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Synthesis and mechanical behaviour of green metal matrix composites using waste eggshells as reinforcement material

  • Shashi Prakash Dwivedi

    Shashi Prakash Dwivedi is pursuing his PhD at Gautam Buddha University, Greater Noida, and working as an Assistant Professor in Noida Institute of Engineering and Technology, Greater Noida. He has published 23 research papers in international and national journals and conferences.

     EMAIL logo     , Satpal Sharma

    Satpal Sharma is currently working as an Assistant Professor in Gautam Buddha University, Greater Noida. He has published 70 research papers in international and national journals and conferences.

         and Raghvendra Kumar Mishra

    Raghvendra Kumar Mishra is currently working as an Assistant Professor in Gautam Buddha University, Greater Noida. He has published 70 research papers in international and national journals and conferences.
Published/Copyright: May 9, 2016
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Green Processing and Synthesis
From the journal Green Processing and Synthesis Volume 5 Issue 3

Abstract

Chicken eggshell (ES) is an aviculture by-product that has been listed worldwide as one of the worst environmental problems. The effective utilisation of ES biowaste is strongly encouraged in our society due to environmental and economic reasons. The aluminium alloy (AA) 2014/5 wt% carbonised ES metal matrix composite used in this study was fabricated by electromagnetic stir casting technique at parameters of 12 A (current), 180 s (time) and 700°C (matrix pouring temperature), respectively, and immediately extruded on universal testing machine at 60 MPa using cylindrical H13 tool steel die coated with graphite to avoid upper flow of ES particles and to improve wettability of carbonised ES with AA2014 alloy. Microstructures of composites show uniform distribution of carbonised ES particles. Density and overall cost of the metal matrix composite decreases 3.57% and 5%, respectively, when carbonised ES particulate is added 5% by weight. Tensile strength, hardness, toughness and fatigue strength of AA2014/5 wt% carbonized eggshell composite were also measured. Results show an improvement in these mechanical properties with addition of ES in the matrix alloy.

Keywords: aviculture by-product; density; eggshells; hazardous; mechanical properties

1 Introduction

The ever-increasing demand for low-cost reinforcement encouraged interest towards production and utilisation of using by-products from industry as reinforcement since they are readily available or are naturally renewable at affordable cost. Many researchers have used clay, fly-ash, rice husk ash and red mud etc. as a reinforcement in aluminium matrix; they all reported good dispersion and recovery of the particles in the composite castings [1–4].

Chicken eggshell (ES) waste is an industrial by-product, and its disposal constitutes a serious environmental hazard. Chicken ES can be used in commercial products to produce new materials, and it has been highlighted in recent investigation because of its renovation prospective. Even though there have been several attempts to use chicken ES components for a variety of applications, its chemical composition and accessibility makes chicken ES a probable source of biofiller-reinforced composites giving additional or improved thermal and mechanical properties. The other advantages of using chicken ES are that it is available in bulk quantity with lightweight and is economical and environmentally friendly. Investigation of various properties, like mechanical and physical, of aluminium metal matrix composites (MMC) reinforced by ES particulate is a remarkable area of research. These composites are mainly produced by various casting processes such as mechanical stir casting and electromagnetic stir casting [5, 6].

Hassan and Aigbodion [5] studied the effects of ES particles on the microstructures and properties of Al-Cu-Mg/ES particulate composites. These results showed that using the carbonised ES as reinforcement in the Al-Cu-Mg alloy gives better physical and mechanical properties as compared to uncarbonised ES particles. Mechanical results concluded that ES particles up to 12 wt% can be used to enhance the properties. Yew et al. [6] evaluated the effect of chicken ES as a biofiller on the adhesion strength and thermal stability of acrylic coatings. The improvement in the properties of the coating was attributed to the even distribution of ES particles and better ES/matrix interface. Toro et al. [7] used different proportions of chicken ES as biofiller in polypropylene composite with different particle sizes and proportions. The Young’s modulus (E) had been improved with the increment of ES content. Severa et al. [8] described the suitability and applicability of the nano-indentation method for the determination of the micromechanical properties of a hen’s ES. Chen et al. [9] made an investigation on solar photocatalytic activity of TiO2/ES, TiO2/Clamshell and TiO2/CaCO3. Lunge et al. [10] synthesised a new alumina-supported carbon composite material called “eggshell composite” (EC) from ES waste as calcium source for selective fluoride adsorption from water. EC proved to be a potential, indigenous and economic adsorbent for fluoride removal. Mosaddegh [11] prepared the nano ES powder by ultrasound irradiation and used it as a novel and biodegradable catalyst with high catalytic activity and reusability in green synthesis of 2-aminochromenes via condensation of α- or β-phathol, malononitrile and aromatic aldehydes at 120°C under solvent-free conditions. Bootklad and Kaewtatip [12] prepared thermoplastic starch using compression moulding and chicken ES. Mosaddegh and Hassankhan [13] developed an efficient and eco-friendly method for the synthesis of 7,8-dihydro-4H-chromen-5(6H)-ones by using ES as a natural and heterogeneous catalyst. Hassan et al. [14] developed a novel combination of mechanochemical and sonochemical to produce high surface area, bio-based calcium carbonate (CaCO3) nanoparticles from ESs. Mosaddegh and Hassankhan [15] developed a general and efficient catalytic system for Pd/C-catalyzed ligand-free aerobic suzuki cross-coupling reactions. M R Salleh et al. [16] prepared the ES by blending and sieving them into granule size of <160 μm. The ES filler had improved creep strain and creep modulus for the operating temperatures of 34°C and 80°C. Mosaddegh et al. [17] synthesised the ES-supported Cu(OH)2 nanoribbons as a novel and heterogeneous catalyst by simply adding an aqueous solution of CuSO4 on the ES support at ambient temperature. Mosaddegh and Hassankhan [18] synthesised the Ca2CuO3/CaCu2O3/CaO nanocomposite via coprecipitation and thermal decomposition methods using CuSO4 and ES wastes as inexpensive starting materials. Mosaddegh et al. [19] synthesised an ES/Fe3O4 nanocomposite using recycled ES biowaste as a starting material and an aqueous solution of FeSO4 as a coating agent without any additional alkali or a protective atmosphere.

From the literature, it was observed that very few researchers used chicken ES as reinforcement material to fabricate aluminium base green MMC. Some of the researchers fabricated MMC using ES by mechanical stir casting route. However, in mechanical stir casting process, when an external stirrer is used, higher porosity is observed due to low density of the ES. Very few researchers discussed the effective utilisation of hazardous reinforcement materials and fabrication of green MMC by electromagnetic stir casting process with low cost and density. For this reason, the aim of the present work is to examine the mechanical and physical properties of AA2014/ES particulate MMC by using electromagnetic stir casting process.

2 Materials and methods

2.1 Matrix material

Aluminium alloy AA2014 is a high-mechanical-strength alloy, which is used for various applications such as aircraft structures (wings and fuselages). AA2014 alloy is, furthermore, exploited in high-temperature applications, for example, in automobile engines and in other rotating and reciprocating parts such as brake-rotors, drive shafts, piston and other structural parts which require lightweight and high-strength materials [20]. The chemical and mechanical properties of AA2014 alloy are given in Tables 1 and 2, respectively.

Table 1:

Chemical composition of AA2014 alloy (wt%).

SiFeCuMnMgZnTiNiCrAl
0.5–0.90.53.9–5.00.4–1.20.2–0.80.250.20.10.1Balance
Table 2:

Measured properties of AA2014 alloy.

PropertiesValues
Melting point640°C
Density (g/cm3)2.8
Tensile strength (MPa)185
Hardness (BHN)60
Toughness (Joule)12
Ductility (percentage elongation)13
Fatigue strength (MPa) for 1×107 cycles90

2.2 Reinforcement material

Figure 1A shows the photograph of hen ES. Hen ESs unsurprisingly consist of ceramic materials. The chemical composition (by weight) of by-product ES has been reported as follows: calcium carbonate (94%), magnesium carbonate (1%), calcium phosphate (1%) and organic matter (4%) [10].

Figure 1: Photograph of (A) hen eggshells, (B) dried eggshells, (C) eggshell powder, and (D) carbonised eggshell powder.
Figure 1:

Photograph of (A) hen eggshells, (B) dried eggshells, (C) eggshell powder, and (D) carbonised eggshell powder.

The hen ES was cleaned and sun dried to eliminate the covering layer of ES as shown in Figure 1B. The dried ES was ball milled to obtain ES powder. It was then carbonised to 500°C for 3 h to remove the carbonaceous materials. The particle size examination of the ES particles was carried out; 25 μm particle size of ES powder was observed (Figure 1C and D). XRD pattern of carbonised ES powder was carried out to identify the composition of reinforcement particles. The XRD analysis of carbonised ES powder in Figure 2 confirms the presence of CaCO3 and Mg. The amount of CaCO3 is highest at about 94%, followed by little amount of Mg.

Figure 2: Typical XRD spectrum of carbonised eggshell powder consisting of about 94% CaCO3.
Figure 2:

Typical XRD spectrum of carbonised eggshell powder consisting of about 94% CaCO3.

2.3 Development of AA2014/ES particulate MMC

Figure 3 shows the schematic diagram of the electromagnetic stir casting setup to develop AA2014/5 wt% ES particulate MMC. Matrix material was heated above its liquidus temperature in muffle furnace. Carbonised ES particulate was also preheated about 500°C to avoid wettability problem. The liquid AA2014 aluminium alloy at temperature of 700°C was poured into a graphite crucible. A thermocouple was inserted in graphite crucible for temperature measurement of AA2014/5 wt% ES particulate MMC during stirring. The argon gas was used during the mixing of ES particulate in melt of AA2014 alloy.

Figure 3: Schematic diagram of electromagnetic stir casting setup [21].
Figure 3:

Schematic diagram of electromagnetic stir casting setup [21].

After the preparation of the AA2014/5 wt% carbonised ES slurry by the electromagnetic stir casting technique, the melt AA2014/ES was transferred to the cast iron chamber which was clamped with machine base of universal testing machine (UTM). The cylindrical die punch was used to apply high squeeze pressure to the melt. The pressure was applied in the mushy zone to eliminate the porosity and solidification shrinkage as shown in Figure 4. Cylindrical H13 tool steel die coated with graphite (avoid any type of chemical reactions with MMC) was attached with load cell on the moving cross head of UTM. Before attaching to UTM, the die was preheated to about 350°C. After the solidification, the prepared samples were removed from the crucible as shown in Figure 5. The upper and lower regions of each sample were removed. The samples for further study were selected from the middle regions of the AA2014 ES composites.

Figure 4: Schematic diagram of squeeze casting process on UTM.
Figure 4:

Schematic diagram of squeeze casting process on UTM.

Figure 5: Prepared MMCs.
Figure 5:

Prepared MMCs.

2.4 Sample preparation for microstructure and mechanical properties

The developed composites were characterised in terms of tensile strength, fatigue strength, hardness (10 mm×10 mm×25 mm) and toughness (10 mm×10 mm×55 mm with 45° V notch at centre of 2 mm depth). The sample sizes for tensile strength and fatigue strength shown in Figure 6A and B were prepared on CNC lathe machine as shown in Figure 7. Five samples as per specification were prepared for each test, and the average value has been reported [3].

Figure 6: Sample specification: (A) tensile sample and (B) fatigue sample [18].
Figure 6:

Sample specification: (A) tensile sample and (B) fatigue sample [18].

Figure 7: Sample preparation.
Figure 7:

Sample preparation.

Metallographic preparation of particle-reinforced MMC is quite a challenge, as the reinforcement carbonised ES particles have lower density. This combination of higher and lower density materials makes it difficult to avoid damages like cracks and broken reinforcement particles. The cast samples are cut in the transverse direction with the help of power hexa. The cut samples prepared above had an uneven surface. So the cut samples were then taken for grinding/polishing operation. The sample was first held over a grinding machine with a moving belt to obtain a smooth surface. The grinding was done in such a way so that all the scratches are in the same direction and the grinded surface becomes flat. After this the samples were polished properly using different grits of emery papers. The sample being aluminium alloy which is considered soft, it is rubbed over the emery paper for a short time. Then, it was rubbed over an emery paper of 400 grit and then over a very fine emery paper of 600 grit for a considerable time in order to get a smooth and clear surface of the samples. The sample was then polished on a fine polishing machine using alumina/diamond polishes. This was done to get a well-polished and a smooth surface required for the further characterisation of the samples. Similarly, all the samples were polished for a considerable time, over and over again until a very fine and smooth surface was obtained for further analysis. Polished unetched samples can show macroscopic cracks, pits, and so on, but no microstructural details because there is not yet any contrast-producing feature on the surface. These will be revealed by the etching process. Etching process was carried out in Kellers solutions (distilled water, nitric acid, hydrochloric acid, and hydrofluoric acid). Microstructure of AA2014/5 wt% green MMCs was measured using metallurgical microscope as shown in Figure 8.

Figure 8: Metallurgical microscope.
Figure 8:

Metallurgical microscope.

2.5 Mechanical properties testing machine

A tensometer for testing machine is used for tensile testing as shown in Figure 9A. It is used to test the tensile stress of AA2014/5 wt% carbonised ES composite. Hardness is a characteristic of a material, not a fundamental physical property. It is defined as resistance to indentation, and it is determined by measuring the permanent depth of the indentation. More simply put, when using a fixed force (load) and a given indenter, the smaller the indentation, the harder the material. Hardness of MMC is measured by hardness testing machine as shown in Figure 9B. Toughness is measured on impact testing machine as shown in Figure 9C. The Charpy impact test is also known as the Charpy V-notch test. It is a standardised high-strain-rate test which determines the amount of energy absorbed by a material during fracture. Fatigue strength is calculated on a fatigue testing machine (Figure 9D). Fatigue testing machines apply cyclic loads to test specimens. Fatigue testing is a dynamic testing mode and can be used to simulate how a material will behave under real-life loading conditions.

Figure 9: Mechanical properties testing machine; (A) tensometer for tensile testing, (B) hardness testing machine, (C) impact testing machine, and (D) fatigue testing machine.
Figure 9:

Mechanical properties testing machine; (A) tensometer for tensile testing, (B) hardness testing machine, (C) impact testing machine, and (D) fatigue testing machine.

3 Results and discussion

3.1 Microstructure analysis

Figure 10 displays optical micrographs taken at magnification of 500× from AA2014/5 wt% ES MMC. The microstructure analysis of AA2014/5 wt% ES MMC shows the presence of dispersed phase; i.e. carbonised ES particles are homogeneously distributed in the AA2014 matrix. The microstructure of AA2014/5 wt% carbonised ES particulate MMCs shows a good bond between AA2014 alloy and ES particles, and very low porosity was observed.

Figure 10: Microstructure of AA2014/5 wt% carbonised eggshell particles.
Figure 10:

Microstructure of AA2014/5 wt% carbonised eggshell particles.

3.2 Density analysis

For density analysis of AA2014 with 0% ES and with 5 wt% ES particulate MMCs, five samples of AA2014/5 wt% ES MMCs have been prepared, and results are shown in Table 3. In the present investigation, results show that the density of the samples of AA2014/5 wt% ES particulate MMCs is lower than the density of the samples of AA2014/0 wt% ES particulate MMCs. The densities of AA2014 alloy and ES particles were 2.80 and 2.47 g/cm3, respectively. After being carbonised, the density of ES particles was observed to be 2 g/cm3. The density of the MMC with 5 wt% ES particulate (average 2.70) was found to be about 3.57% lower than the AA2014. This shows that AA2014-based alloy composites can be made lighter using ES particles.

Table 3:

Observations of the density and mechanical properties of AA2014/5 wt% ES particulate MMC.

Sample numberDensity (g/cc)Tensile strength (MPa)Hardness (BHN)Toughness (Joule)Fatigue strength (MPa at 1×107 cycles)Ductility (percentage elongation)
12.72242.575111159
22.7023485101258
32.712568291059.5
42.692427689510.5
52.7025577109810
Average values2.70245.9799.6107.69.4

3.3 Analysis of mechanical properties

The results of hardness testing of composites are shown in Table 3. It was found that the average value of five samples of AA2014 matrix alloy and AA2014/5 wt% ES composite was 60 BHN and 79 BHN, respectively. It was reported by various previous researchers that the presence of Al2O3, CaCO3 and MnO2 phases increases the hardness of MMC.

The toughness and ductility of AA2014/5 wt% ES particulate composite is shown in Table 3. It was found that the value of toughness and ductility (percentage elongation) of the AA2014 alloy is 12 and 13 J, whereas the average value of toughness and ductility (percentage elongation) of AA2014/5 wt% ES composite is 9.6 and 9.4 J. By mixing the ES particles appropriately in AA2014 alloy, the toughness and ductility (percentage elongation) of AA2014/5 wt% ES composites was reduced by about 20% and 27.69%, respectively. The reduction in ductility and elongation may be due to the presence of hard Al2O3 and CaCO3 phases in the MMC.

In this study, it was observed that the experimental tensile strength of the AA2014/5 wt% ES particulate composites are higher than that of AA2014 alloy. It is noticeable that additions in the weight fraction of carbonised ES particles consequently enhance the tensile strength. The tensile strength of AA2014 alloy is 185 MPa, while the experimental tensile strength (average of five samples) of AA2014/5 wt% composite is 245.9 MPa. The fatigue strength of AA2014 alloy is 90 MPa at 1×107 cycles, while the average value of fatigue strength of AA2014/5 wt% ES composite is 107.6 MPa at 1×107 cycles. There is approximately 20% increase in fatigue strength of the composites. This improvement in fatigue strength may be due to surrounded hard phases like CaCO3, Al2O3 and MnO2 in the MMCs which act as obstacle that opposes the plastic deformation of composites when it is subjected to fatigue testing.

3.4 Cost estimation

The cost of AA2014 is about 300 INR, and as we know the ES particles are available as waste, so the ES particles are available free of cost. In the present investigation, 5 wt% ES carbonised particles were mixed with AA2014 alloy. The cost of AA2014/5 wt% ES composite is estimated to be 285 INR. The cost of MMC with 5 wt% ES particulate was found to be about 5% lower than the cost of AA2014.

4 Conclusions

Eggshell particles can be adapted favourably for the fabrication of green AA2014/5 wt% carbonised ES particulate MMCs as a reinforcement material. The microstructure of composites revealed good bonding between AA2014 alloy and ES particles, and very low porosity was observed. The density and cost of MMC with 5 wt% ES particulate was found to be 3.57% and 5%, respectively, lower than the matrix material (AA2014). Hardness, tensile strength and fatigue strength were improved 31.66%, 32.9% and 19.55%, respectively, by addition of 5 wt% carbonised ES particles in AA2014 alloy. While toughness and ductility were reduced about 20% and 27.69%, respectively.

About the authors

Shashi Prakash Dwivedi

Shashi Prakash Dwivedi is pursuing his PhD at Gautam Buddha University, Greater Noida, and working as an Assistant Professor in Noida Institute of Engineering and Technology, Greater Noida. He has published 23 research papers in international and national journals and conferences.

Satpal Sharma

Satpal Sharma is currently working as an Assistant Professor in Gautam Buddha University, Greater Noida. He has published 70 research papers in international and national journals and conferences.

Raghvendra Kumar Mishra

Raghvendra Kumar Mishra is currently working as an Assistant Professor in Gautam Buddha University, Greater Noida. He has published 70 research papers in international and national journals and conferences.

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Received: 2016-1-13
Accepted: 2016-2-23
Published Online: 2016-5-9
Published in Print: 2016-6-1

©2016 by De Gruyter

This article is distributed under the terms of the Creative Commons Attribution Non-Commercial License, which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.

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https://doi.org/10.1515/gps-2016-0006
Keywords for this article
aviculture by-product; density; eggshells; hazardous; mechanical properties
Creative Commons
BY-NC-ND 3.0

Articles in the same Issue

  1. Frontmatter
  2. In this issue
  3. Original articles
  4. Regioselective alkylation of 1,2,4-triazole using ionic liquids under microwave conditions
  5. A continuous flow process for the green and sustainable production of N-alkyl imidazoles
  6. Microwave-assisted one-pot syntheses of 4-aminoquinazolines
  7. Microwave assisted adsorption based elution: a benign green process optimized by Box-Behnken modeling yields pure vasicine from Adhatoda vasica
  8. Pretreatment of arsenic-bearing gold ore with microwave-assisted alkaline leaching
  9. Synthesis and mechanical behaviour of green metal matrix composites using waste eggshells as reinforcement material
  10. Efficient green synthesis of monomethine cyanines via grinding under solvent-free conditions
  11. Green chemistry preparation of MgO grit like nanostructures: efficient catalyst for the synthesis of 4H-pyrans and α,α′-bis(substituted-benzylidene) cycloalkanone derivatives
  12. An improved method for aldol condensation catalyses by Amberlyst A-26 OH: application in the synthesis of pseudoionone derivative, 11,15-dimethylhexadeca-8,10,14-trien-7-one
  13. Synthesis and characterization of amorphous Al2O3 and γ-Al2O3 by spray pyrolysis
  14. Synergetic surface modification effect of argon and oxygen for diamond films by MPCVD
  15. Optimization of process variables in the synthesis of butyl butyrate using amino acid-functionalized heteropolyacids as catalysts
  16. A new and facile method for the functionalization of a Merrifield resin with terpyridines: application as a heterogeneous catalyst for the synthesis of biaryls in environmentally friendly solvents
  17. Conference announcements
  18. International Conference on Green Chemistry and Sustainable Engineering (Rome, Italy, 20–22 July, 2016)
  19. International MicroNanoConference (Amsterdam, The Netherlands, December 13–14, 2016): where science and business discuss microfluidics, photonics and nanoinstrumentation
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