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Category: Indentation | Creep and Relaxation

 

Mechanical Properties of Hydrogel

MECHANICAL PROPERTIES OF HYDROGEL

USING NANOINDENTATION

Prepared by

DUANJIE LI, PhD & JORGE RAMIREZ

INTRODUCTION

Hydrogel is known for its super absorbency of water allowing for a close resemblance in flexibility as natural tissues. This resemblance has made hydrogel a common choice not only in biomaterials, but also in electronics, environment and consumer good applications such as contact lens. Each unique application requires specific hydrogel mechanical properties.

IMPORTANCE OF NANOINDENTATION FOR HYDROGEL

Hydrogels create unique challenges for Nanoindentation such as test parameters selection and sample preparation. Many nanoindentation systems have major limitations since they were not originally designed for such soft materials. Some of the nanoindentation systems use a coil/magnet assembly to apply force on the sample. There is no actual force measurement, leading to inaccurate and non-linear loading when testing soft materials. Determining the point of contact is extremely difficult as the depth is the only parameter actually being measured. It is almost impossible to observe the change of slope in the Depth vs Time plot during the period when the indenter tip is approaching the hydrogel material.

In order to overcome the limitations of these systems, the nano module of the NANOVEA Mechanical Tester measures the force feedback with an individual load cell to ensure high accuracy on all types of materials, soft or hard. The piezo-controlled displacement is extremely precise and fast. This allows unmatched measurement of viscoelastic properties by eliminating many theoretical assumptions that systems with a coil/magnet assembly and no force feedback must account for.

MEASUREMENT OBJECTIVE

In this application, the NANOVEA Mechanical Tester, in Nanoindentation mode, is used to study the hardness, elastic modulus and creep of a hydrogel sample.

NANOVEA

PB1000

nanoindenter and scratch tester Nanovea PB1000
TEST CONDITIONS

A hydrogel sample placed on a glass slide was tested by nanoindentation technique using a NANOVEA Mechanical Tester. For this soft material a 3 mm diameter spherical tip was used. The load linearly increased from 0.06 to 10 mN during the loading period. The creep was then measured by the change of indentation depth at the maximum load of 10 mN for 70 seconds.

APPROACH SPEED: 100 μm/min

CONTACT LOAD
0.06 mN
MAX LOAD
10 mN
LOADING RATE

20 mN/min

CREEP
70 s
RESULTS & DISCUSSION

The evolution of the load and depth as a function of time is shown in FUGURE 1. It can be observed that on the plot of the Depth vs Time, it is very difficult to determine the point of the change of slope at the beginning of the loading period, which usually works as an indication where the indenter starts to contact the soft material. However, the plot of the Load vs Time shows the peculiar behavior of the hydrogel under an applied load. As the hydrogel begins to get in touch with the ball indenter, the hydrogel pulls the ball indenter due to its surface tension, which tends to decrease the surface area. This behavior leads to the negative measured load at the beginning of the loading stage. The load progressively increases as the indenter sinks into the hydrogel, and it is then controlled to be constant at the maximum load of 10 mN for 70 seconds to study the creep behavior of the hydrogel.

FIGURE 1: Evolution of the load and depth as a function of Time.

The plot of the Creep Depth vs Time is shown in FIGURE 2, and the Load vs. Displacement plot of the nanoindentation test is shown in FIGURE 3. The hydrogel in this study possesses a hardness of 16.9 KPa and a Young’s modulus of 160.2 KPa, as calculated based on the load displacement curve using the Oliver-Pharr method.

Creep is an important factor for the study of a hydrogel’s mechanical properties. The close-loop feedback control between piezo and ultrasensitive load cell ensures a true constant loading during the creep time at the maximum load. As shown in FIGURE 2, the hydrogel subsides ~42 μm as a result of creep in 70 seconds under the 10 mN maximum load applied by the 3 mm ball tip.

FIGURE 2: Creeping at a max load of 10 mN for 70 seconds.

FIGURE 3: The Load vs. Displacement plot of the hydrogel.

CONCLUSION

In this study, we showcased that the NANOVEA Mechanical Tester, in Nanoindentation mode, provides a precise and repeatable measurement of a hydrogel’s mechanical properties including hardness, Young’s modulus and creep. The large 3 mm ball tip ensures proper contact against the hydrogel surface. The high precision motorized sample stage allows for accurate positioning of the flat face of the hydrogel sample under the ball tip. The hydrogel in this study exhibits a hardness of 16.9 KPa and a Young’s modulus of 160.2 KPa. The creep depth is ~42 μm under a 10 mN load for 70 seconds.

NANOVEA Mechanical Testers provide unmatched multi-function Nano and Micro modules on a single platform. Both modules include a scratch tester, hardness tester and a wear tester mode, offering the widest and the most user friendly range of testing available on a single
system.

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Creep Deformation of Polymers using Nanoindentation

Creep Deformation of Polymers using Nanoindentation

Learn more
 

CREEP DEFORMATION

OF POLYMERS USING NANOINDENTATION

Prepared by

DUANJIE LI, PhD

INTRODUCTION

As viscoelastic materials, polymers often undergo a time-dependent deformation under a certain applied load, also known as creep. Creep becomes a critical factor when the polymeric parts are designed to be exposed to continuous stress, such as structural components, joins and fittings, and hydrostatic pressure vessels.

IMPORTANCE OF CREEP MEASUREMENT FOR POLYMERS

The inherent nature of viscoelasticity plays a vital role in the performance of polymers and directly influences their service reliability. The environmental conditions such as loading and temperature affect the creep behavior of the polymers. Creep failures often occur due to the lack of alertness of the time-dependent creep behavior of the polymer materials used under specific service conditions. As a result, it is important to develop a reliable and quantitative test of the viscoelastic mechanical behaviors of the polymers. The Nano module of the NANOVEA Mechanical Testers applies the load with a high-precision piezo and directly measures the evolution of force and displacement in situ. The combination of accuracy and repeatability makes it an ideal tool for creep measurement.

MEASUREMENT OBJECTIVE

In this application, we showcased that
the NANOVEA PB1000 Mechanical Tester
in Nanoindentation mode is an ideal tool
for studying viscoelastic mechanical properties
including hardness, Young’s modulus
and creep of polymeric materials.

NANOVEA

PB1000

nanoindenter and scratch tester Nanovea PB1000
TEST CONDITIONS

Eight different polymer samples were tested by nanoindentation technique using the NANOVEA PB1000 Mechanical Tester. As the load linearly increased from 0 to 40 mN, the depth progressively increased during the loading stage. The creep was then measured by the change of indentation depth at the maximum load of 40 mN for 30 s.

MAXIMUM LOAD 40 mN
LOADING RATE
80 mN/min
UNLOADING RATE 80 mN/min
CREEP TIME
30 s

INDENTER TYPE

Berkovich

Diamond

*setup of the nanoindentation test

RESULTS & DISCUSSION

The load vs displacement plot of the nanoindentation tests on different polymer samples is shown in FIGURE 1 and the creep curves are compared in FIGURE 2. The hardness and Young’s modulus are summarized in  FIGURE 3, and the creep depth is shown in FIGURE 4. As an examples in FIGURE 1, the AB, BC and CD portions of the load-displacement curve for the nanoindentation measurement represent the loading, creep and unloading processes, respectively.

Delrin and PVC exhibit the highest hardness of 0.23 and 0.22 GPa, respectively, while LDPE possesses the lowest hardness of 0.026 GPa among the tested polymers. In general, the harder polymers show lower creep rates. The softest LDPE has the highest creep depth of 798 nm, compared to ~120 nm for Delrin.

The creep properties of the polymers are critical when they are used in structural parts. By precisely measuring the hardness and creep of the polymers, a better understanding of the time-dependent reliability of the polymers can be obtained. The creep, change of the displacement at a given load, can also be measured at different elevated temperatures and humidity using the NANOVEA PB1000 Mechanical Tester, providing an ideal tool to quantitatively and reliably measure the viscoelastic mechanical behaviors of polymers
in the simulated realistic application environment.

FIGURE 1: The load vs displacement plots
of different polymers.

FIGURE 2: Creeping at a maximum load of 40 mN for 30 s.

FIGURE 3: Hardness and Young’s modulus of the polymers.

FIGURE 4: Creep depth of the polymers.

CONCLUSION

In this study, we showcased that the NANOVEA PB1000
Mechanical Tester measures the mechanical properties of different polymers, including hardness, Young’s modulus and creep. Such mechanical properties are essential in selecting the proper polymer material for intended applications. Derlin and PVC exhibit the highest hardness of 0.23 and 0.22 GPa, respectively, while LDPE possesses the lowest hardness of 0.026 GPa among the tested polymers. In general, the harder polymers exhibit lower creep rates. The softest LDPE shows the highest creep depth of 798 nm, compared to ~120 nm for Derlin.

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 wildest and most user-friendly range of testing available on a single system.

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Stress Relaxation Measurement using Nanoindentation
 

INTRODUCTION

Viscoelastic materials are characterized as having both viscous and elastic material properties. These materials are subject to time-dependent stress decrease (stress ‘relaxation’) under constant strain, leading to a significant loss of initial contact force. Stress relaxation is dependent on the type of material, texture, temperature, initial stress, and time. Understanding stress relaxation is critical in selecting optimal materials that have the strength and flexibility (relaxation) required for specific applications.

Importance of Stress Relaxation Measurement

As per ASTM E328i, “Standard Test Methods for Stress Relaxation for Materials and Structures”, an external force is initially applied on a material or structure with an indenter until it reaches a predetermined maximum force. Once the maximum force is reached, the position of the indenter is held constant at this depth. Then the change in external force necessary to maintain the indenter’s position is measured as a function of time. The difficulty in stress relaxation testing is maintaining the depth constant. The Nanovea Mechanical Tester’s nanoindentation module accurately measures the stress relaxation by applying a closed (feedback) loop control of the depth with a piezo-electric actuator. The actuator reacts in real-time to keep the depth constant, while the change in load is measured and recorded by a highly sensitive load sensor. This test can be performed on virtually all types of materials without the need for stringent sample dimension requirements. Additionally, multiple tests can be performed on a single flat sample to ensure test repeatability

MEASUREMENT OBJECTIVE

In this application, the Nanovea Mechanical Tester’s nanoindentation module measures the stress relaxation behavior of an acrylic and copper sample. We showcase that the Nanovea Mechanical Tester is an ideal tool for evaluating the time-dependent viscoelastic behavior of polymer and metal materials.

TEST CONDITIONS

The stress relaxation of an acrylic and a copper sample was measured by the Nanovea Mechanical Tester’s nanoindentation module. Different indentation loading rates were applied ranging from 1 to 10 µm/min. The relaxation was measured at a fixed depth once the target maximum load was reached. A 100 second holding period was implemented at a fixed depth and the change in load was recorded as the holding time elapsed. All of the tests were conducted at ambient conditions (room temperature of 23 °C) and the indentation test parameters are summarized in Table 1.

RESULTS AND DISCUSSION

Figure 2 shows the evolution of displacement and load as a function of time during the stress relaxation measurement of an acrylic sample and an indentation loading rate of 3 µm/min as an example. The entirety of this test can be broken down into three stages: Loading, Relaxation and Unloading. During the Loading stage, the depth linearly increased as the load progressively increased. The Relaxation stage was initiated once the maximum load was reached. During this stage a constant depth was maintained for 100 seconds by using the closed feedback loop depth control feature of the instrument and it was observed that the load decreased over time. The entire test concluded with an unloading stage in order to remove the indenter from the acrylic sample.

Additional indentation tests were conducted using the same indenter loading rates but excluding a relaxation (creep) period. Load vs. displacement plots were acquired from these tests and were combined in the graphs in Figure 3 for the acrylic and copper samples. As the indenter loading rate decreased from 10 to 1 µm/min, the load-displacement curve shifted progressively towards higher penetration depths for both Acrylic and Copper. Such a time-dependent increase in strain results from the viscoelastic creep effect of the materials. A lower loading rate allows a viscoelastic material to have more time to react to the external stress it experiences and to deform accordingly..

The evolution of load at a constant strain using different indentation loading rates were plotted in Figure 4 for both materials tested. The load decreased at a higher rate in the early stages of the relaxation stage (100 second hold period) of the tests and slowed down once the hold time reached ~50 seconds. Viscoelastic materials, such as polymers and metals, exhibit greater load loss rate when they are subjected to higher indentation loading rates. The load loss rate during relaxation increased from 51.5 to 103.2 mN for Acrylic, and from 15.0 to 27.4 mN for Copper, respectively, as the indentation loading rate increased from 1 to 10 µm/min, as summarized in Figure 5.

As mentioned In ASTM Standard E328ii, the major problem encountered in stress relaxation tests is an instrument’s inability of maintaining a constant strain/depth. The Nanovea Mechanical Tester provides excellent accurate stress relaxation measurements due to its ability to apply a closed feedback loop control of the depth between the fast acting piezo-electric actuator and the independent capacitor depth sensor. During the relaxation stage, the piezo-electric actuator adjusts the indenter to maintain its constant depth constraint in real-time while the change in load is measured and recorded by an independent high precision load sensor.

CONCLUSION

The stress relaxation of an acrylic and a copper sample were measured using the nanoindentation module of the Nanovea Mechanical Tester at different loading rates. A greater maximum depth is reached when indentations are performed at lower loading rates due to the creep effect of the material during loading. Both the acrylic and the copper sample exhibit stress relaxation behavior when the indenter position at a targeted maximum load is held constant. Larger changes in load loss during the relaxation stage were observed for the tests with higher indentation loading rates.

The stress relaxation test produced by the Nanovea Mechanical Tester showcase the instruments ability to quantify and reliably measure the time-dependent viscoelastic behavior of polymer and metal materials. It has an unmatched multi-function Nano and Micro modules on a single platform. Humidity and temperature control modules can be paired with these instruments for environmental testing capabilities applicable to a wide range of industries. Both the Nano and Micro modules include scratch testing, hardness testing, and wear testing modes, providing the widest and most user-friendly range of mechanical testing capabilities available on a single system.

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Controlled Humidity Nanoindentation of Polymer Films

The mechanical properties of polymer is modified as the environmental humidity elevates. Transient moisture effects, a.k.a. mechano-sorptive effects arises as the polymer absorbs high moisture content and experiences accelerated creep behavior. The higher creep compliance is a result of complex combined effects such as increased molecular mobility, sorption-induced physical aging and sorption-induced stress gradients.

Therefore, a reliable and quantitative test (Humidity Nanoindentation)of the sorption-induced influence on the mechanical behavior of polymeric materials at different moisture level is in need. The Nano module of the Nanovea Mechanical Tester applies the load by a high-precision piezo and directly measures the evolution of force and displacement. Uniform humidity is created surrounding the indentation tip and the sample surface by an isolation enclosure, which ensures measurement accuracy and minimizes the influence of drift caused by humidity gradient.

Controlled Humidity Nanoindentation of Polymer Films

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