Investigation of Mechanical Properties of Granular γ-Alumina using Experimental Nano indentation and Nano scratch Tests

doi:10.21203/rs.3.rs-2633302/v1

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Investigation of Mechanical Properties of Granular γ-Alumina using Experimental Nano indentation and Nano scratch Tests

https://doi.org/10.21203/rs.3.rs-2633302/v1

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The mechanical properties of ceramic granular γ-alumina, including resistance and stability, were examined using Nano indentation and Nano scratch tests. In so doing, surface morphology, topography, and roughness of the surface of the granular ceramic were evaluated using a scanning electron microscope and atomic force microscopy. Moreover, the elasticity modulus and hardness of granular γ-alumina were estimated using a Nanoindentation method under different loads. It is showed the nanoparticles of this coarse material are about 17 nm on average. Besides, the results demonstrated that the modulus of elasticity and hardness did not follow a particular process when the load increased. In other words, these features increased or decreased within specific ranges. The modulus of elasticity and hardness of granular γ-alumina was obtained equal to 12.6 GPa and 0.433 GPa, respectively. The plasticity index of granular alumina was also examined, and the results showed that it was highly plastic with a plasticity index of 0.83. Nano scratch tests were performed under two different forces to obtain the scratch resistance of granular γ-alumina. The results revealed that the scratch resistance also surged by increasing the indenter force.

Granular alumina

Nano indentation

Nano scratch

Mechanical Properties

Atomic force microscopy

Alumina or aluminum oxide is used as an amorphous ceramic material in different industries, including the pharmaceutical industry, to produce dental implants and various types of composites. Due to the lower prices of alumina, in comparison to other nanotubes, it can be used in the fabrication of nanocomposite specimens [1]. In addition, alumina demonstrates its preferred mechanical and superficial properties, and it can be produced in the granular form at an industrial scale. Given the practical reasons mentioned above, it is necessary to create this ceramic granular material in the lab and study its mechanical properties.

Primarily, it is highly essential to understand that alumina is a porous material. Researchers use the scanning electron microscope (SEM) to examine the porosity and mechanical properties of materials [2, 3]. Atomic force microscopy (AFM) is used as a significant device to study the properties of materials at the nanoscale [4]. The mechanical behavior of the material, especially ceramic material, is essential for engineering applications. The mechanical properties of ceramic materials, which include hardness, elasticity modulus, stiffness, roughness, scratch resistance, friction coefficient, and pile-up, have been widely studied [5, 6]. In doing so, researchers have used Nano indentation [7–13] and Nano scratch tests [14–16].

Nanoindentation indicates the value of surface variation, and it was used as a standard and specific device for identifying the mechanical properties of ceramic materials, including the hardness and modulus of elasticity based on a small specimen. By obtaining the load-displacement curve, it is possible to determine the mechanical properties of a specimen. Every specimen has its universal figure of the load-displacement curve, and these differences between various materials usually indicate different mechanical properties. The scratch test was also used to study the resistance and tribological behavior of materials [17]. The scratch morphology on the surface presents a picture of the material's deformation mechanisms in the scratch test, including friction coefficient, scratch resistance, pile-up, and scratch hardness.

Shokrieh et al. [18] investigated the effect of graphene nanoparticles (GNPs) on the mechanical properties of polymeric nanocomposites by using nanoindentation and nano scratch tests. By implementing the indentation tests, both the elastic and hardness modules were amplified by adding 0.005 mass percent of GNP. Moreover, the scratch test revealed that the pile-ups decreased, and wear resistance increased. According to [18], the mechanical properties of pure polymer matrix upturns with the amplification of a small amount of GNP. Molazemhosseini et al. [19] carried out a study on the mechanical properties of hybrid composites based on Polyether ether ketone (PEEK) reinforced by short carbon fibers and SiO₂ nanoparticles using the Nano indentation and Nano scratch tests. The results represented a significant increase in the hardness and elastic modulus, which was due to the reinforcing agents.

Ahangari et al. [20] conducted a study on the effects of nanoparticles on the mechanical, superficial, and surface properties of Polyurea-Formaldehyde (PUF) composite microcapsules. The elastic modulus and hardness of microcapsules with and without roof wall reinforced carbon nanotube, and Nano alumina was studied using the nanoindentation. Additionally, the surface morphology, topography, and roughness were estimated using SEM, optical microscope (OM), and aFm. Ahangari and Fereidoon [21] studied the mechanical properties and morphology of self-healing Nanocomposite epoxy using healing micro-capsules and reported actual results. They investigated the mechanical properties of microcapsules using the nanoindentation test under three different loads before and after the healing and monitored the topography of the softened surface using AFM. They also showed the effects of healing using AFM after the scratch test on the composite surfaces. Using SEM, they characterized the microstructures of intact and healed composites using self-healings.

Yahyaei and Mohseni [22] achieved the mechanical properties of a sol-gel, which was prepared by nanocomposite films onto polycarbonate via the Nano scratch tests. Fereidoon et al. [23] described how the nanoindentation method was performed on the Nano scratch resistance of Polystyrene Polymethyl Methacrylate (PS/PMMA) in the presence of Multi-Walled Carbon Nanotubes (MWCNTs). Liu et al. [24] utilized AFM for estimating the scratch at the scale of nano and frictional behavior of Polycarbonate (PC). They performed a Nano scratch test under various normal loads by a probe with a tip radius of 20 nm. Furthermore, AFM was employed to display the surface morphology after scratching. The results of this paper can be used as a useful guide for understanding the mechanical mechanisms for Nano scratch polymeric materials; therefore, it can improve the scratch performance on nanoscale.

Moreover, many types of research have been carried out on the mechanical properties of various composite materials and ceramics and comparing them with a pure substance of the same type. Very little research has been conducted on the mechanical properties and surface morphology of a particular kind of material [25]. Besides, there is almost no research on the mechanical properties of alumina granules using Nano indentation and Nano scratch tests.

At first, granular γ-Alumina was prepared; then, SEM and FESEM were used to observe the morphology of the material in full detail and to find the size of pores and nanoparticles, which built the specimens. Experimental Nano indentation and Nano scratch tests were utilized under different normal loads to study the mechanical properties of the material. Moreover, surface topography was examined using AFM before and after the above criteria, and the correlations between the results of Nano indentation, Nano scratch, and AFM were studied in detail.

This section examines the required documents as well as the methods used for laboratory work.

2.1. Materials

Commercial gamma-alumina powder (PURALOX) was supplied by Sasol (Germany) with BET surface areas of 220 m2.g-1 and pore volume of 0.75 cm³.g^− 1.

2.2. Nanoindentation

Nanoindentation is a sensor that can be used for applications such as controlled load to the surface of a material to create a local superficial deformation. The general objective of the nanoindentation is to extract the elastic modulus and hardness of articles based on the determined load-displacement curves. This advanced characterizing technique has a normal workload range of about 1 µN to 500 MN, and its contact depth ranges from 1 nm to 20 µm [19]. During the test, the load and displacements were monitored continuously and recorded (Fig. 1). The maximum load (${\text{P}}_{\text{m}\text{a}\text{x}}$), the maximum depth (${\text{h}}_{\text{m}\text{a}\text{x}}$), contact depth (${\text{h}}_{\text{c}}$), and final depth (${\text{h}}_{\text{f}}$) are important factors that should be obtained from the load-displacement diagram [18]. The interactions between the indenter tip and sample during the process are shown in Fig. 2.

The reduced elastic modulus was premeditated using the Oliver and Pharr method [26]. The contact stiffness S, was introduced as the slope at the beginning of the unloading curve:

$$\text{S}=\frac{\text{d}\text{P}}{\text{d}\text{h}}$$

Where $\text{P}$ is the indentation load, and $\text{h}$ is the indentation depth for calculating the slope. The power-law sets the first part of the unloading curve:

$$\text{S}=\frac{2{\beta }}{\sqrt{{\pi }}}{\left(\frac{1}{{\text{E}}_{\text{r}}}\right)}^{-1}\sqrt{{\text{A}}_{\text{c}}}$$

Where ${\text{E}}_{\text{r}}$ is the reduced elastic modulus of the indentation surface of the indent contact, ${\text{A}}_{\text{c}}$ is the contact area of the indenter, and β is a constant for the indenter geometry. ${\text{E}}_{\text{r}}$ is related to the elastic modulus of the sample and the elastic modulus of the indenter is calculated by:

$$\frac{1}{{\text{E}}_{\text{r}}}=\frac{1-{{\nu }}^{2}}{\text{E}}+\frac{1-{{{\nu }}_{\text{i}}}^{2}}{{\text{E}}_{\text{i}}}$$

Where $\text{E}$ is the elastic modulus of the test sample, ${\text{E}}_{\text{i}}$ and ${{\nu }}_{\text{i}}$ are the elastic modulus, and Poisson’s ratio of the indenter and ${\nu }$ is the Poisson’s ratio of the test specimen. For the Berkovich indenter, ${\text{E}}_{\text{i}}$ and ${{\nu }}_{\text{i}}$ are 1140 GPa and 0.07, respectively [18]. As a result, the reduced elastic modulus${\text{E}}_{\text{r}}$, is defined as follows:

$${\text{E}}_{\text{r}}=\frac{\sqrt{{\pi }}}{2{\beta }}\frac{\text{S}}{\sqrt{{\text{A}}_{\text{c}}}}$$

If the indenter is highly stiffer than the probe’s substance, the hardness is calculated by:

$$\text{H}=\frac{{\text{P}}_{\text{m}\text{a}\text{x}}}{{\text{A}}_{\text{c}}}$$

Where ${\text{P}}_{\text{m}\text{a}\text{x}}$ is the achieved peak of the loading force. Furthermore, the plasticity index, ${\psi }$, is usually used for describing the elastic-plastic reaction of material under applied stress and strain. In the nanoindentation test, the plasticity index of the specimen was obtained as [21]:

$${\psi }=\frac{{\text{A}}_{1}-{\text{A}}_{2}}{{\text{A}}_{1}}$$

Where ${\text{A}}_{1}$ and ${\text{A}}_{2}$ denote the areas under the loading and unloading curves, respectively (Fig. 1). For more details, see [27].

Nanoindentation tests were performed using Triboscope® system that was armed with the Berkovich type indenter tip. The calibrated contact range function was derived from a nanoindentation test that has been previously performed on a fused quartz standard sample. A loading–unloading function with three various types of loads with maximum normal loads of 200 µN, 300 µN, and 400 µN was applied (Fig. 3). The full load was obtained in 5s, and then the load was removed. The retention time was about 5s. In each situation, three indentation tests were performed randomly to achieve reliable results. This system was accompanied by a Nano scope E type AFM digital apparatus, which was used to study the topography of the surface of the samples under indentation and scratch tests.

2.3. Nano scratch

The Nano scratch test was performed by moving the indenter tip, which is in contact with the sample surface. Moreover, two different normal loads of 300 µN and 400 µN were applied. The load function for the scratch test was schematically shown in Fig. 4. As the experiments were performed, the standard and tangential displacement of the indenter tip and regular and tangential loads were simultaneously recorded. In a Nano scratch test, the friction coefficient (${\mu }$) was determined from the fraction of the lateral load, ${\text{F}}_{\text{L}}$ (tangent force) to the average load, ${\text{F}}_{\text{N}}$. The surface topography of the sample after the nano scratch and nanoindentation tests could be directly determined using the AFM. Friction coefficient, µ, could be easily calculated following [18]:

$${\mu }=\frac{{\text{F}}_{\text{L}}}{{\text{F}}_{\text{N}}}$$

Moreover, the scratch hardness is a useful method for assessing the relative scratch resistance. The scratch hardness (${\text{H}}_{\text{s}}$) was defined by analyzing the indentation hardness. With regards to using the Berkovich indenter, the scratch hardness could be obtained as [18]:

$${\text{H}}_{\text{s}}=\frac{{\text{F}}_{\text{N}}}{\text{A}}=2.31\frac{{\text{F}}_{\text{N}}}{{\text{d}}^{2}}$$

where ${\text{F}}_{\text{N}}$ is the maximum applied average load on the indenter during the Nano scratch test, $\text{A}$ is the residual scratch groove area, and $\text{d}$ is the extra scratch width.

This section discusses and analyzes the effects of Nano indentation and Nano scratch tests.

3.1. Nanoindentation

SEM and FESEM were used to observe the surface of the particle and its properties. Figure 5 gives the topography of the surface of the produced granular alumina, its nanoparticles, and the holes on the covers. Figure 5(a) demonstrates the body of this article with a magnification of 37, and a diameter of 1.7 mm. FESEM images were taken with the embellishment of 1 µm and 200 nm (Figs. 5(b-d)) to see a better view of the surface of their holes. Additionally, Fig. 5(b and d) delineates the pores with diameters of 264.17 nm and 551.59 nm, which are abundant on the surface. Thus, this material contains porosity in the range of micrometers and even nanometers. Also, Fig. 5(c) shows the nanoparticles of this granular material, which is about 17 nm on average. It should be noted that the nanoparticles are firmly attached.

Figure 6 delineates the energy-dispersive X-ray spectroscopy analysis of this particle (EDX diagram), which was taken from the SEM test. This figure shows the volume of elements in the particle. As can be seen from the picture, this substance is almost pure and consists only of aluminum and oxygen elements, which form the parts of alumina. The other peaks in the figure represent the gold element, which is also visible in the EDX diagram as the material is gold-coated for the SEM test.

To find the roughness of the nanoscale granules of alumina, AFM was used to observe the surface morphology in a state where there was no indentation and no scratch on the material. The surface shown in the image is the surface of the produced specimen. Figure 7(a) demonstrates the morphology of the alumina surface. There are many ups and downs on the surface due to porosity. As seen in Fig. 7(b), the roughness of the material is about 31.524 nm on average, and as expected, granular nanoparticles of alumina have a high hardness. One reason for this is the porosity of the specimen.

As stated above, the mechanical properties of the nanoparticles were obtained from the load-displacement curves. Therefore, the nanoindentation testing was done to achieve these results. Figure 8 displays the nanoindentation test of alumina nanoparticles under three different normal loads of 200 µN, 300 µN, and 400 µN. Consistently, Fig. 8(b) illustrates the morphology of the surface of the alumina nanoparticle in the indentation area under 400 µN using an AFM. Figure 8(a) represents the load-displacement diagram for these three normal loads. Conducting these tests is hard, which is due to the excessive porosity of the material -i.e., there is no smooth and uniform surface. However, three different types of nanoindentation testing were conducted using each force to improve the chance of obtaining mechanical properties. The reason for the fact that under each power, the depth of penetration in the particle is very different at each indentation, and suddenly a significant change in intensity is observed is the nature of the sample that is very porous. The tip begins to indent and then encounters the porous space, and suddenly the underneath is emptied, followed by a notable change in the specimen. The lab results from support such behavior.

The load-displacement curve also demonstrates reduced elastic modulus. So that the slope of the curve in the unload region expresses the reduced elastic modulus. Consequently and having the reduced modulus of elasticity and modulus of elasticity of the indenter’s tip, the modulus of elasticity of alumina nanoparticles is obtained from Eq. (3). Figure 9(a) illustrates the reduced elastic modulus under three forces of 200 µN, 300 µN, and 400 µN for granules of alumina nanoparticles. The reduced elastic modulus does not follow a particular process with an increase in the force. That is, with the rise of the load, the reduced elastic modulus increases at first and then decreases. It should be noted that three types of indentation were conducted under all three different forces. The figure illustrates each of these indentations under each force with an error value of less than 5%. Moreover, the values of the modulus of elasticity do not differ significantly under all three forces. With an error value of less than 5%, this difference is within a specific range. Consequently, by taking the average value into account, the reduced elastic modulus is equal to 12.6 GPa. In other words, under these three different forces (200 µN, 300 µN, and 400 µN), the reduced elastic modulus of alumina nanoparticles reached 12.3 GPa, 12.9 GPa, and 12.6 GPa, respectively. In addition, this process is uncharacteristic due to the number of holes and pores of the produced material, which is justifiable. Meanwhile, to find the reduced elastic modulus, the hardness of the nanoparticles can also be calculated from the load-displacement curve. Figure 8 and Eq. (5) were used to obtain these results, and the obtained values were shown in Fig. 9(b). This shape is irregular, and as the force increases, the hardness decreases at first and then increases, which means that the mechanical properties of the material do not depend on the load. In other words, with an error approximation of about 16%, the hardness value for granules of alumina nanoparticles is 0.433 GPa. Moreover, the hardness under the forces 200 µN, 300 µN, and 400 µN are 0.43 GPa, 0.4 GPa, and 0.47 GPa, respectively.

Due to the reasons given above and to determine whether plastic or elastic deformations are more evident in the material under study, the plasticity index was obtained using Eq. (6) and Fig. 8, under three different forces of 200 µN, 300 µN, and 400 µN (Fig. 10). This figure shows that the plasticity index increases and then decreases with an increase in the force and does not follow the incremental and declining trend like the elastic modulus and hardness. It is also due to the number of holes and pores in the material. Moreover, as shown in the chart, the plasticity index has the same trend as the modulus of elasticity. The plasticity coefficients under these three different forces are equal to 0.8, 0.88, and 0.81, respectively, with an error of less than 10%. As a result, the magnitude of the plasticity index of the produced granular alumina nanoparticles is 0.83, which indicates that this material has a higher plasticity property than its elastic property. Therefore, this specimen is a relatively plastic material.

3.2. Nano scratch

The scratch process is the introduction of an indenter to the surface, which moves laterally. There have been many efforts to determine this trend in the past years. A Nano scratch test can present the qualitative assessment of the tribological specifications of the surface layer of the materials. This method was used by Hodzic et al. [27]. The Nano scratch test on the material surface was performed under two different normal loads. Then, surface morphology was characterized using the AFM to extract typical longitudinal and cross-sections profile. It was also used to obtain the groove and pile-up areas that were determined using the integration method. Many useful things can be observed from scratch tests in two different normal loads 300 µN and 400 µN, as it is seen in the following figures. However, none of the attempts achieved a scratch test at 200 µN, which is only due to the high porosity of the surface, which is not a smooth and uniform surface. Figure 11 represents the three-dimensional (3D) images of the surface morphology of two different normal loads. With the increase of the average load, the scratch grooves turn to be more visible. As seen in this figure, there are several ups and downs in the surface of specimens. Figure 12 delineates the typical longitudinal section profiles of these visible scratch grooves. It was demonstrated that the scratch depths increase from 300 µN to 400 µN.

Figure 13 demonstrates a specific cross-section profile of the scratch groove at the average loads of 300 µN and 400 µN. Pile-ups and scratch widths are critical factors that can be used for understanding the mechanisms related to nano scratch behavior. Clearly, as the scratch test proceeds, the scratch depth becomes more profound due to the average load increase. Also, the material pile-up exists on both sides and the two ends of the scratch. Pile-ups form and their height are identical to both parties. Furthermore, the scratch viewpoint shows the initial resistance. It is due to the light scatter from the surface. The scratch depth, scratch width, and pile-ups are considered as the signs of scratch resistance obtained from AFM images that are calculated according to Figs. 11 and 13. These parameters are listed in Table 1. As listed, with an increase in the average scratch load, the pile-ups of the scratch depth grow. Thereby, high plasticity could be observed, and many ripples on the surface of both sides and the pile-up height. Furthermore, we know that pile-up is due to plastic deformation; therefore, more pile-ups are related to more plastic deformation. Consequently, the scratch width increases. About the scratch width, it is notable that the specimens or forces with more plastic deformation (or more pile-up) have more scratched width. These results are consistent with the findings of Liu et al. [24] in various normal loads on polycarbonate (PC).

Table 1
Parameters deduced from a cross-section of the scratch test
Load	Scratch depth	Scratch width	Pile-up
300 µN	121.83 nm	1.160 µm	48.573 nm
400 µN	135.20 nm	1.328 µm	56.965 nm

Figure 14 illustrates the coefficient of friction on the surface of the produced granular alumina nanoparticles under 300 µN and 400 µN at the surface of the scratches. As shown, the friction coefficient grows with an increase in the force. More specifically, the point of the friction coefficient is the same as the scratch resistance under various effects, which increases with the induced effect. Clearly, by increasing the force, the tip of the indenter goes further inside the material, and the contact surface of the material improves. It improves the scratch resistance, so the coefficient of friction can also be enhanced. The precise numerical value of the friction coefficient was calculated from the diagram where the graph is almost flat or fluctuates within a given range. In other words, under 300 µN and 400 µN, coefficients of friction are equal to 0.72 and 0.9, respectively. Moreover, this excessive oscillation in the diagram happens due to the holes and pores of the material

Finally, Fig. 15 indicates the scratch hardness of the granular alumina nanoparticles compared with the average hardness of this material obtained from the nanoindentation test, under 300 µN and 400 µN. Typical and scratch hardness was defined based on the capacity of the material to resist deformation. However, there are several differences in the mechanism. Despite mainly dynamic scratch hardness, the typical indentation hardness is usually quasi-static. In the nanoindentation test, a stiff and rigid indenter penetrates the specimen surface and slides. Therefore, the frictional resistance between the indenter, the substance, and the side-force is inevitable. Such parameters are not seen in the nanoindentation test, which explains the difference between the average and scratch hardness. As shown in the figure, by increasing the reasonable force from 300 µN to 400 µN, both scratch hardness and typical hardness demonstrate the same rising trend so that the increase of typical hardness is more intense than the enhancement of the scratch hardness. It is also illustrated that the scratch hardness is always more than the typical hardness. It is because scratching hardness is a dynamic process and includes frictional forces. Thus, the indenter requires more load to defeat these obstructions. Therefore, the scratch hardness increases significantly more than typical hardness.

The granular γ-alumina ceramic nanoparticles were prepared. The nanoindentation and nano scratch tests were utilized for determining the mechanical properties. Furthermore, to obtain the topography and surface morphology, SEM, FESEM, and AFM were used. So the following results were obtained:

The SEM, FESEM, and AFM images were indicative of high material strength so that its roughness was significantly elevated and equal to 31.52 nm. Also, it is showed the nanoparticles of this granular material, which is about 17 nm on average. Plus, the nanoparticles are attached due to having muscular strength.
According to the load-displacement curves under three different loads of 200 µN, 300 µN, and 400 µN, none of the elastic modulus, hardness, and plasticity index followed a specific trend when the load increased. Still, their values remained at a particular range. Application of the interpolation, elastic modulus, hardness, and plasticity index was obtained equal to about 12.6 GPa, 0.433 GPa, and 0.83, respectively. These figures are indicative of a plastic material.
Using the scratch test under two different loads of 300 µN and 400 µN, it was clear that the scratch depth, scratch width, and pile-ups increased with loading. Moreover, with the increase of load, scratch resistance, which is a representative of the friction coefficient, increased from 0.72 to 0.9. Finally, the scratch hardness increased with the load, and it was higher than the indentation hardness.

Data Avalibility Statement

The datasets generated during and/or analysed during the current study are available from the corresponding author on reasonable request.

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No competing interests reported.

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Investigation of Mechanical Properties of Granular γ-Alumina using Experimental Nano indentation and Nano scratch Tests

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Abstract

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1. Introduction

2. Materials And Methods

2.1. Materials

2.2. Nanoindentation

2.3. Nano scratch

3. Result And Discussion

3.1. Nanoindentation

3.2. Nano scratch

4. Conclusion

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References

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