Effect of Sintering Temperature and Heating Rate on Crystallite Size, Densification Behaviour and Mechanical Properties of Al-MWCNT Nanocomposite Consolidated via Spark Plasma Sintering

doi:10.1007/s40195-018-0795-4

Abstract

Abstract:

Powder mixture of ball-milled aluminium and functionalized multi-walled carbon nanotubes was compacted via spark plasma sintering (SPS) to study effects of sintering temperature and heating rate. An increase in sintering temperature led to an increase in crystallite size and density, whereas an increase in heating rate exerted the opposite effect. The crystallite size and relative density increased by 85.0% and 14.3%, respectively, upon increasing the sintering temperature from 400 to 600 °C, whereas increasing the heating rate from 25 to 100 °C/min led to respective reduction by 30.0% of crystallite size and 1.8% of relative density. The total punch displacement during SPS for the nanocomposite sintered at 600 °C (1.96 mm) was much higher than that of the sample sintered at 400 °C (1.02 mm) confirming positive impact of high sintering temperature on densification behaviour. The maximum improvement in mechanical properties was exhibited by the nanocomposite sintered at 600 °C at a heating rate of 50 °C/min displaying microhardness of 81?±?3.6 VHN and elastic modulus of 89?±?5.3 GPa. The nanocomposites consolidated at 400 °C and 100 °C/min, in spite of having relatively smaller crystallite size, exhibited poor mechanical properties indicating the detrimental effect of porosity on the mechanical properties.

Key words: Al nanocomposite, Multi-walled carbon nanotubes, Ball milling, Spark plasma sintering, Densification behavior, Mechanical properties

Lavish Kumar Singh, Alok Bhadauria, Subhodeep Jana, Tapas Laha. Effect of Sintering Temperature and Heating Rate on Crystallite Size, Densification Behaviour and Mechanical Properties of Al-MWCNT Nanocomposite Consolidated via Spark Plasma Sintering[J]. Acta Metallurgica Sinica (English Letters), 2018, 31(10): 1019-1030.

Figures/Tables 12

Table 1 Sintering parameters (sintering temperature and heating rate) used by different researchers for consolidating Al-CNT nanocomposite via spark plasma sintering

Sintering temperature (°C)	Heating rate (°C/min)	References
600	40	[4]
500	-	[29]
350-550	100	[53]
600	50	[54]
480-600	40	[55]
580	100	[56]
600	40	[57]
580	50	[58]
600	40	[59]
600	-	[60]

Fig. 1 SEM images of starting materials: a as-received microcrystalline Al powders of 7-15 μm size; b as-received pristine MWCNTs of diameter 40-70 nm and length 0.2-0.5 μm

Fig. 2 Schematic diagram of experimental procedure followed in the present study to synthesize Al-0.5 wt% MWCNT nanocomposite

Table 2 Sintering parameters for consolidating Al-0.5 wt% MWCNT nanocomposites

Sample	Sintering temperature (°C)	Heating rate (°C/min)	Pressure (MPa)	Holding time (min)
ST400	400	50	80	20
ST500	500	50	80	20
ST600	600	50	80	20
HR25	500	25	80	20
HR100	500	100	80	20

Fig. 3 SEM images of a ball-milled Al powders, b physio-chemically functionalized MWCNTs, c TEM image of a MWCNT embedded in ball-milled Al powder particles

Fig. 4 a XRD patterns of spark plasma-sintered Al-0.5 wt% MWCNT nanocomposites consolidated at different sintering temperatures and heating rates, b TEM image of a MWCNT dispersed in Al matrix, c high-resolution TEM image showing clean interface between Al and MWCNT (ST400, ST500 and ST600 stand for samples sintered at 400, 500 and 600 °C with a hearting rate of 50 °C/min; HR25 and HR100 stand for samples sintered at 500 °C with hearting rates of 25 and 100 °C/min, respectively)

Table 3 Crystallite size, relative density, average pore diameter, number of pores and total punch displacement of synthesized Al-0.5 wt% MWCNT nanocomposites

Nanocomposite	Crystallite size (nm)	Relative density (%)	Average pore diameter (μm)	Number of pores	Total punch displacement (mm)
ST400	53	86.3	87	1885	1.02
ST500	62	95.1	46	357	1.36
ST600	98	98.7	17	24	1.96
HR25	83	96.0	39	290	1.46
HR100	58	94.3	61	623	1.33

Fig. 5 SEM micrographs showing presence of significant amount of porosities and interparticle boundaries at low a and high b magnification in sample sintered at 400 °C and heating rate 50 °C/min, homogeneous consolidation in sample sintered at 600 °C and heating rate 50 °C/min c, relatively homogeneous consolidation with the presence of small amount of porosities in the sample sintered at 500 °C at a heating rate of 100 °C/min d

Fig. 6 Top a-c, front d-f and side g-i views of a slice from Al-MWCNT nanocomposites sintered at sintering temperatures of 400 °C a, d, g, 500 °C b, e, h, 600 °C c, f, i, respectively (Dark blue colour represents porosity volume of ~?0-0.05 μm3, sky blue colour represents porosity volume of ~?0.05-0.15 μm3, and green colour represents porosity volume of ~?0.15-0.3 μm3). (Color figure online)

Fig. 7 Variation of punch movement within die with respect to sintering temperature while carrying out spark plasma sintering of Al-MWCNT powder mixture: a displacement versus sintering temperature; b displacement rate versus sintering temperature

Fig. 8 a Vickers microhardness values of synthesized nanocomposites and SEM micrographs showing microhardness indent marks on samples sintered at b 400 °C, c 500 °C, d 600 °C at heating rate of 50 °C/min

Fig. 9 a Load-displacement curves, b elastic modulus, c nanohardness values of Al-0.5 wt% MWCNT nanocomposites obtained from nanoindentation experiment under a peak load of 2000 μN

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