time, and pH, the increase in the reaction performance of the catalyst was observed. The results reveal that 98.5 % adsorption degradation efficiency increased with the increase in catalyst dosage, contact time, and pH. The as-fabricated photocatalyst generated reactive species that were involved in the degradation of methylene blue (MB) dye upon exposure to visible light irradiation.
在此,我们制备了一种高效的氧掺杂氮化石墨碳(O-CN)和层状双氢氧化物(LDH)纳米复合光催化剂,并将其用于降解废水中的有机染料。研究人员利用傅立叶变换红外光谱、紫外可见光谱、扫描电子显微镜(SEM)、扫描电子显微镜-电子衍射、能量色散 X 射线(EDX)和 X 射线衍射(XRD)等不同技术对该复合材料的结构、形态和不同的光学特征进行了研究。与掺氧 g-C3N4 的无定形性质相反,该复合材料呈现出晶体结构。利用各种实验参数,包括染料浓度、可见光、辐照时间、催化剂剂量、接触时间和 pH 值,观察到催化剂反应性能的提高。结果表明,随着催化剂用量、接触时间和 pH 值的增加,吸附降解效率提高了 98.5%。制成的光催化剂在可见光照射下产生了参与亚甲基蓝(MB)染料降解的活性物种。
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引用次数: 0
Incredible electrochemical performance of ZnWO4/PANI as a favorable electrode material for supercapacitor 作为超级电容器电极材料的 ZnWO4/PANI 具有令人难以置信的电化学性能
Pub Date : 2024-03-15 DOI: 10.1515/zpch-2023-0523
Sastipriyaa Padmanaaban, Yadhukrishnan Kakkad Vasudevan, Raja Viswanathan, Sujin P. Jose, Gopinathan Chellasamy
ZnWO4/PANI was synthesized through the in-situ polymerization technique, revealing the wolframite monoclinic phase in its XRD pattern. The distinctive morphology of ZnWO4/PANI observed in the SEM image, exhibits enhanced redox sites, thereby improving its electrochemical performance. Cyclic voltammetry and galvanostatic charge-discharge studies confirm the pseudocapacitive behavior of ZnWO4/PANI, showcasing an impressive capacitance of 908 F g−1 at 1 A g−1 in 1 M KOH, along with a capacitive retention of 94 % over 5000 cycles. The robust conductivity of PANI and the narrow ion transport channels along with multiple oxidation states of ZnWO4 contribute to the higher specific capacity, guiding the movement of electrons and ions. This study suggests a synergistic effect in ZnWO4/PANI, resulting in remarkable electrochemical performance enhancements.
ZnWO4/PANI 是通过原位聚合技术合成的,在其 XRD 图谱中显示出黑钨矿单斜相。在扫描电镜图像中观察到的 ZnWO4/PANI 的独特形貌显示出增强的氧化还原位点,从而提高了其电化学性能。循环伏安法和电静态充放电研究证实了 ZnWO4/PANI 的伪电容行为,在 1 M KOH 溶液中,1 A g-1 时的电容值为 908 F g-1,5000 次循环后的电容保持率为 94%。PANI 的强导电性和 ZnWO4 的窄离子传输通道以及多种氧化态有助于提高比容量,引导电子和离子的运动。这项研究表明,ZnWO4/PANI 具有协同效应,可显著提高电化学性能。
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引用次数: 0
Comparison of different iron oxides for degradation of tetracycline anti-bacterial drug 比较不同氧化铁对四环素抗菌药物的降解作用
Pub Date : 2024-03-14 DOI: 10.1515/zpch-2024-0606
Radhakrishnan Velayudan, Jeyakumaran Natarajan
Nanomaterials have a wide range of applications including novel biomedical studies are devoted to improving the functionality and effectively of traditional and unmodified systems, both drug carriers and common scaffolds for tissue engineering or advanced hydrogels for wound healing purposes. In this regard, metal oxide nanoparticles show great potential as versatile tools in biomedical science. In particular, iron oxide nanoparticles with different shape and sizes hold outstanding physiochemical characteristics, such as high specific area and structure that make them unique nanomaterials to be used in diverse aspects of medicine and biological systems. The challenges associated with the uncontrolled presence of antibiotics such as tetracycline in the environment have necessitated their removal through different techniques. Tetracycline is hard to degrade in living organisms and can even be converted to more toxic substances. In this article different type of iron oxides were subjected to photo degradation of antibacterial drug Tetracycline under UV light illumination and direct sunlight and the results were promising to degrade the drug within 20 min. The SEM, TEM, EDAX and XRD for the catalyst were characterized to confirm the presence of iron oxide, the size and shape of the particle. The kinetics of photo degradation of tetracycline followed the pseudo-first-order mechanism, proceeding through hydroxyl radicals generated under illumination. Moreover, the photo generated hydrogen peroxide could lead to heterogeneous photocatalytic processes on the surface of iron oxide nanoparticles; additionally generating hydroxyl and hydroperoxyl radicals enables photo degradation of tetracycline.
纳米材料具有广泛的应用,其中包括新型生物医学研究,这些研究致力于提高传统和未改性系统的功能和有效性,包括药物载体、用于组织工程的普通支架或用于伤口愈合的先进水凝胶。在这方面,金属氧化物纳米粒子显示出作为生物医学科学多功能工具的巨大潜力。特别是具有不同形状和尺寸的氧化铁纳米粒子,具有突出的理化特性,如高比面积和结构,使其成为独特的纳米材料,可用于医学和生物系统的各个方面。四环素等抗生素在环境中的无节制存在带来了挑战,因此有必要通过不同的技术去除它们。四环素在生物体内很难降解,甚至会转化为毒性更强的物质。本文采用不同类型的铁氧化物,在紫外光和阳光直射下对抗菌药物四环素进行光降解,结果表明在 20 分钟内就能降解药物。对催化剂的 SEM、TEM、EDAX 和 XRD 进行了表征,以确认氧化铁的存在、颗粒的大小和形状。四环素的光降解动力学遵循伪一阶机制,通过光照下产生的羟自由基进行。此外,光产生的过氧化氢可导致氧化铁纳米粒子表面的异相光催化过程;另外,产生的羟自由基和氢过氧自由基可实现四环素的光降解。
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引用次数: 0
Evaluation of magnetic and electrochemical performance of copper oxide nanoparticles using Myristica fragrans (mace) extract 使用肉豆蔻提取物评估纳米氧化铜的磁性和电化学性能
Pub Date : 2024-03-14 DOI: 10.1515/zpch-2024-0582
Shandhiya Murugan, Deepika Balraj, Saranya Amirtharajan, Ramesh P Manimuthu, Rama R N Venkata, Janarthanan Balasundaram, Mohamed R Ziaudeen, Sharmila Saminathan
The synthesis of metal oxide nanoparticles using natural extract encourages the futuristic design of an environmentally friendly system by getting rid of the dangerous, toxic substances. The food industry in India is paying a lot of attention to Myristica fragrans, often known as mace, due to its rich medicinal significance. In the current study, M. fragrans (Mace) aqueous extract was used to prepare copper oxide (CuO) nanoparticles. Phytochemical screening confirms the presence of bioactive substances such as alkaloids, sterols, glycosides, and flavonoids in the extract. XRD and SEM measurements show that the nanoparticles have a monoclinic structure with polyhedral shape. Using the Debye-Scherrer formula, the material’s average crystallite size was found to be 85 nm. Based on the Tauc plot, an optical band gap of the prepared CuO NPs was calculated as 2.6 eV. At room temperature, the material’s magnetic property was investigated using VSM analysis. Congo red was used to examine the photocatalytic properties of the materials with various timings. CuO nanoparticles’ antibacterial activity was evaluated at various doses against Staphylococcus aureus and Klebsiella pneumoniae. Almost, CuO NPs exhibit better response against both the bacteria. Moreover, research investigations using cyclic voltammetry was carried out to assess the produced nanoparticles’ pseudocapacitive qualities. At a scan rate of 10 mV s−1, the material produced a good specific capacitance of 233.8 F/g with 1 M of KOH as an electrolyte.
利用天然提取物合成金属氧化物纳米粒子,可以摆脱危险的有毒物质,从而促进未来环保系统的设计。由于肉豆蔻具有丰富的药用价值,印度的食品工业对肉豆蔻(Myristica fragrans)给予了极大的关注。在本研究中,肉豆蔻水提取物被用来制备纳米氧化铜(CuO)颗粒。植物化学筛选证实了提取物中生物活性物质的存在,如生物碱、甾醇、苷和黄酮类化合物。XRD 和 SEM 测量结果表明,纳米颗粒具有单斜多面体结构。根据 Debye-Scherrer 公式,该材料的平均结晶尺寸为 85 nm。根据陶克曲线图,计算出制备的 CuO NPs 的光带隙为 2.6 eV。在室温下,使用 VSM 分析法研究了材料的磁性。刚果红被用来检测材料在不同时间段的光催化特性。在不同剂量下,评估了 CuO 纳米粒子对金黄色葡萄球菌和肺炎克雷伯氏菌的抗菌活性。结果表明,CuO NPs 对这两种细菌都有较好的抗菌效果。此外,研究人员还利用循环伏安法评估了所制备纳米粒子的假电容特性。在 10 mV s-1 的扫描速率下,以 1 M 的 KOH 作为电解质,该材料产生了 233.8 F/g 的良好比电容。
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引用次数: 0
Gamma radiation-induced degradation of Acid Violet 49 in the presence of hydrogen peroxide (H2O2) in an aqueous medium 水介质中过氧化氢(H2O2)存在时伽马辐射诱导酸性紫 49 降解
Pub Date : 2024-03-14 DOI: 10.1515/zpch-2022-0165
T. H. Bokhari, Aqsa Iqbal, Muhammad Usman, Maryam Al Huwayz, Mazhar Iqbal, Abid Ali, N. Alwadai, Munawar Iqbal, A. Nazir, Umer Younas
The present study is about the effect of gamma radiations on the degradation of Acid Violet 49 (AV49) in the presence of H2O2 (γ/H2O2). The Cs-137 radiation source was calibrated to irradiate the aqueous solution of AV49 within the 1 kGy, 5 kGy & 10 kGy dose range. The results showed that 50–150 mg/L of AV49 was effectively degraded by γ radiation (85 %), however, the concentration of H2O2 in the range of 0.2–0.6 mL promoted degradation to 90 % and 98 %, respectively. It was observed that all absorption bands declined with rising irradiation dose and disappeared completely after 10 kGy applied dose. pH conditions (3, 5,7, and 9) were used in the radio-lytic degradation of AV49, the results showed that the best degradation efficiency has been found for pH 9. The optimum degradation rate is higher (98 %) with a 50 mg/L concentration of AV49, 0.6 mL H2O2, and pH 9 at a 10 kGy absorbed dose. In addition, the influence of various parameters on the rate of degradation such as the effect of irradiation dose, pH, H2O2, and dye (AV49) concentration was also studied. Furthermore, the removal of total organic carbon TOC was not as effective as that of the AV 49. Total nitrogen TN was not completely removed even at high dosage. Radio-lytic degradation of AV49 was analyzed by using Fourier transform infrared spectroscopy (FTIR) and liquid chromatography coupled to mass spectrometry (LC-MS) as an analytical technique. Results revealed that the proposed methodology for degradation of dyes is effective and probably could be applied for the removal of other toxic pollutants.
本研究是关于在 H2O2(γ/H2O2)存在下伽马辐射对酸性紫 49(AV49)降解的影响。校准铯-137 辐射源,在 1 kGy、5 kGy 和 10 kGy 剂量范围内辐照 AV49 水溶液。结果表明,γ 辐射可有效降解 50-150 mg/L 的 AV49(85%),但 0.2-0.6 mL 浓度的 H2O2 可使降解率分别达到 90% 和 98%。在对 AV49 进行放射性水解降解时,采用了 pH 值(3、5、7 和 9)条件,结果表明 pH 值为 9 时降解效率最高。 在吸收剂量为 10 kGy 时,AV49 的浓度为 50 mg/L、H2O2 的浓度为 0.6 mL、pH 值为 9 时,最佳降解率较高(98%)。此外,还研究了各种参数对降解率的影响,如辐照剂量、pH 值、H2O2 和染料(AV49)浓度的影响。此外,总有机碳 TOC 的去除效果不如 AV49。即使在高剂量下,总氮 TN 也没有被完全去除。利用傅立叶变换红外光谱法(FTIR)和液相色谱耦合质谱法(LC-MS)作为分析技术,对 AV49 的放射性水解降解进行了分析。结果表明,所提出的染料降解方法是有效的,并有可能用于去除其他有毒污染物。
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引用次数: 0
Amidoxime functionalized mesoporous silica nanoparticles for pH-responsive delivery of anticancer drug 脒肟功能化介孔二氧化硅纳米颗粒用于 pH 值响应性递送抗癌药物
Pub Date : 2024-03-12 DOI: 10.1515/zpch-2023-0488
M. Santhamoorthy, Ranganathan Suresh, Vanaraj Ramkumar, L. Guganathan, Kokila Thirupathi, G. Periyasami, Anandhu Mohan, Seong-Cheol Kim
In recent decades, nanomedicine has attracted much attention at the forefront of nanotechnology, gaining great expectations in the biomedical sectors. Among various nanomaterials, silica nanoparticles-based drug delivery is considered effective owing to their physicochemical stability and biological compatibility. Surface grafting and chemical conversion techniques were used to create an amphoteric functional ligand known as amidoxime ligand (AL) modified mesoporous silica material (MS-AL NPs). With this technique, amidoxime ligand groups can be introduced in greater concentration to the silica surface without compromising its structure. The active surface allows for surface functionalization and integration of medicinal substances. They are widely employed in the bio-medical industry for diagnostics, target administration of drugs, bio-sensing, cellular absorption, and so on. The function of the produced MS-AL NPs as a regulated drug delivery system was studied utilizing doxorubicin (Dox) as a model anticancer drug. Using the MCF-7 cell line, the biocompatibility and cellular uptake characteristics were investigated. Considering all factors, the MS-AL NPs may be used as pH-responsive drug carriers in cancer treatment applications.
近几十年来,纳米医学在纳米技术的前沿领域备受关注,在生物医学领域被寄予厚望。在各种纳米材料中,基于二氧化硅纳米颗粒的药物递送因其物理化学稳定性和生物相容性而被认为是有效的。研究人员利用表面接枝和化学转化技术创造了一种两性功能配体,即脒肟配体(AL)修饰介孔二氧化硅材料(MS-AL NPs)。利用这种技术,可以在不破坏二氧化硅结构的情况下,在二氧化硅表面引入更高浓度的脒氧肟配体基团。这种活性表面可实现表面功能化,并与药用物质结合。它们被广泛应用于生物医疗行业的诊断、靶向给药、生物传感、细胞吸收等领域。以多柔比星(Dox)为抗癌药物模型,研究了所制备的 MS-AL NPs 作为调节给药系统的功能。以 MCF-7 细胞系为研究对象,考察了其生物相容性和细胞吸收特性。考虑到所有因素,MS-AL NPs 可作为 pH 值响应型药物载体应用于癌症治疗。
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引用次数: 0
Exploration of facile hydrothermally produced pure nickel oxide nanostructures as an effective electrode material for the enhanced supercapacitor applications 探索水热法生产的纯氧化镍纳米结构作为一种有效电极材料在超级电容器中的增强应用
Pub Date : 2024-03-12 DOI: 10.1515/zpch-2024-0004
Leekeshwer Upadhyay, S. Dhanapandian, Selvakumar Suthakaran, Krishnamoorthi Ashokkumar, V. Sathana, Ayyar Dinesh, Manikandan Ayyar
This research work concerns with the magnetic and electrochemical characteristics of hydrothermally prepared nickel oxide (NiO) nanoparticles for their use as working electrode material in supercapacitor. Through the use of thermal gravimetric (TG-DTA), the thermal stability and heat adsorption/desorption characteristics of the as-produced NiO nanoparticles were examined. By using X-ray diffraction (XRD) technique at ambient, 600 °C and 800 °C annealing temperatures, the trigonal and cubic structure of the as prepared and annealed nanoparticles was discovered. The spherical and cubic morphology of the as synthesized and annealed (800 °C) NiO nanoparticles was confirmed through field emission scanning electron microscope (FESEM), energy dispersive X-ray (EDAX) analysis. The functional groups, optical bandgap energy, surface chemistry, specific surface area and superparamagnetic behavior of the annealed (800 °C) NiO nanoparticles were determined through Fourier transform infra-red (FT-IR), UV-DRS, XPS, BET and VSM characterization approaches, respectively. At the lowest scan rates of 10 mVs−1 and 0.5 Ag−1, the pseudocapacitive behavior was noticed utilizing CV and GCD analyses. An excellent electrical conductivity for the supercapacitor application was also shown by the Nyquist plot of the produced NiO electrode.
这项研究工作涉及水热法制备的纳米氧化镍(NiO)颗粒的磁性和电化学特性,以便将其用作超级电容器的工作电极材料。通过使用热重法(TG-DTA),研究了制备的纳米氧化镍颗粒的热稳定性和吸热/脱热特性。通过在环境温度、600 ℃ 和 800 ℃ 退火温度下使用 X 射线衍射(XRD)技术,发现了制备和退火纳米粒子的三方和立方结构。通过场发射扫描电子显微镜(FESEM)和能量色散 X 射线(EDAX)分析,确认了合成和退火(800 ℃)后的氧化镍纳米粒子的球形和立方体形貌。通过傅立叶变换红外(FT-IR)、紫外-可见光谱(UV-DRS)、XPS、BET 和 VSM 表征方法,分别测定了退火(800 ℃)后的氧化镍纳米颗粒的官能团、光带隙能、表面化学性质、比表面积和超顺磁性。在 10 mVs-1 和 0.5 Ag-1 的最低扫描速率下,利用 CV 和 GCD 分析发现了伪电容行为。所制备的氧化镍电极的奈奎斯特图也显示了其在超级电容器应用中的优异导电性。
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引用次数: 0
Synergistic enhancement of electrochemical supercapacitor efficiency via Co3O4/GO composite electrode 通过 Co3O4/GO 复合电极协同提高电化学超级电容器的效率
Pub Date : 2024-03-12 DOI: 10.1515/zpch-2024-0584
Indira Priyadharsini Chinnuraj, Marimuthu Ganesan, Govindasamy Palanisamy, P. M. Anbarasan, Ikhyun Kim, Imran Hasan, Sivaprakash Paramasivam
In recent times, the convergence of metal oxide adorned graphene oxide (GO) composites has ignited substantial notice, driven by their potential to revolutionize electrochemical energy storage applications, particularly in the realm of supercapacitors. This surge in attention is attributable to the harmonious amalgamation of metal oxide nanoparticles with the versatile GO sheets, resulting in intricately nanostructured materials. The present investigation the synthesis of hybrid done by hydrothermal route, yielding nanostructured Co3O4/GO. Extensive electrochemical assessment reveals a pinnacle specific capacitance of 786.69 F/g at 1 mA/cm2 current density within a 3 mol L−1 KOH aqueous medium, accompanied by commendable rate-handling capabilities.
近来,金属氧化物与氧化石墨烯(GO)复合材料的融合引起了广泛关注,因为它们具有彻底改变电化学储能应用的潜力,特别是在超级电容器领域。这种备受关注的现象归因于金属氧化物纳米颗粒与多用途的 GO 片的和谐结合,从而产生了错综复杂的纳米结构材料。本研究通过水热法合成了纳米结构的 Co3O4/GO。广泛的电化学评估显示,在 3 mol L-1 KOH 水介质中,电流密度为 1 mA/cm2 时,该材料的比电容高达 786.69 F/g,同时还具有值得称赞的速率处理能力。
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引用次数: 0
Exploring optical and electrochemical studies on thulium selenite (TmSeO3) 探索硒化铥(TmSeO3)的光学和电化学研究
Pub Date : 2024-03-12 DOI: 10.1515/zpch-2023-0404
Ariponnammal Shanmuga Sundaram, Basil Ralph Nesam Gregory, Shanmugha Soundare Sivakumar
Thulium selenite (TmSeO3) has been synthesized by precipitation method. It shows interesting smooth surface with nearly non-symmetric texture similar to water droplets spreading on hydrophobic surface. TmSeO3 is found to be monoclinic structure with lattice parameters a = 5.919±0.01 Å, b = 12.422±0.01 Å, c = 8.717±0.01 Å, α = γ = 90°, β = 106.01° and V = 616.1 Å3. Fourier transform infrared spectroscopy confirms the presence of Tm–Se bonding. X-ray photo emission spectrum confirmed the presence of thulium, selenium and oxygen in the samples in oxide form. Magnetic study between 300 and 20 K, shows decrease of magnetic moment with temperature, then reaches saturation and aligns all thulium spins. This results cooperative interaction of thulium spins. M–H curve at 300 K confirms the paramagnetic nature of sample. Cyclic voltammogram of three electrode system, manifests electric double layer capacitance with a potential window of 0.55 V. Specific capacitance is 102 F/g. Chronopotentiometry analysis shows 75 F/g specific capacitance, 11 Wh kg−1 energy density, and 275 W kg−1 power density. Impedance analysis confirms electric double layer capacitor behavior. Hence, TmSeO3 electrode based symmetric supercapacitor device was successfully fabricated and tested by two electrode configuration in aqueous electrolyte of KOH. A specific capacitance of 64.60 F/g at 1 A/g within a potential window of 1.85 V was achieved. Impedance analysis also confirms electric double layer capacitor nature with low series resistance of 0.2596 Ω and charge transfer resistance of 1.6352 Ω. The improved cycling performance after 4000 cycles is 51.5 % specific capacitance retention. Thus, symmetric supercapacitor electrodes based TmSeO3 materials are expected to have good electrochemical properties and good stability for energy storage and conversion applications. Furthur, optical parameters 5.28 eV energy gap, 0.4924 eV Urbach energy value and 1.959 refractive index are determined.
硒铥(TmSeO3)是通过沉淀法合成的。它显示出有趣的光滑表面,具有类似于水滴在疏水表面扩散的非对称纹理。TmSeO3 呈单斜结构,其晶格参数为 a = 5.919±0.01 Å,b = 12.422±0.01 Å,c = 8.717±0.01 Å,α = γ = 90°,β = 106.01°,V = 616.1 Å3。傅立叶变换红外光谱证实了 Tm-Se 键的存在。X 射线光发射光谱证实样品中存在氧化物形式的铥、硒和氧。在 300 至 20 K 之间进行的磁性研究表明,磁矩随温度的升高而减小,然后达到饱和状态并使所有铥自旋对齐。这导致了铥自旋的协同作用。300 K 时的 M-H 曲线证实了样品的顺磁性。三电极系统的循环伏安图显示了双电层电容,电位窗口为 0.55 V。比电容为 102 F/g。计时电位分析表明,比电容为 75 F/g,能量密度为 11 Wh kg-1,功率密度为 275 W kg-1。阻抗分析证实了双层电容器的特性。因此,基于 TmSeO3 电极的对称超级电容器装置被成功制造出来,并在 KOH 水电解质中通过双电极配置进行了测试。在 1.85 V 的电位窗口内,1 A/g 时的比电容为 64.60 F/g。阻抗分析也证实了双层电容器的性质,其串联电阻为 0.2596 Ω,电荷转移电阻为 1.6352 Ω。经过 4000 次循环后,比电容保持率提高了 51.5%。因此,基于 TmSeO3 材料的对称超级电容器电极有望在能量存储和转换应用中具有良好的电化学性能和稳定性。此外,还测定了光学参数 5.28 eV 能隙、0.4924 eV 厄巴赫能值和 1.959 折射率。
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