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Refined Method for Estimating the Interlayer Shear Modulus by Correcting the Deflection of Polymer Composite Specimens 通过修正聚合物复合材料试样挠度估算层间剪切模量的改进方法
IF 0.8 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-07-30 DOI: 10.1134/s0020168524700183
A. N. Polilov, D. D. Vlasov, N. A. Tatus

Abstract

The shear and interlayer characteristics of polymer fiber composites, in contrast to metals, play a decisive role in the deformation and fracture processes. In view of this, special methods have been developed to determine the interlayer flexional strength of a short beam and the interlayer shear modulus by the deflection correction. At the same time, the accepted hypotheses about the distribution of shear stresses, for example, those based on the Zhuravsky formula, are too simple and do not provide the determination of the correction and calculation of the shear modulus with a high accuracy. The use of the Saint-Venant–Lekhnitzky solution for an orthotropic beam instead of the simplest parabolic distribution potentially makes it possible to take into account all shear stresses occurring in a beam and their distribution over the beam height and width, which should increase the accuracy of determining the deflection correction and interlayer shear modulus, respectively. Since the strict solution is presented in a series of hyperbolic functions, its practical use is rather difficult. In this study, an exact approximation of the strict solution by simpler quadratic dependences is proposed, which makes it possible to determine the deflection correction and shear modulus with a high accuracy. It is shown using the proposed approximation that, for real beam-type composite specimens, the use of the refined shear stress distribution with allowance for the nonuniformity of stresses over the beam width yields a deflection correction negligibly small as compared with the case of the simplified parabolic distribution according to the Zhuravsky formula. The numerical verification using the finite element method has been carried out. Special three-point bending tests of fiberglass specimens of different widths have also showed no deflection growth with increasing beam width, which points out an insignificant impact of the heterogeneity of shear stresses on the deflection.

摘要与金属相比,聚合物纤维复合材料的剪切和层间特性在变形和断裂过程中起着决定性作用。有鉴于此,我们开发了特殊方法,通过挠度修正来确定短梁的层间抗弯强度和层间剪切模量。同时,关于剪应力分布的公认假设,例如基于 Zhuravsky 公式的假设,过于简单,无法提供高精度的校正确定和剪切模量计算。对正交梁采用 Saint-Venant-Lekhnitzky 解法,而不是最简单的抛物线分布,有可能考虑到梁中出现的所有剪应力及其在梁高和梁宽上的分布,从而分别提高确定挠度修正和层间剪切模量的精度。由于严格的解法是以一系列双曲函数的形式呈现的,因此其实际应用相当困难。本研究提出了用更简单的二次函数对严格解进行精确近似的方法,从而可以高精度地确定挠度修正和剪切模量。使用所提出的近似方法表明,对于实际的梁型复合材料试样,在考虑到梁宽度上应力不均匀性的情况下,使用细化的剪应力分布与根据 Zhuravsky 公式简化的抛物线分布相比,所产生的挠度修正小得可以忽略不计。使用有限元方法进行了数值验证。对不同宽度的玻璃纤维试样进行的特殊三点弯曲试验也表明,挠度不会随着梁宽的增加而增加,这说明剪应力的异质性对挠度的影响微乎其微。
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引用次数: 0
Fields of Residual Stresses near Open Assemblage Holes of Aircraft Wing Panel 飞机机翼面板装配孔附近的残余应力场
IF 0.8 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-07-30 DOI: 10.1134/s0020168524700298
S. I. Eleonsky, M. D. Zaitsev, Yu. G. Matvienko, V. S. Pisarev

Abstract

The results of fatigue tests of two geometrically identical and similar in design models of the lower wing panel of a commercial aircraft were analyzed. The panels differed in the way of installing mounting bolts, which connect the skin and stringers. Cold expansion of holes drilled both in the skin and stringer was performed for the first panel before joining. The second panel included no additional treatment after drilling pilot holes and final reaming. The bolts were mounted with an interference fit varying from 1.3 to 2.1% and from 2.9 to 3.2% for the first and the second panel, respectively. Changes in the interference fit were the consequence of a scatter attributed to the presence of a tolerance zone for the diameters of both bolts and mounting holes. A two-step comparison of both technologies was based on the experimental study of residual stress fields. The first stage, being a subject of the present study, included the analysis of residual stress fields arising after removal of the bolts and separation of the skin from stringers. Hole drilling and gradual crack growth were used to determine the components of residual stresses. The deformation response was measured by electronic speckle pattern interferometry. High quality interferograms, which provided a reliable resolution of the interference fringes of ultimate density over the hole edge or directly along the notch borders, were obtained for both ways of local removal of the material. The first (pointwise) method, based on drilling a probe hole, provided a quantitative determination of the residual stress components, starting from 1.4 mm distance from the assemblage hole edge. The second technique implements the crack compliance method of subsequent lengthening of the notch, starting directly from the mounting hole edge. This approach provided for a quantitative analysis of residual stress fields, related to different bolt mounting technologies, proceeding from the comparison of SIF values. A high level of compressive residual stresses near open holes was characteristic for both types of panels. Both experimental approaches showed the benefits of joints, where bolts are mounted into cold-expanded (reinforced) holes. For this case, the estimation of the relaxation parameters of the principal component of residual stresses in the direction of the external load is presented.

摘要 分析了两架几何形状相同、设计相似的商用飞机下翼板模型的疲劳试验结果。这两种机翼面板在连接蒙皮和弦杆的安装螺栓方式上有所不同。第一块面板在连接前对蒙皮和弦杆上的钻孔进行了冷膨胀处理。第二块面板在钻孔和最后铰孔之后没有进行额外处理。安装螺栓时,第一块面板和第二块面板的过盈配合分别为 1.3%至 2.1%和 2.9%至 3.2%。过盈配合的变化是由于螺栓和安装孔的直径存在公差带而造成的。根据残余应力场的实验研究,对两种技术进行了两步比较。第一阶段是本研究的主题,包括分析螺栓拆除和蒙皮与弦杆分离后产生的残余应力场。采用钻孔和裂纹逐渐增长的方法来确定残余应力的成分。变形响应是通过电子斑点模式干涉仪测量的。两种局部去除材料的方法都能获得高质量的干涉图,对孔边缘或直接沿缺口边界的极限密度干涉条纹提供可靠的分辨率。第一种(点式)方法以钻探孔为基础,从距装配孔边缘 1.4 毫米处开始定量测定残余应力成分。第二种技术采用了裂纹顺应法,即直接从装配孔边缘开始,对缺口进行后续加长。这种方法通过比较 SIF 值,对与不同螺栓安装技术相关的残余应力场进行了定量分析。两种类型的面板在开孔附近都存在较高的压缩残余应力。两种实验方法都显示了将螺栓安装到冷膨胀(加固)孔中的接头的优点。针对这种情况,介绍了外部载荷方向残余应力主分量松弛参数的估算。
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引用次数: 0
Actual Problems of Creating Digital Twins of Machine Engineering Products in Terms of Durability Assessment 在耐久性评估方面创建机械工程产品数字孪生产品的实际问题
IF 0.8 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-07-30 DOI: 10.1134/s0020168524700237
A. V. Erpalov, K. A. Khoroshevskii, I. V. Gadolina

Abstract

The global digitalization of production opens new opportunities for predictive diagnostics of the technical condition of mechanical engineering products. The issues attributed to assessing their technical condition, primarily to the determination of the residual life of mechanical engineering products, are considered. Currently, a class of virtual models, digital twins of the residual life, is distinguished. Apart from the functions of monitoring and predicting the stability of structures, they can possess a feedback and control the durability by simulating and optimizing the real technological process, taking into account the possibility of achieving the limit state of the structure. The problems of existing methods of assessing the durability in the time and frequency domains are considered in detail from the viewpoint of using the residual resource of structures as the basis of an algorithmic support of digital twins. We also marked the possible variety of obtaining initial data for assessing the durability, namely, fatigue diagrams of materials for different types and schemes of loading. The fatigue diagram is greatly affected by the loading process (regular, random, or mixed), while in the actual work the nonstationary random loading prevails. The methods used for assessing the durability of nonstationary loading are poorly studied and often resolve into simplification of a nonstationary process. The study is focused on nonstationary loading processes, since the creation of digital twins implies a continuous analysis of the durability of the structure for real operational loads. Other problems that can arise when developing digital twins of structures are also considered and discussed.

摘要 全球生产数字化为机械工程产品技术状况的预测诊断提供了新的机遇。本文探讨了评估机械工程产品技术状况的问题,主要是确定机械工程产品的残余寿命。目前,有一类虚拟模型,即残余寿命的数字孪生模型被区分开来。除了具有监测和预测结构稳定性的功能外,它们还可以通过模拟和优化实际技术过程来反馈和控制耐用性,同时考虑到实现结构极限状态的可能性。从使用结构残余资源作为数字孪生算法支持的基础的角度,详细考虑了现有时域和频域耐久性评估方法的问题。我们还指出了获取评估耐久性初始数据的各种可能方式,即不同类型和不同加载方案下的材料疲劳图。疲劳图受加载过程(常规、随机或混合)的影响很大,而在实际工作中,非稳态随机加载占主导地位。用于评估非稳态加载耐久性的方法研究较少,通常会简化非稳态过程。本研究的重点是非稳态加载过程,因为创建数字孪生结构意味着要对结构在实际运行荷载下的耐久性进行持续分析。此外,还考虑并讨论了在开发数字孪生结构时可能出现的其他问题。
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引用次数: 0
Analysis of the Electromagnetic Properties of 2000NN/2000NM Composites with Ferroelectric and Polymer Matrices 带有铁电和聚合物基质的 2000NN/2000NM 复合材料的电磁特性分析
IF 0.8 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-07-30 DOI: 10.1134/s002016852470016x
V. G. Kostishin, R. I. Shakirzyanov, I. M. Isaev, E. S. Savchenko, B. M. Skibo

Abstract

The results of studying the electrical properties of ferrite-dielectric composites containing inclusions of Mn-Zn and Ni-Zn spinel ferrites with the same initial magnetic permeability (grades 2000NM and 2000NN, respectively) and different electrical resistance are presented. Polymer and ceramic dielectrics with different values of dielectric permeability were used as matrices of composites: polystyrene (PS525), polyvinylidene fluoride (grade F2MB), lead zirconate titanate (PZT-21), and barium titanate (TBK-3). Experimental samples of composites were obtained by hot pressing (for a polymer matrix) or cold pressing with a binder (for a ferroelectric ceramic matrix). It has been shown that the radio-absorbing properties of the obtained composites strongly depend on the electrical properties of a dielectric matrix and on the electrical resistivity of a filler. The highest attenuation of electromagnetic waves of 25–27 dB in the frequency range of 4–5 GHz is observed for ferrite-polymer composites with a 2000NM semiconductor filler with a 6-mm-thick radio-absorbing material. For composites filled with a Mn-Zn ferrite, a pronounced shift in the dispersion region of magnetic permeability is also observed, which in turn changes the frequency position of peak radio absorption. For the composites with a ferroelectric matrix, the operating frequency range for both fillers was shifted toward the low-frequency region of 1–4 GHz with maximum attenuation of up to 22 dB at the same thickness of the material. It was experimentally confirmed that, at a weight content Cm of ferrite of 40 wt %, an increase in the dielectric permeability of the matrix results in a decrease in frequency fc of the center of minimum absorption and in a decrease in minimum reflection coefficient (K_{{{text{refl}}}}^{{min }}) at a metallic plate for a 2000NN filler with a high electrical resistance. For the composites with a 2000NM filler, the dependence of (K_{{{text{refl}}}}^{{min }}) (ε' of the matrix) passes through a minimum. The obtained composites can be considered as effective radio-absorbing materials for the frequency range of 1–6 GHz with peak attenuation of an electromagnetic wave in the range of 14–27 dB and with the operating frequency band of 1.1–2.5 GHz (at a level less than 10 dB).

摘要 本文介绍了对铁氧体-电介质复合材料电气特性的研究结果,这些复合材料含有具有相同初始磁导率(等级分别为 2000NM 和 2000NN)和不同电阻值的锰锌和镍锌尖晶石铁氧体夹杂物。具有不同介电渗透率值的聚合物和陶瓷电介质被用作复合材料的基体:聚苯乙烯(PS525)、聚偏氟乙烯(F2MB 级)、锆钛酸铅(PZT-21)和钛酸钡(TBK-3)。复合材料的实验样品是通过热压(聚合物基体)或使用粘合剂冷压(铁电陶瓷基体)获得的。实验表明,所获复合材料的无线电吸收特性在很大程度上取决于电介质基体的电特性和填料的电阻率。在 4-5 GHz 频率范围内,铁氧体-聚合物复合材料对电磁波的最高衰减为 25-27 dB,其中半导体填充物为 2000NM,无线电吸收材料为 6 毫米厚。对于填充了 Mn-Zn 铁氧体的复合材料,还观察到磁导率色散区域的明显偏移,这反过来又改变了无线电吸收峰值的频率位置。对于含有铁电基体的复合材料,两种填料的工作频率范围都向 1-4 GHz 的低频区域转移,在材料厚度相同的情况下,最大衰减可达 22 dB。实验证实,当铁氧体的重量含量 Cm 为 40 wt % 时,对于具有高电阻的 2000NN 填料,基体介电渗透率的增加会导致最小吸收中心频率 fc 的降低以及金属板上最小反射系数 (K_{{text/{refl}}}}^{/min}}/)的降低。对于使用 2000NM 填料的复合材料,(K_{{text/{refl}}}}^{min }})(基体的 ε')的依赖性通过了一个最小值。所获得的复合材料可视为 1-6 GHz 频率范围内的有效无线电吸收材料,其电磁波峰值衰减范围为 14-27 dB,工作频段为 1.1-2.5 GHz(电平小于 10 dB)。
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引用次数: 0
Diametral Compression of Short Cylinders with a Central Hole as a Method for Assessing the Tensile Strength of Brittle Materials 用带中心孔的短圆柱体直径压缩法评估脆性材料的抗拉强度
IF 0.8 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-07-30 DOI: 10.1134/s0020168524700201
V. Yu. Goltsev, A. V. Osintsev, A. S. Plotnikov, V. I. Polskij

Abstract

The possibility of assessing the fracture resistance of brittle materials by testing short cylinders, solid and with a central hole, under diametral compression has been investigated. The computational analysis was performed using the finite element method with the ANSYS program. It was shown that the stress distribution in a disk with a hole is similar to that in a disk without a hole, but it has disturbances caused by the stress concentrator in the form of the hole. The normalized values of the maximum principal stresses for a disk with a hole are more than 5 times higher than those for a disk without a hole. Experimental analysis was carried out by testing short cylinders made of brittle materials—cast iron and graphite—both solid and with a central hole. It was found that the fracture resistance determined by the formula of the ASTM D3967-95a standard is practically the same for solid cast iron specimens, while for graphite specimens it differs by 1.5 times from the true fracture resistance of the materials. When testing specimens of cast iron and graphite with a central hole, the fracture resistance differs from the standard by 1.5 and almost 2.5 times, respectively. The different nature of specimen failure was also noted—slow controlled fracture for cast iron and dynamic fracture for graphite, according to their respective deformation diagrams. As an example, the results of testing real cylindrical specimens with a central hole—uranium dioxide fuel pellets—are presented. It is shown that the results of testing graphite ARV-1 specimens and fuel pellets are in good agreement. Thus, the possibility of testing small short cylinders using the diametral compression scheme for indirect assessment of tensile strength of brittle materials is confirmed. A calculation equation is proposed for the indirect assessment of the tensile strength of brittle materials based on the results of testing small short cylinders with and without a central hole under diametral compression.

摘要 研究了在直径压缩条件下,通过测试实心和带中心孔的短圆柱体来评估脆性材料抗断裂性的可能性。计算分析采用 ANSYS 程序的有限元法进行。结果表明,带孔圆盘中的应力分布与无孔圆盘中的应力分布相似,但由于孔的形式存在应力集中器,因此会产生扰动。有孔圆盘的最大主应力归一化值是无孔圆盘的 5 倍多。实验分析是通过测试由脆性材料(铸铁和石墨)制成的短圆柱体,包括实心圆柱体和带中心孔的圆柱体。结果发现,根据 ASTM D3967-95a 标准公式确定的实心铸铁试样的抗断裂强度几乎相同,而石墨试样的抗断裂强度与材料的真实抗断裂强度相差 1.5 倍。在测试带有中心孔的铸铁和石墨试样时,断裂抗力分别与标准相差 1.5 倍和近 2.5 倍。此外,还注意到试样破坏的不同性质--根据各自的变形图,铸铁为缓慢受控断裂,石墨为动态断裂。举例来说,我们展示了带中心孔的真实圆柱形试样--二氧化钛燃料颗粒--的测试结果。结果表明,石墨 ARV-1 试样和燃料颗粒的测试结果非常一致。因此,使用直径压缩方案测试小型短圆柱体以间接评估脆性材料抗拉强度的可能性得到了证实。根据有中心孔和无中心孔短圆柱体在直径压缩下的测试结果,提出了间接评估脆性材料抗拉强度的计算公式。
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引用次数: 0
Study of the Generalized Curves of the Static and Cyclic Deformation, Damage, and Fracture 静态和循环变形、损伤和断裂的广义曲线研究
IF 0.8 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-07-30 DOI: 10.1134/s0020168524700195
N. A. Makhutov, M. M. Gadenin

Abstract

It is shown that materials on the metal, nonmetal, or composite base under the static and cyclic loading have individual deformation diagrams, which relate stresses and strains. These diagrams are obtained during the standard tensile, compression, torsion, or bending testing of laboratory samples with the detection of forces and deformations of their working parts under loading. In this case, the diagram for a single static deformation in the stress–strain coordinates covers both the elastic deformation region and the elastoplastic deformation region, when deformations are localized in the neck of a loaded sample until its destruction at a critical stress level. It is shown that obtained deformation diagrams are often described by a linear, fractional-linear, and power approximation of the obtained deformation curve. The direct experiments, theory of dislocations, and statistical theory of strength confirm the priority of the power approximation of the investigated diagrams. At the same time, for all construction materials, the generalized deformation diagram in relative coordinates is described by a single power equation with the individual hardening parameter, which is determined experimentally or theoretically from the dependences relating data on the elastic modulus, yield stress, strength, and ultimate plasticity of a material. The cyclic elastoplastic deformation diagrams in the form of plastic hysteresis loops are recorded by analogy with the static tension diagrams with the stress–strain axes in conditional and true relative values. The generalized deformation diagrams for a single static and cyclic loading form a scientific basis for plotting a generalized fatigue curve using the deformation fracture criterion for a wide range of cycles to failure. An effective solution to the strength and service life problems for the most complex engineering objects, such as nuclear reactors, aircraft, and rocket and space systems, can be achieved by considering the generalized deformation and fracture diagrams and relevant calculations. Their importance will especially increase in the design and implementation of new unique high-tech facilities.

摘要 研究表明,金属、非金属或复合材料在静态和循环载荷作用下会产生单独的变形图,这些变形图与应力和应变有关。这些变形图是在对实验室样品进行标准拉伸、压缩、扭转或弯曲试验时,通过检测其工作部件在加载下的力和变形而获得的。在这种情况下,应力-应变坐标中的单个静态变形图既包括弹性变形区,也包括弹塑性变形区,此时变形集中在加载样品的颈部,直到其在临界应力水平上被破坏。研究表明,所获得的变形曲线图通常用线性、分数线性和幂近似来描述。直接实验、位错理论和强度统计理论证实了所研究图表的幂近似的优先性。同时,对于所有建筑材料而言,相对坐标上的广义变形图都是由单个幂等式和单个硬化参数来描述的,而硬化参数是通过实验或理论确定的,与材料的弹性模量、屈服应力、强度和极限塑性相关。以塑性滞后环的形式记录循环弹塑性变形图,与静态拉伸图进行类比,应力-应变轴为条件相对值和真实相对值。单次静态和循环加载的广义变形图为使用变形断裂准则绘制广义疲劳曲线提供了科学依据,该曲线适用于各种失效循环。对于最复杂的工程对象,如核反应堆、飞机、火箭和太空系统,通过考虑广义变形和断裂图以及相关计算,可以有效地解决强度和使用寿命问题。特别是在设计和实施新的独特的高科技设施时,它们的重要性将与日俱增。
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引用次数: 0
On the Reasons for the Premature Failure of Safety Valve Springs in the Equipment of Primary Oil Refining 论一次炼油设备安全阀弹簧过早失效的原因
IF 0.8 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-07-30 DOI: 10.1134/s0020168524700213
M. A. Tupitsin, I. A. Trishkina, E. I. Storozheva

Abstract

The reasons for the premature failure of a spring (made of 50KhFA steel) used in the safety valve of the column head part are analyzed. The failure of the spring occurred after 7 years of operation at a temperature below 90°C in a working environment of light oil products (sulfurous gasoline). Visual and measurement control, general chemical analysis of the composition of the steel, energy-dispersive analysis of the metal in local areas, measurements of hardness and microhardness, microstructural analysis of the metal, macro- and electron fractography, phase chemical and X-ray structural analyses, and recovering heat treatment are used for the studies. The characteristic external signs, typical microdamages, and mechanisms of sulfide (hydrogen) corrosion cracking of high-strength 50KhFA steel with the most dangerous accompanying process, hydrogenation, are revealed. The analysis of the chemical composition and hardness of the metal meets the requirements of the standards for this steel. The microstructure of the metal under study is tempered martensite with the presence of a decarburized layer of up to 0.158 mm in the surface layers. The results of the study show that the premature failure of the spring is attributed both to the technological heredity and operational factors (contact with the working environment beyond the design basis). Ulcerative damage of the metal surface with the penetration of corrosion products into the deep layers due to the violation of the integrity of the coating of the spring are noted, which indicates low resistance of 50KhFA steel to low-temperature hydrogen sulfide corrosion. The failure predominantly occurs near nonmetallic inclusions along the boundaries of the primary austenite grains, where the largest precipitates of chromium carbides are located, as well as along the interphase boundaries of oriented carbide plates.

摘要 分析了用于柱头部分安全阀的弹簧(由 50KhFA 钢制成)过早失效的原因。在轻质油品(含硫汽油)的工作环境中,弹簧在低于 90°C 的温度下工作 7 年后发生故障。研究中使用了目视和测量控制、钢成分的一般化学分析、金属局部区域的能量色散分析、硬度和显微硬度测量、金属的微观结构分析、宏观和电子分形、相化学和 X 射线结构分析以及恢复热处理。揭示了高强度 50KhFA 钢硫化物(氢)腐蚀开裂的外部特征、典型微损伤和机理,以及最危险的伴随过程--析氢。对金属化学成分和硬度的分析符合该钢种的标准要求。所研究金属的微观结构为回火马氏体,表层存在长达 0.158 毫米的脱碳层。研究结果表明,弹簧过早失效的原因既有技术遗传因素,也有操作因素(与工作环境的接触超出了设计基础)。由于弹簧涂层的完整性受到破坏,金属表面出现溃疡性损伤,腐蚀产物渗入深层,这表明 50KhFA 钢对低温硫化氢腐蚀的抵抗力较低。失效主要发生在沿初级奥氏体晶粒边界的非金属夹杂物附近(最大的铬碳化物析出物位于此处),以及沿取向碳化物板的相间边界。
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引用次数: 0
Quantification of Calcium, Phosphorus, and Cerium in Novel Biocompatible Materials by Total Reflection X-Ray Fluorescence Spectroscopy 利用全反射 X 射线荧光光谱法量化新型生物兼容材料中的钙、磷和铈
IF 0.8 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-07-19 DOI: 10.1134/s0020168524700055
A. A. Samoilova, N. V. Petrakova, N. A. Andreeva, T. N. Penkina, S. G. Dorofeev, D. G. Filatova

Abstract

An approach to determining the composition of new biocompatible materials based on cerium-containing calcium phosphates using the TXRF method is proposed. The ranges of analyte contents in solutions were determined for the correct determination of Ca, P, and Ce using the external reference method. A systematic underestimation of the calcium signal was noted when its content in the analyzed composite sample was above 30 mg/L. In order to assess the compliance of the sample with the thin layer criterion, an analysis of the Compton scattering spectra for the ceramic sample solution was carried out; the maximum value was 16.8 keV (96°). According to the plot of the mass attenuation coefficient for a film of a given composition, the attenuation of the intensity of the calcium line perpendicular to the substrate is not associated with absorption of the sample. Internal reference samples (Gd and Cu) were selected and conditions were found for determining micro- and macrocomponents in solutions and suspensions of samples. It has been shown that, when the calcium content in the sample is up to 50 mg/L, it is possible to correctly determine Ca, P, and Ce using the TXRF method in solutions and suspensions with Sr of 0.05 and 0.09, respectively. The convergence of the results obtained using the external and internal reference methods with appropriate dilutions of solutions and suspensions was noted.

摘要 提出了一种使用 TXRF 方法测定基于含钙磷酸盐的新型生物兼容材料成分的方法。使用外部参照法确定了溶液中分析物含量的范围,以便正确测定钙、磷和铈。当分析的复合样品中钙含量超过 30 mg/L 时,钙信号被系统性低估。为了评估样品是否符合薄层标准,对陶瓷样品溶液的康普顿散射光谱进行了分析;最大值为 16.8 keV (96°)。根据特定成分薄膜的质量衰减系数图,垂直于基底的钙线强度衰减与样品的吸收无关。选择了内部参考样品(钆和铜),并找到了测定样品溶液和悬浮液中微观和宏观成分的条件。结果表明,当样品中的钙含量高达 50 毫克/升时,使用 TXRF 方法可以在 Sr 分别为 0.05 和 0.09 的溶液和悬浮液中正确测定 Ca、P 和 Ce。在适当稀释溶液和悬浮液的情况下,使用外部和内部参考方法得出的结果趋于一致。
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引用次数: 0
Assessing the Reliability of the Forensic Technique for the Identification Study of Motor Gasoline Using Gas-Liquid Chromatography 评估使用气-液色谱法鉴定车用汽油的法医技术的可靠性
IF 0.8 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-07-19 DOI: 10.1134/s0020168524700134
G. I. Bebeshko, G. G. Omel’yanyuk, O. V. Samoilova, A. I. Usov

Abstract

A new approach to solving the problems of forensic examination of petroleum products, fuels, and lubricants associated with establishing whether motor gasoline belongs to a common/different identification variety is proposed. A technique for the identification of gasoline using quantitative results of chromatographic determination of controlled parameters and subsequent evaluation of the results in pairwise compared samples according to the established criteria is developed. The following parameters were selected as controlled parameters: values of research octane number (RON), concentrations of hydrocarbon groups (paraffins, isoparaffins, arenes, naphthenes, olefins) and oxygenates. Their determination was carried out using standardized methods. We used the hardware and software complex of the Chromatec-Crystal 5000 series, including the Chromatec-DHA data processing program. Estimated criteria or decision-making rules regarding the issues posed to an expert were determined to classify gasoline under one product name (generic variety), one production technology (group variety), or a common source of origin (one production batch, storage tank, etc.). The reliability of the method was assessed using a validation procedure consisting of three stages. We used a collection of AI-92 motor gasoline, selected at gas stations of four oil companies during six months of 2022 in various districts of Moscow. At the first stage, the performer analyzed 12 aliquots of each of four gasoline samples (samples that previously belonged to the common volume) at different times. It was established that the quality indicators of the proposed technique (standard deviation of the repeatability and reproducibility, expanded uncertainty, limits of the repeatability and reproducibility) for each of the determined controlled indicators did not exceed the permissible errors established by standardized methods. At the second stage of the experiment, the performer combined 12 test samples into four groups from each manufacturer (one production technology) with three samples of different production times (different batches). By comparing the discrepancies in the measured values of the same controlled indicators between pairs of samples within groups and the discrepancy in average indicators between pairs of groups, the performer establish gasolines manufactured using the same technology; gasolines produced by the same technology, but at different times (different batches); and with a probability of 95%, gasolines having a common source of origin (previously belonging to a common volume). The conclusions of the validation study matched the original data on the samples, which confirmed the correctness of the developed comparison criteria. At the third stage (blind test), the performer examined seven gasoline samples information about the composition and properties of which was not provided to him. The results of the blind test w

摘要 提出了一种新方法来解决与确定车用汽油是否属于共同/不同鉴定品种有关的石油产品、燃料和润滑油的法医检验问题。利用色谱法测定受控参数的定量结果以及随后根据既定标准对成对比较样品的结果进行评估,开发了一种鉴定汽油的技术。选定以下参数作为控制参数:研究辛烷值 (RON)、烃类(石蜡、异构烷烃、炔烃、环烷烃、烯烃)和含氧化合物的浓度。它们的测定采用标准化方法进行。我们使用了 Chromatec-Crystal 5000 系列的硬件和软件,包括 Chromatec-DHA 数据处理程序。就专家提出的问题确定了估计标准或决策规则,以便将汽油归类为一个产品名称(通用品种)、一种生产技术(群体品种)或一个共同来源(一个生产批次、储罐等)。该方法的可靠性通过由三个阶段组成的验证程序进行评估。我们使用了 2022 年 6 个月期间在莫斯科各区四家石油公司加油站收集的 AI-92 车用汽油。在第一阶段,执行人员在不同时间分别对四个汽油样品(之前属于共同体积的样品)中的 12 个等分样品进行了分析。结果表明,所建议技术的质量指标(重复性和再现性的标准偏差、扩大的不确定性、重复性和再现性的极限)的每一个确定的控制指标都没有超过标准方法规定的允许误差。在实验的第二阶段,执行人员将每个生产商(一种生产技术)的 12 个测试样品分成四组,每组有三个不同生产时间(不同批次)的样品。通过比较组内各组样品之间相同受控指标测量值的差异和各组之间平均指标的差异,执行者确定了采用相同技术生产的汽油;采用相同技术生产但生产时间不同(不同批次)的汽油;以及具有共同来源(以前属于同一批次)的汽油,概率为 95%。验证研究的结论与样品的原始数据相吻合,证实了所制定的比较标准的正确性。在第三阶段(盲测),表演者检查了 7 个汽油样品,但没有向他提供这些样品的成分 和特性信息。盲测结果令人满意。因此,验证结果表明,该方法适用于解决与车用汽油有关的法医鉴定问题,而且执行人员有能力实施该技术。
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引用次数: 0
Express X-Ray Fluorescence Analysis of Technical-Grade Tantalum and Niobium: from Raw Materials to Products 技术级钽和铌的快速 X 射线荧光分析:从原材料到产品
IF 0.8 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Pub Date : 2024-07-19 DOI: 10.1134/s0020168524700067
L. Yu. Mezhevaya, M. N. Filippov, O. I. Lyamina, G. E. Mar’ina, A. A. Arkhipenko, V. B. Baranovskaya

Abstract

The available approaches to detecting impurities in Ta- and Nb-based materials involve transferring a sample into a solution with subsequent isolation of impurities. This procedure is quite complicated and time-consuming. Therefore, it is interesting to study the possibilities of direct, in particular, X-ray fluorescence (XRF), analysis of solid samples of these materials. The conventional XRF scheme, which involves the experimental construction of calibration characteristics for each element being determined, requires a large number of reference samples containing a very wide range of impurities. In this work, a preliminary characterization of samples of technical tantalum and niobium and products based on them has been carried out. It is shown that, for initial materials, the XRF method can establish only a significant absence of impurities; however, even for sintered niobium hydride and tantalum powder, XRF can be used for the express estimation of the composition. It is proposed to use a Spectroscan MAX-GVM crystal diffraction spectrometer for the analysis and to construct the calibration using the standard software that implements the fundamental parameter method. In this case, the resulting impurity contents can differ from reference values by one to two orders of magnitude. Such accuracy is often sufficient to adjust the technology. The limits of the XRF detection of impurities in Ta- and Nb-based materials have been established. For the elements determined by K-series lines (from Ti to Co), the detection limits range within 30–60 ppm; for the elements determined by M-series lines (Ta), the detection limit is approximately 200 ppm; and for L-series lines (Nb), it is from 100 to 150 ppm.

摘要 检测钽基和铌基材料中杂质的现有方法涉及将样品转移到溶液中,然后分离杂质。这一过程相当复杂且耗时。因此,研究对这些材料的固体样品进行直接分析,特别是 X 射线荧光分析(XRF)的可能性很有意义。传统的 X 射线荧光分析法需要在实验中为每种待测元素建立校准特征,这就需要大量含有各种杂质的参考样品。在这项工作中,我们对工业钽和铌样品以及以它们为基础的产品进行了初步表征。结果表明,对于初始材料,XRF 方法只能确定明显不含杂质;但是,即使对于烧结的氢化铌和钽粉,XRF 也可用于明确估算成分。建议使用 Spectroscan MAX-GVM 晶体衍射光谱仪进行分析,并使用执行基本参数法的标准软件进行校准。在这种情况下,得出的杂质含量可能与参考值相差一到两个数量级。这种精度通常足以调整技术。钽基和铌基材料中杂质的 XRF 检测极限已经确定。对于 K 系列线测定的元素(从钛到钴),检测限在 30-60 ppm 范围内;对于 M 系列线测定的元素(钽),检测限约为 200 ppm;对于 L 系列线(铌),检测限为 100-150 ppm。
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引用次数: 0
期刊
Inorganic Materials
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