Application Note | Fossil Mechanical Properties

Ammonite Fossil Mechanical Properties Using Nanoindentation

Non-Destructive Hardness and Modulus Mapping Across Light and Dark Areas of a Fossil Shell

Nanoindentation tip above an ammonite fossil

Research & Experimental Testing

Duanjie Li

Visual Design & Editorial

Andrew Shore

Introduction

As the remaining traces of plants, animals and other organisms that once lived on the ancient earth, fossils preserve information on the evolution of life. The oldest fossils can be traced back as far as the Archaean Eon, about 3.48 billion years old1, 2. Paleontology studies the formation mechanism and evolutionary relationships of fossils across geological time. The fossilization process includes several major mechanisms depending on the tissue type and external conditions, such as permineralization, casts and molds, authigenic mineralization, replacement and recrystallization.

Importance of Nanoindentation for Fossil Study

Fossils possess different mechanical properties determined by the stage and mechanism of the fossilization process. For instance, shells and bones can be replaced with different types of minerals when they are exposed to various environments. At different stages of the recrystallization process, the hardness of the fossil changes as well.

Nanoindentation precisely measures the mechanical behaviors of materials at small scales3, 4. The high-resolution load-displacement curves from the nanoindentation measurement can provide a variety of physico-mechanical properties, including hardness, Young’s modulus, creep, fracture toughness and many others. A mechanical property mapping of the fossil sample can play a key role in determining the mechanism and stages of the fossilization process. The small indentation force applied using the nanoindentation technique provides an ideal non-destructive mechanical testing solution to prevent damage to fossils under test.

Measurement Objective

In this application, the NANOVEA Mechanical Tester, in nanoindentation mode, is used to map the mechanical properties of different locations of an ammonite fossil sample. We would like to showcase the capacity of the NANOVEA Mechanical Tester in performing nanoindentation mapping on a fossil sample with high precision and reproducibility.

NANOVEA PB1000 Large Platform

Mechanical Tester

Nanoindenter and scratch tester platform NANOVEA PB1000 with nano and micro modules
Nanoindentation tip lowered onto a polished ammonite fossil
Fig. 1: Nanoindentation tip on the ammonite fossil sample.

Test Conditions

The Nano Module of the NANOVEA Mechanical Tester was applied to perform a series (3 × 3, spaced 0.08 mm apart, 9 indents in total) of nanoindentations on the top of an ammonite fossil sample using a Berkovich indenter. All indentations were performed to a maximum load of 50 mN. The distribution of the indentations is illustrated in Fig. 2 and the test conditions are summarized in Table 1.

Ammonite cross-section with two marked spots and micrographs of the 3 × 3 indent grids in the dark and light areas
Fig. 2: Location of indentations on the ammonite fossil sample.
ParameterValue
Maximum force (mN)50
Loading rate (mN/min)100
Unloading rate (mN/min)100
Creep (s)5
Indenter typeBerkovich

Table 1: Test conditions of the nanoindentation mapping.

Results and Discussion

The images of the 3 × 3 indentation matrix in the dark and light areas are displayed in Fig. 2. Two representative load-displacement curves of the indentations on the dark and light areas are shown in Fig. 3, and the corresponding hardness and Young’s modulus calculated using the Oliver and Pharr method5 are summarized and compared in Fig. 4. The light area possesses an average hardness of ~4.9 GPa and Young’s modulus of ~90.4 GPa, compared to ~4.1 GPa and ~87.2 GPa, respectively, for the dark area.

Load-displacement curves to 50 mN for the dark and light areas, the light area reaching a shallower depth
Fig. 3: Load-displacement curves of the indentations.
Bar chart of hardness and Young’s modulus for the dark and light areas with error bars
Fig. 4: Hardness and Young’s modulus at the dark and light areas of the fossil sample.

Such a 3 × 3 indentation matrix was carried out with superior accuracy and repeatability, thanks to the high-precision piezo load control and the direct load/displacement measurement by the NANOVEA Mechanical Tester. The excellent position control of the sample stage allows users to precisely pinpoint the target area for mechanical properties mapping. This makes mapping of the mechanical properties substantially less time-consuming and user friendly. It provides a solution for detecting different materials, phases and fossilization stages at different locations of the fossil sample.

We welcome further discussion and comments on the correlation of the hardness/Young’s modulus and the stage of fossilization and recrystallization, which will be a useful tool that provides insight into the mechanism of fossil formation and the fossil’s age.

Conclusion

In this study, we showcased the capacity of the NANOVEA Mechanical Tester in performing nanoindentation mapping on a fossil sample. The precise position control and accurate measurement of hardness and Young’s modulus enable identification of the mechanical properties of the materials at different locations on the fossil surface, which may be related to the stage of fossilization and recrystallization, as well as the fossil’s age. The tested ammonite fossil sample possesses varied hardness from 4.1 to 4.9 GPa at different locations.

The Nano, Micro or Macro modules of the NANOVEA Mechanical Tester 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. In addition, optional 3D non-contact profiler and AFM Module are available for high resolution 3D imaging of indentation, scratch and wear track in addition to other surface measurements such as roughness.

References

1. Noffke, N.; Christian, D.; Wacey, D.; Hazen, R. M., Astrobiology, 13 (12), pp. 1103–1124.
2. Borenstein, S., Oldest fossil found: Meet your microbial mom, Associated Press, 15 November 2013.
3. Oliver, W. C.; Pharr, G. M., Journal of Materials Research, Volume 19, Issue 1, January 2004, pp. 3–20.
4. Schuh, C. A., Materials Today, Volume 9, Issue 5, May 2006, pp. 32–40.
5. Oliver, W. C.; Pharr, G. M., Journal of Materials Research, Volume 7, Issue 6, June 1992, pp. 1564–1583.

Frequently Asked Questions About Fossil Nanoindentation

Why measure the mechanical properties of fossils?

Fossils take on different mechanical properties depending on the stage and mechanism of fossilization; shells and bones are replaced by different minerals, and hardness changes through recrystallization, so a property map can help identify the mechanism and stage.

Is nanoindentation destructive?

The small indentation force makes it an ideal non-destructive mechanical test that prevents damage to the fossil being tested.

How was the ammonite tested?

A 3 × 3 matrix of indents spaced 0.08 mm apart with a Berkovich indenter to 50 mN, on a dark and a light area of the fossil, analysed by the Oliver and Pharr method.

What did the light and dark areas show?

The light area averaged ~4.9 GPa hardness and ~90.4 GPa Young’s modulus, against ~4.1 GPa and ~87.2 GPa for the dark area.

How is the indentation location chosen?

Precise positioning of the sample stage lets the target area be pinpointed under the microscope, making property mapping faster and easier.

What else can nanoindentation measure?

The load-displacement curve also gives creep and, with suitable tests, fracture toughness, along with hardness and Young’s modulus.

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