journal article·2023-10-14

Addressing nanomechanical testing irregularities in molecular organic crystals to determine mechanical properties

Hugh P. Grennan, Alexandra C. Burch, Bryce C. Tappan, Virginia W. Manner, David F. Bahr

Journal of Materials Research· Volume 38· Issue 19
Publisher page

Abstract

Molecular crystals often form noncubic crystal structures which can lead to anisotropic or limited slip conditions that lead to the inability to accommodate arbitrary plastic deformation. In certain molecular crystal systems, such as diaminoazoxyfurazan (DAAF), limited slip conditions are present. Indentations on DAAF produced an irregular (non-parabolic) “mechanical fingerprint”, while similarly structured molecular crystals hexanitrohexaazaisowurtzitane (CL-20), azodiaminoazoxyfurazan (ADAAF), and 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) behaved predictably. Indentation impressions on DAAF were often non-conforming to the indenter tip and produced a higher-than-expected coefficient of variation in calculated properties. These behaviors are not identified in other materials with chemical and crystallographic similarities to DAAF, therefore, non-conformal behavior is not governed by these attributes alone. However, once this novel mechanical fingerprint was identified, extracting material properties from nanoindentation was still possible. The elastic modulus and hardness of DAAF is 14.3 and 0.67 GPa, respectively; CL-20 has a modulus and hardness of 25.5 and 1.18 GPa, respectively.Graphical abstract
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Research context

OpenAlex topics: Metal and Thin Film Mechanics · Force Microscopy Techniques and Applications · Energetic Materials and Combustion

SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.

References (31)

Show source-provided references
1. L. Baraldi et al., Mechanical characterization of pharmaceutical powders by nanoindentation and correlation with their behavior during grinding. Pharmaceutics 14(6), 1146 (2022). https://doi.org/10.3390/pharmaceutics1406114610.3390/pharmaceutics14061146 ↗
2. G.R. Miller, A.N. Garroway, A Review of the Crystal Structures of Common Explosives Part I: RDX, HMX, TNT, PETN, and Tetryl (Naval Research Lab, Washington DC, 2001)
3. R.J.J. Hinch, 93. Hexahydro-1,3,5-trinitroso-s-triazine (1,3,5-Trinitroso-1,3,5-triazacyclohexane). Am. Chem. Soc. 27(4), 569–570 (1955)
4. R.W. Beal, C.D. Incarvito, B.J. Rhatigan, A.L. Rheingold, T.B. Brill, X-ray crystal structures of five nitrogen-bridged bifurazan compounds. Propellants, Explos., Pyrotech. 25(6), 277–283 (2000). https://doi.org/10.1002/1521-4087(200012)25:6%3c277::AID-PREP277%3e3.0.CO;2-P10.1002/1521-4087(200012)25:6<277::AID-PREP277>3.0.CO;2-P ↗
5. N.B. Bolotina, M.J. Hardie, R.L. Speer, A.A. Pinkerton, Energetic materials: variable-temperature crystal structures of γ- and ε-HNIW polymorphs. J Appl Crystallogr 37(5), 808–814 (2004). https://doi.org/10.1107/S002188980401783210.1107/S0021889804017832 ↗
6. J.M. Veauthier, D.E. Chavez, B.C. Tappan, D.A. Parrish, Synthesis and characterization of furazan energetics ADAAF and DOATF. J. Energ. Mater. 28(3), 229–249 (2010). https://doi.org/10.1080/0737065100360176910.1080/07370651003601769 ↗
7. H.H. Cady, A.C. Larson, The crystal structure of 1,3,5-Triamino-2,4,6-trinitrobenzene. Acta Cryst. (1965). https://doi.org/10.1107/S0365110X6500107X10.1107/S0365110X6500107X ↗
8. D.F. Bahr, D.J. Morris, Nanoindentation: localized probes of mechanical behavior of materials, in Springer handbook of experimental solid mechanics. ed. by W. Sharpe (Springer, New York, 2008), pp.389–40810.1007/978-0-387-30877-7_16 ↗
9. W.C. Oliver, G.M. Pharr, An improved technique for determining hardness and elastic modulus using load and displacement sensing indentation experiments. J Mater Res 7(6), 1564–1583 (1992). https://doi.org/10.1557/jmr.1992.156410.1557/jmr.1992.1564 ↗
10. R. von Mises, Mechanik der plastischen Formänderung von Kristallen. ZAMM 8(3), 161–185 (1928). https://doi.org/10.1002/zamm.1928008030210.1002/zamm.19280080302 ↗
11. G.W. Groves, A. Kelly, Independent slip systems in crystals. Phil. Mag. 8(89), 877–887 (1963). https://doi.org/10.1080/1478643630821384310.1080/14786436308213843 ↗
12. M.F. Doerner, W.D. Nix, A method for interpreting the data from depth-sensing indentation instruments. J Mater Res 1(4), 601–609 (1986). https://doi.org/10.1557/JMR.1986.060110.1557/JMR.1986.0601 ↗
13. T.F. Page, S.V. Hainsworth, Using nanoindentation techniques for the characterization of coated systems: a critique. Surf Coat Technol 61, 201 (1993)10.1016/0257-8972(93)90226-E ↗
14. M.K. Mishra, G.R. Desiraju, U. Ramamurty, A.D. Bond, Studying microstructure in molecular crystals with nanoindentation: intergrowth polymorphism in Felodipine. Angew. Chem. 126(48), 13318–13321 (2014). https://doi.org/10.1002/ange.20140689810.1002/ange.201406898 ↗
15. S. Varughese, M.S.R.N. Kiran, K.A. Solanko, A.D. Bond, U. Ramamurty, G.R. Desiraju, Interaction anisotropy and shear instability of aspirin polymorphs established by nanoindentation. Chem Sci 2(11), 2236–2242 (2011). https://doi.org/10.1039/c1sc00430a10.1039/c1sc00430a ↗
16. D.J. Morris, S.B. Myers, R.F. Cook, Sharp probes of varying acuity: instrumented indentation and fracture behavior. J. Mater. Res. 19(1), 165–175 (2004)10.1557/jmr.2004.19.1.165 ↗
17. E.R. Weppelmann, J.S. Field, M.V. Swain, Influence of spherical indentor radius on the indentation-induced transformation behaviour of silicon. J Mater Sci 30, 2455–2462 (1995)10.1007/BF01184600 ↗
18. M.S.R.N. Kiran, S. Varughese, C.M. Reddy, U. Ramamurty, G.R. Desiraju, Mechanical anisotropy in crystalline saccharin: nanoindentation studies. Crystal Growth Design 10, 4650–4655 (2010). https://doi.org/10.1021/cg100936210.1021/cg1009362 ↗
19. K.J. Ramos, D.F. Bahr, Mechanical behavior assessment of sucrose using nanoindentation. J Mater Res 22(7), 2037–2045 (2007). https://doi.org/10.1557/jmr.2007.024910.1557/jmr.2007.0249 ↗
20. Y. Jing, Y. Zhang, J. Blendell, M. Koslowski, M.T. Carvajal, Nanoindentation method to study slip planes in molecular crystals in a systematic manner. Cryst Growth Des 11(12), 5260–5267 (2011). https://doi.org/10.1021/cg200689a10.1021/cg200689a ↗
21. K.J. Ramos, D.E. Hooks, D.F. Bahr, Direct observation of plasticity and quantitative hardness measurements in single crystal cyclotrimethylene trinitramine by nanoindentation. Phil. Mag. 89(27), 2381–2402 (2009). https://doi.org/10.1080/1478643090312033510.1080/14786430903120335 ↗
22. X. Zhou et al., Mechanical anisotropy of the energetic crystal of 1,1-Diamino-2,2-dinitroethylene (FOX-7): a study by nanoindentation experiments and density functional theory calculations. J. Phys. Chem. C 120(25), 13434–13442 (2016). https://doi.org/10.1021/acs.jpcc.6b0461210.1021/acs.jpcc.6b04612 ↗
23. W.C. Duncan-Hewitt, G.C. Weatherly, Evaluating the fracture toughness of sucrose crystals using microindentation techniques. Pharm Res 6(5), 373–378 (1989)10.1023/A:1015923229999 ↗
24. F. Liu, D.E. Hooks, N. Li, N.A. Mara, J.A. Swift, Mechanical properties of anhydrous and hydrated uric acid crystals. Chem. Mater. 30(11), 3798–3805 (2018). https://doi.org/10.1021/acs.chemmater.8b0093910.1021/acs.chemmater.8b00939 ↗
25. C.M. Barr, M. Cooper, J. Lechman, D.C. Bufford, The mechanical response of micron-sized molecular crystals. MRS Adv 6(27), 674–681 (2021). https://doi.org/10.1557/s43580-021-00124-y10.1557/s43580-021-00124-y ↗
26. T.Y.-J. Han et al., The solubility and recrystallization of 1,3,5-triamino-2,4,6-trinitrobenzene in a 3-ethyl-1-methylimidazolium acetate–DMSO co-solvent system. New J. Chem. 33(1), 50–56 (2009). https://doi.org/10.1039/B810109D10.1039/B810109D ↗
27. D.F. Bahr, D.E. Kramer, W.W. Gerberich, Non-linear deformation mechanisms during nanoindentation. Acta mater. 46(10), 3605–3617 (1997)10.1016/S1359-6454(98)00024-X ↗
28. M.R. Taw, J.D. Yeager, D.E. Hooks, T.M. Carvajal, D.F. Bahr, The mechanical properties of as-grown noncubic organic molecular crystals assessed by nanoindentation. J Mater Res 32(14), 2728–2737 (2017). https://doi.org/10.1557/jmr.2017.21910.1557/jmr.2017.219 ↗
29. N. Lease, M.D. Holmes, M.A. Englert-Erickson, L.M. Kay, E.G. Francois, V.W. Manner, Analysis of ignition sites for the explosives 3,3′-Diamino-4,4′-azoxyfurazan (DAAF) and 1,3,5,7-Tetranitro-1,3,5,7-tetrazoctane (HMX) using crush gun impact testing. ACS Mater. Au 1(2), 116–129 (2021). https://doi.org/10.1021/acsmaterialsau.1c0001310.1021/acsmaterialsau.1c00013 ↗
30. M.R. Maughan, M.T. Carvajal, D.F. Bahr, Nanomechanical testing technique for millimeter-sized and smaller molecular crystals. Int J Pharm 486(1–2), 324–330 (2015). https://doi.org/10.1016/j.ijpharm.2015.03.06210.1016/j.ijpharm.2015.03.062 ↗
31. P.R. Spackman et al., CrystalExplorer: a program for Hirshfeld surface analysis, visualization and quantitative analysis of molecular crystals. J. Appl. Cryst. 54(3), 1006–1011 (2021). https://doi.org/10.1107/S160057672100291010.1107/S1600576721002910 ↗