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Catalytic Activity of MWCNTs Doped with Some Transition Metal Phthalocyanines and Modified with Silver in ORR 掺杂某些过渡金属酞菁并用银修饰的 MWCNT 在 ORR 中的催化活性
IF 0.5 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-07-01 DOI: 10.3103/S1061386224700080
K. Yu. Vinogradov, R. V. Shafigulin, V. M. Davydov, S. V. Vostrikov, M. V. Kuznetsov, A. V. Safonov, O. V. Belousova, A. V. Bulanova

Bimetallic oxygen reduction reaction (ORR) catalysts based on multi-walled carbon nanotubes (MWCNTs) doped with cobalt, copper, and nickel phthalocyanines and modified with silver (MWCNT–CoPc–Ag, MWCNT–CuPc–Ag, and WMCNT–NiPc–Ag) were obtained using high-temperature synthesis. The synthesis was carried out at 900°C in a nitrogen atmosphere. Scanning electron microscopy (SEM), low-temperature nitrogen adsorption–desorption, Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and powder X-ray diffraction (XRD) were used to determine the physicochemical properties of the synthesized catalysts. The effect of high-temperature synthesis on the textural and morphological properties of materials was also studied. It was shown that the physicochemical parameters of materials largely depend on the nature of the metal in the composition of original phthalocyanine. The electrocatalytic activity of the materials was studied by linear voltammetry in a three-electrode cell with a rotating disk electrode and mercury oxide reference electrode. The MWCNT–CoPc–Ag catalyst showed high electrocatalytic activity in ORR, comparable to that of a commercial platinum catalyst, as well as high corrosion resistance.

摘要 利用高温合成技术获得了基于掺杂钴、铜和镍酞菁并用银修饰的多壁碳纳米管(MWCNT)的双金属氧还原反应(ORR)催化剂(MWCNT-CoPc-Ag、MWCNT-CuPc-Ag 和 WMCNT-NiPc-Ag)。合成过程在 900°C 的氮气环境中进行。利用扫描电子显微镜(SEM)、低温氮吸附-解吸、拉曼光谱、X 射线光电子能谱(XPS)和粉末 X 射线衍射(XRD)测定了合成催化剂的理化性质。此外,还研究了高温合成对材料质构和形态特性的影响。结果表明,材料的物理化学参数在很大程度上取决于原始酞菁成分中金属的性质。在带有旋转盘电极和氧化汞参比电极的三电极电池中,通过线性伏安法研究了材料的电催化活性。MWCNT-CoPc-Ag 催化剂在 ORR 中表现出很高的电催化活性,可与商用铂催化剂相媲美,同时还具有很高的耐腐蚀性。
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引用次数: 0
The Effect of Impurity Gas on the Combustion Mode of Granular Mixtures Ti–C–B 杂质气体对 Ti-C-B 粒状混合物燃烧模式的影响
IF 0.5 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-07-01 DOI: 10.3103/S106138622470002X
D. S. Vasilyev, B. S. Seplyarskii, R. A. Kochetkov, T. G. Lisina, T. G. Akopdzhanyan

Experimental studies of the combustion of granular mixtures (100 – X)(Ti + C) + X(Ti + 2B), 0 ≤ X ≤ 100 wt %, were carried out. Granules 0.6 and 1.7 mm in size were made using an alcoholic solution of polyvinyl butyral. The combustion velocity dependence on X showed two characteristic areas with a boundary between them near X = 60 wt %. At X > 60 wt %, the combustion velocity increased significantly which allowed us to assume a convective mechanism of combustion due to the release of impurity gas. This assumption was verified by experiments in which the impurity gases were filtered through the side surface of samples to exclude the effect of a convective heat transfer. The necessary conditions for the transition to the convective combustion mode were formulated. Calculations showed that the critical conditions were met for mixture 40%(Ti + C) + 60%(Ti + 2B) with granule size of 1.7 mm. The content of impurity gas (presumably hydrogen) for mixtures burning in convective mode was estimated.

摘要 对颗粒状混合物(100 - X)(Ti + C)+ X(Ti + 2B)(0 ≤ X ≤ 100 wt %)的燃烧进行了实验研究。使用聚乙烯醇缩丁醛的酒精溶液制成 0.6 毫米和 1.7 毫米大小的颗粒。燃烧速度与 X 的关系显示出两个特征区域,在 X = 60 wt % 附近,这两个区域之间有一个边界。在 X > 60 wt % 时,燃烧速度显著增加,因此我们可以假定由于杂质气体的释放而产生了对流燃烧机制。为了排除对流传热的影响,我们通过实验对杂质气体进行了过滤,从而验证了这一假设。实验还提出了过渡到对流燃烧模式的必要条件。计算表明,颗粒尺寸为 1.7 毫米的 40%(Ti + C) + 60%(Ti + 2B) 混合物满足临界条件。估算了以对流模式燃烧的混合物中杂质气体(可能是氢)的含量。
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引用次数: 0
The Structure and Properties of the Promising Ultra-High-Temperature HfB2–HfC–SiC Ceramics Obtained from Heterophase SHS Powders 利用异相 SHS 粉末制备的前景广阔的超高温 HfB2-HfC-SiC 陶瓷的结构与性能
IF 0.5 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-07-01 DOI: 10.3103/S1061386224700067
A. A. Zaitsev, Yu. S. Pogozhev, A. Yu. Potanin, A. N. Astapov, I. O. Vakhrusheva, V. V. Korolev, S. I. Rupasov, E. A. Levashov

This work continues the earlier studies focusing on fabrication of heterophase micropowders and consolidated ceramics based on HfB2–HfC–SiC ultra-high-temperature boride/carbide compositions via self-propagating high-temperature synthesis (SHS) and hot pressing (HP). The effect of NH4Cl addition on the morphology and microstructure of the SHS powders was studied. Composite micropowders characterized by particle size of 0.2–10 μm and 40–50% content of the submicron-sized fraction were fabricated. The structure, mechanical and thermophysical properties, kinetics and mechanism of high-temperature oxidation of hot-pressed ceramic materials composed of 57–72 wt % HfB2, 14–20 wt % HfCx, 10–14 wt % SiC, and 8–15 wt % HfO2 were studied. They are found to have hardness up to 18.9 GPa, crack resistance up to 9.7 MPa m0.5, bending strength up to 400 MPa, temperature diffusivity up to 22.6 mm2/s, and thermal conductivity up to 59 W/(m K). The power law describes their oxidation kinetics. The protection mechanism against oxidation involves the formation of a multilayered heterogenous oxide film consisting of HfO2, HfSiO4, and borosilicate glass.

摘要 这项工作延续了先前的研究,重点是通过自蔓延高温合成(SHS)和热压(HP)法制备基于 HfB2-HfC-SiC 超高温硼化物/碳化物组合物的异相微粉和固结陶瓷。研究了 NH4Cl 添加量对 SHS 粉末形貌和微观结构的影响。制备出的复合微粉的粒度为 0.2-10 μm,亚微米级部分的含量为 40-50%。研究了由 57-72 wt % HfB2、14-20 wt % HfCx、10-14 wt % SiC 和 8-15 wt % HfO2 组成的热压陶瓷材料的结构、机械和热物理性能、高温氧化动力学和机理。研究发现,它们的硬度高达 18.9 GPa,抗裂性高达 9.7 MPa m0.5,抗弯强度高达 400 MPa,温度扩散率高达 22.6 mm2/s,热导率高达 59 W/(m K)。幂律描述了它们的氧化动力学。氧化保护机制包括形成一层由 HfO2、HfSiO4 和硼硅玻璃组成的多层异质氧化膜。
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引用次数: 0
Features of Front Propagation during Combustion of a Thermite-Type Mixture FeO/TiO2/B2O3/Cr2O3/CaCrO4/Al/C under Gravity Forces 在重力作用下 FeO/TiO2/B2O3/Cr2O3/CaCrO4/Al/C 热亚铁型混合物燃烧过程中的前沿传播特征
IF 0.5 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-07-01 DOI: 10.3103/S1061386224700043
S. L. Silyakov, N. Yu. Khomenko, A. E. Sytschev

The effect of the angle of inclination of a cylindrical reaction volume relative to the horizontal position on the combustion characteristics of a multicomponent thermite-type mixture FeO/TiO2/B2O3/Cr2O3/CaCrO4/Al/C was experimentally studied. It was shown that the combustion parameters, the burning velocity, material loss caused by sputtering, and the yield of target metallic phase into ingot, are unaffected by the angle of inclination. The dynamics of combustion front orientation relative to the burning velocity vector as the front propagates when the cylindrical reaction volume was tilted from 0° to 90° was revealed.

摘要 实验研究了圆柱形反应体积相对于水平位置的倾斜角度对多组分热敏型混合物 FeO/TiO2/B2O3/Cr2O3/CaCrO4/Al/C 燃烧特性的影响。结果表明,燃烧参数、燃烧速度、溅射造成的材料损失以及目标金属相成锭率均不受倾角的影响。研究还揭示了当圆柱形反应体积从 0° 倾斜到 90° 时,燃烧前沿方向相对于燃烧速度矢量的动态变化。
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引用次数: 0
Study of the Adsorption Properties of Mesoporous Silica Modified with Silver and Doped with Cerium or Terbium Using Inverse Gas Chromatography 利用反相气相色谱法研究银修饰和掺杂铈或铽的介孔二氧化硅的吸附特性
IF 0.5 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-07-01 DOI: 10.3103/S1061386224700079
A. A. Tokranov, E. O. Tokranova, D. V. Ovchinnikova, R. V. Shafigulin, A. V. Bulanova, M. V. Kuznetsov, A. V. Safonov, O. V. Belousova

Samples of mesoporous silica gel doped with cerium and terbium and modified with silver were synthesized using the template method. The textural and morphological characteristics of the samples were studied using scanning electron microscopy, inductively coupled plasma mass spectrometry, X-ray diffraction analysis, Fourier-transform infrared (FT-IR) spectroscopy, and nitrogen adsorption-desorption analysis. Moreover, thermodynamic characteristics of adsorption (differential heats and entropies) of test organic compounds were obtained using the inverse gas chromatography method. It was established that the nature of the dopant leads to changes in the textural characteristics of the samples and the heat of adsorption for hydrocarbons and compounds prone to various types of specific interactions.

摘要 采用模板法合成了掺杂铈和铽以及银修饰的介孔硅胶样品。利用扫描电子显微镜、电感耦合等离子体质谱、X 射线衍射分析、傅立叶变换红外光谱和氮吸附-解吸分析研究了样品的纹理和形态特征。此外,还利用反气相色谱法获得了测试有机化合物的吸附热力学特性(差热和熵)。结果表明,掺杂剂的性质会导致样品的纹理特征发生变化,并导致碳氢化合物和易发生各种特定相互作用的化合物的吸附热发生变化。
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引用次数: 0
High-Temperature Synthesis of Cast Ceramic Material Al2O3–Cr2O3 + ZrO2 高温合成铸造陶瓷材料 Al2O3-Cr2O3 + ZrO2
IF 0.5 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-07-01 DOI: 10.3103/S1061386224700055
P. A. Miloserdov, V. A. Gorshkov

A cast oxide ceramic material consisting of Al2O3–Cr2O3 solid solution and ZrO2 inclusions uniformly distributed in it was prepared through metallothermic SHS from highly exothermic thermite-type mixtures containing molybdenum (VI) and chromium (III) oxides and Al/Zr as a combined reducing agent. The influence of green mixture mass on the synthesis parameters, composition, and microstructure of the final products was studied. The optimal conditions for high-temperature synthesis of cast composite oxide material consisting of 80 wt % Al2O3, 10 wt % Cr2O3, and 10 wt % ZrO2 were determined.

摘要 从含有钼(VI)和铬(III)氧化物以及 Al/Zr 作为联合还原剂的高放热热石型混合物中,通过金属热 SHS 法制备了由 Al2O3-Cr2O3 固溶体和均匀分布在其中的 ZrO2 夹杂物组成的铸造氧化物陶瓷材料。研究了绿色混合物质量对最终产品的合成参数、成分和微观结构的影响。确定了高温合成由 80 wt % Al2O3、10 wt % Cr2O3 和 10 wt % ZrO2 组成的铸造复合氧化物材料的最佳条件。
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引用次数: 0
Solution Combustion Synthesis and Kinetic Measurements in Ni(NO3)2–C6H8O7 System. Preparation of Nickel Powder Ni(NO3)2-C6H8O7 体系中的溶液燃烧合成和动力学测量。制备镍粉
IF 0.5 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-07-01 DOI: 10.3103/S1061386224700031
N. Amirkhanyan

Solution combustion synthesis (SCS) is a widely used method to prepare nanomaterials tailored for specific applications, with a primary focus on understanding the influence of precursors on material properties and microstructure evolution. There is also a lack of systematic studies to understand the kinetics of SCS reactions. This work reports on the preparation of pure nickel by the combustion of Ni(NO3)2 + citric acid (C6H8O7) solution and the investigation of SCS reaction mechanism by thermal analysis technique. The lower and upper combustion limits were determined depending on the citric acid to Ni(NO3)2 ratio. The optimal composition of the initial mixture was revealed to prepare nickel powder without using an additional post–synthesis reduction of metal oxides. Ozawa’s method was employed to calculate the effective activation energy (∼101 ± 5 kJ mol–1) of the nickel formation reaction based on the TGA data. The magnetization of the nickel powder agglomerates with ∼80–200-nm nanoscale particles was measured to be 55.1 Am2 kg–1.

摘要 溶液燃烧合成(SCS)是一种广泛用于制备特定应用纳米材料的方法,其主要重点是了解前驱体对材料特性和微观结构演变的影响。目前还缺乏了解 SCS 反应动力学的系统研究。本研究报告介绍了通过燃烧 Ni(NO3)2 + 柠檬酸 (C6H8O7) 溶液制备纯镍的过程,并通过热分析技术研究了 SCS 反应机理。根据柠檬酸与 Ni(NO3)2 的比例确定了燃烧下限和上限。结果表明,初始混合物的最佳成分可用于制备镍粉,而无需在合成后额外还原金属氧化物。根据 TGA 数据,采用小泽法计算了镍形成反应的有效活化能(∼101 ± 5 kJ mol-1)。测得镍粉团聚体的磁化率为 55.1 Am2 kg-1,其纳米级颗粒为 80-200 nm。
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引用次数: 0
Rapidly Synthesizing Cu2Sb Phase of Tetragonal Structure by Electrothermal Explosion 通过电热爆炸快速合成四方结构的 Cu2Sb 相
IF 0.5 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-03-14 DOI: 10.3103/S1061386224010035
A. Hafs, T. Hafs, D. Berdjane, L. Yandjah

In our study, we aimed to synthesize the Cu2Sb phase with a tetragonal structure. We achieved this by subjecting compacts (2Cu + Sb) to electrothermal explosion (ETE) with a high current density of 500 Å. To analyze the constituent phases of the alloy composite, we employed X-ray diffraction analysis with the MAUD program, which utilizes the Rietveld method, as well as scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) techniques. Furthermore, we investigated the mechanical properties through Vickers indentation and compression techniques.

摘要 在我们的研究中,我们的目标是合成具有四方结构的 Cu2Sb 相。为了分析合金复合材料的组成相,我们采用了利用里特维尔德法的 MAUD 程序进行的 X 射线衍射分析,以及扫描电子显微镜(SEM)和能量色散 X 射线(EDX)技术。此外,我们还通过维氏压痕和压缩技术研究了其机械性能。
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引用次数: 0
Impact of Magnesium on Structural and Morphological Study of Co–Zn Ferrites 镁对共锌铁氧体结构和形态研究的影响
IF 0.5 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-03-14 DOI: 10.3103/S1061386224010047
R. Y. Kolekar, S. B. Kapatkar, Sushant S. Kakati, S. N. Mathad

The Co0.8–xMgxZn0.2Fe2O4 (x = 0.00 to 0.56) ferrites were prepared by solid state reaction route. The phase composition and morphology of the synthesized ferrites were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. From the XRD results, single phase cubic spinal structure with space group Fd-3m was confirmed. The lattice constant (a), particle size (D), hopping lengths (LA and LB), bond lengths (A–O and B–O), ionic radii (rA and rB), microstrain (ε,) and dislocation density (ρD) were reported. The lattice constant increased as magnesium additive increased. The SEM image affirmed size and shape of particles. Crystallite size and microstrain were realized by W–H plot and SSP.

摘要 采用固态反应路线制备了 Co0.8-xMgxZn0.2Fe2O4(x = 0.00 至 0.56)铁氧体。分别用 X 射线衍射(XRD)和扫描电子显微镜(SEM)对合成铁氧体的相组成和形貌进行了表征。从 X 射线衍射结果来看,确定了空间群为 Fd-3m 的单相立方脊柱结构。报告了晶格常数(a)、粒度(D)、跳跃长度(LA 和 LB)、键长(A-O 和 B-O)、离子半径(rA 和 rB)、微应变(ε, )和位错密度(ρD)。晶格常数随着镁添加剂的增加而增加。扫描电镜图像证实了颗粒的大小和形状。晶体尺寸和微应变通过 W-H 图和 SSP 得到。
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引用次数: 0
Combustion Synthesis of Cermets from Granular Mixtures Ti–C–NiCr for Protective Coatings 从用于保护涂层的 Ti-C-NiCr 粒状混合物燃烧合成金属陶瓷
IF 0.5 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-03-14 DOI: 10.3103/S1061386224010072
B. S. Seplyarskii, R. A. Kochetkov, T. G. Lisina, N. I. Abzalov

The combustion modes of granular mixtures (100 – X)(Ti + C) + XNiCr, X = 0–30%, were studied. The experimental setup provided filtration of impurity gases released during combustion, either in the direction of propagation of the combustion front, or through the side surface of the sample. The comparison of burning velocities in different gas filtration schemes indicates the influence of convective heat transfer on the combustion patterns of mixtures with X < 30%. A method was proposed for determining the composition of the mixture in which the transition to the convective combustion mode occurs. The content of impurity gases in mixtures of different compositions was estimated quantitively. The comparison of experimental data with calculations based on the theory of filtration combustion showed that there is a conductive combustion mode for all mixtures of 0.6-mm granules and a mixture of 1.7-mm granules with X = 30%. XRD analysis of the synthesis products revealed no intermetallic phases, regardless of the size of the granules.

摘要 研究了颗粒状混合物 (100 - X)(Ti + C) + XNiCr(X = 0-30%)的燃烧模式。实验装置对燃烧过程中释放的杂质气体进行了过滤,过滤的方向可以是燃烧前沿的传播方向,也可以是通过样品的侧表面。不同气体过滤方案下燃烧速度的比较表明,对流传热对 X < 30% 混合物的燃烧模式有影响。提出了一种方法来确定向对流燃烧模式过渡的混合物成分。对不同成分混合物中杂质气体的含量进行了定量估算。实验数据与基于过滤燃烧理论的计算结果的比较表明,所有 0.6 毫米颗粒的混合物以及 X = 30% 的 1.7 毫米颗粒的混合物都存在传导燃烧模式。对合成产物的 XRD 分析表明,无论颗粒大小如何,都没有金属间相。
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引用次数: 0
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International Journal of Self-Propagating High-Temperature Synthesis
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