Title: Nanomechanical testing of freestanding polymer films: in situ tensile testing and Tg measurement

Journal Article · · Journal of Materials Research

Abstract A method for small-scale testing and imaging of freestanding, microtomed polymer films using a push-to-pull device is presented. Central to this method was the development of a sample preparation technique which utilized solvents at cryogenic temperatures to transfer and deposit delicate thin films onto the microfabricated push-to-pull devices. The preparation of focused ion beam (FIB)-milled tensile specimens enabled quantitative in situ TEM tensile testing, but artifacts associated with ion and electron beam irradiation motivated the development of a FIB-free specimen preparation method. The FIB-free method was enabled by the design and fabrication of oversized strain-locking push-to-pull devices. An adaptation for push-to-pull devices to be compatible with an instrumented nanoindenter expanded the testing capabilities to include in situ heating. These innovations provided quantitative mechanical testing, postmortem TEM imaging, and the ability to measure the glass transition temperature, via dynamic mechanical analysis, of freestanding polymer films. Results for each of these mentioned characterization methods are presented and discussed in terms of polymer nanomechanics. Graphic Abstract

Research Organization:
Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)
Sponsoring Organization:
USDOE; USDOE Office of Science (SC), Basic Energy Sciences (BES)
Grant/Contract Number:
AC02-05CH11231
OSTI ID:
1773925
Journal Information:
Journal of Materials Research, Journal Name: Journal of Materials Research Journal Issue: 12 Vol. 36; ISSN 0884-2914
Publisher:
Cambridge University Press (CUP)Copyright Statement
Country of Publication:
United States
Language:
English

References (19)

Micrometer-Scale Tensile Testing of Biological Attachment Devices journal April 2006
The glass transition temperature of polystyrene: Results of a round robin test journal March 1996
Homogeneous and Localized Deformation in Poly(Methyl Methacrylate) Nanocutting journal February 2019
Effects of pre-strain on the compressive stress–strain response of Mo-alloy single-crystal micropillars journal October 2008
Dislocation starvation and exhaustion hardening in Mo alloy nanofibers journal March 2012
Mixed mode fracture toughness as a separation parameter when cutting polymers journal December 2009
Polymer fracture and deformation during nanosectioning in an ultramicrotome journal September 2017
Radiation damage in the TEM and SEM journal August 2004
Relating nanoscale plasticity to bulk ductility in aluminum alloys journal November 2008
Minimization of focused ion beam damage in nanostructured polymer thin films journal February 2011
Extreme Ductility in Freestanding Polystyrene Thin Films journal September 2020
Mechanics and Dynamics of the Strain-Induced M1–M2 Structural Phase Transition in Individual VO 2 Nanowires journal August 2011
Superglide at an Internal Incommensurate Boundary journal February 2010
Mechanical properties of ultrahigh-strength gold nanowires journal June 2005
Gallium, neon and helium focused ion beam milling of thin films demonstrated for polymeric materials: study of implantation artifacts journal January 2019
An investigation on focused electron/ion beam induced degradation mechanisms of conjugated polymers journal January 2011
Sample Dimensions Influence Strength and Crystal Plasticity journal August 2004
Yielding and Strain Hardening in Metallic Thin Films on Substrates: an Edge Dislocation Climb Model journal January 2009
Overview on established and novel FIB based miniaturized mechanical testing using in-situ SEM journal August 2009