Results and Discussion

4.5 Nano Mg(OH)2: PA Composites

4.5.1 Physical properties of nano Mg(OH)2: PA composites

4.5.1.1 Hardness of nano Mg(OH)2: PA composites

The effect of weight percentage of filler loading (nano and Commercial Mg(OH)2 on

hardness of polyamide composites is shown in fig 4.41. It is observed that

hardness of nano Mg(OH)2 filled polyamide nanocomposites was higher than that

of commercial Mg(OH)2 filled polyamide composites. Also the hardness of 11nm

Mg(OH)2 found to be more improved than that of 24 and 20 nm sizes of Mg(OH)2.

The hardness is recorded as 89 and 77 for 1 wt % loading of 11 nm and

commercial Mg(OH)2 respectively, while 4 wt % loadings of 11 nm and commercial

Mg(OH)2 showed hardness 101 and 82 respectively. This might be due to uniform

dispersion of nano Mg (OH) 2, which makes the surface of the composite hard and

tough. The improvement in hardness of polyamide composites is evidenced from

the results of elongation at break of polyamide composites [8-11].

Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon Page 112
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Fig 4.41: Hardness of PA filled with different sizes of Mg(OH)2

4.5.2 Mechanical properties of nano Mg(OH)2: PA composites

4.5.2.1 Tensile strength of nano Mg(OH)2: PA composites

A relation between weight percentage of filler loading nano and Commercial

Mg(OH)2 and tensile strength of polyamide composites is shown in fig 4.42. It is

observed that tensile strength of nano Mg(OH)2 filled polyamide nanocomposites

was higher than that of commercial Mg(OH)2 filled polyamide composites. Also the

tensile strength of 11 nm Mg(OH)2 was found to be more improved than that of 24

and 20 nm sizes of Mg(OH)2. The tensile strength is recorded as 106 MPa and 97

MPa for 1 wt % loading of 11 nm and commercial Mg(OH)2 respectively.

Whereas, 4 wt % loading of 11 nm and commercial Mg(OH)2 shows tensile

strength 137 MPa and 104 MPa respectively. It means nano filler provides higher

tensile strength compared to commercial Mg(OH)2. This increment in tensile

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 Results and Discussion

strength is due to uniform dispersion of nano filler throughout the matrix. Also due

to reduction in particles size of Mg(OH)2 that forms smaller spherullits for shorter

period of time [9, 10,11]. Moreover, during processing, rate of transfer of heat is

uniform from particle to particle due to fine sizes of nano Mg(OH)2, which leads in

formation of composite without any failure .The uniform dispersion of nano

Mg(OH)2 is evidenced from AFM images as shown in fig 4.43 and 4.44. During

tensile test the fine cracks are developed on specimen shown in AFM photograph

(fig 4.43 and 4.44).

Fig 4.42: Tensile strength of PA filled with different fillers Mg(OH)2

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Fig 43- AFM micrograph of 4-wt % of 11nm Mg(OH)2 polyamide composite

Fig 4.44 AFM 3D Photograph showing Crack and Filler Dispersion in PA 66 –

11 nm Ca3(PO4)2 Nanocomposite

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 Results and Discussion

4.5.2.2 Elongation at break of nano Mg (OH) 2: PA composites

Fig 4.45 shows elongation at break of polyamide nanocomposites with varying wt

% loading. It was found that with increase in weight percentage of filler loading,

elongation at break decreased. There was continuous decrement in elongation at

break with increase in amount of filler loading for all compositions. 11 nm Mg(OH)2

filled polyamide composite showed more decrement in elongation at break

compared to other sizes of Mg(OH)2. This might be due to hard nature of

polyamide as well as nano inorganic filler. 1 % loading of nano Mg(OH)2 shows

elongation at break 19.14, 19.98, 18.12 and 16.58% for commercial, 24,20 and 11

nm Mg(OH)2 respectively. Whereas, 4 wt % loadings of commercial, 24,20, and 11

nm Mg(OH)2 shows elongation at break 14.67, 14.34, 11.43 and 9.15%

respectively. Addition of filler decreases the elongation at break of composites.

This is due to the increment in spherullits formation with reduction in size and

increase in percentage of filler. Moreover it provides catastrophic failure to the

specimen with crack propagation [13], and thus decreases the extensibility of the

composite. This crack development is evidenced by AFM (figs 4.43 and 4.44).

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Fig 4.45: Elongation at break of PA filled with different sizes of

Mg(OH)2

4.5.2.3 Young’s modulus of nano Mg(OH)2: PA composites

A relation between weight percentage of filler loading (nano and Commercial

Mg(OH)2) and Young’s modulus of polyamide composites is shown in fig 4.46. It is

observed that Young’s modulus of nano Mg(OH)2 filled polyamide nanocomposites

was higher than that of commercial Mg(OH)2 filled polyamide composites. Also, the

Young’s modulus of 11 nm Mg(OH)2 was found to be more than that of 24 and 20

nm sizes of Mg(OH)2. 1 wt % loading of 11 nm Mg(OH)2 showed Young’s modulus

3804 Mpa, while 3652 Mpa for same wt % of loading of commercial Mg(OH)2.

Whereas, 4 wt % loadings of 11 nm Mg(OH)2 and commercial Mg(OH)2 showed

Young’s modulus as 4004 Mpa and 3727 Mpa [10,11].

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 Results and Discussion

Fig 4.46 Young’s modulus of PA filled with different sizes of

Mg(OH)2

4.5.3 Thermal properties of nano Mg(OH)2: PA composites

4.5.3.1 Thermal gravimetric analysis of nano Mg(OH)2: PA composites

Fig 4.47 to 4.49 shows thermal properties of pristine, commercial Mg(OH)2 and

nano Mg(OH)2 (24, 20, 11nm) filled polyamide composites. The incorporation of

nano Mg(OH)2 into polyamide composites with reduced particle size shows better

thermal stability than that of commercial Mg(OH)2 filled polyamide composite. 24,

20, 11 nm Mg(OH)2 shows decomposition temperature at 502, 550, and 570o C at

1 wt % loading, while 4 wt % loading shows decomposition temperatures 570, 585

and 590 o C respectively. The enhancement in thermal stability was due to uniform

dispersion and reduced particle size of nano Mg(OH)2, which is responsible for the

uniform absorption of heat that prevent decomposition of composite.

It can be summarized from the results that the reduced nanosizes of Mg(OH)2

provides better thermal, and mechanical properties than that of commercial

Mg(OH)2 in polyamide- 6,6. It can also be observed from a morphological study

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 Results and Discussion

that the nanoparticles dispersed uniformly throughout the matrix up to a 4-wt %

loading. As the uniform dispersion of nano- Mg(OH)2 brings the chains closer and

keeps them intact with nanoparticles and provides more strength and toughness

to composites than commercial Mg(OH)2, whereas reduced nanosizes showed

more enhancement in the hardness in comparison to commercial Mg(OH)2. This is

also due to uniform dispersion of nanoparticles in the polymer matrix. As the

nanoparticles are so small that they disperse uniformly in the matrix and

intercalate polymer chains to provide them with order i.e. orientation of molecules

is taking place. However, the amount of loading of nano- Mg(OH)2 causes

decrement in elongation at break this decrement in elongation at break is not due

to agglomeration of nanoparticles but due to catastrophic failure to the specimen

with crack propagation, and thus decreases the extensibility of the composite.

Fig 4.47 TGA of 24 nm Mg(OH)2polyamide Mg(OH)2composite

Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon Page 119
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Fig 4.48 TGA of 20 nm Mg(OH)2polyamide Mg(OH)2composite

Fig 4.49 TGA of 11 nm Mg(OH)2polyamide Mg(OH)2 Composite

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 Results and Discussion

4.5.3.2 Differential scanning colorimetric of nano Mg(OH)2: PA composites

Figs 4.50 to 4.52 show the DSC thermograms of pure polyamide and the

polyamide/ Mg(OH)2 nanocomposites. The glass transition temperature (Tg) of the

nanocomposites are found to be 55, 62, and 78 oC, respectively for 24, 20 and 11

nm Mg(OH)2. Where as pure polyamide shows Tg at 50 oC. The increment in Tg is

more compared to that of pure polyamide. Moreover the melting temperatures of

nanocomposites are found to be 275,294, and 302 respectively for 24, 20 and 11

nm Mg(OH)2. Where as pure polyamide melts at 263 oC. It is likely to say that

polyamide chains in the nanocomposites are immobilized inside and/or onto the

nano Mg(OH)2 particles, which prevents the segmental motion of the polymer

chains, similar to the case of polystyrene/MMT system (9). In other way can say

that, the confinement of the polyamide chains within the nano particles with a

restriction in the mobility of the polymer chains. Also due to proper processing of

polyamide matrix with uniform distribution of heat throughout the sheet voids in

between the polymer chains get minimized and thus the increment in glass

transition temperature is obtained [5,9].

[

Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon Page 121
 Results and Discussion

Fig 4.50. DSC of 24 nm-Polyamide Composite

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 Results and Discussion

Fig 4.51. DSC of 20 nm-Polyamide Nanocomposites

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 Results and Discussion

Fig 4.52 DSC of 11 nm-Polyamide Nanocomposites

4.5.3.3 Flammability of nano Mg (OH) 2: PA composites

The rates of flame retardency of different filler compositions are shown in fig 4.53.

The nanosize Mg(OH)2 filled in polyamide shows significant improvement in

flammability compared to that of commercial Mg(OH)2 filled polyamide. The

flammability values are 0.239 and 0.393 mm/sec for 1 wt % of 11 nm size Mg(OH)2

and commercial Mg(OH)2 respectively. It means, reduction in nanosize shows

better improvement in flame retarding properties. This might be due to the nano

filler, which creates the effective char layer on the surface, and it absorbs the heat

of burning (endothermic). In addition, Mg(OH)2 can delay the time before ignition

and suppress the release of smoke. Mg(OH)2 with high activity can also absorb

many substances, including free radical and carbon [9].

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 Results and Discussion

Fig 4.53: Flame retardancy of PA filled with different sizes of Mg(OH) 2

4.5.3.4 Vicat softening temperature of nano Mg (OH) 2: PA composites

The nano size Mg(OH)2 filled in polyamide shows significant improvement in vicat

softening temperature compared to that of commercial Mg(OH)2 filled polyamide

composite as shown in fig 4.54. The vicat softening temperatures are 308 and

247 oC for 1 wt % of 48 nm size Mg(OH)2 and commercial Mg(OH)2 respectively.

It means that reduction in nano sizes shows better enhancement in vicat

softening temperature of polyamide composites. This might be due to the nano

filler, which absorbs the heat as mentioned in earlier text (endothermic). Also due

to uniform transfer of heat throughout the polymer matrix that makes the surface

hard and rigid.

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 Results and Discussion

Fig 4.54: Vicat Softening Temperature of PA filled with different sizes of

Mg(OH) 2

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