Pub Date : 2024-02-22DOI: 10.26896/1028-6861-2024-90-2-39-46
A. L. Zhaludkevich, S. Karpushenkov, L. Karpushenkava, A. V. Konovalova, O. V. Ignatenko, T. V. Shoukavaya
A low wear resistance is a significant disadvantage of magnesium-based alloys widely used in industry. The results of plasma electrolytic oxidation (PEO) carried out in an aqueous-alkaline phosphate electrolyte with the addition of hexagonal boron nitride (h-BN) powder to obtain coatings with greater wear resistance on the surface of AZ31 magnesium alloy are presented. The PEO method is one of the most promising for surface treatment of magnesium alloys, since oxidation is carried out in alkaline aluminate, silicate or phosphate electrolytes with various functional additives. The addition of nanocrystalline hexagonal h-BN powder in the form of a suspension into the electrolyte volume does not affect the electrical parameters of PEO, and h-BN particles are incorporated into the structure of the formed composite coating, increasing the wear resistance. It is shown that the resulting coatings have a relief typical of PEO with developed morphology and porosity, which change depending on the oxidation time. In this case, the incorporation of h-BN particles into the coating occurs by an inert mechanism, since they do not undergo chemical transformations with the formation of new phases. Composite coatings obtained on the surface of the AZ31 magnesium alloy by the PEO method consist of crystalline phases of MgO and Mg3(PO4)2, regardless of the addition of h-BN particles to the electrolyte. The wear resistance of coatings is 6 – 8 times higher compared to the untreated alloy. The results obtained can be used to produce PEO coatings with increased wear resistance and use them in various sectors of the economy.
{"title":"Study of the wear resistance of composite coatings modified with h-BN particles on AZ31 magnesium alloy","authors":"A. L. Zhaludkevich, S. Karpushenkov, L. Karpushenkava, A. V. Konovalova, O. V. Ignatenko, T. V. Shoukavaya","doi":"10.26896/1028-6861-2024-90-2-39-46","DOIUrl":"https://doi.org/10.26896/1028-6861-2024-90-2-39-46","url":null,"abstract":"A low wear resistance is a significant disadvantage of magnesium-based alloys widely used in industry. The results of plasma electrolytic oxidation (PEO) carried out in an aqueous-alkaline phosphate electrolyte with the addition of hexagonal boron nitride (h-BN) powder to obtain coatings with greater wear resistance on the surface of AZ31 magnesium alloy are presented. The PEO method is one of the most promising for surface treatment of magnesium alloys, since oxidation is carried out in alkaline aluminate, silicate or phosphate electrolytes with various functional additives. The addition of nanocrystalline hexagonal h-BN powder in the form of a suspension into the electrolyte volume does not affect the electrical parameters of PEO, and h-BN particles are incorporated into the structure of the formed composite coating, increasing the wear resistance. It is shown that the resulting coatings have a relief typical of PEO with developed morphology and porosity, which change depending on the oxidation time. In this case, the incorporation of h-BN particles into the coating occurs by an inert mechanism, since they do not undergo chemical transformations with the formation of new phases. Composite coatings obtained on the surface of the AZ31 magnesium alloy by the PEO method consist of crystalline phases of MgO and Mg3(PO4)2, regardless of the addition of h-BN particles to the electrolyte. The wear resistance of coatings is 6 – 8 times higher compared to the untreated alloy. The results obtained can be used to produce PEO coatings with increased wear resistance and use them in various sectors of the economy.","PeriodicalId":504498,"journal":{"name":"Industrial laboratory. Diagnostics of materials","volume":"52 4","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140440489","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-02-22DOI: 10.26896/1028-6861-2024-90-2-53-61
S. Monin, M. A. Gorbovets, I. A. Khodinev
Using a sample of test results from 68 compact eccentric tensile specimens made of titanium alloys, nickel alloys and steel, the effect of the choice of numerical differentiation method (secant method and the method of differential polynomials on three, five and seven points) used to calculate the fatigue crack growth rate on characteristics of the linear section of the kinetic diagram of the fatigue failure. The purpose of the study is to determine the advantages, disadvantages and consistent patterns of the considered methods. The coefficient of determination R 2, integral criterion χ which characterizes the difference between the predicted and actual number of cycles corresponding to the section of stable crack growth, and correlation between the logarithms of the Paris constants for alloys of the same class were used as criteria for the correct choice of the method of numerical differentiation. The main results and conclusions of the study: the use of the method of differential polynomials over three points compared to the secant method slightly increases the correlation between the logarithms of the fatigue crack growth rate and the range of the stress intensity factor (an increase in R 2) and increases the difference between the calculated and experimental number of cycles corresponding to stable crack growth (an increase in χ). However, when determining the fatigue crack growth rate by the method of differential polynomials for five and seven points, a more significant smoothing of the experimental data is observed, accompanied by a significant increase in R 2 and a decrease in χ; proximity to zero of the integral accuracy parameter χ is a necessary but not sufficient criterion for good agreement between the test result and the mathematical model that describes it, while the combination of parameters χ and R 2 uniquely forms this criterion; the choice of the method of numerical differentiation does not affect the correlation of the logarithms of the constants of the Paris equation.
利用 68 个由钛合金、镍合金和钢制成的紧凑型偏心拉伸试样的测试结果样本，研究了用于计算疲劳裂纹生长率的数值微分法（三次方法和三点、五点和七点微分多项式法）的选择对疲劳破坏动力学图线性截面特征的影响。研究的目的是确定所考虑方法的优缺点和一致模式。确定系数 R 2、表征稳定裂纹增长段对应的预测循环数与实际循环数之间差异的积分标准 χ 以及同类合金的巴黎常数对数之间的相关性被用作正确选择数值微分方法的标准。研究的主要结果和结论：与正割法相比，使用三点微分多项式法会略微增加疲劳裂纹增长速率对数与应力强度因子范围之间的相关性（R 2 增加），并增加稳定裂纹增长对应的计算循环次数与实验循环次数之间的差异（χ 增加）。然而，当采用微分多项式法确定五点和七点的疲劳裂纹生长率时，实验数据出现了更明显的平滑，同时 R 2 显著增加，χ 下降；积分精度参数 χ 接近于零是试验结果与描述试验结果的数学模型之间保持良好一致性的一个必要但不充分的标准，而参数 χ 和 R 2 的组合则唯一地构成了这一标准；数值微分方法的选择并不影响巴黎方程常数对数的相关性。
{"title":"On the application of numerical differentiation methods to the determination of the fatigue crack growth rate","authors":"S. Monin, M. A. Gorbovets, I. A. Khodinev","doi":"10.26896/1028-6861-2024-90-2-53-61","DOIUrl":"https://doi.org/10.26896/1028-6861-2024-90-2-53-61","url":null,"abstract":"Using a sample of test results from 68 compact eccentric tensile specimens made of titanium alloys, nickel alloys and steel, the effect of the choice of numerical differentiation method (secant method and the method of differential polynomials on three, five and seven points) used to calculate the fatigue crack growth rate on characteristics of the linear section of the kinetic diagram of the fatigue failure. The purpose of the study is to determine the advantages, disadvantages and consistent patterns of the considered methods. The coefficient of determination R 2, integral criterion χ which characterizes the difference between the predicted and actual number of cycles corresponding to the section of stable crack growth, and correlation between the logarithms of the Paris constants for alloys of the same class were used as criteria for the correct choice of the method of numerical differentiation. The main results and conclusions of the study: the use of the method of differential polynomials over three points compared to the secant method slightly increases the correlation between the logarithms of the fatigue crack growth rate and the range of the stress intensity factor (an increase in R 2) and increases the difference between the calculated and experimental number of cycles corresponding to stable crack growth (an increase in χ). However, when determining the fatigue crack growth rate by the method of differential polynomials for five and seven points, a more significant smoothing of the experimental data is observed, accompanied by a significant increase in R 2 and a decrease in χ; proximity to zero of the integral accuracy parameter χ is a necessary but not sufficient criterion for good agreement between the test result and the mathematical model that describes it, while the combination of parameters χ and R 2 uniquely forms this criterion; the choice of the method of numerical differentiation does not affect the correlation of the logarithms of the constants of the Paris equation.","PeriodicalId":504498,"journal":{"name":"Industrial laboratory. Diagnostics of materials","volume":"18 9‐10","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140438635","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-02-22DOI: 10.26896/1028-6861-2024-90-2-29-38
E. G. Vinokurov, C. R. Gainetdinov, R. V. Grafushin, V. D. Skopintsev, V. V. Vasilev, T. F. Burukhina
The surface roughness of coatings has a significant impact on their functional properties and efficiency. We present the results of studying the effect of the main technological parameters on the roughness of chemical coatings with Ni – P and Ni – Cu – P alloys. The key factors affecting the roughness of coatings were determined by the Taguchi method. Parameters of the coating process were varied in the experiments: concentration of components in solution, pH, temperature, and the time of deposition. It is found that the surface roughness increases linearly with the thickness of coatings. The concentration of sodium hypophosphite and pH value have the greatest influence on the development of roughness. It is shown that the lowest roughness is observed at concentrations of sodium hypophosphite and copper salt 0.358 and 0.0012 mol/liter, pH 5.8 and temperature 90 °C. The rate of the surface roughness development for Ni – P and Ni – Cu – P coatings under optimal conditions is 0.68 and 0.97 %/μm (before optimization — 6.72 %/μm). The obtained results can be used to improve the methodology for reducing the roughness of coatings with Ni – P and Ni – Cu – P alloys and, accordingly, to improve the functionality, wear resistance and quality of coatings.
涂层的表面粗糙度对其功能特性和效率有重大影响。我们介绍了主要技术参数对镍-铂和镍-铜-铂合金化学涂层粗糙度影响的研究结果。采用田口方法确定了影响涂层粗糙度的关键因素。实验中改变了涂层工艺的参数：溶液中成分的浓度、pH 值、温度和沉积时间。结果发现，表面粗糙度随涂层厚度的增加而线性增加。次磷酸钠浓度和 pH 值对粗糙度的发展影响最大。结果表明，当次磷酸钠和铜盐的浓度分别为 0.358 和 0.0012 摩尔/升、pH 值为 5.8、温度为 90 ℃ 时，粗糙度最低。在最佳条件下，Ni - P 和 Ni - Cu - P 涂层的表面粗糙度变化率分别为 0.68 和 0.97 %/μm（优化前为 6.72 %/μm）。所得结果可用于改进降低镍-磷和镍-铜-磷合金镀层粗糙度的方法，从而提高镀层的功能性、耐磨性和质量。
{"title":"Study of crucial factors for minimizing the roughness of chemical coatings with Ni – P and Ni – Cu – P alloys","authors":"E. G. Vinokurov, C. R. Gainetdinov, R. V. Grafushin, V. D. Skopintsev, V. V. Vasilev, T. F. Burukhina","doi":"10.26896/1028-6861-2024-90-2-29-38","DOIUrl":"https://doi.org/10.26896/1028-6861-2024-90-2-29-38","url":null,"abstract":"The surface roughness of coatings has a significant impact on their functional properties and efficiency. We present the results of studying the effect of the main technological parameters on the roughness of chemical coatings with Ni – P and Ni – Cu – P alloys. The key factors affecting the roughness of coatings were determined by the Taguchi method. Parameters of the coating process were varied in the experiments: concentration of components in solution, pH, temperature, and the time of deposition. It is found that the surface roughness increases linearly with the thickness of coatings. The concentration of sodium hypophosphite and pH value have the greatest influence on the development of roughness. It is shown that the lowest roughness is observed at concentrations of sodium hypophosphite and copper salt 0.358 and 0.0012 mol/liter, pH 5.8 and temperature 90 °C. The rate of the surface roughness development for Ni – P and Ni – Cu – P coatings under optimal conditions is 0.68 and 0.97 %/μm (before optimization — 6.72 %/μm). The obtained results can be used to improve the methodology for reducing the roughness of coatings with Ni – P and Ni – Cu – P alloys and, accordingly, to improve the functionality, wear resistance and quality of coatings.","PeriodicalId":504498,"journal":{"name":"Industrial laboratory. Diagnostics of materials","volume":"9 6","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140438944","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-02-22DOI: 10.26896/1028-6861-2024-90-2-47-52
A. B. Ankudinov, M. I. Alymov, V. Zelensky, R. Kapustin, A. E. Sychev, V. S. Shustov
Data on pore size distribution in solids are obtained by pycnometric density-based methods for measuring the pore structure of materials. The results of measuring open porosity by weighing a dry sample followed by evacuation and saturation with distilled water at atmospheric pressure, impregnation with water under pressure using a hydrostat and mercury porosimetry are presented. The samples of porous nickel obtained using powder technology by sintering of the compacts from mixtures of nickel nanopowder with powder ammonium bicarbonate NH4HCO3 (a blowing agent), the volume fractions of which were 80 and 20%, respectively, were studied. A powder blowing agent with a particle size of 63 – 125, 140 – 200, and 250 – 315 μm was used. A theoretical estimation of the pore size available for the penetration of the impregnating liquid was carried out for three methods used for the determination of open porosity. It is shown that upon water saturation after evacuation the liquid can penetrate only into pores larger than 3 μm. Moreover, in porous structures with a large fraction of submicron pores, the actual values of the open porosity are significantly underestimated when using the method of saturation with distilled water after evacuation. The higher the fraction of fine pores in the material, the lower the open porosity value. The difference between the open porosity values determined by methods of water impregnation using a hydrostat and mercury porosimetry was negligible. It has been established that among three considered methods for measuring open porosity, only the method of saturation with distilled water after evacuation cannot be used in analysis of structures with submicron pores. The results obtained can be used to develop porous functional materials and products with a given porosity structure.
{"title":"Determination of the porosity characteristics by pycnometric methods","authors":"A. B. Ankudinov, M. I. Alymov, V. Zelensky, R. Kapustin, A. E. Sychev, V. S. Shustov","doi":"10.26896/1028-6861-2024-90-2-47-52","DOIUrl":"https://doi.org/10.26896/1028-6861-2024-90-2-47-52","url":null,"abstract":"Data on pore size distribution in solids are obtained by pycnometric density-based methods for measuring the pore structure of materials. The results of measuring open porosity by weighing a dry sample followed by evacuation and saturation with distilled water at atmospheric pressure, impregnation with water under pressure using a hydrostat and mercury porosimetry are presented. The samples of porous nickel obtained using powder technology by sintering of the compacts from mixtures of nickel nanopowder with powder ammonium bicarbonate NH4HCO3 (a blowing agent), the volume fractions of which were 80 and 20%, respectively, were studied. A powder blowing agent with a particle size of 63 – 125, 140 – 200, and 250 – 315 μm was used. A theoretical estimation of the pore size available for the penetration of the impregnating liquid was carried out for three methods used for the determination of open porosity. It is shown that upon water saturation after evacuation the liquid can penetrate only into pores larger than 3 μm. Moreover, in porous structures with a large fraction of submicron pores, the actual values of the open porosity are significantly underestimated when using the method of saturation with distilled water after evacuation. The higher the fraction of fine pores in the material, the lower the open porosity value. The difference between the open porosity values determined by methods of water impregnation using a hydrostat and mercury porosimetry was negligible. It has been established that among three considered methods for measuring open porosity, only the method of saturation with distilled water after evacuation cannot be used in analysis of structures with submicron pores. The results obtained can be used to develop porous functional materials and products with a given porosity structure.","PeriodicalId":504498,"journal":{"name":"Industrial laboratory. Diagnostics of materials","volume":"29 18","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140442164","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-02-22DOI: 10.26896/1028-6861-2024-90-2-62-72
A. Polovyi, N. Lisachenko
A method for calculating the stress-strain state of layers of cross-ply laminate based on an experimental deformation diagram under uniaxial tension is proposed. The essence of the method consists in solving a system of two equations describing the experimental curves σx = f(εx) and σx = f(εy), which allows determination of two unknown parameters related to the secant elastic characteristics of the material layers. The law of change in the remaining unknown parameters is set by assumptions regarding deformation of the polymer matrix composite and its layers during loading. To carry out the calculation, it is necessary to set the initial values of the elastic properties of the unidirectional material of the layers, which should be well consistent with the initial values of the elastic properties of the structure under study determined from the experiment. According to the developed algorithm, calculated dependences between average stresses, deformations and secant elastic properties of the layers of the structure are obtained (0°/90°/90°/0°) made of fiberglass E-Glass/MY750 using experimental data from the literature. Calculations carried out for three sets of initial values of the elastic properties of the material under study showed qualitatively identical results. The transverse tensile stress in the 90° layer reaches a maximum in the first half of the stress-strain diagram, and then decreases to zero. A similar stress in the 0° layer reaches a maximum at the failure point of the structure under study. It is revealed that the maximum calculated values of transverse stresses acting in layers 0° and 90° noticeably exceed the transverse tensile strength of the material specified in the literature. The longitudinal tensile stress in the 0° layer reaches a maximum at the failure point and corresponds to 95% of the value of the longitudinal tensile strength of the material. The longitudinal compressive stress in the 90° layer is at a low level throughout the deformation process of the structure under study. The results of this study can be recommended for developing models of the behavior of layers with cracks in the matrix when loading a polymer matrix composite.
{"title":"Calculation of the stress-strain state of layers of cross-ply laminate based on an experimental stress-strain curves under uniaxial tension","authors":"A. Polovyi, N. Lisachenko","doi":"10.26896/1028-6861-2024-90-2-62-72","DOIUrl":"https://doi.org/10.26896/1028-6861-2024-90-2-62-72","url":null,"abstract":"A method for calculating the stress-strain state of layers of cross-ply laminate based on an experimental deformation diagram under uniaxial tension is proposed. The essence of the method consists in solving a system of two equations describing the experimental curves σx = f(εx) and σx = f(εy), which allows determination of two unknown parameters related to the secant elastic characteristics of the material layers. The law of change in the remaining unknown parameters is set by assumptions regarding deformation of the polymer matrix composite and its layers during loading. To carry out the calculation, it is necessary to set the initial values of the elastic properties of the unidirectional material of the layers, which should be well consistent with the initial values of the elastic properties of the structure under study determined from the experiment. According to the developed algorithm, calculated dependences between average stresses, deformations and secant elastic properties of the layers of the structure are obtained (0°/90°/90°/0°) made of fiberglass E-Glass/MY750 using experimental data from the literature. Calculations carried out for three sets of initial values of the elastic properties of the material under study showed qualitatively identical results. The transverse tensile stress in the 90° layer reaches a maximum in the first half of the stress-strain diagram, and then decreases to zero. A similar stress in the 0° layer reaches a maximum at the failure point of the structure under study. It is revealed that the maximum calculated values of transverse stresses acting in layers 0° and 90° noticeably exceed the transverse tensile strength of the material specified in the literature. The longitudinal tensile stress in the 0° layer reaches a maximum at the failure point and corresponds to 95% of the value of the longitudinal tensile strength of the material. The longitudinal compressive stress in the 90° layer is at a low level throughout the deformation process of the structure under study. The results of this study can be recommended for developing models of the behavior of layers with cracks in the matrix when loading a polymer matrix composite.","PeriodicalId":504498,"journal":{"name":"Industrial laboratory. Diagnostics of materials","volume":"17 9","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140440882","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-02-22DOI: 10.26896/1028-6861-2024-90-2-73-82
V. V. Mylnikov, E. A. Dmitriev, D. I. Shetulov
Manufacture of parts operating under difficult conditions of cyclic loading, as well as products with stable dimensions necessitates the use of materials with minimal manifestations of inelastic properties. Study of these materials suggests conducting specialized narrowly focused tests using newly developed machines and installations with appropriate experimental techniques. We present the design, operation and control features of the original electromagnetic installation for testing fatigue and frequency stability and operating in a self- oscillating mode, which provides the equality of the frequency of cyclic loading and natural frequency of the sample. The system of the installation control contains two closed circuits: for excitation of self-oscillations and for stabilization of the oscillation amplitude. The sample is loaded by electromagnetic force, and unloading occurs due to the elastic forces of the material. The methodology and algorithms for calculating the stresses of samples of various geometric shapes for estimating changes in amplitude-frequency characteristics are presented. The calculated relationship between the force applied to the sample and its movement at the point of application of force is derived with subsequent determination of the stress by a known force. The results of calibration tests for the static mode of sample loading are presented and the forces acting on the sample (external, inertia, and elastic forces) are evaluated taking into account the maximum stress and maximum strain amplitude. Static and cyclic loading modes are compared. The frequency characteristics obtained during testing steel samples according to the proposed method are obtained. The experimental results of tests with interruptions in the process of cyclic loading and continuous testing are analyzed. It is shown that interruptions in cyclic tests lead to a jump-like increase in the frequency, whereas continuous tests revealed no jumps. At the same time, a comparative analysis with the results of continuous tests showed that the overall frequency deviation is approximately the same for the entire operating cycle in both cases. It is shown that an increase in the frequency after rest is random and does not depend on the number of operating cycles.
{"title":"Installation and test procedure for frequency stability under cyclic loading of metals and alloys","authors":"V. V. Mylnikov, E. A. Dmitriev, D. I. Shetulov","doi":"10.26896/1028-6861-2024-90-2-73-82","DOIUrl":"https://doi.org/10.26896/1028-6861-2024-90-2-73-82","url":null,"abstract":"Manufacture of parts operating under difficult conditions of cyclic loading, as well as products with stable dimensions necessitates the use of materials with minimal manifestations of inelastic properties. Study of these materials suggests conducting specialized narrowly focused tests using newly developed machines and installations with appropriate experimental techniques. We present the design, operation and control features of the original electromagnetic installation for testing fatigue and frequency stability and operating in a self- oscillating mode, which provides the equality of the frequency of cyclic loading and natural frequency of the sample. The system of the installation control contains two closed circuits: for excitation of self-oscillations and for stabilization of the oscillation amplitude. The sample is loaded by electromagnetic force, and unloading occurs due to the elastic forces of the material. The methodology and algorithms for calculating the stresses of samples of various geometric shapes for estimating changes in amplitude-frequency characteristics are presented. The calculated relationship between the force applied to the sample and its movement at the point of application of force is derived with subsequent determination of the stress by a known force. The results of calibration tests for the static mode of sample loading are presented and the forces acting on the sample (external, inertia, and elastic forces) are evaluated taking into account the maximum stress and maximum strain amplitude. Static and cyclic loading modes are compared. The frequency characteristics obtained during testing steel samples according to the proposed method are obtained. The experimental results of tests with interruptions in the process of cyclic loading and continuous testing are analyzed. It is shown that interruptions in cyclic tests lead to a jump-like increase in the frequency, whereas continuous tests revealed no jumps. At the same time, a comparative analysis with the results of continuous tests showed that the overall frequency deviation is approximately the same for the entire operating cycle in both cases. It is shown that an increase in the frequency after rest is random and does not depend on the number of operating cycles.","PeriodicalId":504498,"journal":{"name":"Industrial laboratory. Diagnostics of materials","volume":"34 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140440823","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-02-21DOI: 10.26896/1028-6861-2024-90-2-12-18
R. R. Izmailov, V. A. Drozdov, R. M. Mironenko, A. Lavrenov
Catalytic processes and technologies are the structure-forming elements of modern chemical, petrochemical and pharmaceutical industries. Prospects of their development are strongly determined by continuous improvement of the existing catalysts and developing the advanced and more efficient ones. Among the available catalysts, an important place belongs to palladium catalysts with carbon supports. Palladium as an active component exhibits unique catalytic properties in various transformations of organic substances: hydrogenation, dehydrogenation, isomerization, dehydrocyclization, carbonylation, oxidation, etc. To control the content of the active component of a catalyst, precise and rapid physicochemical methods are used. ICP-AES shows a good performance in the analytical practice due to the rapidity, sensitivity, high accuracy and selectivity in determining various elements. The aim of the study was to develop a scientifically grounded methodological approach to estimate the palladium content in the catalysts synthesized on different carbon supports made of carbon black and Sibunit, which combines only the acidic decomposition of a sample and analysis by ICP-AES. A series of palladium catalysts synthesized on the carbon supports with different structural and textural characteristics was studied. An urgent goal is to control the content of the active component in the composition of catalysts. This characteristic affects the phase and electronic state of the metal, the structural and textural characteristics and thus determines the activity and selectivity of catalysts during operation. Therefore, quantitative chemical analysis is one of the main methods used to control the quality of catalysts. A method for quantitative determination of palladium concentration, which combines acidic decomposition of a sample and ICP-AES has been developed. The carbon support type was shown to exert no effect on the accuracy and reproducibility of data obtained by the analysis of supported palladium catalysts. The content of palladium in such catalysts can be measured using analytical lines 340.458 and 360.955 nm without lowering the measurement accuracy. The selected conditions of sample preparation make it possible to carry out a quantitative analysis of metal systems based on the carbon support with high accuracy. The relative error in determining the elements did not exceed 4%, the relative standard deviation was no more than 0.04. The results of this work can be used to analyze catalysts of similar chemical composition by ICP-AES.
{"title":"Determination of palladium content in catalysts based on different carbon supports by inductively coupled plasma — atomic emission spectrometry (ICP-AES)","authors":"R. R. Izmailov, V. A. Drozdov, R. M. Mironenko, A. Lavrenov","doi":"10.26896/1028-6861-2024-90-2-12-18","DOIUrl":"https://doi.org/10.26896/1028-6861-2024-90-2-12-18","url":null,"abstract":"Catalytic processes and technologies are the structure-forming elements of modern chemical, petrochemical and pharmaceutical industries. Prospects of their development are strongly determined by continuous improvement of the existing catalysts and developing the advanced and more efficient ones. Among the available catalysts, an important place belongs to palladium catalysts with carbon supports. Palladium as an active component exhibits unique catalytic properties in various transformations of organic substances: hydrogenation, dehydrogenation, isomerization, dehydrocyclization, carbonylation, oxidation, etc. To control the content of the active component of a catalyst, precise and rapid physicochemical methods are used. ICP-AES shows a good performance in the analytical practice due to the rapidity, sensitivity, high accuracy and selectivity in determining various elements. The aim of the study was to develop a scientifically grounded methodological approach to estimate the palladium content in the catalysts synthesized on different carbon supports made of carbon black and Sibunit, which combines only the acidic decomposition of a sample and analysis by ICP-AES. A series of palladium catalysts synthesized on the carbon supports with different structural and textural characteristics was studied. An urgent goal is to control the content of the active component in the composition of catalysts. This characteristic affects the phase and electronic state of the metal, the structural and textural characteristics and thus determines the activity and selectivity of catalysts during operation. Therefore, quantitative chemical analysis is one of the main methods used to control the quality of catalysts. A method for quantitative determination of palladium concentration, which combines acidic decomposition of a sample and ICP-AES has been developed. The carbon support type was shown to exert no effect on the accuracy and reproducibility of data obtained by the analysis of supported palladium catalysts. The content of palladium in such catalysts can be measured using analytical lines 340.458 and 360.955 nm without lowering the measurement accuracy. The selected conditions of sample preparation make it possible to carry out a quantitative analysis of metal systems based on the carbon support with high accuracy. The relative error in determining the elements did not exceed 4%, the relative standard deviation was no more than 0.04. The results of this work can be used to analyze catalysts of similar chemical composition by ICP-AES.","PeriodicalId":504498,"journal":{"name":"Industrial laboratory. Diagnostics of materials","volume":"11 4","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140442931","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-02-21DOI: 10.26896/1028-6861-2024-90-2-5-11
M. Y. Lepilina, E. V. Yakubenko, T. N. Ermolaeva, V. B. Baranovskaya
A technique for X-ray fluorescence spectral analysis of zinc-aluminum- magnesium alloys has been developed, which allows the determination of Mg, Al, Pb, Si, Cu, Mn, Fe, Ni content in the alloy. The effect of the sample preparation method on the linearity of calibration graphs is revealed. The conditions for determining the main alloying (Al, Mg) and impurity (Pb, Fe, Cu, Si, Mn, Ni) elements by X-ray fluorescence spectrometry were studied. It is proposed to use the correction of the matrix effect by selecting alpha coefficients for the intensity of X- ray radiation with subsequent automatic conversion of the function into a linear form. Calibration graphs for determination of the elements in the corresponding ranges, i.e., Mg (0.00019 – 5.04%), Al (0.0002 – 12.4%), Pb (0.0012 – 2.07%), Si (0.0005 – 0.12%), Cu (0.0006 – 5.95%), Mn (0.0004 – 0.00524%), Fe (0.0009 – 0.41%), Ni (0.0009 – 0.27%), were obtained using standard reference samples and production samples of the alloys, the chemical composition of which was previously determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The correctness of the developed methodology was confirmed by analysis of standard samples and comparative analysis of the obtained results using the Student’s t-test.
开发了一种锌铝镁合金 X 射线荧光光谱分析技术，可测定合金中的镁、铝、铅、硅、铜、锰、铁、镍含量。揭示了样品制备方法对校准图线性的影响。研究了用 X 射线荧光光谱法测定主要合金元素（Al、Mg）和杂质元素（Pb、Fe、Cu、Si、Mn、Ni）的条件。建议通过选择 X 射线辐射强度的阿尔法系数来校正矩阵效应，随后自动将函数转换为线性形式。测定相应范围内元素的校准图，即镁（0.00019 - 5.04%）、铝（0.0002 - 12.4%）、铅（0.0012 - 2.07%）、硅（0.0005 - 0.12%）、铜（0.0006 - 5.95%）、锰（0.0004 - 0.00524%）、铁（0.0009 - 0.41%）、镍（0.0009 - 0.27%），这些数据是使用标准参考样品和合金生产样品获得的，合金的化学成分之前是通过电感耦合等离子体原子发射光谱法（ICP-AES）测定的。通过分析标准样品和使用学生 t 检验对所获结果进行比较分析，确认了所开发方法的正确性。
{"title":"Development of a technique for X-ray fluorescence analysis of zinc-aluminum-magnesium alloys","authors":"M. Y. Lepilina, E. V. Yakubenko, T. N. Ermolaeva, V. B. Baranovskaya","doi":"10.26896/1028-6861-2024-90-2-5-11","DOIUrl":"https://doi.org/10.26896/1028-6861-2024-90-2-5-11","url":null,"abstract":"A technique for X-ray fluorescence spectral analysis of zinc-aluminum- magnesium alloys has been developed, which allows the determination of Mg, Al, Pb, Si, Cu, Mn, Fe, Ni content in the alloy. The effect of the sample preparation method on the linearity of calibration graphs is revealed. The conditions for determining the main alloying (Al, Mg) and impurity (Pb, Fe, Cu, Si, Mn, Ni) elements by X-ray fluorescence spectrometry were studied. It is proposed to use the correction of the matrix effect by selecting alpha coefficients for the intensity of X- ray radiation with subsequent automatic conversion of the function into a linear form. Calibration graphs for determination of the elements in the corresponding ranges, i.e., Mg (0.00019 – 5.04%), Al (0.0002 – 12.4%), Pb (0.0012 – 2.07%), Si (0.0005 – 0.12%), Cu (0.0006 – 5.95%), Mn (0.0004 – 0.00524%), Fe (0.0009 – 0.41%), Ni (0.0009 – 0.27%), were obtained using standard reference samples and production samples of the alloys, the chemical composition of which was previously determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The correctness of the developed methodology was confirmed by analysis of standard samples and comparative analysis of the obtained results using the Student’s t-test.","PeriodicalId":504498,"journal":{"name":"Industrial laboratory. Diagnostics of materials","volume":"17 2","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140444127","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-02-21DOI: 10.26896/1028-6861-2024-90-2-19-28
E. I. Denisov, V. S. Semenishchev, M. V. Voitenko, D. V. Ryansky
X-ray fluorescent (XRF) analysis is one of the most widely used methods for analytical control of soil and rock samples, which allows determining a wide range of elements using a single sample with minimum costs. This work is aimed to expand the XRF capabilities in terms of obtaining calibration dependences for various types of samples. The work presents the results of the experimental assessment of the accuracy of the method of fundamental parameters for analysis of soil samples on a Quant’X energy dispersive spectrometer with the UniQuant software using artificial samples. The suggested methodical approach has shown the potentiality of using a Quant’X energy dispersive spectrometer with the UniQuant software for analysis of soil samples prepared by different methods (fused, pressed and bulk). The systematic deviation from the target value and a random error were estimated. For fused soil samples, deviations from the target value for most of the major components were (1.01) with a random error of 0.01 – 0.06. A Quant’X spectrometer with the UniQuant software allows determining light elements in fused samples with an error of up to 0.06. For the majority of impurity elements, a significant deviation was found, more than one (an underestimation of the determination results by an average of 1.18 times). This requires correction of the results obtained and the analysis error will be determined by values?? ranging from 0.01 to 0.1. In most cases, the deviation from the target value and the error of the element determination decreased as the sample preparation became more complex. After adjustment, bulk soil samples showed the highest error of the analysis results (from 0.1 to 0.2 for the major elements and 0.05 – 0.10 for impurity elements). The detection limits of some elements in fused soil samples were estimated. When the component content in the soil is more than 0.1%, the best option is to analyze fused samples. To determine concentration levels of about 50 ppm, it is proposed to measure pressed samples and take into account the increased error.
{"title":"Assessment of the accuracy of the method of fundamental parameters for XRF analysis of soil samples using an ARL Quant’X energy dispersive spectrometer with the UniQuant software","authors":"E. I. Denisov, V. S. Semenishchev, M. V. Voitenko, D. V. Ryansky","doi":"10.26896/1028-6861-2024-90-2-19-28","DOIUrl":"https://doi.org/10.26896/1028-6861-2024-90-2-19-28","url":null,"abstract":"X-ray fluorescent (XRF) analysis is one of the most widely used methods for analytical control of soil and rock samples, which allows determining a wide range of elements using a single sample with minimum costs. This work is aimed to expand the XRF capabilities in terms of obtaining calibration dependences for various types of samples. The work presents the results of the experimental assessment of the accuracy of the method of fundamental parameters for analysis of soil samples on a Quant’X energy dispersive spectrometer with the UniQuant software using artificial samples. The suggested methodical approach has shown the potentiality of using a Quant’X energy dispersive spectrometer with the UniQuant software for analysis of soil samples prepared by different methods (fused, pressed and bulk). The systematic deviation from the target value and a random error were estimated. For fused soil samples, deviations from the target value for most of the major components were (1.01) with a random error of 0.01 – 0.06. A Quant’X spectrometer with the UniQuant software allows determining light elements in fused samples with an error of up to 0.06. For the majority of impurity elements, a significant deviation was found, more than one (an underestimation of the determination results by an average of 1.18 times). This requires correction of the results obtained and the analysis error will be determined by values?? ranging from 0.01 to 0.1. In most cases, the deviation from the target value and the error of the element determination decreased as the sample preparation became more complex. After adjustment, bulk soil samples showed the highest error of the analysis results (from 0.1 to 0.2 for the major elements and 0.05 – 0.10 for impurity elements). The detection limits of some elements in fused soil samples were estimated. When the component content in the soil is more than 0.1%, the best option is to analyze fused samples. To determine concentration levels of about 50 ppm, it is proposed to measure pressed samples and take into account the increased error.","PeriodicalId":504498,"journal":{"name":"Industrial laboratory. Diagnostics of materials","volume":"52 9","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140444963","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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