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Category: Mechanical Tester

 

Multiphase Material using Nanoindentation NANOVEA

Metallurgy Study of Multiphase Material

Metallurgy Study of Multiphase Material using Nanoindentation

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METALLURGY STUDY
OF MULTIPHASE MATERIAL

USING NANOINDENTATION

Prepared by

DUANJIE LI, PhD & ALEXIS CELESTIN

INTRODUCTION

Metallurgy studies the physical and chemical behavior of metallic elements, as well as their intermetallic compounds and alloys. Metals that undergo working processes, such as casting, forging, rolling, extrusion and machining, experience changes in their phases, microstructure and texture. These changes result in varied physical properties including hardness, strength, toughness, ductility, and wear resistance of the material. Metallography is often applied to learn the formation mechanism of such specific phases, microstructure and texture.

MPORTANCE OF LOCAL MECHANICAL PROPERTIES FOR MATERIALS DESIGN

Advanced materials often have multiple phases in a special microstructure and texture to achieve desired mechanical properties for target applications in industrial practice. Nanoindentation is widely applied to measure the mechanical behaviors of materials at small scales i ii. However, it is challenging and time-consuming to precisely select specific locations for indentation in a very small area. A reliable and user-friendly procedure of nanoindentation testing is in demand to determine the mechanical properties of different phases of a material with high precision and timely measurements.

MEASUREMENT OBJECTIVE

In this application, we measure mechanical properties of a multiphase metallurgical sample using the Most Powerful Mechanical Tester: the NANOVEA PB1000.

Here, we showcase the capacity of the PB1000 in performing nanoindentation measurements on multiple phases (grains) of a large sample surface with high precision and user friendliness using our Advanced Position Controller.

NANOVEA

PB1000

TEST CONDITIONS

In this study, we use a metallurgical sample with multiple phases. The sample had been polished to a mirror-like surface finish before the indentation tests. Four phases have been identified in the sample, namely PHASE 1, PHASE 2, PHASE 3 and PHASE 4 as shown below.

The Advanced Stage Controller is an intuitive sample navigation tool which automatically adjusts the speed of sample movement under the optical microscope based on position of the mouse. The further the mouse is away from the center of field of view, the faster the stage moves toward the mouse’s direction. This provides a user-friendly method to navigate the entire sample surface and select the intended location for mechanical testing. The coordinates of the test locations are saved and numbered, along with their individual test setups, such as loads, loading/unloading rate, number of tests in a map, etc. Such a test procedure allows users to examine a large sample surface for specific areas of interest for indentation and perform all the indentation tests at different locations in one time, making it an ideal tool for mechanical testing of metallurgical samples with multiple phases.

In this study, we located the specific phases of the sample under the optical microscope integrated in the NANOVEA Mechanical Tester as numbered on FIGURE 1. The coordinates of the selected locations are saved, followed by automatic nanoindentation tests all at once under the test conditions summarized below

FIGURE 1: SELECTING NANOINDENTATION LOCATION ON THE SAMPLE SURFACE.
RESULTS: NANOINDENTATIONS ON DIFFERENT PHASES

The indentations at the different phases of the sample are displayed below. We demonstrate that the excellent position control of the sample stage in the NANOVEA Mechanical Tester allows users to precisely pinpoint the target location for mechanical properties testing.

The representative load-displacement curves of the indentations are shown in FIGURE 2, and the corresponding hardness and Young’s Modulus calculated using Oliver and Pharr Methodiii are summarized and
compared in
FIGURE 3.


The
PHASES 1, 2, 3 and 4 possess an average hardness of ~5.4, 19.6, 16.2 and 7.2 GPa, respectively. The
relatively small size for
PHASES 2 contributes to its higher standard deviation of the hardness and Young’s
Modulus values.

FIGURE 2: LOAD-DISPLACEMENT CURVES
OF THE NANOINDENTATIONS
FIGURE 2: HARDNESS & YOUNG’S MODULUS
OF DIFFERENT PHASES

CONCLUSION

In this study, we showcased the NANOVEA Mechanical Tester performing nanoindentation measurements on multiple phases of a large metallurgical sample using the Advanced Stage Controller. The precise position control allows users to easily navigate a large sample surface and directly select the areas of interest for nanoindentation measurements.

The location coordinates of all the indentations are saved and then performed consecutively. Such a test procedure makes measurement of the local mechanical properties at small scales, e.g. the multi-phase metal sample in this study, substantially less time-consuming and more user friendly. The hard PHASES 2, 3 and 4 improve the mechanical properties of the sample, possessing an average hardness of ~19.6, 16.2 and 7.2 GPa, respectively, compared to ~5.4 GPa for PHASE 1.

The Nano, Micro or Macro modules of the instrument all include ISO and ASTM compliant indentation, scratch and wear tester modes, providing the widest and most user friendly range of testing available in a single system. NANOVEA‘s unmatched range is an ideal solution for determining the full range of mechanical properties of thin or thick, soft or hard coatings, films and substrates, including hardness, Young’s modulus, fracture toughness, adhesion, wear resistance and many others.

i Oliver, W. C.; Pharr, G. M., Journal of Materials Research., Volume 19, Issue 1, Jan 2004, pp.3-20
ii Schuh, C.A., Materials Today, Volume 9, Issue 5, May 2006, pp. 32–40
iii Oliver, W. C.; Pharr, G. M., Journal of Materials Research, Volume 7, Issue 6, June 1992, pp.1564-1583

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DMA Frequency Sweep on Polymer Using Nanoindentation

DMA Frequency Sweep on Polymer Using Nanonindentation

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DMA FREQUENCY SWEEP

ON POLYMER USING NANOINDENTATION

Prepared by

Duanjie Li, PhD

INTRODUCTION

IMPORTANCE OF DMA FREQUENCY SWEEP TEST

The changing frequency of the stress often leads to variations in the complex modulus, which is a critical mechanical property of polymers. For example, tires are subjected to cyclical high deformations when vehicles are running on the road. The frequency of the pressure and deformation changes as the car accelerates to higher speeds. Such a change can result in variation in the viscoelastic properties of the tire, which are important factors in the car performance. A reliable and repeatable test of the viscoelastic behavior of polymers at different frequencies is in need. The Nano module of the NANOVEA Mechanical Tester generates sinusoidal load by a high precision piezo actuator and directly measures the evolution of force and displacement using ultrasensitive load cell and capacitor. The combination of easy setup and high accuracy makes it an ideal tool for DMA frequency sweep.

Viscoelastic materials exhibit both viscous and elastic characteristics when undergoing deformation. Long molecular chains in polymer materials contribute to their unique viscoelastic properties, i.e. a combination of the characteristics of both elastic solids and Newtonian fluids. Stress, temperature, frequency and other factors all play roles in the viscoelastic properties. Dynamic Mechanical Analysis, also known as DMA, studies the viscoelastic behavior and complex modulus of the material by applying a sinusoidal stress and measuring the change of strain.

MEASUREMENT OBJECTIVE

In this application, we study viscoelastic properties of a polished tire sample at different DMA frequencies using the Most Powerful Mechanical Tester, NANOVEA PB1000, in Nanoindentation mode.

NANOVEA

PB1000

TEST CONDITIONS

FREQUENCIES (Hz):

0.1, 1.5, 10, 20

CREEP TIME AT EACH FREQ.

50 sec

OSCILLATION VOLTAGE

0.1 V

LOADING VOLTAGE

1 V

indenter type

Spherical

Diamond | 100 μm

RESULTS & DISCUSSION

The DMA frequency sweep at the maximum load allows a fast and simple measurement on the viscoelastic characteristics of the sample at different loading frequencies in one test. The phase shift and the amplitudes of the load and displacement waves at different frequencies can be used to calculate a variety of fundamental material viscoelastic properties, including Storage Modulus, Loss Modulus and Tan (δ) as summarized in the following graphs. 

Frequencies of 1, 5, 10 and 20 Hz in this study, correspond to speeds of about 7, 33, 67 and 134 km per hour. As the test frequency increases from 0.1 to 20 Hz, it can be observed that both Storage Modulus and Loss Modulus progressively increase. Tan (δ) decreases from ~0.27 to 0.18 as the frequency increases from 0.1 to 1 Hz, and then it gradually increases to ~0.55 when the frequency of 20 Hz is reached. DMA frequency sweep allows measuring the trends of Storage Modulus, Loss Modulus and Tan (δ), which provide information on the movement of the monomers and cross-linking as well as the glass transition of polymers. By raising the temperature using a heating plate during the frequency sweep, a more complete picture of the nature of the molecular motion under different test conditions can be obtained.

EVOLUTION OF LOAD & DEPTH

OF THE FULL DMA FREQUENCY SWEEP

LOAD & DEPTH vs TIME AT DIFFERENT FREQUENCIES

STORAGE MODULUS

AT DIFFERENT FREQUENCIES

LOSS MODULUS

AT DIFFERENT FREQUENCIES

TAN (δ)

AT DIFFERENT FREQUENCIES

CONCLUSION

In this study, we showcased the capacity of the NANOVEA Mechanical Tester in performing the DMA frequency sweep test on a tire sample. This test measures the viscoelastic properties of the tire at different frequencies of stress. The tire shows increased storage and loss modulus as the loading frequency increases from 0.1 to 20 Hz. It provides useful information on the viscoelastic behaviors of the tire running at different speeds, which is essential in improving the performance of tires for smoother and safer rides. The DMA frequency sweep test can be performed at various temperatures to mimic the realistic working environment of the tire under different weather.

In the Nano Module of the NANOVEA Mechanical Tester, the load application with the fast piezo is independent from the load measurement done by a separate high sensitivity strain gage. This gives a distinct advantage during DMA since the phase between depth and load is measured directly from the data collected from the sensor. The calculation of phase is direct and does not need mathematical modeling that adds inaccuracy to the resulting loss and storage modulus. This is not the case for a coil-based system.

In conclusion, DMA measures loss and storage modulus, complex modulus and Tan (δ) as a function of contact depth, time and frequency. Optional heating stage allows determination of materials phase transition temperature during DMA. The NANOVEA Mechanical Testers provide unmatched multi-function Nano and Micro modules on a single platform. Both the Nano and Micro modules include scratch tester, hardness tester and wear tester modes, providing the widest and most user friendly range of testing available on a single module.

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Microparticles: Compression Strength and Micro Indentation by Testing Salts

Microparticles: Compression Strength & Micro Indentation by Testing Salts

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MICROPARTICLES

COMPRESSION STRENGTH & MICRO INDENTATION
BY TESTING SALTS​

Author:
Jorge Ramirez

Revised by:
Jocelyn Esparza

INTRODUCTION

Compression strength has become vital to quality control measurement in developing and improving new and existing microparticles and micro features (pillars and spheres) seen today. Microparticles have various shapes, sizes and can be developed from ceramics, glass, polymers, and metals. Uses include drug delivery, food flavor enhancement, concrete formulations among many others. Controlling the mechanical properties of microparticles or microfeatures are critical for their success and requires the ability to quantitatively characterize their mechanical integrity  

IMPORTANCE OF DEPTH VERSUS LOAD COMPRESSION STRENGTH

Standard compressive measurement instruments are not capable of low loads and fail to provide adequate depth data for microparticles. By using Nano or Microindentation, the compression strength of nano or microparticles (soft or hard) can be accurately and precisely measured.  

MEASUREMENT OBJECTIVE

In this application note we measure  the compression strength of salt with the NANOVEA Mechanical Tester in micro indentation mode.

NANOVEA

CB500

TEST CONDITIONS

maximum force

30 N

loading rate

60 N/min

unloading rate

60 N/min

indenter type

Flat Punch

Steel | 1mm Diameter

Load vs depth curves

Results & Discussion

Height, failure force and strength for Particle 1 and Particle 2

Particle failure was determined to be the point where the initial slope of the force vs. depth curve began to noticeably decrease.This behavior shows the material has reached a yield point and is no longer able to resist the compressive forces being applied. Once the yield point is surpassed, the indentation depth begins to exponentially increase for the duration of the loading period. These behaviors can be seen in Load vs Depth Curves for both samples.

CONCLUSION

In conclusion, we have shown how the NANOVEA Mechanical Tester in micro indentation mode is a great tool for compression strength testing of microparticles. Although the particles tested are made of the same material, it is suspected that the different failure points measured in this study were likely due to pre-existent micro cracks in the particles and varying particle sizes. It should be noted that for brittle materials, acoustic emission sensors are available to measure the beginning of crack propagation during a test.


The
NANOVEA Mechanical Tester offers depth displacement resolutions down to the sub nanometer level,
making it a great tool for the study of very fragile micro particles or features as well. For soft and fragile
materials, loads down to 0.1mN are possible with our nano indentation module

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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.

Click to read the full application note!

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 dierent 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 signicant 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 different 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 aects 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 info@nanovea.com 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.

Viscoelastic Analysis of Rubber

Tires are subjected to cyclical high deformations when vehicles are running on the road. When exposed to harsh road conditions, the service lifetime of the tires is jeopardized by many factors, such as the wear of the thread, the heat generated by friction, rubber aging, and others.

As a result, tires usually have composite layer structures made of carbon-lled rubber, nylon cords, and steel wires, etc. In particular, the composition of rubber at different areas of the tire systems is optimized to provide different functional properties, including but not limited to wear resistant thread, cushion rubber layer, and hard rubber base layer.

A reliable and repeatable test of the viscoelastic behavior of rubber is critical in quality control and R&D of new tires, as well as evaluation of the life span of old tires. Dynamic Mechanical Analysis(DMA) during Nanoindentation is a technique of characterizing the viscoelasticity. When controlled oscillatory stress is applied, the resulting strain is measured, allowing users to determine the complex modulus of the tested materials.

 

Click to read the full Application Note!

A BETTER Look at Polycarbonate Lens

Polycarbonate lenses are commonly used in many optical applications. Their high impact resistance, low weight, and cheap cost of high-volume production makes them more practical than traditional glass in various applications [1].

Some of these applications require safety (e.g. safety eyewear), complexity (e.g. Fresnel lens) or durability (e.g. traffic light lens) criteria that are difficult to meet without the use of plastics. Its ability to cheaply meet many requirements while maintaining sufficient optical qualities makes plastic lenses stand out in its field. Polycarbonate lenses also have limitations. The main concern for consumers is the ease at which they can be scratched. To compensate for this, extra processes can be carried out to apply an anti-scratch coating.

Nanovea takes a look into some important properties of plastic lens by utilizing our three metrology instruments: Profilometer, Tribometer, and Mechanical Tester.

 

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