2| EXPERIMENTAL DETAILS

2.1 | Materials preparation

Polypropylene noted (PP) used in this work was supplied by TASNEE (density = 0.9 g/cm3,
melting point = 163°C). Thermoplastic Polyurethane (noted TPU) was obtained from (density
= …. g/cm3, melting point = …. °C) . Raw Fly Ash (noted raw FA) was originated by thermal
power plant of OCP Jorf-Lasfar El-Jadida, Morocco.

2.1.1 | FA preparation

By means of a vibratory sieve shaker (FRITSCH- Analysette 3 PRO) and a 63 μm sieve, the
raw FA was sieved and separated into two groups with various particle size ranges (higher
than 63µm and less than 63µm).

The particle size having less than 63µm was used for the preparation of the composites at 5,
10, 15, 20 wt% FA content.

2.1.2 | Master Batch preparation

A master batch with a composition of 50/50 wt% PP/FA were elaborated using FA with a
particle size less than 63µm and PP pellets obtained via extrusion of PA granules.

The extrusion process of master batch was achieved using a Leistritz ZSE-18 twin-screw
extruder L/D = 40 (LEISTRITZ EXTRUSIONSTECHNIK GMBH, Germany). Compounding
was performed using a speed of 125 rpm. Temperature profile Temperature profile of the
extruder barrel’s night zones was set, from hopper to die, at respectively 200, 200, 200, 200,
190, 190, 190, and 190 °C respectively. The extrudate were cooled in a water bath and then
pelletized into pellets of 2–3 mm in length using (THERMO Fisher, UK). The
latter were dried in vacuum oven at 80°C for 2h.
 2.1.3 | Polymer composites preparation

Three lots have been prepared using PP as a matrix and using a reinforcement agent
containing 100% FA, 80%FA/20%TPU and 50%FA/50%TPU respectively, with the same
amounts of FA in each lot (5, 10, 15 and  20 wt%) . The specimens for mechanical tests were
molded by a laboratory scale injection molding machine at the barrel temperature of 210°C,
the nozzle temperature of 202°C and the mold temperature of 30°C. The mold opened after a
cooling time of 6 s and the dosing volume of a small dumbbell and a disc was 12 cm3. The
formulations coded as PP/80FA/20TPU/X refer to the samples of second lot with the
reinforcement agent containing 80%FA/20%TPU, where X indicates the weight loading of
FA (X = 5,10,15 and 20 wt%). For better understanding of the properties of reinforced PP,
neat PP was also molded. Formulations of composites are shown in Table 1. 

T ABLE 1 Formulations of samples .

Samples PP (wt%) FA (wt%) TPU (wt%)

PP/100FA/0 100 0 0
PP/100FA/5 95 5 0
PP/100FA/10 90 10 0
PP/100FA/15 85 15 0
PP/100FA/20 80 20 0

PP/80FA/20TPU/5 93.75 5 1.25

PP/80FA/20TPU/10 87.5 10 2.5
PP/80FA/20TPU/15 81.25 15 3.75
PP/80FA/20TPU/20 75 20 5

PP/50FA/50TPU/5 90 5 5
PP/50FA/50TPU/10 80 10 10
PP/50FA/50TPU/15 70 15 15
PP/50FA/50TPU/20 60 20 20

Abbreviations: PP: Polypropylene, FA: Fly ash , TPU: Thermoplastic polyurethane

2.2 | Characterization techniques

 2.2.1 | Scanning electron microscope

Zeiss EVO 10 SEM (Carl Zeiss Microscopy, GmbH, Jena,Germany) was used to evaluate
particle dispersion/distribution of FA in the polymeric matrix and to illustrate the morphology
of FA powders. In order to obtain clean and accurate fracture faces, all composite samples
were cryo-fractured under liquid nitrogen. To make the samples conductive, a gold coating
was applied by sputtering technique.

2.2.2 | Fourier transform infrared spectroscopy

FTIR spectra of the composites were recorded using an ABB Bomem FTLA 2000-102
spectrometer (ATR: Specac Golden Gate). The spectra were obtained with an accumulation of
16 scans and a resolution of 4cm−1 in 600–4000 cm−1 range.

2.2.3 | X-ray diffraction

XRD data were collected using a Bruker D8 Advance X-ray Diffractometer, using Cu Kα
radiation (λ= 1.5418 Å) with a 0.01° 2θ step size in the range of 6°–80°. Ni filtered radiation
with 40 kV voltage and 100 mA intensity. The 3D visualization of the crystal structure was
obtained using VESTA (Visualization for Electronic and Structural Analysis) program.

2.2.4 | Thermogravimetric analysis

The thermal decomposition of FA powder and composites were evaluated using TA

instruments (Discovery TGA). Roughly 20 mg of each sample was placed in a platinum pan
and was heated from room temperature up to 900°C (for FA samples) and to 700°C (for
composite specimens) under nitrogen flow of 20 ml/min at a heating rate of 10 °C·min-1 to
yield the onset temperature of decomposition.

2.2.5 | Tensile tests

Tensile tests were performed according to ISO 527-1:2012 using a universal testing machine
INSTRON 8821S (Instron, USA) at a crosshead speed of 20 mm/min using a 5 kN load cell.
Tensile strength, percentage elongation at break and modulus values were recorded. All the
results were calculated with an average value of three samples for each formulation.

2.2.6 | Torsion tests

Torsion tests were performed on an ARES-LS rheometer operating at room temperature in a

rectangular torsion mode, using 5.5 mm width and 2 mm thick samples with 53,1 mm fixed
length between the rips. The torsion modulus (G*) and the loss modulus factor (tan δ) are
obtained in dynamic frequency sweep tests with frequencies ranging from 0.1 Hz to 40 Hz at
a strain amplitude of 0.02. Two specimens were used for each formulation and the average
values were reported.