Application Note | Biological Materials

Biological Mechanical Properties Study of Oyster Shell

Microindentation Hardness, Modulus and Coefficient of Friction of Two Shell Microstructures

Oyster shell under a micro indenter

Research & Experimental Testing

Frank Liu

Visual Design & Editorial

Andrew Shore

Introduction

As material science evolves, researchers have turned to biological materials for inspiration. The strong mechanical properties and unique structures of biological materials have been heavily researched in an attempt to replicate them. Desirable material properties, such as hardness and flexibility, can be traced to how micro/nano structures are naturally formed. To demonstrate a quantifiable way of collecting data on material properties on biological material, the NANOVEA Mechanical Tester’s Micro module is used to perform indentation and coefficient of friction (COF) tests on different microstructures of an oyster shell.

Importance of Mechanical Testing in Determining Hardness and COF of Biological Materials

The NANOVEA Mechanical Tester’s Micro Module is ideal for collecting local material properties on the surface of the sample. Insights on the relationships between microstructure and mechanical performance can be formed from the material properties each microstructure possesses. This can provide information on the multifunctionality of the biological material and its benefits for the organism’s survival in nature. These insights can also be used to help synthetically replicate biological materials.

Measurement Objective

In this application, the NANOVEA Mechanical Tester’s Micro module is used to measure the hardness (GPa), Young’s Modulus (E), and COF at different microstructures on the interior of an oyster shell. The different microstructures were observed and located under a microscope before indentation and COF testing was performed. The hardness, Young’s Modulus, and COF were compared between the two observable microstructures.

NANOVEA PB1000 Large Platform

Mechanical Tester

Nanoindenter and scratch tester platform NANOVEA PB1000 with nano and micro modules
Microscope view of the oyster shell interior with microstructure 1 and microstructure 2 marked
Fig. 1: The two microstructures on the interior of the oyster shell.

Microindentation

Test Conditions and Procedure

The following indentation parameters were used:

Test parameter (all tests)Value
Maximum force1 N
Loading rate4 N/min
Unloading rate4 N/min
Creep10 s
Computation methodASTM E2546 and Oliver & Pharr
Indenter typeVickers

Table 1: Indentation parameters.

Results

It should be noted that the layers beneath the microstructure can influence the hardness and Young’s modulus. As a result, the values observed should not be taken as an absolute value, but comparative amongst the other microstructures. From the data gathered, Microstructure #2 shows a higher hardness than microstructure #1.

While the standard deviation for hardness and Young’s modulus is large for microstructure #2, the average values between the two microstructures are distinctly different from each other.

TestHardness (Vickers)Hardness (MPa)Young’s modulus (MPa)Max depth (µm)
1186.51973157006.252
2182.91935154906.314
3176.31866153406.387
4193.52047146206.338
5190.82020150106.310
Average186.01968152306.320
Standard deviation6.8724200.049

Table 2: Microindentation results for microstructure #1.

Load versus depth indentation curve on microstructure 1
Fig. 2: Load vs depth curves for microstructure #1.
TestHardness (Vickers)Hardness (MPa)Young’s modulus (MPa)Max depth (µm)
174.70790.691849.041
273.91782.283359.269
377.03815.285849.101
468.63726.3108009.008
570.69748.1100408.985
Average72.99772.593899.081
Standard deviation3.3335.310270.114

Table 3: Microindentation results for microstructure #2.

Load versus depth indentation curve on microstructure 2
Fig. 3: Load vs depth curves for microstructure #2.

Conclusion: Microindentation

The NANOVEA Mechanical Tester’s Micro Module displays its ability to obtain hardness and Young’s modulus on two different microstructures of an oyster shell. The two microstructures have distinct hardness and Young’s modulus values, giving insight into the strength from the arrangement or composition of the microstructures themselves.

While only indentation tests were conducted in this study, these additional functionalities in the NANOVEA Mechanical Tester may prove useful for other biological materials: viscoelastic creep, Martens hardness, ultimate yield strength, multi-cycle test, and fracture toughness. High sensitivity, low load tests can also be conducted with the NANOVEA Mechanical Tester’s Nano Module.

Coefficient of Friction

Test Conditions and Procedure

Test parameter (all tests)Value
Load typeConstant
Applied load0.3 N
Scratch length1 mm
Scratching speed1 mm/min
Indenter geometryBall
Indenter material52100 steel
Ball diameter3 mm

Table 4: Scratch (COF) test parameters.

Results

A coefficient of friction test was conducted by running a linear constant load scratch test. When targeting COF properties, minimal damage and penetration to the sample is desired to minimize influence beyond the surface. As a result, a low load of 300mN and an indenter that will give a large contact area was used.

The results show microstructure #1 has a larger average COF than microstructure #2. Standard deviation for each microstructure is low, showing high consistency for the data collected.

TestMax COFMin COFAverage COF
10.24390.12540.1920
20.25580.12700.1971
30.27310.15230.2241
Average0.25760.13490.2044
Standard deviation0.01200.01230.0141

Table 5: COF results for microstructure #1.

Scratch test graph of normal force, friction coefficient and depth along the 1 mm scratch on microstructure 1
Fig. 4: Constant load scratch on microstructure #1.
TestMax COFMin COFAverage COF
10.19030.08060.1466
20.20280.11330.1492
30.20980.09480.1394
Average0.20100.09620.1451
Standard deviation0.00810.01340.0042

Table 6: COF results for microstructure #2.

Scratch test graph of normal force, friction coefficient and depth along the 1 mm scratch on microstructure 2
Fig. 5: Constant load scratch on microstructure #2.

Conclusion

The study on the COF of different microstructures yielded values of 0.2044 ± 0.0141 and 0.1451 ± 0.0042 for microstructure #1 and #2 respectively. From the tests conducted, the NANOVEA Mechanical Tester’s Micro Module has successfully characterized the COF on the two microstructures of the oyster shell.

In this study, the COF was gathered under normal, dry conditions. The NANOVEA Mechanical Tester can also include other add-ons to conduct testing under different environmental conditions, including lubrication, humidity, and temperature. These testing conditions can also be applied to indentation testing.

Frequently Asked Questions About Mechanical Testing of Biological Materials

Why test the mechanical properties of biological materials?

Biological materials have strong mechanical properties and unique structures that researchers try to replicate. Measuring local properties shows how each micro/nanostructure contributes to hardness and flexibility, informing synthetic replicas.

How were the oyster shell microstructures tested?

Two microstructures on the shell interior were located under a microscope, then indented with a Vickers tip to 1 N following ASTM E2546 and Oliver & Pharr, and scratched at a constant 0.3 N with a 3 mm steel ball to measure friction.

What hardness and modulus were measured?

Microstructure #1 averaged 1968 ± 72 MPa (186.0 HV) with a modulus of 15230 MPa; microstructure #2 averaged 772.5 ± 35.3 MPa (72.99 HV) with 9389 MPa.

Are the values absolute?

No. The layers beneath each microstructure can influence hardness and modulus, so the values should be compared between microstructures rather than taken as absolute.

How was friction measured without damaging the shell?

With a linear constant-load scratch at a low 300 mN and a large ball to minimize penetration. Microstructure #1 gave a COF of 0.2044 ± 0.0141 and microstructure #2 0.1451 ± 0.0042.

What else can be measured on biomaterials?

Viscoelastic creep, Martens hardness, ultimate yield strength, multi-cycle tests and fracture toughness, low-load tests with the Nano module, and tests under lubrication, humidity or temperature.

Characterizing Natural or Biomimetic Materials?