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Pycnometric Determination of Porosity Characteristics 孔隙度特征的计量测定
IF 0.9 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2025-03-10 DOI: 10.1134/S0020168524700651
A. B. Ankudinov, M. I. Alymov, V. A. Zelensky, R. D. Kapustin, A. E. Sychev, V. S. Shustov

Pycnometric methods of characterization of the pore structure of solids, based on density measurements, provide data on the pore size distribution. Here we report results of open porosity determination via weighing of a dry sample, followed by evacuation and saturation with distilled water at atmospheric pressure; via pressure infiltration with water using a manostat system; and by mercury intrusion porosimetry. We have studied porous nickel samples prepared by a powder metallurgy process involving sintering of green compacts consisting of mixtures of nickel nanopowder and ammonium bicarbonate (NH4HCO3) powder as a pore former, with volume fractions of 80 and 20%, respectively. The particle size ranges of the pore former were 63–125, 140–200, and 250–315 μm. For the three methods used to determine open porosity, we theoretically evaluated the size of pores accessible to infiltrating liquid. The results demonstrate that, in the case of saturation with water after evacuation, the liquid can penetrate only pores more than 3 μm in size. Moreover, in the case of porous structures with a large fraction of submicron pores, the open porosity determined via saturation with distilled water after evacuation is considerably underestimated. The larger the fraction of small pores in the material, the larger the underestimation. The difference between the open porosity values obtained via pressure infiltration with water and by mercury porosimetry is insignificant. We demonstrate that, of the three porosity determination methods, only saturation with distilled water after evacuation cannot be used to analyze structures with submicron pores. The results we obtained can be useful in designing porous functional materials and articles with a tailored pore structure.

基于密度测量的固体孔隙结构表征的计量方法提供了孔隙尺寸分布的数据。在这里,我们报告了通过称重干燥样品,然后在常压下用蒸馏水疏散和饱和来确定开孔率的结果;通过压力渗透与水使用稳压系统;通过汞侵入孔隙度测定法。我们研究了通过粉末冶金工艺制备的多孔镍样品,该工艺涉及由镍纳米粉和碳酸氢铵(NH4HCO3)粉末的混合物组成的绿色压块烧结,作为孔隙形成剂,体积分数分别为80%和20%。成孔剂的粒径范围为63 ~ 125 μm、140 ~ 200 μm和250 ~ 315 μm。对于用于确定开孔率的三种方法,我们从理论上评估了可渗透液体的孔隙大小。结果表明,在疏水饱和的情况下,液体只能穿透大于3 μm的孔隙;此外,对于含有大量亚微米孔隙的多孔结构,通过抽提后蒸馏水饱和测定的开孔率被大大低估。材料中小孔隙的比例越大,低估越大。水压力入渗法与汞孔隙度法得到的孔隙度值差异不显著。我们证明,在三种孔隙度测定方法中,仅用抽真空后蒸馏水饱和不能用于分析亚微米孔隙结构。所得结果可用于设计具有定制孔结构的多孔功能材料和制品。
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引用次数: 0
Effect of Chromium on Stereolithographic Printing with Alumina-Based Slurries 铬对铝基浆料立体平版印刷的影响
IF 0.9 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2025-03-10 DOI: 10.1134/S0020168524700754
L. V. Ermakova, V. V. Dubov, R. R. Saifutyarov, D. E. Lelekova, S. K. Belus’, V. G. Smyslova, P. V. Karpyuk, P. S. Sokolov

We have studied the effect of small Cr2O3 and Cr3+ additions on the optical properties of high-purity alumina-based powders and photocurable slurries for 3D printing. The polymerization depth of the slurries has been shown to strongly depend on the amount of the coloring additive in the Al2O3 powders. Using digital light processing (DLP) 3D printing followed by high-temperature sintering, we have obtained thin-walled planar samples of high-density periodic-structure ceramics and studied their microstructure and luminescence properties. Their photoluminescence spectrum contains a sharp strong line in the red spectral region, at 694 nm (characteristic line of ruby). The luminescence decay curves showed single-exponential behavior with a decay time of ~3.7 ms.

我们研究了少量Cr2O3和Cr3+添加量对3D打印用高纯铝基粉末和光固化浆料光学性能的影响。浆料的聚合深度与Al2O3粉末中着色添加剂的含量密切相关。采用数字光处理(DLP) 3D打印和高温烧结的方法,获得了高密度周期结构陶瓷的薄壁平面样品,并对其微观结构和发光性能进行了研究。它们的光致发光光谱在红色光谱区有一条锐利的强谱线,在694 nm处(红宝石的特征谱线)。发光衰减曲线呈单指数性质,衰减时间为~3.7 ms。
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引用次数: 0
Synthesis of a Diatomite-Based Calcium Metasilicate Hydrate and Investigation of Its Adsorptive and Structural Properties 硅藻土基水合偏硅酸钙的合成及其吸附和结构性能研究
IF 0.9 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2025-03-10 DOI: 10.1134/S0020168524700766
A. G. Manukyan

Optimal conditions have been found for lime treatment of diatomite from the Jradzor deposit (Armenia) which ensure that the resulting calcium metasilicate hydrate has a large specific surface area, high adsorption capacity, and good filtration performance. Differential thermal analysis, IR spectroscopy, and X-ray diffraction have been used to identify the mechanism underlying the formation of a C–S–H(I) calcium metasilicate hydrate during lime treatment of diatomite. Water and benzene vapor adsorption isotherms have been used to assess adsorptive and structural properties of the C–S–H(I) calcium metasilicate hydrate and calculate parameters of its pore structure. It is shown that C–S–H(I) calcium metasilicate hydrate can be effectively used as a filtration material and adsorbent.

已经找到了用石灰处理来自亚美尼亚 Jradzor 矿床的硅藻土的最佳条件,这些条件可确保生成的偏硅酸钙水合物具有较大的比表面积、较高的吸附能力和良好的过滤性能。差热分析、红外光谱和 X 射线衍射被用来确定硅藻土在石灰处理过程中形成 C-S-H(I)偏硅酸钙水合物的机理。利用水和苯蒸汽吸附等温线评估了 C-S-H(I)偏硅酸钙水合物的吸附和结构特性,并计算了其孔隙结构参数。结果表明,C-S-H(I) 偏硅酸钙水合物可有效用作过滤材料和吸附剂。
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引用次数: 0
High-Voltage Power Supply for X-ray Control of the Structure of Materials 用于材料结构x射线控制的高压电源
IF 0.9 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2025-03-10 DOI: 10.1134/S0020168524700699
A. S. Dmitriev, A. D. Kuleshov, N. N. Potrakhov, Yu. N. Potrakhov, K. K. Guk

A high-voltage power supply, along with an X-ray tube, is one of the main components of X-ray machines widely used in studying the structure of materials, estimating the internal structure of components and mechanisms, and nondestructive testing of technological processes. In monoblock devices, an X-ray tube and power supply are located in a common housing, while in cable-type setups, an X-ray emitter with the tube and a power supply are connected by a high-voltage cable. In this study, the results of creation of a stabilized high-voltage power supply for X-ray tubes as a part of a cable-type machine are reported. The electric circuits and design of the power supply based on a full-bridge voltage inverter built on power bipolar transistors are developed. The output voltage and power of the source are adjusted through the pulse width modulation of the rectified mains voltage applied to the primary winding of a high-voltage transformer. The use of a solid-state compound with increased thermal conductivity has made it possible to limit the design to forced air cooling of the source and place it within the Rack Mount standard dimensions (4U form factor). The experience of the power supply operation at a large industrial enterprise has shown that its electrical and dimensional parameters provide the possibility of successful use in X-ray machines for structure control of materials.

高压电源和x射线管是x射线机的主要部件之一,广泛应用于材料结构的研究、构件内部结构和机构的估计以及工艺过程的无损检测。在单块装置中,x射线管和电源位于一个共同的外壳中,而在电缆型装置中,x射线管和电源通过高压电缆连接。在这项研究中,报告了为x射线管作为电缆型机器的一部分创建稳定高压电源的结果。研究了基于功率双极晶体管的全桥电压逆变器的电源电路和设计。该源的输出电压和功率通过施加于高压变压器初级绕组的整流电源电压的脉宽调制来调节。使用具有更高导热性的固态化合物,可以将设计限制为强制空气冷却源,并将其放置在机架安装标准尺寸(4U形状因子)内。某大型工业企业电源运行的经验表明,它的电气参数和尺寸参数为x射线机成功应用于材料结构控制提供了可能。
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引用次数: 0
Root Cause Analysis of the Brittle Fracture of Pipes of Boiler Heating Surfaces after Long-Term Operation 锅炉受热面管道长期运行脆性断裂的根本原因分析
IF 0.9 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2025-03-10 DOI: 10.1134/S0020168524700559
A. V. Nechaeva, V. A. Polyanskii, A. M. Polyanskii, V. V. Shalagaev, Yu. A. Yakovlev

The study of the causes of destruction of power equipment is necessary for their elimination or limitation, as well as for the development and improvement of methods of technical diagnostics. The latter is especially important, since accidents or unplanned shutdowns of power equipment cause great economic damage. Standard methods of technical diagnostics in assessing the residual life of equipment include mechanical testing of samples cut out of equipment parts, determination of their chemical composition, structural studies, and fractography of the metal. Both fractures of samples specially cut for mechanical testing and surfaces of destruction that occurred during operation are studied. The danger of developing hydrogen embrittlement in metals is well known. The presence of brittle fracture areas or facets is usually associated with hydrogen-induced destruction or hydrogen embrittlement. Direct measurements of the concentration of hydrogen dissolved in metal samples are not regulated by standards; therefore, diagnostics of the development of hydrogen embrittlement is only qualitative. Our studies show that standard approaches are insufficient for technical diagnostics of the pipes of heating surfaces of boiler equipment. Hydrogen accumulation during operation may not have visible signs of corrosion or structural changes. It was found that hydrogen and external thermomechanical load induce anisotropy of mechanical and structural properties of steels of pipes of heating surfaces. As a result, the nature of destruction of samples cut from pipe walls depends on the orientation of test loads relative to the main axes of the stress tensor of operational (working) loads. The obtained experimental data allow us to conclude that, when establishing the causes of accidents and examining working heat exchangers in order to assess their residual life, it is necessary to additionally measure the distribution of the concentration of dissolved hydrogen in the metal and mechanically test ring samples.

研究电力设备的破坏原因,对于消除或限制电力设备的破坏,以及发展和改进技术诊断方法都是必要的。后者尤其重要,因为电力设备的意外或意外停机会造成巨大的经济损失。评估设备剩余寿命的技术诊断的标准方法包括对从设备部件中切割出来的样品进行机械测试、测定其化学成分、结构研究和金属断口学。对力学试验专用试样的断口和运行过程中产生的破坏面进行了研究。金属发生氢脆的危险是众所周知的。脆性断裂区域或断面的存在通常与氢致破坏或氢脆有关。直接测量金属样品中溶解氢的浓度没有标准规定;因此,对氢脆发展的诊断只是定性的。研究表明,对于锅炉设备受热面管道的技术诊断,标准的方法是不够的。操作过程中氢气的积累可能没有明显的腐蚀或结构变化迹象。结果表明,氢气和外部热机械载荷会导致受热面钢管力学性能和组织性能的各向异性。因此,从管壁上切下的试样的破坏性质取决于试验载荷相对于运行(工作)载荷应力张量主轴的方向。所获得的实验数据使我们得出结论,在确定事故原因和检查工作中的热交换器以评估其剩余寿命时,有必要额外测量金属中溶解氢浓度的分布和机械测试环样品。
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引用次数: 0
Effect of Organoalumoxanes on the Microstructure and Density of Al2O3f/Al2O3 Composites 有机铝氧烷对Al2O3f/Al2O3复合材料微观结构和密度的影响
IF 0.9 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2025-03-10 DOI: 10.1134/S0020168524700924
M. S. Varfolomeev, G. I. Shcherbakova

We describe binders and impregnating mixtures based on chelated organoalumoxanes, which are used as precursors to highly thermally stable matrices and protective coatings. Using the polymer impregnation and pyrolysis (PIP) process, we have fabricated Al2O3f/Al2O3 ceramic-matrix composites. Ceramic micropowders resulting from pyrolysis of the precursors have been shown to have an advantageous effect on the microstructure and properties of the material. We have studied the microstructure and density of Al2O3f/Al2O3 composites produced using chelated organoalumoxane-based binders and impregnating mixtures. The relative density of the composites, 3.1 g/cm3, considerably exceeds the initial density of the porous preform: 2.5 g/cm3.

我们描述了基于螯合有机铝氧烷的粘合剂和浸渍混合物,它们被用作高度热稳定的基质和保护涂层的前体。采用聚合物浸渍热解(PIP)工艺制备了Al2O3f/Al2O3陶瓷基复合材料。由前驱体热解得到的陶瓷微粉对材料的微观结构和性能有有利的影响。我们研究了用螯合有机铝基粘合剂和浸渍混合物制备的Al2O3f/Al2O3复合材料的微观结构和密度。复合材料的相对密度为3.1 g/cm3,大大超过了多孔预制体的初始密度2.5 g/cm3。
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引用次数: 0
Synthesis and Thermodynamic Properties of the Ca3Sc2Ge3O12 Germanate 锗酸Ca3Sc2Ge3O12的合成及热力学性质
IF 0.9 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2025-03-10 DOI: 10.1134/S0020168524700912
L. T. Denisova, L. G. Chumilina, Yu. F. Kargin, G. V. Vasil’ev, V. V. Beletskii, V. M. Denisov

The calcium strontium germanate Ca3Sc2Ge3O12 has been prepared by solid-state reaction, by firing a stoichiometric mixture of CaO, Sc2O3, and GeO2 in air at temperatures from 1273 to 1623 K. Using X-ray diffraction data for single-phase samples, we have determined the unit-cell parameter of Ca3Sc2Ge3O12 crystals (garnet structure, sp. gr. Ia(bar {3})d, a = 12.508(48) Å, V = 1956.92(2) Å3). The heat capacity of polycrystalline samples has been determined in the range 320–1050 K using differential scanning calorimetry. The results have been used to calculate thermodynamic functions of the calcium strontium germanate.

在1273 ~ 1623 K的温度下,将CaO、Sc2O3和GeO2的化学计量混合物在空气中烧制,通过固相反应制备了锗酸锶钙Ca3Sc2Ge3O12。利用单相样品的x射线衍射数据,我们确定了Ca3Sc2Ge3O12晶体(石榴石结构,sp. gr. Ia (bar {3}) d, a = 12.508(48) Å, V = 1956.92(2) Å3)的单胞参数。用差示扫描量热法测定了多晶样品在320 - 1050k范围内的热容。所得结果已用于计算锗酸锶钙的热力学函数。
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引用次数: 0
Installation and Testing Methods for Frequency Stability under Cyclic Loading of Metals and Alloys 金属和合金循环载荷下频率稳定性的安装和试验方法
IF 0.9 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2025-03-10 DOI: 10.1134/S0020168524700523
V. V. Mylnikov, E. A. Dmitriev, D. I. Shetulov

For manufacturing parts operating under complex conditions of cyclic loading, as well as products with stable dimensions, materials with minimal manifestations of inelastic properties are required. To study them, it is necessary to conduct specialized narrow-focus tests using machines and installations with appropriate experimental techniques. This paper presents the design of an electromagnetic installation for fatigue and frequency stability testing operating in a self-oscillating mode, in which the cyclic loading frequency is always equal to the natural frequency of oscillations of a sample. The installation control system contains two closed loops—for excitation of self-oscillations and for the oscillation amplitude stabilization. The sample is loaded by electromagnetic force and unloaded owing to the elastic forces of the material. This work presents a technique and algorithms for calculating the stresses of samples of various geometric shapes to assess changes in the amplitude–frequency characteristics. A calculated relationship is established between the force applied to the sample and its displacement at the point of force application, followed by determining the stress by the known force. The results of calibration tests for the static loading mode of samples are presented and the forces acting on the sample (external, inertia, elasticity) are estimated taking into account the maximum stress and maximum deformation amplitude. Static and cyclic loading modes are compared. The frequency characteristics are obtained when testing steel samples according to the proposed method. An analysis of the experimental results of tests with breaks during cyclic loading and continuous tests is carried out. It is shown that breaks in cyclic tests lead to an abrupt increase in frequency, while such jumps are absent during continuous tests. At the same time, a comparative analysis of the results of the considered types of tests showed that the total frequency deviation for the entire operating cycle is approximately the same in both cases. It is shown that the increase in frequency after rest is random and does not depend on the number of operating cycles.

为了制造在复杂循环载荷条件下工作的零件,以及尺寸稳定的产品,需要具有最小非弹性性能表现的材料。为了研究它们,有必要使用具有适当实验技术的机器和装置进行专门的窄焦点测试。本文设计了一种在自振荡模式下工作的电磁疲劳与频率稳定性试验装置,在这种模式下,循环加载频率总是等于试样的振荡固有频率。安装控制系统包括自激振荡和稳定振荡幅值两个闭环。样品由电磁力加载,由材料的弹性力卸载。这项工作提出了一种计算各种几何形状样品应力的技术和算法,以评估幅频特性的变化。建立了施加在试样上的力与其在施力点的位移之间的计算关系,然后通过已知的力确定应力。给出了试样静态加载模式的标定试验结果,并在考虑最大应力和最大变形幅值的情况下,估计了作用在试样上的力(外力、惯量、弹性)。对静荷载和循环荷载进行了比较。根据提出的方法对钢样进行测试,得到了频率特性。对循环加载和连续加载时的断裂试验结果进行了分析。结果表明,在循环试验中,中断会导致频率的突然增加,而在连续试验中则不会出现这种跳跃。同时,对所考虑的测试类型的结果进行比较分析表明,在这两种情况下,整个工作周期的总频率偏差大致相同。结果表明,静息后频率的增加是随机的,与工作循环次数无关。
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引用次数: 0
A Study of α-Zn2P2O7 Hygroscopicity α-Zn2P2O7的吸湿性研究
IF 0.9 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2025-03-10 DOI: 10.1134/S0020168524700936
D. A. Vatlin, O. G. Reznitskikh, E. A. Sherstobitova, O. V. Bushkova

We have studied water vapor absorption by the α-phase of zinc pyrophosphate, Zn2P2O7, at 25°C. This compound has been found to be highly hygroscopic owing to the formation of a crystalline hydrate with the composition Zn2P2O7∙5H2O. Removal of its water of crystallization has been shown to occur in three steps, starting at 60°C and reaching completion at 400°C. The phase composition of the dehydration product depends on heat treatment temperature. Below 500°C, we observe considerable amorphization and predominant formation of γ-Zn2P2O7, whereas phase-pure α-Zn2P2O7 can be obtained as a result of annealing at temperatures above 600°C.

我们研究了焦磷酸锌(Zn2P2O7) α-相在25℃时的水蒸气吸收率。该化合物被发现具有高度的吸湿性,因为它形成了一种晶体水合物,组成为Zn2P2O7∙5H2O。它的结晶水的去除有三个步骤,从60°C开始,到400°C完成。脱水产物的相组成取决于热处理温度。在500℃以下,我们观察到γ-Zn2P2O7的大量非晶化和主要形成,而在600℃以上退火可以得到相纯的α-Zn2P2O7。
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引用次数: 0
Characteristic Features of the Extraction of Rare-Earth Elements from Phosphogypsum 从磷石膏中提取稀土元素的特点
IF 0.9 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2025-03-10 DOI: 10.1134/S0020168524700857
I. S. Nikulin, T. B. Nikulicheva, A. V. Gal’tsev, D. A. Kolesnikov, V. S. Zakhvatinskii, A. O. V’yugin, N. V. Anosov

This paper examines how the gypsum-containing waste processing procedure influences the degree of rare-earth metal (REM) extraction from the waste. Gypsum-containing waste from the production of phosphoric acid was treated with aqueous solutions of various acids in the temperature range 25–140°C at solid : liquid ratios from 1 : 1 to 1 : 3. The results demonstrate that the largest REM extraction from phosphogypsum can be reached by treating with hydrochloric or nitric acid at the boiling point of the aqueous solution of the acid. Nitric acid is preferable because, after the acid treatment, the gypsum contains a large amount of nitrates, which can be used as agricultural fertilizers. Treatment of phosphogypsum at elevated temperatures and pressures leads to dissolution of a larger amount of gypsum, without increasing the REM yield. The highest economic efficiency of REM extraction from phosphogypsum is ensured by a solid : liquid ratio of about 1 ; 2, treatment temperature of 103–105°C, and cascade time no more than 10 min.

本文考察了含石膏废物处理工艺对废物中稀土金属提取率的影响。用不同酸的水溶液在25-140℃的温度范围内,以1:1至1:3的固液比处理磷酸生产中的含石膏废料。结果表明,在硫酸水溶液的沸点下,用盐酸或硝酸处理磷石膏可获得最大的REM萃取量。硝酸是最好的,因为经过酸处理后,石膏中含有大量的硝酸盐,可以用作农业肥料。在高温高压下处理磷石膏会导致大量石膏溶解,但不会增加REM收率。从磷石膏中提取REM的经济效益最高,固液比约为1;2、处理温度103-105℃,且串级时间不大于10 min。
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引用次数: 0
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Inorganic Materials
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