Abstract
The mechanical properties and stress relaxation behavior of annealed aluminum-carbon nanotube composite were studied and compared with those of pure aluminum. The composite was prepared using an induction furnace, where 1.6 vol.% of multiwall carbon nanotubes were added in aluminum as strengthening material. It was found that the mechanical strength of the annealed composite was almost twice that of aluminum. The stress relaxation behavior of both materials was logarithmic in nature. However, the stress relaxation, hardening component, and intrinsic height of the thermally activated barrier were significantly influenced by the presence of nanotubes in the aluminum matrix. It was found that the stress relaxation rate of the composite was reduced (>30%) and the hardening component was increased (>100%) compared with that of aluminum. The calculated strengths of the thermally activated barriers for aluminum and the composite were 1.7 and 2.6 eV, respectively.
1 Introduction
In the class of contemporary metal matrix composites, the aluminum-carbon nanotube (Al-CNT) composite has many attractive properties, including high specific strength, low density, formability, excellent surface finish, and electrical conductivity [1, 2]. The Al-CNT composite is a potential candidate material for many applications from structural to electrical contact materials in the aerospace and automobile industries.
Stress relaxation is an intrinsic property of a material, in which the material decreases the applied load held at constant strain with the passage of time. The total strain remains constant; however, a fraction of the elastic strain transforms into plastic strain [3]. The stress relaxation characteristics of a material become vital when designing mechanical fasteners, riveted or bolted assemblies, shrink or press-fit components, solderless electrical connectors, etc. Moreover, stress relaxation data could be beneficial in predicting necessary heat treatment to relieve the residual stresses in castings, forgings, cold rolled, or welding assemblies [4].
Previously, many researchers investigated stress relaxation in pure metals, for example aluminum [5], copper [6], nickel [7], iron [8], etc. Their work encompassed primarily the development of stress relaxation mechanisms and models. Many works on the stress relaxation behavior of alloys are also available in compiled form [3, 9]. However, any significant work on metal matrix composites, especially on Al-CNT composites, could not be found in available literature resources. Therefore, the main objective of the present work was to investigate the stress relaxation behavior of the Al-CNT composite.
2 Materials and methods
High-purity aluminum (AA1199) was used for the matrix material. The chemical composition of the matrix material is given in Table 1. The multiwall carbon nanotubes (MWCNTs) used to fabricate the composite were synthesized using chemical vapor deposition [10]. The composite was fabricated using induction melting, having 1.6 vol.% MWCNTs. The detailed fabrication and characteristics of the composite are discussed elsewhere [11]. The composite was rolled down to 0.4-mm thin strips and annealed at 240°C for 30 min in an inert atmosphere. Pure aluminum specimens, having the same processing conditions, were also prepared for comparison and evaluation. For mechanical testing, specimens were machined according to ASTM E8 standard, using the electric discharge wire-cut method.
Chemical composition of pure aluminum grade AA1199.
| Elements | Al | Cu | Fe | Mg | Mn | Si | Zn | Others |
|---|---|---|---|---|---|---|---|---|
| AA1199 | >99.99 | <0.006 | <0.006 | <0.006 | <0.002 | <0.006 | <0.006 | <0.002 |
To evaluate mechanical properties, tensile tests were performed using an INSTRON universal testing machine (INSTRON, UK) at 0.02 s−1 and 25 mm strain rate and gauge length, respectively. To find the stress relaxation behavior, specimens were tested in accordance with ASTM E328-02 at a strain rate of 1×10−4 s−1. Stress relaxation data were acquired using a digital interface operating at 500 Hz. At a certain stress level (σo), the cross-head movement of the machine was arrested for a relaxation time of 300 s in each case. All tests were carried out at room temperature.
3 Results and discussion
3.1 Tensile test
The tensile curves of annealed specimens of pure aluminum and Al-CNT composite are given in Figure 1. The results of pure aluminum are comparable with the mechanical properties of standard AA1199-O4, with minor deviations. The deviations could be attributed to the processing conditions and/or purity level. To have a justified comparison, the processing conditions were kept the same for the fabrication of Al-CNT composites. In Al-CNT composite specimens, the yield and tensile strengths increased from 29 and 56 MPa to 97 and 109 MPa, respectively. However, a decrease in elongation from 22.6% to 7.4% was observed. It is believed that the amelioration of mechanical strength is a synergistic effect of the strengthening by the nanotubes, increased lattice strain, and refinement in crystallite size. Table 2 shows the results of tensile testing along with the percent change in various mechanical properties.

Superimposed tensile stress-strain curves of annealed aluminum and Al-CNT composite. Inset is an image of the finished tensile specimen used for the testing according to ASTM E8 specifications.
Results of mechanical testing.
| Specimens | Yield strength (MPa) | Tensile strength (MPa) | Elongation (%) |
|---|---|---|---|
| Aluminum | 29±6 | 56±5 | 22.6±1.4 |
| Al-CNT | 97±3 | 109±3 | 7.4±0.8 |
| Net change (%) | >230 | >90 | <65 |
The nanotubes affect the strengthening of metal-matrix-CNT composites by both of their elastic and plastic behaviors. Empirically, the Maxwell model could be used to explain the deformation behavior of the composite under unidirectional loading [12], as shown in Figure 2, where a linear spring element (representing elastic strains) and a linear viscous dashpot element (representing plastic strains) are connected in series. According to the model, the total strain (εt) in the composite will be the sum of the change in elastic (εe) and plastic (εp) strains:

Maxwell model showing a schematic of elastic and plastic behaviors.
In stage I (i.e. in the beginning of tensile curve, Figure 1), the matrix (aluminum) and strengthening material (MWCNTs) deform elastically, and it continues till the yield point of the matrix (i.e. 29 MPa). If the composite is unloaded at this stage, the elastic strain (εe) and plastic strain (εp) will be zero. Therefore
However, at stress levels above the yield point (>29 MPa), the matrix deforms plastically, whereas the nanotubes still deform elastically. This is stage II, and here the composite behaves in a quasi-elastic way; therefore, on unloading
The unloading affects the elastic retention of the CNTs and compression strains within the matrix. Stage II persists until the yield point of the composite, beyond which both aluminum and the nanotubes undergo plastic deformation. This is stage III, which features delamination of the Al-CNT interphase. Therefore, unloading of the composite will demonstrate permanent deformation attributed to plastic strains of the matrix (εpm) and the reinforcement (εpr)
Finally, at stage IV, crack initiation growth occurs, which continues until fracture [13].
3.2 Stress relaxation test
The experimental stress relaxation curves of both tested materials are presented in Figure 3. The inset of Figure 3 is a schematic of the curve’s segment where the cross-head movement of the testing machine was stopped and the applied stress was relaxed for a specific time period (i.e. 300 s). Point “A” represents the initial stress (σ˳) at t=0, point “B” represents the relaxed stress (σ) after t=300 s, and point “C” represents the instantaneous rise in the stress (σ′) after t=300 s when the cross-head movement is again started.

Experimental stress relaxation curves of aluminum and Al-CNT composite. Inset is the schematic of the curve segment during relaxation time.
3.2.1 Stress relaxation and hardening
According to Choudhry and Ashraf [14], stress relaxation Δσ(t) and hardening component Δσ′(t) can be determined using Eqs. (5) and (6), respectively:
The values of Δσ(t) and Δσ′(t) were calculated using experimental stress relaxation curves and plotted against corresponding stresses (σo) to find the trends of stress relaxation and hardening in both materials under investigation (Figure 4). The plots of both materials showed that the hardening component was initially more than stress relaxation; however, as the initial stress increased, a gradual decrease in hardening components occurred. A comparison of the stress relaxation and hardening component values of aluminum and Al-CNT composite is given in Table 3. It was observed that the composite exhibited lower values of stress relaxation and higher values of hardening component, as compared to aluminum.

Plots of stress relaxation Δσ=σo−σ(t), hardening component Δσ′=σ′(t)−σo, and their sum Δσ*=Δσ+Δσ′ manual="yes; between initial stress σo, for a relaxation time of 300 s.
Change in the rate of stress relaxation and hardening component of aluminum and Al-CNT composite.
| Aluminum | Al-CNT composite | Change (%) | |
|---|---|---|---|
| Stress relaxation | 0.13 | 0.09 | <30 |
| Hardening component | −0.05 | −0.02 | >50 |
In case of aluminum, the hardening component (Δσ′) could be attributed to the migration of point defects toward the core of edge dislocations and/or pinning [5]. However, the behavior of the composite was different. Under given strain conditions, dislocation loops were generated around the obstacles (i.e. the nanotubes). Continuing strain at point B (inset of Figure 3) resulted in dislocation multiplication and breakaway; hence, the dislocation density was increased and the hardening component emerged, as manifested by hardening at point C. The hardening component (Δσ′) increased with the strain to a certain tensile stress (σo); afterwards, it decreased and stress relaxation (Δσ) dominated, which was the limit of deformation hardening. The limit of deformation hardening indicated that the nanotubes were effective obstacles to the glide of dislocations until that strain level; afterward, at higher strain levels, dislocation-to-dislocation interaction increased and dominated the deformation mechanism [15, 16]. At low strain conditions, the stress relaxation and deformation hardening of the composite material were similar to aluminum in behavior, although the deformation hardening was twice as much that of aluminum. However, in higher stress conditions, the deformation hardening component decreased rapidly and diminished (Figure 4). This observation suggested that the strengthening in the composite was induced by deformation hardening (i.e. dislocation-to-dislocation interactions) at lower stresses; however, at higher stresses, the dislocation interaction-based hardening mechanism was replaced by strengthening induced by the interaction of the nanotubes itself with the matrix, which doubled the mechanical strength of the material. This phenomenon is known as the shear-lag model, where the load is transferred to the nanotubes from the matrix through interfacial shear stress. Hence, the stiffness of the nanotubes is directly involved in strengthening [17].
3.2.2 Thermally activated barrier
In a crystalline material, the flow stresses could be divided into two components: (i) long-range elastic interactions of the moving dislocations with the microstructure and (ii) the minimum stress required to overcome the opposing local energy barriers, which could be of various types, i.e. an intrinsic lattice resistance, small obstacles (precipitates), or unfavorable dislocation core.
The first component is elastic in nature and fades out as temperature increases; however, the second component dominates the high-temperature deformation behavior of the material. Short-range interaction of dislocations with energy barriers takes place in such a small volume that it is strongly influenced by thermal vibrations. Thermal activation helps dislocations to overcome these barriers, thus resulting in a reduction of stress as the temperature rises. These short-range thermally activated barriers govern almost all temperature-dependent mechanical properties of materials.
These processes are obviously of fundamental importance for the understanding and modeling of strength of structural materials. New materials have rather complex structures, in which dislocation mechanisms are more difficult to identify than in single-phase metals and alloys [18]. The strength of the barriers could be calculated using stress relaxation test data as shown below.
To calculate the strength of thermally activated barrier, graphs of stress relaxation (Δσ) vs. time were plotted at different stress levels (σo). A logarithmic scale was used to express the time axis, which helped reduce the skewness of the data (Figure 5). The slope of the each graph (S) represents the relaxation rate at a particular initial stress level (σo). Therefore, the graphs between initial stress (σo) and slope (S) were plotted, as shown in Figure 6. It is obvious in Figure 6 that the rate of stress relaxation is less in the Al-CNT composite than in aluminum, which suggests that the Al-CNT composite presents more resistance to relaxation in stressed condition than aluminum. Res et al. [19] proposed a single barrier model, where the height of the thermally activated barrier can be calculated using the relaxation rate (S) and initial stress level (σo), according to Eq. (7):

Graphs of stress relaxation data. Note that the time is plotted in logarithmic scale. The graphs have different initial stress (σo) values, which are written on the right margins of the graphs.

Rate of stress relaxation (S) as a function of initial tensile stress (σo) for aluminum and Al-CNT composite.
where Uo is intrinsic height of the thermally activated barrier, m is a constant (~25), K is Boltzmann constant (0.8617×10−4 eV K−1), and T is room temperature (298 K). The values of dσo/dS are calculated from Figure 6 (i.e. 46 and 102 s−1 for aluminum and the composite, respectively). The corresponding values of the strength of the thermally activated barriers for aluminum and the composite are 1.7 and 2.6 eV, respectively. Similar types of results were also deduced by Butt et al. [5] and Choudhry and Ashraf [14] for aluminum and AA7075, respectively, depicting the magnitude in order for processes like cross-slip, vacancy formation, and mutual inhalation of dislocations. The higher values of Uo in case of the composite can be attributed to the impeding of dislocation pile-ups due to fine grain size and the nanotubes, seizing the cross-slip phenomenon and increasing the dislocation density.
4 Conclusions
The mechanical strength of annealed Al-CNT composite was almost double that of annealed aluminum. During deformation in the tensile test, the behavior of the composite was quasi-elastic.
The stress relaxation behavior of both materials (i.e. annealed aluminum and Al-CNT composite) appeared to be logarithmic in nature.
The stress relaxation, hardening component, and intrinsic height of thermally activated barriers were significantly influenced by the presence of nanotubes in the aluminum matrix.
The stress relaxation rate of the composite was >30% less than that of aluminum, whereas the hardening component of the composite was twice more than that of aluminum. At low strains, the hardening component dominated stress relaxation.
The calculated strengths of the thermally activated barrier (Uo) for aluminum and the composite were 1.7 and 2.6 eV, respectively, which are of the order of magnitude for recovery processes. The Uo of the composite was comparable with that of the AA7075 alloy in the annealed condition.
References
[1] Pérez-Bustamante R, Gómez-Esparza CD, Estrada-Guel I, Miki-Yoshida M, Licea-Jiménez L, Pérez-García S, Martínez-Sánchez R. Mater. Sci. Eng. A. 2009, 502, 159–163.10.1016/j.msea.2008.10.047Search in Google Scholar
[2] Rashad RM, Awadallah OM, Wifi AS. J. Achieve. Mater. Manuf. Eng. 2013, 58, 74–80.Search in Google Scholar
[3] Manjoine MJ, Voorhees HR. Compilation of Stress-Relaxation Data for Engineering Alloys, 2nd ed. ASTM Data Series Publication DS 60: Philadelphia, 1982.10.1520/MNL11954DSearch in Google Scholar
[4] ASTM E238-02. American Standard Test Methods. ASTM International: West Conshohocken, PA, 2002, vol. 3.01, pp. 1–13.Search in Google Scholar
[5] Butt MZ, Zubair M, Haq IU. J. Mater. Sci. 2000, 5, 6139–6144.10.1023/A:1026752404893Search in Google Scholar
[6] Dineff P, Dikov V, Tzeneva R. Prz. Elektrotechn. 2013, 89, 242–246.Search in Google Scholar
[7] Trusov LI, Khvostantseva TP, Solov’ev Va, Mel’nikova Va. J. Mater. Sci. 1995, 30, 2956–2961.10.1007/BF00349669Search in Google Scholar
[8] Brunner D, Diehl J. Phys. Status Solidi 1987, 104, 145–155.10.1002/pssa.2211040110Search in Google Scholar
[9] Robey RF, Prangnell PB, Dif R. Mater. Forum 2004, 28, 132–138.10.3828/cfc.2004.28.1.009Search in Google Scholar
[10] Mansoor M, Shahid M, Habib A. Mater. Res. 2014, 17, 739–746.10.1590/S1516-14392014005000070Search in Google Scholar
[11] Mansoor M, Shahid M. J. Appl. Res. Technol. 2016, 14, 215–224.10.1016/j.jart.2016.05.002Search in Google Scholar
[12] Krapf NC. Stress Relaxation of Post-tensioned Stainless Steel Rods for Bridge Pier Cap Shear Strengthening. Georgia: Georgia Institute of Technology, 2010.Search in Google Scholar
[13] Dieter GE. Mechanical Metallurgy. McGraw-Hill: London, UK, 1988.Search in Google Scholar
[14] Choudhry MA, Ashraf M. J. Alloys Compd. 2007, 437, 113–116.10.1016/j.jallcom.2006.07.079Search in Google Scholar
[15] Kwon H, Park DH, Silvain JF, Kawasaki A, Hansang K, Dae HP, Jean FS, Akira K. Compos. Sci. Technol. 2010, 70, 546–550.10.1016/j.compscitech.2009.11.025Search in Google Scholar
[16] Tjong SC. Adv. Eng. Mater. 2007, 9, 639–652.10.1002/adem.200700106Search in Google Scholar
[17] Clyne TW. An Introduction to Metal Matrix Composites. Cambridge University Press: Cambridge, 1995.Search in Google Scholar
[18] Caillard D, Martin JL. Thermally Activated Mechanisms in Crystal Plasticity. Pergamon Materials Series: New York, 2003, vol. 8.Search in Google Scholar
[19] Res C, Butt MZ, Feltham P. Cryst. Res. Technol. 1984, 19, 325–329.10.1002/crat.2170190306Search in Google Scholar
©2018 Walter de Gruyter GmbH, Berlin/Boston
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.
Articles in the same Issue
- Frontmatter
- Review
- Progress in the research and applications of natural fiber-reinforced polymer matrix composites
- Original articles
- Damage assessment of random multiwalled carbon nanotube-reinforced polymer nanocomposites
- A variational approach for predicting initiation of matrix cracking and induced delamination in symmetric composite laminates under in-plane loading
- Processing-structure-property correlations of in situ Al/TiB2 composites processed by aluminothermic reduction process
- Interface transition layer interaction mechanism for ZTAP/HCCI composites
- Mechanical and electrical properties of polylactic acid/carbon nanotube composites by rolling process
- Development of hydroxyapatite-polylactic acid composite bone fixation plate
- Dielectric and thermal properties of magnesium oxide/poly(aryl ether ketone) nanocomposites
- A sustainable approach to optimum utilization of used foundry sand in concrete
- Improving flame-retardant, thermal, and mechanical properties of an epoxy using halogen-free fillers
- Optimization of the PDMS/biochar nanocomposite membranes using the response surface methodology
- Preparation and characterization of low-cost high-performance mullite-quartz ceramic proppants for coal bed methane wells
- Experimental investigation and analysis on the wear properties of glass fiber and CNT reinforced hybrid polymer composites
- Preparation of polyaniline-polyvinyl alcohol-silver nanocomposite and characterization of its mechanical and antibacterial properties
- An effective approach to synthesize carbon nanotube-reinforced Al matrix composite precursor
- Effect of oxygen plasma treatment on tensile strength of date palm fibers and their interfacial adhesion with epoxy matrix
- A novel characterization method of fiber reinforced polymers with clustered microstructures for time dependent mass transfer
- Stress relaxation behavior of annealed aluminum-carbon nanotube composite
- Restrained shrinkage cracking of self-consolidating concrete roads
- The effective ellipsoid: a method for calculating the permittivity of composites with multilayer ellipsoids
Articles in the same Issue
- Frontmatter
- Review
- Progress in the research and applications of natural fiber-reinforced polymer matrix composites
- Original articles
- Damage assessment of random multiwalled carbon nanotube-reinforced polymer nanocomposites
- A variational approach for predicting initiation of matrix cracking and induced delamination in symmetric composite laminates under in-plane loading
- Processing-structure-property correlations of in situ Al/TiB2 composites processed by aluminothermic reduction process
- Interface transition layer interaction mechanism for ZTAP/HCCI composites
- Mechanical and electrical properties of polylactic acid/carbon nanotube composites by rolling process
- Development of hydroxyapatite-polylactic acid composite bone fixation plate
- Dielectric and thermal properties of magnesium oxide/poly(aryl ether ketone) nanocomposites
- A sustainable approach to optimum utilization of used foundry sand in concrete
- Improving flame-retardant, thermal, and mechanical properties of an epoxy using halogen-free fillers
- Optimization of the PDMS/biochar nanocomposite membranes using the response surface methodology
- Preparation and characterization of low-cost high-performance mullite-quartz ceramic proppants for coal bed methane wells
- Experimental investigation and analysis on the wear properties of glass fiber and CNT reinforced hybrid polymer composites
- Preparation of polyaniline-polyvinyl alcohol-silver nanocomposite and characterization of its mechanical and antibacterial properties
- An effective approach to synthesize carbon nanotube-reinforced Al matrix composite precursor
- Effect of oxygen plasma treatment on tensile strength of date palm fibers and their interfacial adhesion with epoxy matrix
- A novel characterization method of fiber reinforced polymers with clustered microstructures for time dependent mass transfer
- Stress relaxation behavior of annealed aluminum-carbon nanotube composite
- Restrained shrinkage cracking of self-consolidating concrete roads
- The effective ellipsoid: a method for calculating the permittivity of composites with multilayer ellipsoids