

Determination of the porosity characteristics by pycnometric methods
https://doi.org/10.26896/1028-6861-2024-90-2-47-52
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.
About the Authors
A. B. AnkudinovRussian Federation
Alexey B. Ankudinov
49, Leninsky prosp., Moscow, 119334
M. I. Alymov
Russian Federation
Mikhail I. Alymov
49, Leninsky prosp., Moscow, 119334
8, ul. Akademika Osipyana, Chernogolovka, Moscow oblast’, 142432
V. A. Zelensky
Russian Federation
Victor A. Zelensky
49, Leninsky prosp., Moscow, 119334
R. D. Kapustin
Russian Federation
Roman D. Kapustin
8, ul. Akademika Osipyana, Chernogolovka, Moscow oblast’, 142432
A. E. Sychev
Russian Federation
Alexander E. Sychev
8, ul. Akademika Osipyana, Chernogolovka, Moscow oblast’, 142432
V. S. Shustov
Russian Federation
Vadim S. Shustov
49, Leninsky prosp., Moscow, 119334
References
1. Qin S., Bo Y., Herzog S., et al. Influence of process parameters on porosity and hot cracking of AISI H13 fabricated by laser powder bed fusion / Powders. 2022. Vol. 1. P. 184 – 193. DOI: 10.3390/powders1030012
2. Lei Luo, Liangshun Luo, Yanqing Su, et al. Reducing porosity and optimizing performance for Al-Cu-based alloys with large solidification intervals by coupling travelling magnetic fields with sequential solidification / Journal of Materials Science & Technology. 2021. Vol. 79. N 20. P. 1 – 14. DOI: 10.1016/j.jmst.2020.11.035
3. Morozov E. M., Alymov M. I. Fracture pressure in microdefects of consolidated materials / Dokl. RAN. Fiz. Khim. 2021. Vol. 501. N 6. P. 56 – 58. DOI: 10.1134/S0012501621110026
4. Alymov M. I., Averin S. I., Morozov E. M., et al. Determination of the pressure inside pores / Industr. Lab. Mater. Diagn. 2021. Vol. 87. N 10. P. 40 – 43 [in Russian]. DOI: 10.26896/1028-6861-2021-87-10-40-43
5. Ketkova L. A. Nature of heterophase inclusions in high-purity optical fiber materials as studied with 3D laser ultramicroscopy / Optical Materials. 2015. Vol. 47. P. 251 – 255.
6. Terris T., Andreau O., Peyre P., et al. Optimization and comparison of porosity rate measurement methods of selective laser melted metallic parts / Additive Manufacturing. 2019. Vol. 28. P. 802 – 813. DOI: 10.1016/j.addma.2019.05.035.hal-02292119
7. Poinern G., Brundavanam R., Le X., Fawcett D. The mechanical properties of a porous ceramic derived from a 30 nm sized particle based powder of hydroxyapatite for potential hard tissue engineering applications / American Journal of Biomedical Engineering. 2012. Vol. 2. P. 278 – 286. DOI: 10.5923/j.ajbe.20120206.07
8. Gausner S. I., Kivilis S. S., Osokina A. P., Pavlovsky A. N. Measurement of mass, volume and density. — Moscow: Izd. standartov, 1972. — 623 p. [in Russian].
9. Kilmametov A., Gröger R., Hahn H., et al. Bulk density measurements of small solid objects using laser confocal microscopy / Adv. Mater. Technol. 2016. 1600115. P. 1 – 12. DOI: 10.1002/admt.201600115
10. Andreola F., Leonelli C., Romagnoli M., Miselli P. Techniques used to determine porosity / American Ceramic Society Bulletin. 2000. P. 49 – 52. www.ceramicbulletin.org
11. Sing K. S. W. Adsorption methods for the characterization of porous materials / Advances in Colloid and Interface Science. 1998. Vol. 76 – 77. P. 3 – 11.
12. Wang Y., Zhou B. Recent progress in single and combined porosity- evaluation techniques for porous materials / Materials. 2022. Vol. 15. P. 1 – 19. DOI: 10.3390/ma15092981
13. Jaques V., Du Plessis A., Zemek M., et al. Review of porosity uncertainty estimation methods in computed tomography dataset / Measurement Science and Technology. 2021. Vol. 32. P. 122001. DOI: 10.1088/1361-6501/ac1b40
14. Oliveira M. V., Ribeiro A. A., Moreira A. C., et al. Comparison of porosity measurement techniques for porous titanium scaffolds evaluation / Materials Science Forum. 2010. Vol. 660 – 661. P. 100 – 105. DOI: 10.4028/www.scientific.net/MSF.660-661.100
15. Martin W. D., Putman B. J. Comparison of methods for measuring porosity of porous paving mixtures / Construction and Building Materials. 2016. Vol. 125. P. 299 – 305. DOI: 10.1016/j.conbuildmat.2016.08.038
16. Murray C., Flannery C., Streiter I., et al. Comparison of techniques to characterise the density, porosity and elastic modulus of porous low-k SiO2 xerogel films / Microelectronic Engineering. 2002. Vol. 60. P. 133 – 141.
17. de Oliveira C., Kohns R., Meyerhofer F., et al. Multi-technique structural characterization of glass foams with complex pore structures obtained through phase separation / Mater. Chem. Front. 2021. Vol. 5. P. 4615 – 4625. DOI: 10.1039/d1qm00383f
18. Rouquerol J., Baron G., Denoyel R., et al. Recommendations for the Characterization of Porous Solids / Pure and Applied Chemistry. 2012. Vol. 84. N 1. P. 107 – 136. DOI: 10.1351/PAC-REP-10-11-19
19. Plachenov T. G., Kolosentsev S. D. Porosimetry. — Leningrad: Khimiya, 1988. — 176 p. [in Russian].
20. Klobes P., Meyer K., Munro R. Porosity and Specific Surface Area Measurements for Solid Materials. — Washington: U.S. Government Printing Office, NIST, 2006. — 89 p.
21. Epishin A. I., Alymov M. I. Determination of the volume fraction of the microporosity in nickel-based superalloy single crystals. / Industr. Lab. Mater. Diagn. Vol. 88. N 11. P. 32 – 40 [in Russian]. DOI: 10.26896/1028-6861-2022-88-11-32-40
22. Chernyavsky K. S. Stereology in metallurgy. — Moscow: Metallurgiya, 1977. — 280 p. [in Russian].
Review
For citations:
Ankudinov A.B., Alymov M.I., Zelensky V.A., Kapustin R.D., Sychev A.E., Shustov V.S. Determination of the porosity characteristics by pycnometric methods. Industrial laboratory. Diagnostics of materials. 2024;90(2):47-52. (In Russ.) https://doi.org/10.26896/1028-6861-2024-90-2-47-52