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AR Category: Indentation | Hardness and Elastic
Biological Tissue Hardness Evaluation using Nanoindentation
Importance of Biological Tissue Nanoindentation
Traditional mechanical tests (hardness, adhesion, compression, puncture, yield strength, etc.) require greater precision and reliability in today’s quality control environments with a wide range of advanced materials from tissues to brittle materials. Traditional mechanical instrumentation fails to provide the sensitive load control and resolution required for advanced materials. The challenges associated with biomaterials require developing mechanical tests capable of accurate load control on extremely soft materials. These materials require very low sub mN testing loads with large depth range to ensure proper property measurement. In addition, many different mechanical test types can be performed on a single system allowing for greater functionality. This provides a range of important measurements on biomaterials including hardness, elastic modulus, loss and storage modulus, and creep in addition to scratch resistance and yield strength failure points.
Measurement Objective
In this application Nanovea’s mechanical tester in nanoindentation mode is used to study the hardness and elastic modulus of 3 separate areas of a biomaterial substitute on fat, light meat, and dark meat regions of prosciutto.
Nanoindentation is based on instrumented indentation standards ASTM E2546 and ISO 14577. It uses established methods where an indenter tip of known geometry is driven into a specific site of the test material with a controlled increasing normal load. When reaching a pre-set maximum depth, normal load is reduced until complete relaxation occurs. Load is applied by a piezo actuator and measured in a controlled loop with a high sensitivity load cell. During experiments the indenter position relative to the sample surface is monitored with a high precision capacitive sensor. The resulting load and displacement curves provide data specific to the mechanical nature of the tested material. Established models calculate quantitative hardness and modulus values with the measured data. Nanoindentation is suited to low load and penetration depth measurements at nanometer scales.
Results and Discussion
These tables below present measured values of hardness and Young’s modulus with averages and standard deviations. High surface roughness may cause large variations in the results due to small indentation size.
The fat area had about half the hardness of the meat areas. Meat treatment caused the darker meat area to be harder than the light meat area. Elastic modulus and hardness are in direct relation to mouth feel chewiness of the fat and meat areas. The fat and light meat area have creep continuing at a higher rate than the dark meat after 60 seconds.
Detailed Results – Fat
Detailed Results – Light Meat
Detailed Results – Dark Meat
Conclusion
In this application, Nanovea’s mechanical tester in nanoindentation mode reliably determined mechanical properties of the fat and meat areas while overcoming high sample surface roughness. This demonstrated the wide and unmatched capability of Nanovea’s mechanical tester. The system simultaneously provides precise mechanical property measurements on extremely hard materials and soft biological tissues.
The load cell in closed loop control with the piezo table ensures precise measurement of hard or soft gel materials from 1 to 5kPa. Using the same system, it is possible to test biomaterials at higher loads up to 400N. Multi-cycle loading can be used for fatigue testing and yield strength information in each zone can be obtained using a flat cylindrical diamond tip. In addition, with Dynamic Mechanical Analysis (DMA), the viscoelastic properties loss and storage moduli can be evaluated with high accuracy using the closed loop load control. Tests at various temperatures and under liquids are also available on the same system.
Nanovea’s mechanical tester continues to be the superior tool for biological and soft polymer/gel applications.
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Tooth Hardness Evaluation using Nanoindentation
Importance of Nanoindentation for Bio Materials
With many traditional mechanical tests (Hardness, Adhesion, Compression, Puncture, Yield Strength, etc.), today’s quality control environments with advanced sensitive materials, from gels to brittle materials, now require greater precision and reliability control. Traditional mechanical instrumentation fails to provide the sensitive load control and resolution required; designed to be used for bulk materials. As the size of material being tested became of greater interest, the development of Nanoindentation provided a reliable method to obtain essential mechanical information on smaller surfaces such as the research being done with biomaterials. The challenges specifically associated with biomaterials have required the development of mechanical testing capable of accurate load control on extremely soft to brittle materials. Also, multiple instruments are needed to perform various mechanical tests which can now be performed on a single system. Nanoindentation provides a wide range of measurement with precise resolution at nano controlled loads for sensitive applications.
Measurement Objective
In this application, the Nanovea Mechanical Tester, in Nanoindentation mode, is used to study the hardness and elastic modulus of the dentin, decay, and pulp of a tooth. The most critical aspect with Nanoindentation testing is securing the sample, here we took a sliced tooth and epoxy mounted leaving all three areas of interest exposed for testing.
Results and Discussion
This section includes a summary table that compares the main numerical results for the different samples, followed by the full result listings, including each indentation performed, accompanied by micrographs of the indentation, when available. These full results present the measured values of Hardness and Young’s modulus as the penetration depth with their averages and standard deviations. It should be considered that large variation in the results can occur in the case that the surface roughness is in the same size range as the indentation.
Summary table of main numerical results:
Conclusion
In conclusion, we have shown how the Nanovea Mechanical Tester, in Nanoindentation mode, provides precise measurement of the mechanical properties of a tooth. The data can be used in the development of fillings that will better match the mechanical characteristics of a real tooth. The positioning capability of the Nanovea Mechanical Tester allows full mapping of the hardness of the teeth across the various zones.
Using the same system, it is possible to test teeth material fracture toughness at higher loads up to 200N. A multi-cycle loading test can be used on more porous materials to evaluate the remaining level of elasticity. Using a flat cylindrical diamond tip can give yield strength information in each zone. In addition, with DMA “Dynamic Mechanical Analysis”, the viscoelastic properties including loss and storage moduli can be evaluated.
The Nanovea nano module is ideal for these tests because it uses a unique feedback response to control precisely the load applied. Because of this, the nano module can also be used to do accurate nano scratch testing. The study of scratch and wear resistance of tooth material and filling materials adds to the overall usefulness of the Mechanical tester. Using a sharp 2-micron tip to quantitatively compare marring on filling materials will allow better prediction of the behavior in real applications. Multi-pass wear or direct rotative wear testing are also common tests providing important information on the long term viability.
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Nano Mechanical Characterization of Spring Constants
A spring’s ability to store mechanical energy has a long history of use. From bows for hunting to locks for doors, spring technology has been around for many centuries. Nowadays we rely on springs, be it from mattresses, pens, or automotive suspension, as they play a vital role in our daily lives. With such a wide variety of use and designs, the ability to quantify their mechanical properties is necessary.
Mechanical Broadview Map Selection Tool
We’ve all heard the term, time is money. Which is why many companies constantly seek methods of expediting and improving various processes, it saves time. When it comes to indentation testing, speed, efficiency and precision can be integrated into a quality control or R&D process when using one of our Nanovea Mechanical Testers. In this application note, we will be showcasing an easy way of saving time with our Nanovea Mechanical Tester and Broad View Map and Selection Tool software features.
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Precise Localized Glass Transition with Nanoindentation DMA
Precise Localized Glass Transition with Nanoindentation DMA
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Imagine a scenario where a bulk sample is uniformly heated at a constant rate. As a bulk material heats up and approaches its melting point, it will start to lose its rigidity. If periodic indentations (hardness tests) are conducted at the same target force, the depth of each indent should be constantly increasing since the sample is becoming softer (see figure 1). This continues until the sample begins to melt. At this point, a large increase in the depth per indent will be observed. Using this concept, phase change in a material can be observed by using dynamic oscillations with a fixed force amplitude and measuring its displacement, i.e. Dynamic Mechanical Analysis (DMA).
Read about Precise Localized Glass Transition!
Stress Relaxation Measurement using Nanoindentation
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Compression on Soft, Flexible Materials
Importance of testing soft, flexible materials
An example of very soft and flexible samples is a microelectromechanical system. MEMS are used in everyday commercial products like printers, mobile phones, and cars [1]. Their uses also include special functions, such as biosensors [2] and energy harvesting [3]. For their applications, MEMS must be able to reversibly transition between their original configuration to a compressed configuration repeatedly [4]. To understand how the structures will react to mechanical forces, compression testing can be conducted. Compression testing can be utilized to test and tune various MEMS configurations as well as testing upper and lower force limits for these samples.
The Nanovea Mechanical Tester Nano Module’s ability to accurately collect data at very low loads and travel over 1mm of distance makes it ideal for testing the soft and exible samples. By having independent load and depth sensors, large indenter displacement does not affect the readings by the load sensor. The ability to carry out low-load testing over a range of more than 1mm of indenter travel makes our system unique compared to other nanoindentation systems. In comparison, a reasonable travel distance for a nanoscale indentation system is typically below 250μm.
Measurement Objective
In this case study, Nanovea conducted compression testing on two uniquely di erent flexible, spring-like samples. We showcase our ability to conduct compression at very low loads and record large displacement while accurately obtaining data at low loads and how this can be applied to the MEMS industry. Due to privacy policies, the samples and their origin will not be revealed in this study
Measurement Parameters
Note: The loading rate of 1 V/min is proportional to approximately 100μm of displacement when the indenter is in the air.
Results and Discussion
The sample’s response to mechanical forces can be seen in the load vs depth curves. Sample A only displays linear elastic deformation with the test parameters listed above. Figure 2 is a great example of the stability that can be achieved for a load vs. depth curve at 75μN. Due to the load and depth sensors stability, it would be easy to perceive any signi cant mechanical response from the sample.
Sample B displays a different mechanical response from Sample A. Past 750μm of depth, fracture-like behavior in the graph begins to appear. This is seen with the sharp drops in load at 850 and 975μm of depth. Despite traveling at a high loading rate for more than 1mm over a range of 8mN, our highly sensitive load and depth sensors allow the user to obtain the sleek load vs depth curves below.
The stiffness was calculated from the unloading portion of the load vs depth curves. Stiffness reflects how much force is necessary to deform the sample. For this stiffness calculation, a pseudo Poisson’s ratio of 0.3 was used since the actual ratio of the material is not known. In this case, Sample B proved to be stiffer than Sample A.
Conclusion
Two diff erent flexible samples were tested under compression using the Nanovea Mechanical Tester’s Nano Module. The tests were conducted at very low loads (<80μN) and over a large depth range (>1mm). Nano-scaled compression testing with the Nano Module has shown the module’s ability to test very soft and flexible samples. Additional testing for this study could address how repeated cyclical loading a ects the elastic recovery aspect of the spring-like samples via the Nanovea Mechanical Tester’s multi-loading option.
For more information on this testing method, feel free to contact us at [email protected] and for additional application notes please browse our extensive Application Note digital library.
References
[1] “Introduction and Application Areas for MEMS.” EEHerald, 1 Mar. 2017, www.eeherald.com/section/design-guide/mems_application_introduction.html.
[2] Louizos, Louizos-Alexandros; Athanasopoulos, Panagiotis G.; Varty, Kevin (2012). “Microelectromechanical Systems and Nanotechnology. A Platform for the Next Stent Technological Era”. Vasc Endovascular Surg.46 (8): 605–609. doi:10.1177/1538574412462637. PMID 23047818.
[3] Hajati, Arman; Sang-Gook Kim (2011). “Ultra-wide bandwidth piezoelectric energy harvesting”. AppliedPhysics Letters. 99 (8): 083105. doi:10.1063/1.3629551.
[4] Fu, Haoran, et al. “Morphable 3D mesostructures and microelectronic devices by multistable bucklingmechanics.” Nature materials 17.3 (2018): 268.
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Mechanical Properties of Silicon Carbide Wafer Coatings
Understanding the mechanical properties of silicon carbide wafer coatings is critical. The fabrication process for microelectronic devices can have over 300 different processing steps and can take anywhere from six to eight weeks. During this process, the wafer substrate must be able to withstand the extreme conditions of manufacturing, since a failure at any step would result in the loss of time and money. The testing of hardness, adhesion/scratch resistance and COF/wear rate of the wafer must meet certain requirements in order to survive the conditions imposed during the manufacturing and application process to insure a failure will not occur.
Mechanical & Tribological Properties of Carbon Fiber
Combined with the wear test by Tribometer and surface analysis by Optical 3D Profilometer, we
showcase the versatility and accuracy of the Nanovea instruments in testing composite materials
with directional mechanical properties.
Biomechanical Hardness Evaluation of Tissue
The ability to accurately measure mechanical properties in the fields of Life Science has recently become an important aspect of many current studies. In some cases, understanding the mechanical properties of soft biological surfaces have helped uncover the mechanical effects of diseases. Understanding mechanical properties provides a context for identifying the local mechanical behavior linked to specific changes. It is also critical in the development of artificial bio-materials. In this application, the Nanovea Mechanical Tester, in Nanoindentation mode, is used to study the biomechanical hardness and elastic modulus of 3 separate areas of prosciutto (fat, light meat and dark meat).
Tooth Hardness Evaluation Using Nanoindentation
In this application, the Nanovea Mechanical Tester, in Nanoindentation mode, is used to study the hardness and elastic modulus of the dentin, decay and pulp of a tooth. The most critical aspect with Nanoidentation testing is securing the sample, here we took a sliced tooth and epoxy mounted leaving all three area of interest exposed for testing.
