An overview of nanoindentation as it applies to battery manufacturing and battery materials research. Topics include battery cell manufacturing, cathode load response, nanomechanical mapping of composite electrodes, in situ particle compression, viscoelastic response of binder materials, and alternative battery materials testing environments.

This work investigates the nanomechanical and elastic properties of a lithium/polymer composite battery cathode, measured by nanoindentation mapping to correlate the life cycle, charge/discharge cycles to the nanomechanical properties of the battery electrode.

The Nano Indenter^® G200 is used with a customizable NanoSuite test method to analyze the integrity of a MEMS-fabricated IC wafer probe; specifically, to determine the magnitude of shear force that the probe can withstand without breaking off its support structure.

Guidelines on geometries and recommended applications for different nanoindentation tips, including Berkovich, Vickers, Cube-Corner, Cone, and Sphere.

The NanoFlip indentation system was used to compress glass microspheres within an SEM chamber. At an elastic strain of 0.2%, the measured Young’s modulus fits exactly within the expected range for soda-lime glass. The results are enhanced by in situ SEM images which reveal both plastic yield and fracture.

Many of the KLA Instruments Nano Indenter^® systems include the capability to measure electromechanical properties. This paper discusses use of the I-V Option for studying Pyrolytic Carbon (PyC).

Using the test method ‘Complex Shear Modulus of Biomaterials’, a KLA nanoindenter performs nanoindentation testing on edible gelatin. Theory, sample preparation and measurement technique are discussed.

A KLA nanoindenter is used with the NanoBlitz 3D option to perform nanoindentation hardness testing on Scalmalloy, a commercial aluminum alloy specifically designed for laser-powder-bed additive manufacturing. NanoBlitz 3D maps of the Scalmalloy cross-section clearly illustrate the layered 3D metal printing process, with a bimodal hardness distribution and a Gaussian modulus distribution.

A KLA-developed technique was used for measuring the storage and loss modulus of artificial tissue samples using dynamic nanoindentation on a KLA Nano Indenter^® G200. Tests were performed using the Continuous Stiffness Measurement (CSM) option, which allows for frequency-specific, dynamic nanoindentation, which provides better spatial resolution for material characterization than traditional bulk DMA analysis.

The Student’s t-test is used in an uncommon way to predict the number of observations, N, which must be made in order to be sensitive to a given difference at a given confidence level. With respect to nanoindentation, this analysis illuminates the benefits of the ultra-fast testing afforded by the Express Test option for the KLA Nano Indenter^® G200 to dramatically improve the sensitivity to significant difference.

Instrumented nanoindentation is used to measure elasticity and strength of bone at the level of individual osteons. Elastic modulus and nanoindenter hardness testing are performed by analyzing the contact stiffness as a continuous function of penetration depth.

Ten different materials are tested with the KLA iNano^® nanoindenter in accordance with ISO 14577-1, including polymers, metals, glasses and single crystals. The same test method measuring Young's modulus values also automatically determines instrumented nanoindentation hardness and the converted Vickers Hardness Number (VHN).

A KLA Nano Indenter^® system is used with the ProbeDMA™ nanoindentation technique to analyze the silicone gel coatings of two automotive MEMS-based pressure sensors. ProbeDMA takes advantage of Continuous Stiffness Measurement (CSM) to provide quantitative results for both DMA (storage) modulus and contact stiffness for the two sensors.

The Nano Indenter^® G200 is used to study the extent of layer damage from charged iron particles and protons into the bulk of irradiated HCM12A steel by measuring indentation hardness as a function of penetration depth.

The Nano Indenter^® G200 is used with the Express Test and the laser-heated tip and stage options for elastic modulus and indentation hardness testing of Ordinary Portland Cement (OPC) paste at temperatures from 20°C to 250°C. NanoVision was also used to generate surface topography measurements.

A KLA nanoindenter utilizing the hot stage, the Continuous Stiffness Measurement (CSM) option and the “Dynamic CSR for Thin Films” test method was used for measuring Young’s modulus and indentation hardness of optical coatings on fused silica substrates. Results were compared for two optical coatings at 22°C, 150°C and 300°C.

A KLA Nano Indenter^® G200 was used for material characterization of both bare M42 steel and its TiN coating. Nanoindentation testing included ISO 14577 semi-static tests and Continuous Stiffness Measurement (CSM) tests.

The KLA InSEM^® HT high temperature nanoindenter was used for material characterization of Physical Vapor Deposition (PVD) ZrN coatings on steel. NanoBlitz 3D was used to compare maps of hard coating modulus and hardness at both 400°C and 660°C.

A KLA Nano Indenter^® was used with NanoBlitz 3D high speed mapping for elastic modulus and nanohardness testing of the bond coat, top coat and interface regions of as-coated and thermally-cycled thermal barrier coatings (TBCs). Excellent correlation was found between the microstructure and the local nanomechanical properties at the micrometer length scale, even at the interface between the various layers of TBC and in the porous top coat.

The interface adhesion energy of low k films is measured using the ISO 14577 standard nanoindentation method with a decremental loading factor. Analysis of the load-displacement curves determined the load at crack initiation/delamination at the film/substrate interface, and the energy dissipated during nanoindentation near the critical load.

The KLA iMicro nanoindenter is used to measure the near-surface indentation hardness of Fe₁₄Cr. Both the irradiated and control Fe₁₄Cr are analyzed using the iMicro nanoindentation test method “Advanced Dynamic E and H" to generate continuous measurement of both Young’s modulus and Vickers hardness.

A KLA nanoindenter is used to perform local dynamic mechanical analysis (DMA) testing on SBR, mounted inside a cold chamber. The ProbeDMA™ nanoindentation testing method measures frequency-specific viscoelastic material properties, and is used here to compare the storage modulus of SBR as a function of temperature and frequency.

A Nano Indenter^® G200X system was used to perform impact nanoindentation testing on aluminum, iron, stainless steel, and commercial purity magnesium. Hardness testing as a function of strain rate was compared for these materials using the ISO 14577 test method and Constant Load and Hold (CLH) testing.

The iMicro nanoindenter was used to generate stress-strain curves for commercially pure titanium using the standard iMicro test method "Flat Punch on Metals for Stress-Strain." The flat-punch geometry is superior to the more commonly used sphere, because both the contact area and the volume of tested material remain constant throughout the nanoindentation test.

This paper, co-authored by Warren C. Oliver and originally published in Materials and Design, discusses high speed nanoindentation mapping using NanoBlitz 3D for local nanomechanical testing of multi-phase alloys and small volumes of materials with high throughput. To determine the minimum spacing between indents required to prevent interactions from neighboring indents, extensive nanoindentation experiments and finite element simulations are performed.

This paper, co-authored by Warren C. Oliver and originally published in Materials and Design, discusses high speed nanoindentation mapping as applied to thermal barrier coatings (TBCs). Extensive nanoindentation tests are performed using NanoBlitz 3D to spatially map the indentation hardness and elastic modulus of the bond coat, top coat and bond coat-top coat interface regions of as-coated and thermally cycled TBCs. The resulting spatial property maps are compared with the corresponding microstructures to establish correlations.

A Nano Indenter^® G200 is used to determine the scratch and wear properties of ten spin-coated low k films on silicon substrates. A ramp-load scratch test is performed, with a single line scan of the coating surface collected before and after the scratch test to determine residual deformation. The NanoVision stage is used to provide high resolution positioning capability for the nanoindentation testing.

Express Test is a method of rapid nanomechanical testing used with a KLA nanoindenter to generate histograms and 3D maps of nanomechanical properties, such as Young's modulus and nanohardness, with negligible thermal drift.

This application note discusses the Continuous Stiffness Measurement (CSM) nanoindentation option, used for applications that must take into account dynamic effects, such as strain rate and frequency. The CSM option for material characterization offers a means of separating the in-phase and out-of-phase components of the load-displacement history.

Instrumented Indentation Testing (IIT) is used to measure strain rate sensitivity (SRS) of thin nickel and copper films on silicon. The Continuous Stiffness Measurement (CSM) nanoindentation option was also used in order to measure indentation hardness and elastic modulus as a continuous function of penetration depth.

Dynamic instrumented indentation was used to measure the complex shear modulus of soft biological tissue under physiological conditions. Continuous Stiffness Method (CSM) nanoindentation was used with the hot stage option to compare the complex shear modulus and confirm the anisotropic nature of muscle tissue.

Instrumented Indentation Testing (IIT) or Depth-Sensing Indentation (DSI) has become the technique of choice for nanomechanical testing and material characterization. This paper discusses the Oliver-Pharr test method, theory and analysis for extraction of Young's modulus, hardness, complex modulus, stress exponent for creep, and fracture toughness.

A KLA nanoindenter using the Continuous Stiffness Measurement (CSM) option to measure the Young's modulus and nanoindentation hardness of three sol-gel coatings. Scratch tests were also performed to evaluate adhesion of the coatings. In the case of adhesive failure, NanoSuite Explorer was used to identify the critical load at failure.

Probe based Dynamic Mechanical Analysis (ProbeDMA™) nanomechanical testing was performed on cross sections of a rubber tire using the Continuous Stiffness Measurement (CSM) technique. The local storage and loss moduli were compared for different material structures along the cross sections.

Nanoindentation hardness testing was used to analyze ultra-thin gold films before and after vacuum annealing, deposited on two different substrates. NanoBlitz 3D and Express Test results showed a significant decrease in indentation hardness of the gold metal films.