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Indentation fracture behavior of energetic and inert molecular crystals

Published online by Cambridge University Press:  22 November 2019

Alexandra C. Burch Open the ORCID record for Alexandra C. Burch [Opens in a new window] ,
John D. Yeager  and
David F. Bahr
Alexandra C. Burch
Affiliation:
School of Materials Engineering, Purdue University, West Lafayette, Indiana 47907, USA; and Explosive Science and Shock Physics, Los Alamos National Laboratory, Los Alamos, New Mexico 87545, USA Explosive Science and Shock Physics, Los Alamos National Laboratory, Los Alamos, New Mexico 87545, USA
John D. Yeager
Affiliation:
Explosive Science and Shock Physics, Los Alamos National Laboratory, Los Alamos, New Mexico 87545, USA
David F. Bahr*
Affiliation:
School of Materials Engineering, Purdue University, West Lafayette, Indiana 47907, USA; and Explosive Science and Shock Physics, Los Alamos National Laboratory, Los Alamos, New Mexico 87545, USA
*
a)Address all correspondence to this author. e-mail: dfbahr@purdue.edu
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Abstract

Measuring the elastic and plastic properties with nanoindentation is predicated on the indentation not fracturing the material. In this study, an unloading curve analysis is used to identify indentation-induced fracture in brittle molecular organic crystals to define conditions, where properties measurements are accurate, and for calculating the toughness. Single crystals of cyclotetramethylene tetranitramine (HMX) and idoxuridine were indented from 1 to 300 mN with indenter probes of varying acuity to identify fracture initiation loads. Idoxuridine displayed no fracture up to and at 100 mN, with fracture occurrence then seen at an increasing rate until every indentation made induced fracture at 300 mN. HMX displayed no fracture up to and at 4 mN, with fracture then occurring at an increasing rate until every sample fractured at 8 mN. The toughness of HMX and idoxuridine is ≈0.28 ≈ 0.4–0.5 MPa/m1/2, respectively.

Keywords

nanoindentationfracturehardness
Type
Article
Information
Journal of Materials Research , Volume 34 , Issue 23 , 16 December 2019 , pp. 3954 - 3963
Copyright
Copyright © Materials Research Society 2019 

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References

Mohammed, H., Briscoe, B.J., and Pitt, K.G.: The interrelationship between the compaction behaviour and the mechanical strength of pure pharmaceutical tablets. Chem. Eng. Sci. 60, 3941–3947 (2005).CrossRefGoogle Scholar
Duncan-Hewitt, W.C. and Weatherly, G.C.: Modeling the uniaxial compaction of pharmaceutical powders using the mechanical properties of single crystals. II: Brittle materials. J. Pharm. Sci. 79, 273–278 (1990).CrossRefGoogle ScholarPubMed
Jain, S.: Mechanical properties of powders for compaction and tableting: An overview. Pharm. Sci. Technol. Today 2, 20–31 (1999).CrossRefGoogle ScholarPubMed
Luscher, D.J., Yeager, J. D., Clausen, B., Vogel, S.C., Higginbotham Duque, A. L., and Brown, D. W.: Using neutron diffraction to investigate texture evolution during consolidation of deuterated triaminotrinitrobenzene (d-TATB) explosive powder. Crystals 7, 138 (2017).CrossRefGoogle Scholar
Elban, W.L. and Chiarito, M.A.: Quasi-static compaction study of coarse HMX explosive. Powder Technol. 46, 181–193 (1986).CrossRefGoogle Scholar
Stepanov, V., Patel, R.B., Mudryy, R., and Qiu, H.: Investigation of nitramine-based amorphous energetics. Propellants, Explos., Pyrotech. 41, 142–147 (2016).CrossRefGoogle Scholar
Yu, L.: Amorphous pharmaceutical solids: Preparation, characterization and stabilization. Adv. Drug Delivery Rev. 48, 27–42 (2001).CrossRefGoogle ScholarPubMed
Bower, J.K., Kolb, J.R., and Pruneda, C.O.: Polymeric coatings effect on surface activity and mechanical behavior of high explosives. Ind. Eng. Chem. Prod. Res. Dev. 19, 326–329 (1980).CrossRefGoogle Scholar
Yeager, J.D., Higginbotham Duque, A.L., Shorty, M., Bowden, P.R., and Stull, J.A.: Development of inert density mock materials for HMX. J. Energ. Mater. 36, 253 (2018).CrossRefGoogle Scholar
Burch, A.C, Yeager, J.D., and Bahr, D.F.: Nanoindentation of HMX and idoxuridine to determine mechanical similarity. Crystals 7, 335 (2017).CrossRefGoogle Scholar
Taw, M.R. and Bahr, D.F.: The mechanical properties of minimally processed RDX. Propellants, Explos., Pyrotech. 42, 659–664 (2017).CrossRefGoogle Scholar
Taw, M.R., Yeager, J.D., Hooks, D.E., Carvajal, T.M., and Bahr, D.F.: The mechanical properties of as-grown noncubic organic molecular crystals assessed by nanoindentation. J. Mater. Res. 32, 2728 (2017).CrossRefGoogle Scholar
Kiran, M.S.R.N., Varughese, S., Reddy, C.M., Ramamurty, U., and Desiraju, G.R.: Mechanical anisotropy in crystalline saccharin: Nanoindentation studies. Cryst. Growth Des. 10, 4650–4655 (2010).CrossRefGoogle Scholar
Olusanmi, D., Roberts, K.J., Ghadiri, M., and Ding, Y.: The breakage behaviour of aspirin under quasi-static indentation and single particle impact loading: Effect of crystallographic anisotropy. Int. J. Pharm. 411, 49–63 (2011).CrossRefGoogle ScholarPubMed
Hudson, R.J., Zioupos, P., and Gill, P.P.: Investigating the mechanical properties of RDX crystals using nano-indentation. Propellants, Explos., Pyrotech. 37, 191–197 (2012).CrossRefGoogle Scholar
Ramos, K.J. and Bahr, D.F.: Mechanical behavior assessment of sucrose using nanoindentation. J. Mater. Res. 22, 2037–2045 (2007).CrossRefGoogle Scholar
Egart, M., Janković, B., Lah, N., Ilić, I., and Srčič, S.: Nanomechanical properties of selected single pharmaceutical crystals as a predictor of their bulk behaviour. Pharm. Res. 32, 469–481 (2015).CrossRefGoogle ScholarPubMed
Mathew, N. and Sewell, T.D.: Nanoindentation of the triclinic molecular crystal 1,3,5-triamino-2,4,6-trinitrobenzene: A molecular dynamics study. J. Phys. Chem. B 120, 8266 (2016).Google Scholar
Elban, W.L., Hoffsommer, J.C., and Armstrong, R.W.: X-ray orientation and hardness experiments on RDX explosive crystals. J. Mater. Sci. 19, 552–566 (1984).CrossRefGoogle Scholar
Ramos, K.J., Hooks, D.E., and Bahr, D.F.: Direct observation of plasticity and quantitative hardness measurements in single crystal cyclotrimethylene trinitramine by nanoindentation. Philos. Mag. 89, 2381–2402 (2009).CrossRefGoogle Scholar
Lawn, B. and Wilshaw, R.: Indentation fracture: Principles and applications. J. Mater. Sci. 10, 1049–1081 (1975).CrossRefGoogle Scholar
Khan, Z., Faisal, H., and Tarefder, R.: Fracture toughness measurement of asphalt concrete by nanoindentation. In Proceedings of the ASME International Mechanical Engineering Congress and Exposition, Vol. 10, Micro- and Nano-Systems Engineering and Packaging (ASME, Tampa, 2017); doi: 10.1115/IMECE2017-71840.Google Scholar
Jungk, J.M., Boyce, B.L., Buchheit, T.E., Friedmann, T.A., Yang, D., and Gerberich, W.W.: Indentation fracture toughness and acoustic energy release in tetrahedral amorphous carbon diamond-like thin films. Acta Mater. 54, 4043–4052 (2006).CrossRefGoogle Scholar
Cai, X., Xu, Y., Zhong, L., and Liu, M.: Fracture toughness of WC–Fe cermet in W–WC–Fe composite by nanoindentation. J. Alloys Compd. 728, 788–796 (2017).CrossRefGoogle Scholar
Guo, H., Jiang, C.B., Yang, B.J., and Wang, J.Q.: On the fracture toughness of bulk metallic glasses under Berkovich nanoindentation. J. Non-Cryst. Solids 481, 321–328 (2018).CrossRefGoogle Scholar
Mannepalli, S. and Mangalampalli, K.: Indentation plasticity and fracture studies of organic crystals. Crystals 7, 324 (2017).CrossRefGoogle Scholar
Yen, C-Y., Jian, S-R., Tseng, Y-C., and Juang, J-Y.: The deformation behavior and fracture toughness of single crystal YSZ(111) by indentation. J. Alloys Compd. 735, 2423–2427 (2018).CrossRefGoogle Scholar
Anstis, G.R., Chantikul, P., Lawn, B.R., and Marshall, D.B.: A critical evaluation of indentation techniques for measuring fracture toughness: I, direct crack measurements. J. Am. Ceram. Soc. 64, 533–538 (1981).CrossRefGoogle Scholar
Chantikul, P., Anstis, G.R., Lawn, B.R., and Marshall, D.B.: A critical evaluation of indentation techniques for measuring fracture toughness: II, strength method. J. Am. Ceram. Soc. 64, 539–543 (1981).CrossRefGoogle Scholar
Fuller, E.R., Quinn, G.D., and Cook, R.F.: Strength and fracture measurements at the nano scale. In AIP Conference Proceedings, Vol. 931: Frontiers of Characterization and Metrology for Nanoelectronics, eds. D.G. Seiler, A.C. Diebold, R. McDonald, C.M. Garner, D. Herr, R.P. Khosla, and E.M. Secula (AIP, Melville, 2007); pp. 156–160.CrossRefGoogle Scholar
Oliver, W.C. and Pharr, G.M.: An improved technique for determining harness and elastic modulus using load and displacement sensing indentation experiments. J. Mater. Res. 7, 1564–1583 (1992).CrossRefGoogle Scholar
Morris, D.J., Myers, S.B., and Cook, R.F.: Sharp probes of varying acuity: Instrumented indentation and fracture behavior. J. Mater. Res. 19, 165 (2004).CrossRefGoogle Scholar
Cook, R.F. and Pharr, G.M.: Direct observation and analysis of indentation cracking in glasses and ceramics. J. Am. Ceram. Soc. 73, 787–817 (1990).CrossRefGoogle Scholar
Jing, Y., Zhang, Y., Blendell, J., Koslowski, M., and Carvajal, M.T.: Nanoindentation method to study slip planes in molecular crystals in a systematic manner. Cryst. Growth Des. 11, 5260–5267 (2011).CrossRefGoogle Scholar
Wildfong, P.L.D., Hancock, B.C., Moore, M.D., and Morris, K.R.: Towards an understanding of the structurally based potential for mechanically activated disordering of small molecule organic crystals. J. Pharm. Sci. 95, 2645–2656 (2006).CrossRefGoogle ScholarPubMed
Morris, D.J.: Instrumented indentation contact with sharp probes of varying acuity. MRS Proc. 1049, AA06–AA09 (2007).CrossRefGoogle Scholar
Mound, B.A. and Pharr, G.M.: Nanoindentation of fused quartz at loads near the cracking threshold. Exp. Mech. 59, 369–380 (2019).CrossRefGoogle Scholar
Jang, J. and Pharr, G.M.: Influence of indenter angle on cracking in Si and Ge during nanoindentation. Acta Mater. 56, 4458–4469 (2008).CrossRefGoogle Scholar
Cook, R.F.: Fracture sequences during elastic–plastic indentation of brittle materials. J. Mater. Res. 34, 1633–1644 (2019).CrossRefGoogle Scholar
Morris, D.J. and Cook, R.F.: Radial fracture during indentation by acute probes: I, description by an indentation wedging model. Int. J. Fract. 136, 237–264 (2005).CrossRefGoogle Scholar
Maughan, M.R., Carvajal, M.T., and Bahr, D.F.: Nanomechanical testing technique for millimeter-sized and smaller molecular crystals. Int. J. Pharm. 486, 324–330 (2015).CrossRefGoogle ScholarPubMed