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Investigation of the mechanical properties of friction stir welded PA6-based

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Investigation of the mechanical properties of friction stir welded PA6-

based polymer nanocomposite and optimizing experimental conditions
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Page 1 of 31 AUTHOR SUBMITTED MANUSCRIPT - MRX-111398.R1

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Investigation of the mechanical properties of friction stir welded PA6-based

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6 polymer nanocomposite and optimizing experimental conditions
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9 Hossein Laieghi, Sina Alipour, Amir Mostafapour *

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11 Faculty of Mechanical Engineering, University of Tabriz, Tabriz, Iran
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Abstract:
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The newly fabricated two-phase composite of polyamide-6/nitrile butadiene rubber reinforced with
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19 halloysite nanotubes was welded by heat-assisted friction stir welding. The welding process was
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21 carried out via a heating system placed inside the stationary shoe-shoulder under different process
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conditions and materials to achieve sound joints. Influence of tool rotational speed, tool traverse

speed, and HNTs content as the three input parameters on mechanical properties has been

investigated using response surface methodology. Analysis of variance was utilized to establish the
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29 significance of independent variables on welding overall quality characteristics. The multi-response
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31 optimized variables were found to be as follows: rotational speed = 900 (RPM), traverse speed = 14
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33 (mm/min), and HNT = 6.72%. Under these conditions, the maximum values attained for tensile
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strength, Young’s modulus and impact strength were 59.1 (MPa), 1416.3 (MPa) and 124.1 (J/m),
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38 respectively. Optimal results have been validated through confirmation experiments. Morphological
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40 and microstructural characterization of the fractured surface of samples using scanning electron
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42 microscopes revealed that the increase of shear stress due to tool stirring action as well as the
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44 addition of halloysite nanotubes improves the interfacial interactions and produce fine rubber phase
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46 of PA6/NBR composites.
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49 Keywords: Friction stir welding; Polymer-matrix composite (PMCs); Mechanical properties;
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51 Microstructures; Statistical Methods; Optimization
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53 *Corresponding author.
54 E-mail addresses: a-mostafapur@tabrizu.ac.ir
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1. Introduction

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8 Thermoplastic elastomers are a plurality of copolymers, which consist of both
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10 thermoplastic and elastomeric properties. Polyamide-6 /nitrile butadiene rubber blends as
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12 an important class of thermoplastic elastomers with excellent mechanical properties could
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be used in different applications[1,2]. Introducing 1D natural nanomaterials into PA6/NBR
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17 blends increases its mechanical properties. For this purpose, HNTs are good candidates in
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19 comparison with carbon nanotubes (CNTs) from the aspect of economy and
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21 biocompatibility[3].
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The two-phase polymeric composite of PA6/NBR reinforced with HNTs is a new

engineering material; therefore, detecting proper method for joining this nanocomposite is
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29 required to fabricate larger and complex parts. Various methodologies have been utilized
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for the joining of polymeric composites including induction welding[4], resistance
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34 welding[5], ultrasonic welding[6], etc. Poor thermal conductivity and low melting
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36 temperature lead to dimensional changes of the composite parts that welded via mentioned
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38 processes. One of the welding methods that are free from these defects is friction stir
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41 welding which is mostly used for metals[7]. Friction stir welding due to its several
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43 advantages such as low temperature, process time, and costs as well as higher weld quality
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45 has found application in various industries. This technique involves a non-consumable
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rotating metal tool owning a shoulder and a pin, in which supplied frictional heat as a result
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50 of high rotational rate caused to softening the materials and providing material flow for mix
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52 and join them together. Compared to conventional welding methods, the FSW process
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avoids solidification problems like thermal residual stress, solidification cracking, porosity,
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and other defects related to fusion. Hence, defect-free welds with desirable mechanical

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7 properties have been made via this solid-state welding method.
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10 Since its development in 1991, FSW has spread out as a selective method in the common
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12 joining of aluminum components[8]. It is currently used on a wide range of materials,
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containing magnesium alloys[9], copper[10], steel[11], and metal matrix composites[12]. In
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17 recent years, friction stir welding of polymers and polymer matrix composites has attracted
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19 the attention of researchers. Elyasi et al.[13] studied the effect of process parameters on
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21 friction stir welding of PMMA T-joint. Welded samples showed excellent results with a
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smooth surface at specified rotation rates and traverse speeds. The tensile and flexural

strength of welded samples achieved about 84% and 93% of parent PMMA strength

respectively while the highest hardness reached up to 85.6 Shore D. Gao et al.[14]
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31 investigated dissimilar submerged FSW of high-density polyethylene (HDPE) and
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33 acrylonitrile butadiene styrene (ABS) sheets reinforced with multiwalled carbon nanotubes
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35 (MWCNTs). They showed that inappropriate processing parameters led to the formation of
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pores and cracks. The obtained maximum tensile strength for joints was more than 65.3 %
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40 of base material strength.
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43 During FSW of polymer matrix composites, mechanical properties of the joints are affected
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45 by process variables. Therefore, Optimization of process variables not only cause to
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increase the efficiency of the method but also improve the mechanical properties of the
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50 joint. Over the last years, response surface methodology which developed by Box and
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52 Wilson[15] in 1951, is used to modeling and optimizing the FSW process. In series of
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investigations have been conducted on modeling and optimization of the friction stir

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7 welding process for polymeric based materials, RSM has played an important role:
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10 Azarsa et al.[16] employed RSM as a statistical method for the prediction of the flexural
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12 behavior of friction stir welded high-density polyethylene sheets and showed a significant
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relationship between considered properties and processing parameters. Rahbarpour et
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17 al.[17] proposed an investigation of the feasibility and quality of friction stir welded wood–
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19 plastic composites. They studied the effect of input variable on the tensile strength of
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21 welded parts with the application of RSM method. It appears that the shoe temperature has
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played an important role to reach the maximum tensile strength. Mostafapour et al.[18]

joined Nylon 6 plates via a novel method of heat-assisted FSW by an external heat source.

They employed RSM based on Box–Behnken design to study the effects of various
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31 operating condition on the tensile strength of joints.
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34 The aim of the present study is attempted to join polyamide 6/NBR sheets via heat-assisted
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36 FSW at the presence of three different percentage of halloysite nanotubes. The effect of
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38 process parameters such as tool traverse and rotational speeds on mechanical properties of
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41 joints have been investigated by employ RSM in conjunction with Box–Behnken design.
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43 The other objective of this research was to figure out the effect of HNTs content on FSW
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45 characteristics. The multi-response optimization is also executed by desirability function.
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Finally, friction stir welded sample compared with based material (fabricated by twin-screw
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50 extruding) using microstructural observation.
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2. Experimental

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8 2.1. Material and Methods
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11 Polyamide 6 (KOPA, KN136) used in this experiments was purchased from KOLON
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13 Plastics, INC. (South Korea). The melt flow index and density of this material are 31.4 g/10
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15 min and 1.14 g/cm3, respectively. Ultrafine grade HNTs with a purity of 98.9% was
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18 supplied by Imerys Tableware Asia Limited, New Zealand. Nitrile butadiene rubber with
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20 the content of 34 wt% acrylonitrile and 0.98 g/cm3 specific gravity was purchased from
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22 KUMHO (South Korea). Mechanical properties of the base material are given in Table 1.
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28 sample Formulation
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Table 1 Mechanical properties of base material

Tensile strength Impact strength Young’s modulus

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(MPa) (j/m) (MPa)
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30 PA6/NBR 80/20 66.4 78.6 1106.2
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34 The blending of PA6/NBR/HNT nanocomposite was carried out in a Brabender co-rotating
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36 twin-screw extruder (ZSK, Germany) with a feeding rate of 0.5 kg/h, the screw speed of 80
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rpm and temperature profile of 195 - 230°C. PA6/NBR/HNT sheets used for the welding
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41 with 80mm × 40mm × 5 mm dimension were prepared using Collin P 200 E-type heat
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43 press. The configuration of the FSW tooling system used in this study illustrated in Fig. 1.
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Tool pin and the shoe material was made of AISI H13 (DIN 1.2344) Hot Worked Steel.
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48 The shoulder’s surface was coated with PTFE (Teflon).
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6 Pin
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8 Thrust bearing
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10 Brass ring
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Heater
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13 Stationary shoe
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Thermoset
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18 Fig. 1 Schematic and actual pictures of FSW tools
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20 2.2. Characterization
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In order to microstructural analyzes, the tensile fracture surface of samples was studied

using a Tescan MIRA3 FEG scanning electron microscope. Prior to taking SEM

micrographs, specimens etched by acetone at room temperature for 24 hours to extract the
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30 NBR domains, then coated with gold to increase their surface conductivity.
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33 The nanocomposite’s tensile properties were measured at across head speed of 5 mm/min
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36 according to ASTM D638, type V by GOTECH AI-7000 universal testing machine. Three
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38 samples were tested under the same conditions to ensure the reliability of test results.
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41 Notched Izod impact strength was reported using a SIT-20D Impact tester at room
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temperature based on ASTM D256 and an average of three measurements. Welded plates
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46 were cut into tensile and impact samples by the 120W KENIVERS® laser machine.
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49 2.3. Planning of experiments
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52 The FSW process was performed under different conditions of material and parameters. A
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been obtained as the following range: rotational speed (N) of 900, 1120 and 1400 rpm,

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7 Traverse speed (V) of 14, 28, 40 mm/min, and HNTs content (H) of 3, 5, 7 wt%. Shoe
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9 temperature set to a constant degree of 140 °C. Primary design of experiments (DOE) was

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11 done using a three-factor Box–Behnken design (BBD) to specify optimum conditions. The
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14 input parameters with three factors that each factor includes three levels determined by the
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16 Design Expert software (See Table 2). After selecting the parameters, FSW procedure was

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18 carried out through a vertical machine center and designed fixture as demonstrated in Fig.
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2.
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FSW process variables
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Table 2 Designed experiments and corresponding results

Mechanical properties
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TS Modulus Impact strength
29 N V H N/V
NO. (MPa) (MPa) (j/m)
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31 Rotational Tool traverse
HNT
32 speed speed Exp. Pred. Exp. Pred. Exp. Pred.
(wt.%)
33 (rpm) (mm/min)
34 N1 1120 40 3 28 36.5 36.4 1085.9 1077.3 117.5 121.4
35 N2 900 14 5 64 61 61.8 1327.2 1326.7 125.4 127.3
36 N3 900 40 5 22.5 46.7 46.3 1296.9 1309 76.3 79.2
37 N4 1120 40 7 28 50.1 51.2 1225.6 1223. 8 67.2 62.9
38 N5 900 28 7 32 56.4 55.6 1404.9 1395.6 67.5 69.4
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39 N6 1120 14 7 80 45.8 45.8 1271.2 1279.3 94.4 91.2

40 N7 900 28 3 32 48.7 49.1 1179.8 1177.5 138 131.4
41 N8 1400 28 7 50 47 46.6 1118 1121.1 36 41.8
42 N9 1400 14 5 100 31.9 32.3 1165.3 1155.4 42.6 40.2
43 N10 1400 40 5 35 50.6 49.9 1078 1076.2 70.9 68.5
44 N11 1120 14 3 80 41.1 39.9 1109 1111.3 118.3 122
45 N12 1400 28 3 50 31.5 32.3 1034.5 1043.1 67.9 67
46 N13 1120 28 5 40 52.4 52.8 1178.6 1165 55.6 51.7
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47 N14 1120 28 5 40 52.7 52.8 1165.1 1165 53.4 51.7

48 N15 1120 28 5 40 53.4 52.8 1151.3 1165 45.9 51.7
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18 Prepared sample for
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21 Fig. 2 FSW of PA6/NBR/HNT nanocomposite plates with fabricated fixture and tooling system
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2.4. Response surface methodology (RSM)
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RSM consists of mathematical and statistical analysis techniques that are useful for
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determining a relationship between independent quantitative variables and obtained
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31 responses. The main purpose of the method is to optimize the responses influenced by input
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33 variables[19]. In order to establish a functional relationship among the responses (Y) and
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input parameters; rotational speed (N), traverse speed (V), and HNTs content are
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38 considered as controllable variables. The response surface can be expressed as follows:
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41 (1) 𝑌 = 𝑓 (𝑁,𝑉,𝐻)
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44 The RSM-based second order polynomial (regression) model utilized to represent the
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46 response surface (Y) which is given by the following equation:
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49 𝑘 𝑘
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Where 𝑌 is the predicted response; ε the random experimental error; 𝛽0 a constant

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13 3. Results and discussion
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16 The common property of all polyamides is the absorption of water through the

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18 environment. The nanotubes diminish the water absorption speed with respect of barrier
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20 properties and compensate the modulus reduction of nanocomposite when moisture is
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absorbed by PA6. However, absorbed moisture at room temperature leads to the creation of

porosities in the PA6-based nanocomposites during the twin-screw extruding as shown in

Fig. 3 (a). Prior to the extrusion process of PA6 granules, these defects were eliminated by
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the use of an oven.
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33 (a) Porosities
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37 (b)
Lack of joining
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Tunnel defect
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43 AS
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48 Voids at the RS Surface lack of filling
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RS
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54 Fig. 3 Typical defects appeared at a) TSEd sample; b) cross section of FSWed sample; c) start and
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The similar defects may occur at the end point of the weld line because of inadequate

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11 retreating side (RS). The Fig. 3 (b) and (c) shows some defects in welded samples at a
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14 distance of 10 mm from the start and end points. Therefore, samples were not picked from
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19 After the welding procedure, various mechanical tests have been conducted to study the
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21 effect of input variables (see Fig. 4). The tensile tests results revealed that almost all
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samples were broken on the area of RS. Through the visual inspection of welded samples,

no macro-scale defects were detected on the surface of weld nuggets; however, the

microstructural image of RS shown in Fig. 5 (a) represented the tunnel defect in the weld
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31 nugget which significantly influences on mechanical properties of joints. As reported by
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33 Balos et al.[20], tunneling defect caused the reduction of mechanical properties by
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35 25%−82%. The formation of tunneling defects is occurred due to insufficient material flow
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from AS to RS. Table 2 shows the finalized mechanical properties of welded specimens in
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40 different conditions. It is observed that the mechanical properties begin to decline with the
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42 increase of rotational speed which might be taking place due to excessive stirring action
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44 resulted in overflowing of plasticized materials, this leads to the upward movement of
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materials and formation of micro-voids at the bottom side of weld nugget as shown in Fig.
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Fig. 4 Picture of samples after tensile and impact tests
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N900-V40

(b)
N1400-V14
AS an RS
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31 Micro voids
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35 Tunnel
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45 Fig. 5 SEM images showing micro defects in FSW along with high magnification
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3.1. Analysis of variance (ANOVA)
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50 ANOVA results for mechanical properties are shown in Table 3-5. In order to evaluate the
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52 significance of model, values for the sum of squares (SS), Degree of freedom (DoF), mean
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54 square (MS), P-value and F-value of each model terms are listed in the Tables.
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As it can be seen from Table 3, the Model F-value of 41.98 for tensile strength indicates

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7 that there is only a 0.04% chance that an F-value this large could occur due to noise. In this
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9 case, corresponding values of ‘P’ for A, B, C, AB, B2, C2 model terms are less than 0.05,

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11 implying that the model is significant. The P-value of 0.052 shows the insignificant extent
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14 for lack-of-fit, whereas we want the model to fit; non-significant lack-of-fit is good. The
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16 model precision determined by the R2. The calculated R2 of the model is 0.9869 as it is

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18 highly close to 1 which implied that the polynomial model was accurate. The Predicted R2
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of 0.7930 is in reasonable agreement with the adjusted R2 of 0.9634, which shows that the
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predicted and experimental values have a high correlation. The value of adequate precision

is 22.249, considering that value greater than 4 is desirable.

The applied same procedure to Young’s modulus is given in Table 4. The F-value (85.65)
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31 and correspondingly P-value (< 0.0001) represent the model is significant. Besides this,
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33 both calculated and adjusted R2 values for the model are above 98% and predict R2 value of
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35 0.9299 is very close to the adjusted R2 of 0.9820. These values demonstrate that the model
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is adequate. Signal to noise ratio is 31.429 that indicates sufficient signal.Table 5 presents
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40 that all input parameters are significant excluding two level interactions of traverse speed
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42 and HNTs content (BC) and the quadratic effect of rotational speed (A2). The R2 value for
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44 impact strength is 0.9854, which shows a desirable model. The Predicted R2 is in
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reasonable agreement with Adjusted R2.
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4 Table 3 ANOVA result for tensile strength

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Source SS DF MS F-value P-value Cont% Probe>F
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8 Model 1013.46 9 112.61 41.98 0.0004 significant
9 A-RPM 365.9 1 365.9 136.42 < 0.0001 35.62%

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10 B-Traverse speed 36.2 1 36.2 13.5 0.0144 3.52%
11 C-HNT 222.81 1 222.81 83.07 0.0003 21.69%
12 AB 265.28 1 265.28 98.9 0.0002 25.83%
13 AC 16.18 1 16.18 6.03 0.0575 1.57%
14 BC 0.005 1 0.005 0.025 0.9656 0.001%
15 A^2 1.14 1 1.14 0.43 0.5426 0.11%
16 B^2 53.09 1 53.09 19.79 0.0067 5.16%

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17 C^2 115.94 1 115.94 43.22 0.0012 11.28%
18 Lack of Fit 12.94 3 4.31 18.38 0.052 insignificant
19 Pure Error 0.47 2 0.23
20 Cor Total 1026.87 14
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Standard deviation
Mean
C.V. (%)
PRESS
1.64
47.06
3.48
212.06
R-Squared

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Adj R-Squared
Pred R Squared
Adeq Precision
0.9869
0.9634
0.7930
22.249
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31 Table 4 ANOVA result for Young's modulus
32
33 Source SS DF MS F-value P-value Cont% Probe>F
34 Model 145339 9 16155.26 85.65 < 0.0001 significant
35 A-RPM 81421.63 1 81421.63 431.68 < 0.0001 55.63%
36 B-Traverse speed 4659 1 4659.01 24.70 0.0042 3.18%
37
C-HNT 43745.26 1 43861.47 232.54 < 0.0001 29.89%
38
AB 951.67 1 951.67 5.05 0.0746 0.65%
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AC 4954.9 1 4947.82 26.23 0.0037 3.38%
41 BC 116.57 1 116.57 0.62 0.4674 0.08%
42 A^2 7041.56 1 7041.56 37.33 0.0017 4.81%
43 B^2 1251.18 1 1251.18 6.63 0.0497 0.85%
44 C^2 551.69 1 551.69 2.92 0.1479 0.37%
45 Lack of Fit 570.7 3 190.23 1.02 0.53 insignificant
46 Pure Error 372.39 2 186.19
Cor Total 146342 14
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49 Standard deviation 13.73 R-Squared 0.9936
50 Mean 1186.09 Adj R-Squared 0.9820
51 C.V. (%) 1.16 Pred R Squared 0.9299
52 PRESS 10261.52 Adeq Precision 31.429
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4 Table 5 ANOVA result for Impact strength

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Source SS DF MS F-value P-value Cont% Probe>F
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Model 14610.42 9 1623.38 37.48 < 0.0001 significant
9 A-RPM 4774.0 1 4774.04 110.23 < 0.0001 32.19%

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10 B-Traverse speed 194.8 1 194.83 4.50 0.0874 1.31%
11 C-HNT 3574.6 1 3574.62 82.54 < 0.0001 24. 1%
12 AB 1477.8 1 1477.84 34.12 0.0021 9.96%
13 AC 342.5 1 342.53 7.91 0.0374 2.30%
14 BC 190.9 1 190.88 4.41 0.0898 1.28%
15 A^2 1
106.9 106.91 2.47 0.1770
16 0.72%

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17 B^2 2137.7 1 2137.72 49.36 0.0009 14.41%
18 C^2 1958.8 1 1958.80 45.23 0.0011 13.21%
19 Lack of Fit 164.78 3 54.93 2.12 0.3362 insignificant
20 Pure Error 51.77 2 25.88
21 Cor Total 14826.96 14
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Standard deviation
Mean
C.V. (%)
PRESS
6.58
78.49
8.38
2771.6
R-Squared
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Adj R-Squared
Pred R Squared
Adeq Precision
0.9854
0.9591
0.8131
16.970
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30
31 From the analysis of data (Tables 3-5), standard Pareto charts (see Fig. 6) revealed for
32
33 factors ranking based on effectiveness or non-effectiveness. It was noticed that the
34
35
rotational speed (factor A) is the most efficient parameter compared to others. The
36
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38 contribution percentages of tool rotational speed for Young’s modulus and impact strength
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40 were 55.63% and 32.19% respectively, which followed by HNTs content of 29.89% and
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42 24.1%, respectively. The figure for tensile strength stood at 35.62% followed by the
43
44
45 combined two factors; rotational speed and traverse speed (factor AB) 25.83%. Factor AB
46
was slightly more effective than HNTs content.
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50 The mathematical models were established for mechanical properties with respect to input
51
52 parameters (in terms of coded units) using Design Expert 10 software (Version 10.0.7.0),
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55 and substituting the values in equations (3) - (5), respectively.
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(3) Tensile strength = 51.96 ― 6.77𝑁 + 2.13𝑉 + 5.3𝐻 ― 0.57𝑁2 ―3.82𝑉2 ―5.6𝐻2

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7 +8.1(𝑁 ∗ 𝑉) +2(𝑁 ∗ 𝐻) ―0.037(𝑉 ∗ 𝐻)
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9

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10 (4) Young’s Modulus = 1153.84 ― 101.03 𝑁 ― 24.22 𝑉 + 74.42 𝐻 + 44.46 𝑁2
11
12 +18.54 𝑉2 ―12.22 𝐻2 ―15.35(𝑁 ∗ 𝑉) ―35.04(𝑁 ∗ 𝐻) ―5.39(𝑉 ∗ 𝐻)
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(5) Impact strength = 49.10 ― 24.46𝑁 ― 4.95𝑉 ― 21.25𝐻 + 5.48𝑁2 +24.24𝑉2
16

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18 +23.03𝐻2 +19.12(𝑁 ∗ 𝑉) +9.22(𝑁 ∗ 𝐻) ―6.90(𝑉 ∗ 𝐻)
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55.63%
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35.62%

25.83%
21.69%

11.28%

5.16%
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29 1.57%
3.38% 3.18%

30 0.11%
0.85% 0.65%
0.37%
31 0.001%
0.08%

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35 32.19%

36 24.1%

37 14.41%
38 13.21%
9.96%
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41 2.30%
1.31% 1.28%
42 0.72%

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44
45
46 Fig. 6 Pareto charts, effectiveness of input parameters on: a) Tensile strength; b) Young’s modulus;
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c) Impact strength
48
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50 Fig. 7 displayed the predicted values of mechanical properties versus actual ones in the
51
52 variety of input parameters. The comparison results proved that predicted values of
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54 parameters are close to experimentally recorded data.
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Fig. 7 Plots of predicted response vs. actual value for: a) Tensile strength; b) Young’s modulus; c)
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31 Impact strength
32
33 3.2. Effect of input parameters on responses
34
35
36 3.2.1. Effect of independent parameters on responses
37
38
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39 During the FSW process, tool rotational speed and traverse speed (N and V) control the
40
41 amount of heat input in the stir zone which influences the mechanical and microstructure
42
43
44 properties. Low heat input leads to the smaller the crystallinity, but there must be sufficient
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46 to soften the materials and to avoids the formation of tunneling defect and voids that caused
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48 by decreased materials flow in the stir zone[21]. However, excessive heat generation
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51 attributed to molecular weight reduction and thermal degradation resulted in lower weld
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strength. The non-dimensional speed ratio by combining N and V can be used as a concise

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7 manner to represent the FSW process parameters, which is given in Eq. (6):
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9

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10 𝑁
(6) 𝑅=
11 𝑉
12
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14 Increasing speed ratio leads to higher frictional heat and easy material flow. As listed in
15
16 Table 2, to obtain acceptable mechanical properties, limited range of speed ratio determined

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18 for the mechanical properties (22.5<R<100) through the experimental works. For the speed
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21 ratios less than 22.5, PA6/NBR/HNT sheets have not welded due to insufficient heat
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PA6. an
transfer while the higher amounts of speed ratio limited due to the narrow melting range of

Fig. 8 illustrates the perturbation plots for responses of joints. This plot shows the
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alterations of responses while each parameter moves from the center point (set the coded
31
32
33 zero level for each parameter by software) in the design space. According to Fig. 8 and a
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35 sharp curvature in rotational speed (parameter A), the rotational speed had a significant
36
37 effect on responses compared to other variables. Tensile strength, Young’s modulus and
38
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40 impact strength of all samples decreased with an increase in the rotational speed, which is
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42 related to the burning of polymeric materials due to excessive generated heat[22,18].
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44 Increasing the rotational speed due to overheating causes turbulence in the nugget zone
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46
(NZ). Through this turbulence, the outpouring of material on the upward surface of the
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49 specimen formed as flash. Subsequently, weld nugget tends to the formation of the tunnel
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51 defect. Another reason for the reduction in mechanical properties was increased rotational
52
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speed resulted in excessive heat input generated which squeezed out the materials from the
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nugget zone and decreased the thickness of NZ. Introducing of HNTs into the two-phase

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7 PA6/NBR matrix improves the tensile properties meanwhile reduced impact strength. The
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9 enhanced tensile properties of FS welded nanocomposite samples ascribed to the higher

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11 amount and uniform dispersion of HNTs in the matrix and intercalated polymer chains
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13
14 within the halloysite nanotubes. More distribution of halloysite nanotubes within the matrix
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16 leads to much more decrease in impact strength, considering that higher rotational speed by

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18 increase of shear stress developed the dispersion in the processed zone. These results are
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21
corroborated by the morphological observations. As is evident from the figure, smaller the
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properties achieved at the middle level. an
traverse speed, better the obtained impact strength, while maximum values of tensile
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42 Fig. 8 Perturbation diagram of the process variable effects on the main responses
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44 3.2.2. Interactions effect of parameters on tensile strength
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46
The effects of different input variables on the responses, in the form of three-dimensional
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49 surface graphs and contour plots, are shown in Fig. 9-11.
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52 During FSW, tool rotational and traverse speeds have had a substantial influence on the
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55 thermal cycle and material flow of the polymer nanocomposite to obtain sound joint. Thus,
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the optimal combination of them has been concluded to achieve high-quality joint, so the

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7 low rotational speed combined with low traverse speed improved joint formation and
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9 decreased cooling rate. Fig. 9 (a) illustrates that with simultaneous reduction of rotational

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11 and traverse speeds, the tensile strength rises steadily in the FS welded samples from 30.1
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14 to 60.2 MPa. The interaction plots of Fig. 9 (b) displayed that the increase in factor C and a
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16 decrease of factor A at the same time leads to raising about 70% in tensile strength despite

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18 the considerable effect of rotational speed. It is noticeable that the effect of traverse speed
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without adding nanotubes is negligible [see Fig. 9 (c)].
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46 Fig. 9 Surface and contour plots showing the interaction effects of independent variables on the
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Tensile strength
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3.2.3. Interactions effect of parameters on Young’s modulus
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52
By keeping HNTs content at the center level, the mutual effect of rotation rate and traverse
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55 speed are demonstrated in Fig. 10 (a). Since rotational speed has the greatest effect on the
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modulus, increasing this parameter will reduce the amount of modulus at all values of

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7 traverse speeds. Fig. 10 (b) reveals that the maximum modulus (above 1350 MPa) obtained
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9 at HNTs content higher than 6% and a rotational speed of 900 rpm. Halloysite nanotubes

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11 reduce the size of rubber phase and causes a rougher fracture surface that leads to an
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14 increase in Young’s modulus as demonstrated by Paran et al.[23]. It can be observed in part
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16 (c) of this figure that the Young’s modulus tends to increase, with the decrease of term B

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18 and increase of term C simultaneously. The highest modulus obtained at less than 17
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mm/min traverse speeds and 7% HNTs, which is above 1250 MPa.
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47 Fig. 10 Surface and contour plots showing the interaction effects of independent variables Young’s
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modulus
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3.2.4. Interactions effect of parameters on impact strength

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8 As can be obtained from parts (a) and (b) of Fig. 11, interaction among terms A and B
9

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10 affects the impact strength mutually. Also, the rotational speed and HNTs content had a
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12 similar reversed effect on the impact strength. The amount of impact strength increased
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14
substantially from just under 40 j/m to around 130 j/m, a rise of about 225% in FS welded
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16

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17 samples obtained at HNTs of 3% and rotational speed of 900 rpm. Regarding the part (c)
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19 and Table 5, the interaction effect of traverse speed and HNTs content (BC) are not
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21 significant.
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48 Fig. 11 Surface and contour plots showing the interaction effects of independent variables Impact
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3.3. Optimization of parameters using desirability function methodology

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8 One of the main goals in this research was to maximize the response variables of FS welded
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10 PA6/NBR/HNT sheets and find the optimal values of input parameters. The determined
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12 criteria for the optimization of each factor and responses are summarized in Table 6.
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15 Table 6 Goals and factors ranges for multi-response optimization
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18 Name Goal Lower limit Upper limit Lower weight Upper weight importance
19 A:N is in range 900 1400 1 1 3
20 B:V is in range 14 40 1 1 3
21 C:H is in range 3 7 1 1 3
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Tensile strength
Young’s Modulus
Impact strength
maximize
maximize
maximize
31.5
1034.6
36.1
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1404.9
138.1
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42 Desirability = 0.932
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45 Fig. 12 Ramp function graph of combined optimization
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47 The combined optimization results and values of optimal input variables are presented in
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49 Fig. 12. Obtained results as follows:
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Optimum rotational speed (N) = 900 (rev/min).
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Optimum traverse speed (V) = 14 (mm/min).

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8 Optimum HNTs content (H) = 6.72%
9

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11 In addition, maximized responses predicted as follows:
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14 Tensile strength = 59.05 MPa; Young’s modulus = 1416.3 MPa; Impact strength = 124.1
15
16 (j/m).

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19 Fig. 13 shows the desirability of friction stir welding conditions and responses in the form
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22 of a bar graph. The desirability of parameters and responses together depicted by combined
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desirability = 0.93
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46 Fig. 13 Bar graph of desirability for combined optimization
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3.4. Confirmation tests
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The final step after evaluating the optimal parameter settings is checking the validity of
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54 proposed models by performing seven different experiments. The results obtained are
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shown in Table 7 and Fig. 14. Confirmation runs were conducted under random conditions

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7 that have not been used in the design matrix but are within the range of defined levels. The
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9 first confirmation test for each response includes an optimum level of parameters. Final

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11 empirical test including multi-response optimized parameters was performed and average
12
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14 error for responses 2.56% achieved. Good agreement has been observed between the actual
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16 and predicted results. The regression models [equations (3) – (5)] were reasonably accurate

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18 as all experimental results are within the confidence interval of the predicted values. FSW
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of the samples using optimal input parameters produced good quality and defect-free joint
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as presented in Fig. 15.

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Table 7 Confirmation experiments
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29 Process parameters Mechanical properties
30
Run Error%
31 N V H Actual Predicted
32 Tensile strength (MPa)
33
34 1 900 14 5.7% 60.6 61.5 1.42%
35 2 1120 28 3% 44.1 42.8 2.88%
36
37 Young’s modulus (MPa)
38 1 900 14 7% 1415.1 1429.4 1%
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39 2 1400 28 6% 1123.9 1110.8 1.18%

40
41 Impact strength (j/m)
42 1 900 14 3% 167.7 173.9 3.56%
43
2 1120 40 5% 72.3 69.1 4.71%
44
45 Multi-response optimization
46 Tensile strength 57.5 59.1
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47 Young’s modulus 900 14 6.7% 1387.1 1416.3 2.56%

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49 Impact strength 127.2 124.1
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22 Fig. 14 Verification results of the responses
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(a)
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34 (c) (d)
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43 Fig. 15 FSWed sample through optimum process parameters (N900, V14) and a) 3% HNTs content;
44 b) 5.7% HNTs content; c) 6.7% HNTs content; d) 7% HNTs content
45
46 In order to have a better resolution of obtained results, Fig. 16 shows SEM micrographs of
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48 the multi-response optimized joint in comparison with twin-screw extruded (base material)
49
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51 specimen. The tensile fracture surface of FS Welded sample illustrated a rougher surface,
52
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53 indicating ductile fracture behavior[24]. As can be seen in Fig. 16 (b) as dark holes, rubber
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droplets dispersed uniformly throughout the PA6 matrix due to the further mixing of NBR

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7 phase via FSW processing. The area distribution charts of rubber phase represent reduces in
8
9 the NBR droplets size from 1.11 µm to 0.899 µm by addition of HNTs content and

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11 performing of the welding process. NBR droplets size reduction attributed to rising in
12
13
14 viscosity of PA6 matrix and droplet shearing mechanism[25]. Addition of HNTs into PA6
15
16 matrix cause to increase the viscosity of PA6 phase, which leads to decrease of NBR/PA6

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18 viscosity ratio, on the other hand, the rise in the shear stress occurs as a result of rotational
19
20
21
movement[26]. Higher mechanical properties of PA6/NBR composite joint could be
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parameters. an
achieved in the presence of HNTs as reinforcement and setting proper FSW process
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Fig. 16 SEM fractographs of tensile testing; a) base material; b) FSWed sample
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According to Fig. 17, the elemental analysis of multi-response optimized joint and 5 wt.%

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7 HNTs loaded PA6/NBR blend (TSE) indicated that all the HNTs elements are distributed in
8
9 the samples. However, Uniform distributions of HNTs without any clusters in the FS

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11 welded sample attributed to tool stirring action which is responsible for the fragmentation
12
13
14 of clusters of HNTs and redistributing broken particles. It should be noted that the high
15
16 peak in the chart is related to the gold coating of the sample surface.

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42 Fig. 17 EDX-mapping of; a) TSE; b) multi-response optimized FSW samples
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45 4. Conclusion
46
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48 Improving of weld quality within an operating range of input parameters was performed in
49
50
the FSW process of polymeric nanocomposites. Modeling and determination of the
51
52
optimum input variables were then focused on maximizing the mechanical properties using
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55 RSM and desirability function. The main results can be drawn as follows:
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 Lower rotational and traverse speeds are required to attain defects free welds as well

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7 as desirable mechanical properties.
8
9  Among the three independent variables, the rotational speed was the most effective

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12
parameter for responses followed by HNTs content and traverse speed.
13
14  According to ANOVA results, the correlation coefficients for the predictive models
15
16 of tensile strength, Young’s modulus and impact strength were found 98.69%; 99.36%

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and 98.54% respectively, which represent reliability of the developed models.
19
20
21  The optimal parameters leading to maximal responses, which is recommended in
22
23
24
25
26
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28
an
multi-response optimization, are: N = 900 rev/min, V= 14 mm/min and H = 6.72%.

 The combined optimization results revealed that the values for impact strength and

Young’s modulus improved up to around 60% and 30% respectively compared to base
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30 material while tensile strength reached up to 90% of the base material strength.
31
32
 Confirmation tests of the response surface model were carried out for optimal (in
33
34
35 the cases of single-response and multi-response) and random condition. The developed
36
37 models were reasonably accurate since the percentages of error values were not higher
38
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39 than 4.71%.
40
41
42  The area distribution charts of rubber phase represent that the NBR droplets size
43
44 was smaller for FS welded nanocomposites with respect to presence of HNTs content
45
46 and performing of the FS welding process.
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7 References:
8
9 1. Chowdhury R, Banerji M, Shivakumar K. (2007). Polymer blends of carboxylated

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butadiene acrylonitrile copolymer (nitrile rubber) and polyamide 6 developed in twin screw
11
12 extrusion. J Appl Polym Sci. 104 (1):372-377
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14 2. Chavarria F, Paul D. (2004). Comparison of nanocomposites based on nylon 6 and nylon
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