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Vol. 9. Issue 1.
Pages 404-412 (January - February 2020)
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Vol. 9. Issue 1.
Pages 404-412 (January - February 2020)
Original Article
DOI: 10.1016/j.jmrt.2019.10.069
Open Access
Enhanced tensile properties and corrosion resistance of stainless steel with copper-coated graphene fillers
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Zhiqiang Lia,b,d, Hongwei Nia,b,
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nihongwei@wust.edu.cn

Corresponding authors.
, Zhong Chend,
Corresponding author
ASZChen@ntu.edu.sg

Corresponding authors.
, Junjie Nid,e, Rongsheng Chenc, Xi’an Fana,b, Yang Lia,b, Yibo Yuana,b
a The State key Laboratory of Refractories and Metallurgy, Wuhan University of Science and Technology, Wuhan, China
b Key Laboratory for Ferrous Metallurgy and Resource Utilization of Ministry of Education, Wuhan University of Science and Technology, Wuhan, China
c School of Chemistry and Chemical Engineering, Wuhan University of Science and Technology, Wuhan, China
d School of Materials Science and Engineering, Nanyang Technological University, Singapore
e School of Materials Science and Engineering, Liaocheng University, Liaocheng, China
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Tables (4)
Table 1. Weight and volume percentages of Gr in Gr-Cu/SS composites.
Table 2. Mechanical properties of stainless steel and its composites.
Table 3. Corrosion resistance behavior of stainless steel composites.
Table 4. Comparison of tensile stress of PM 316L processed with various reinforcements.
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Abstract

Graphene (Gr) can significantly improve the mechanical properties of metal matrix materials. However, the reinforcing effect of Gr on stainless steel (SS) has rarely been investigated due to the difficulty in its uniform dispersion. In this study, 316L stainless steel was reinforced with copper-coated graphene (Gr-Cu/SS) through molecular level mixing, ball milling, and spark plasma sintering (SPS). The tensile strength and yield strength of Gr-Cu/SS have increased by 74.0% and 65.5%, respectively, with 0.2 wt% graphene added. The improvement on the tensile strength and yield strength of Gr-Cu/SS is attributed to the effective load transfer and the increase of relative density due to the addition of graphene. Moreover, the corrosion resistance of Gr-Cu/SS was improved, attributed to the low cathodic overvoltage of copper and the prevention of ionic transfer between stainless steel grains by graphene.

Keywords:
Graphene
Stainless steel
Powder metallurgy
Mechanical properties
Spark plasma sintering
Full Text
1Introduction

Stainless steel (SS) components have been routinely prepared by powder metallurgy (PM) because of its outstanding characteristics of near neat shape and high raw materials utilization [1–3]. However, the mechanical strength and the corrosion resistance of PM-SS was lower than that of wrought stainless steel. The weaknesses in mechanical strength and corrosion resistance of PM-SS were attributed to its lower relative density when prepared by the powder metallurgy process [4,5]. Previous research indicates that both the relative density and mechanical strength of PM-SS could be improved through adding metallic, intermetallic or ceramic additives [6–11], and coupled with compaction when necessary. For instance, the addition of 4wt% of copper has led to increase of the tensile and yield strengths of 316L stainless steel by 20.0% and 12.7%, respectively [4]. In another report, the yield strength of power sintered 316L SS increased from ∼250MPa to ∼350MPa with 6wt% addition of tin, and the variation in the yield strength with the amount of additives seems to be well correlated with the sintered density [6]. Farid et al. found that 316L stainless steel with the addition of 5.0wt% of MoS2 particles can significantly enhance the densification, hardness and ultimate tensile strength [11]. However, the mechanical properties of stainless steel prepared by powder metallurgy were still lower than those of the wrought counterpart, which has limited the scope of application of stainless steel prepared by powder metallurgy.

A further improvement of mechanical properties would enlarge the scope of PM-SS application. The further improvement would probably be achieved by adding a reinforcing additive with stronger mechanical properties. Among all kinds of additives, graphene exhibits great potential in enhancing the mechanical properties of metal matrix materials.

Graphene (Gr) is a new material with large specific surface area and very high mechanical strengths [12–16]. It has been applied as a reinforcing additive for improving the mechanical properties of metal matrix materials [16–20]. For instance, the addition of 8vol% Gr resulted in the significant increase in yield strength of copper by 114% [18]. However, limited attention has been paid on the reinforcement of PM-SS using Gr because of the difficulty in its homogeneous dispersion in the stainless steel particles due to the big difference in their densities. Moreover, Gr, as a carbon-based material, would react with stainless steel when they are sintered at high temperatures and under strong compacting pressure [21–24]. The reaction would reduce the reinforcing effect of Gr on the mechanical properties of PM-SS.

In this study, Gr was coated with a layer of copper with the purposes to increase its density and to prevent the reaction between Gr and 316L SS particles. 316L stainless steel reinforced with copper-coated graphene (Gr-Cu/SS) was prepared by mixing, ball milling and spark plasma sintering (SPS). The effect of Gr content on the mechanical properties and corrosion resistance of PM-SS was investigated. The method taken in this study could be extended to reinforcement of graphene to other metallic materials.

2Experiment2.1Preparation of Gr-Cu

The copper-coated graphene (Gr-Cu) was prepared by molecular mixing, as shown in Fig. 1. Firstly, graphene oxide (GO) nanosheets (45mg, Suzhou graphene nanotechnology company) were dispersed into deionized water (90ml) by ultrasonication to obtain an aqueous dispersion with a concentration of 0.5mg/ml. Cu(CH3COO)2·H2O (2.35g, Aladdin, analysis agent) was mixed with NH4OH·(100ml, Aladdin) to obtain a copper ammonia solution. The GO aqueous solution (0, 30 or 60ml, as listed in Table 1) and the copper ammonia solution were mixed and evaporated at around 100℃ to obtain a slurry mixture of copper-coated GO (GO-Cu). Then, the slurry mixture was dried and subsequently reduced in hydrogen atmosphere at 200°C for 2h to obtain the copper-coated graphene (Gr-Cu) additives.

Fig. 1.

Schematic of fabrication process of Gr-Cu/SS composites: (a) as-received GO nanosheet; (b) GO nanosheet-Cu; (c) as-received stainless steel powder; (d) Gr-Cu nanosheet; (e) Gr-Cu/SS mixed powder and (f) Gr-Cu/SS sample.

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Table 1.

Weight and volume percentages of Gr in Gr-Cu/SS composites.

Sample 
Name  SS  0.1 Gr-Cu/SS  0.2 Gr-Cu/SS 
Weight of SS, g  15  15  15 
Weight of graphene oxide, mg  15  30 
Concentration of GO solution, mg/ml  0.5  0.5 
Volume of GO solution, ml  30  60 
Weight percentage of Gr, wt%  0.1  0.2 
Volume percentage of Gr, vol%  0.35  0.70 
2.2SPS sintering of Gr-Cu/SS

The Gr-Cu/SS composites were prepared through ball milling and sintered by spark plasma sintering (SPS), as shown in Fig. 1(c–f). 316L SS powder (15g, with a mean size of 15μm), the Gr-Cu additives and milling ball (150g, stainless steel) were placed into a stainless steel pot and milled with a rotating speed of 200rpm for 2h. During the ball milling process, anhydrous ethyl alcohol (15ml) was added as a process control agent to avoid the oxidization of Gr. Finally, the mixed powder was sintered by SPS at 1000°C in argon atmosphere to obtain Gr–Cu/SS samples with the size 50×10×3mm (Fig. 1(f)). The heating rate and the holding time were 50°C/min and 10min, respectively. A uniaxial pressure of 50MPa was applied during the sintering process. The amount of Gr added was 0%, 0.1% and 0.2wt%, based on the total weight of Gr and the SS powder, and the sintered samples are denoted as SS, 0.1 Gr-Cu/SS and 0.2 Gr-Cu/SS. The small amount of Cu coating (as shown later) on the surface of Gr was ignored in the weight percent calculation.

2.3Characterizations

The morphologies of GO and Gr-Cu/SS powder were observed through a field emission scanning electron microscope (FESEM FEI Nova400) with an accelerating voltage of 20kV. Energy dispersive spectroscope (EDS IE350 Penta FETX-3) was used to verify the chemical composition. The variation of functional groups in GO, GO-Cu and Gr-Cu/SS was evaluated by Fourier Transform Infrared Spectroscopy (FT-IR VERTEX 70) and X-ray Photoelectron Spectroscopy (XPS PHI Quantera II). Archimedes’ principle was used to measure the relative densities of samples. The tensile test was carried out using an Instron-5569 mechanical tester with the crosshead speed of 0.5mm/min at room temperature. The sample for tensile test was machined as a dog-bone shape with a gage length of 20mm and a width of 4mm. The result of tensile test was an average of three samples for each sample condition. The fracture surfaces after the tensile test were also observed by the FESEM. In addition, the corrosion resistance was evaluated through Tafel plot using an electrochemical workstation with a scanning rate of 0.001V/s in H2SO4 (0.5wt%) solution. During the measurement of the Tafel curves, the sample was used as the working electrode, and a saturated calomel electrode and a platinum silk were used as the reference electrode and the counter electrode, respectively.

3Results and discussions3.1Morphology and chemical compositions

The morphology and the FT-IR specta of GO are shown in Fig. 2. The as-received GOs were transparent and wrinkled as shown in Fig. 2(a), which implies that they are few layers in the thickness. From the FT-IR analysis in Fig. 2(b), the characteristic peaks at 3423, 1712, 1628 and 1052cm−1 in FT-IR represents the stretching vibrations of OH, CC, C–OH and C–O-C functional groups, respectively [25]. These functional groups exist on the surface of GO. The functional groups not only can facilitate the homogeneous dispersion of GO in water, but also provide a number of active depositing positions for the copper ions [26].

Fig. 2.

(a) SEM image and (b) FT-IR of as-received GO.

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Copper ions in the copper ammonia solution were deposited on the surface of GO to generate the cooper coated GO (Cu-GO) particles during the mixing and evaporating process. Subsequently, the Cu-GO particles were reduced to copper coated graphene (Cu-Gr) during the reducing process. The morphology and chemical compositions of Cu-Gr were examined by SEM and EDS as shown in Fig. 3. It can be seen from Fig. 3 (a) that a number of nanoparticles were deposited on the surface of Gr. The EDS mapping in Fig. 3(b) revealed a good coverage of the Gr surface by copper. The composition can be estimated from the EDS results as shown in Fig. 3(c). The amount of copper was about 14.54 at% (47.35wt%) in the prepared Cr-Cu filler (ignoring O and Si).

Fig. 3.

(a) SEM image and (b) EDS mapping of Cu in Gr-Cu.(c) EDS composition of Gr-Cu.

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In order to investigate the chemical reaction between GO and copper ammonia solution during the evaporating and reducing process, the variation of functional groups in GO, GO-Cu and Gr-Cu/SS composite was analyzed by XPS, as shown in Fig. 4. The functional groups of sp2 CC, sp3 CC, C–O, CO and OCO could be characterized by the peaks at 284.7 eV, 285.9 eV, 286.7 eV, 287.9 eV and 288.8 eV in the C 1s XPS spectra [26]. It is worth mentioning that the peaks of C–O and CO functional groups of GO-Cu and Gr-Cu/SS have declined in comparison with those of GO, while no distinct change was found in the peaks of sp2 CC and sp3 CC functional groups. Specifically, the peak of C–O functional group in GO-Cu decreased significantly in comparison with that in GO, suggesting that the copper salt primarily reacted with the C–O functional groups of GO. Meanwhile, the slight decrease of CO peak in GO-Cu indicates that CO functional groups also took part in the reaction between GO and copper ammonia solution. Thereafter, the peaks of C–O and CO functional groups in Gr-Cu/SS further decreased, indicating that the GO-Cu was reduced. On the contrary, the structure of Gr remained stable as there was no distinct change in the peaks of sp2 CC and sp3 CC.

Fig. 4.

C 1s XPS spectra of (a) GO, (b) GO-Cu and (c) Gr-Cu/SS.

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The effectiveness of Gr reinforcement on the mechanical properties of SS is critically dependent on the distribution of the Gr-Cu particles in the SS matrix. The distribution of Gr-Cu among SS powder as well as on the surface of Gr-Cu/SS composite was examined through FESEM. As shown in Fig. 5, the surface of SS particles was smooth, while Gr-Cu nanosheets located at the intervals and adhered well to the surface of SS particles after the ball milling. Afterwards, mixed powders were sintered to produce bulk samples. A number of pores were observed on the surface of sintered SS without filler addition, suggesting that the SS powder could not be fully-densely sintered. By contrast, no visible pores were observed on the surface of Gr-Cu/SS composite. Moreover, the elemental analysis of point “A” in the matrix and the point “B” at the filler spot on the surface of Gr-Cu/SS composite confirms that these white spots are the Gr-SS fillers and they are uniformly dispersed in the matrix (Fig. 5e and f).

Fig. 5.

SEM images of (a) SS powder, (b) Gr-Cu/SS powder and surfaces of (c) SS without any filler, (d) Gr-Cu/SS sintered samples. EDS of (e) point A and (f) point B in Gr-Cu/SS sintered sample. Point A corresponds to the matrix, and point B corresponds to the Gr-Cu filler.

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3.2Mechanical properties of Gr-Cu/SS composites

To evaluate the reinforcing effect of Gr-Cu on SS, the relative density and tensile strength were measured at room temperature (Table 2). The relative density of Gr-Cu/SS composites increased from 91.9% to 98.5% with increased amount of Gr-Cu addition from 0wt% to 0.2wt%. The tensile stress-strain curves of SS and Gr-Cu/SS composite are shown in Fig. 6. The average tensile and yield strength of SS material were 315MPa and 275MPa, respectively. These mechanical properties were enhanced by the Gr-SS addition. The tensile and yield strength of Gr-Cu/SS composite were 548MPa and 455MPa, respectively with a 0.2wt% filler addition. Moreover, the ductility of Gr-Cu/SS composites was improved with increasing Gr-Cu addition.

Table 2.

Mechanical properties of stainless steel and its composites.

  Gr content wt% vol%Tensile strength, MPa  0.2% Yield strength, MPa  Relative density, % 
SS  315±275±91.9±0.2 
0.1 Gr-Cu/SS  0.1  0.35  428±370±96.5±0.1 
0.2 Gr-Cu/SS  0.2  0.70  548±455±98.5±0.2 
Fig. 6.

Tensile stress-strain curves of SS and Gr-Cu/SS composites.

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The fracture morphology of SS material and Gr-Cu/SS composites is shown in Fig. 7. The SS particles and voids between these particles are easily visible on the fractured SS without the additional of the Gr-Cu fillers. On the fractured surface of Gr-Cu/SS samples, however, the number of voids has clearly decreased, while the number of dimples increased significantly. The size of dimples decreased with increasing Gr-Cu filler content. The variation of fracture morphology supports the observed improvement in the tensile and ductile properties of Gr-Cu/SS samples. Moreover, it could be seen clearly from the enlarged view of the 0.2 Gr-Cu/SS sample that Gr sheet was pulled out at the edges of the dimples, as shown in Fig. 7(d).

Fig. 7.

SEM images of tensile fractured surface of (a) SS, (b) 0.1Gr-Cu/SS, (c) 0.2Gr-Cu/SS and (d) its magnified view.

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3.3Corrosion resistance test

The effect of Gr-Cu reinforcement on the corrosion resistance of 316L stainless steel was also evaluated through the Tafel plot, as shown in Fig. 8. Corrosion potential and corrosion current density are listed in Table 3.

Fig. 8.

Corrosion resistance of stainless steel composites reinforced with Gr-Cu filler.

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Table 3.

Corrosion resistance behavior of stainless steel composites.

  Corrosion potential, V  Corrosion current density, 10−5 A/cm2 
SS  −0.346  15.4 
0.1 Gr-Cu/SS  −0.326  4.44 
0.2 Gr-Cu/SS  −0.227  0.38 

The corrosion potential has shifted positively with the addition of the Gr-Cu fillers, which is an indication of improved corrosion resistance. Meanwhile, the corrosion current density has decreased by two orders of magnitude when 0.2wt% of Gr-Cu is added. The 0.2 Gr-Cu/SS exhibited the best corrosion resistance among all examined samples.

3.4Discussion

A comparison of reinforcing performance among the Gr-Cu composites in the present study and several other reinforcements (including tin, babbitt and hard particles) for improving the mechanical properties of 316L SS matrix composites is shown in Table 4. It is worth mentioning that a small addition of Gr has resulted in the greatest improvement in mechanical properties of 316L SS. To achieve effective enhancement in the tensile strength of powder sintered 316L SS, the early reports used a relatively large amount of metal or intermetallic fillers, ranging from 2 to 6wt%. In contrast, the present study finds that only adding a very small amount of Gr-Cu into SS is effective if achieving great improvement. The tensile and yield strengths of SS with the 0.2wt% Gr addition have reached 548MPa and 455MPa, which represent an increase of 13.5% and 164.5%, respectively, when compared with the wrought 316L stainless steel.

Table 4.

Comparison of tensile stress of PM 316L processed with various reinforcements.

Materials  UTS, MPa  YS, MPa  Reference 
Wrought 316483  172  [1] 
PM 316315  275  Present work 
PM 316335  –  [11] 
PM 316431  207  [1] 
PM 316L +4wt% tin  481  297  [6] 
PM 316L +6wt% tin  471  352  [6] 
PM 316L +6wt% babbitt  454  323  [6] 
PM 316L +3wt% AlCr2  350  –  [10] 
PM 316L +1.5wt% Cr2Ti  430  –  [10] 
PM 316L +1.5wt% SiC  375  –  [10] 
PM 316L +1.5wt% VC  390  –  [10] 
PM 316L +5wt% MoSi2  486  –  [11] 
PM 316L +0.2wt% Gr  548  455  Present work 

The significant improvement in mechanical properties of Gr-Cu/SS composites is attributed to the increase of relative density, the great stiffness and strength of graphene as well as the high efficiency of load transfers from stainless steel matrix to graphene. The relative density of Gr-Cu/SS composites (Table 2) increased with increasing Gr addition, this finding is consistent with early reports that the pores in sintered SS material were filled by the fillers. With reduced porosity, there are more boundaries between the fillers and the SS matrix, which is beneficial for load transfer [6,11]. The Cu coating on Gr surface has also ensured effective strengthening by Gr through improved filler dispersion and enhanced wettability between Gr and SS matrix [6,26,27]. Finally, the high specific surface area, high stiffness and great strength of Gr would prevent the rupture and shearing of composites [16,19]. The high specific surface provides a large interfacial region at the Gr/SS boundary, which is beneficial for the load transfer [19,27]. The Gr addition with high stiffness and great strength could be used to endure more load transferred from the SS matrix, ensuring the much improved mechanical properties in the Gr-Cu/SS composites [28].

Both the strength and ductility have increased with the increase of Gr-Cu filler in the current work, which is different from the previous research in which the ductility of the metal composites usually decreased with Gr filler addition [16,17,25,27]. The difference might be attributed to unique combination, in the current work, of the small amount of fillers and the significantly improved density (Table 2). From Table 4, the amount of fillers used in the current work is much smaller than other reports. This might have prevented the trade-off between strength and ductility due to the damage to the matrix, especially when the sample density has increased. In addition, the addition of metal element could improve the ductile of stainless steel. For instance, the addition of Sn not only improved the yield strength of 316L stainless steel, but also increased the elongation [29]. However, since the amount of Cu is very small in this work, addition of Cu is unlikely to be the main factor.

The improvement in the corrosion resistance of Gr-Cu/SS is attributed to the presence of copper and graphene, as well as the increased density. Firstly, copper is a heavy metal with a low cathodic overvoltage. It is beneficial for the corrosion resistance of Gr-Cu/SS sample by significantly reducing chromium nitride precipitation [30,31]. The passivation of Gr-Cu/SS composite and the cathodic reactions can be promoted by the addition of copper. Secondly, compared with the reference stainless steel, Gr-Cu/SS composites presented a sharp decrease in the anodic reaction rates, suggesting that the graphene has protected the underlying surface by slowing down the ionic transfer between the bulk solution and their reaction with the metal surface [32,33]. Last, the increase in relative density of Gr-Cu/SS composites also plays a role in hindering the electrochemical reaction.

4Conclusions

Stainless steel samples reinforced with copper-coated graphene (Gr-Cu/SS) particles were prepared by molecule mixing, ball milling and spark plasma sintering. After the mixing and ball milling processes, the Gr-Cu fillers were uniformly dispersed in the SS matrix. With only 0.2wt% Gr added, the tensile strength and yield strength of Gr-Cu/SS composite increased from 315MPa and 275MPa to 548MPa and 455MPa, respectively. The reinforcing effect of Gr on the mechanical properties of SS is attributed to the increase in relative density and high efficiency of load transfer. In addition, the corrosion resistance of Gr-Cu/SS was also improved. The Gr-Cu/SS with 0.2wt% Gr addition has let to a more positive corrosion potential at -0.227V and a two-orders of magnitude lower corrosion current density (3.8×10−6 A/cm2). The improvement in the corrosion resistance of Gr-Cu/SS is derived from the low cathodic overvoltage of copper and the low ionic transfer in SS. In summary, graphene exhibits a huge potential as reinforcement fillers to improve the mechanical properties and corrosion resistance of stainless steel prepared by powder metallurgy.

Conflicts of interest

The authors have no conflicts of interest to declare.

Acknowledgements

This work was supported by the National Natural Science Foundation of China (No. 51471122 and No. 51604202), the State Key Laboratory of Refractories and Metallurgy Foundation (No. 2016QN13), and China Postdoctoral Science Foundation (No. 2015M582284).

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