Chapter 4b
This document was uploaded by user and they confirmed that they have the permission to share it. If you are author or own the copyright of this book, please report to us by using this DMCA report form. Report DMCA
Overview
Download & View Chapter 4b as PDF for free.
More details
- Words: 1,627
- Pages: 14
Results and Discussion
4.4 Nano Ca3(PO4)2: PA Composites 4.4.1 Physical properties of nano Ca3(PO4)2: PA composites 4.4.1.1 Hardness of nano Ca3(PO4)2: PA composites Fig 4.30 The effect of weight percentage of filler loading (nano and commercial Ca3(PO4)2 on hardness of polyamide composites. It is observed that hardness of nano Ca3(PO4)2 filled polyamide nanocomposites is higher than that of commercial Ca3(PO4)2 filled polyamide composites. Also the hardness of 11 nm Ca 3(PO4)2 found to be more improved than that of 23 and 17 nm sizes of Ca 3(PO4)2. The hardness is recorded as 86 and 77 for 1 wt % loading of 11 nm and commercial Ca3(PO4)2 respectively, while 4 wt % loadings of 11 nm and commercial Ca3(PO4)2 showed hardness 98 and 82 respectively. This might be due to uniform dispersion of nano Ca3(PO4)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 [8-13].
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 98
Results and Discussion
Fig 4.30: Hardness of PA filled with different fillers 4.4.2 Thermal properties of nano Ca3(PO4)2: PA composites 4.4.2.1 Thermal gravimetric analysis of nano Ca3(PO4)2: PA composites Fig 4.31 to 4.33 shows thermal properties of pristine, commercial Ca3(PO4)2 and nano Ca3(PO4)2
(23, 17, and 11 nm) filled polyamide composites. The
incorporation of, nano Ca3(PO4)2 into polyamide composites with reduced particle size shows better thermal stability than that of commercial Ca3(PO4)2 filled polyamide composite. 23, 17, 11 nm Ca3(PO4)2 shows decomposition temperature at 500, 520, and 542 oC at 1 wt % loading, while 4 wt % loading shows decomposition temperatures 543, 557 and 570o C respectively. The enhancement in thermal stability is due to uniform dispersion and reduced particle size of nano Ca3(PO4)2, which is responsible for the uniform absorption of heat and prevent out diffusion of volatile decomposition products. It can be summarized from the results Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 99
Results and Discussion
that the reduced nanosizes of Ca3(PO4)2 provides better thermal, and mechanical properties than that of commercial Ca3(PO4)2 in polyamide- 6, 6. It can also be observed from a morphological study that the nanoparticles dispersed uniformly throughout the matrix up to a 4-wt % loading. As the uniform dispersion of nanoCa3(PO4)2 brings the chains closer and keeps them intact with nanoparticles and provides more strength and toughness to composites than commercial Ca3(PO4)2 , whereas reduced nanosizes showed more enhancement in the hardness in comparison to commercial Ca3(PO4)2. This is also due to the uniform dispersion of the nanoparticles in the polymer chains [10-11]. As the nanoparticles are so small that they dispersed 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- Ca3(PO4)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.
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 100
Results and Discussion
Fig 4.31 TGA of 11 nm Ca3(PO4)2 polyamide filled with various sizes of CaSO4
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 101
Results and Discussion
Fig 4.32 TGA of 17 nm Ca3(PO4)2 polyamide filled with various sizes of CaSO4
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 102
Results and Discussion
Fig 4.33 TGA of 21 nm Ca3(PO4)2 polyamide filled with various sizes of CaSO4
4.4.2.2 Flammability of nano Ca3(PO4)2: PA composites The rates of flame retardency of different filler compositions are shown in fig 4.34. The nanosize Ca3(PO4)2 filled in polyamide shows significant improvement flammability compared to that of commercial Ca3(PO4)2 filled polyamide. The flammability values are 3.4 and 2.5 sec/mm for 1 wt % of 11 nm size Ca3(PO4)2 and commercial Ca3(PO4)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, Ca3(PO4)2 can delay the time before ignition
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 103
Results and Discussion
and suppress the release of smoke. Ca3(PO4)2 with high activity can also absorb many substances, including free radical and carbon[8-11].
Fig 4.34: Rate of flame retardancy of PA filled with different fillers
4.4.2.3 Vicat softening temperature of nano Ca3(PO4)2: PA composites The nano size Ca3(PO4)2 filled in polyamide shows significant improvement in vicat softening temperature compared to that of commercial Ca3(PO4)2 filled polyamide composite shown in fig 4.35. The vicat softening temperatures are 304 and 247o C for 1 wt % of 11 nm size Ca3(PO4)2 and commercial Ca3(PO4)2 respectively. It means that reduction in nano sizes shows better enhancement in vicat softening temperature of polyamide composites [11]. it absorbs
heat
uniformly. Uniform transfer of heat throughout the polymer matrix that makes the surface hard and
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 104
Results and Discussion
rigid.
Fig 4.35 VST of PA filled with different Nanofillers
4.4.3 Mechanical properties of nano Ca3(PO4)2: PA composites 4.4.3.1 Tensile strength of nano Ca3(PO4)2: PA composites A relation between weight percentage of filler loading (nano and commercial Ca3(PO4)2 and tensile strength of polyamide composites is shown in fig 4.38. It is observed that tensile strength of nano Ca3(PO4)2 filled polyamide nanocomposites is higher than that of commercial Ca3 (PO4)2 filled polyamide composites [13]. Also the tensile strength of 11 nm Ca3 (PO4)2 is found to be more improved than that of 23 and 17 nm sizes of Ca3(PO4)2 . The tensile strength is recorded as 109 MPa and 96 MPa for 1 wt % loading of 11 nm and
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 105
Results and Discussion
commercial Ca3(PO4)2 respectively. Whereas, 4 wt % loading of 11 nm and commercial Ca3(PO4)2 shows tensile strength 102 MPa and 139 MPa respectively. It means nano filler provides higher tensile strength compared to commercial Ca3(PO4)2. This increment in tensile strength is due to uniform dispersion of nano filler throughout the matrix [8, 10, and 11]. Also due to reduction in particles size of Ca3 (PO4)2, that forms smaller spherullits for shorter period of time. Moreover, during processing, rate of transfer of heat is uniform from particle to particle due to fine sizes of nano Ca3(PO4)2 , which leads in formation of composite without any failure .The uniform dispersion of nano Ca3 (PO4)2 is evidenced from AFM images as shown in fig10 (a-b). During tensile test the fine cracks are developed on specimen shown in AFM photograph (fig 4.36 and 4.37).
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 106
Results and Discussion
Fig 4.36 AFM Photograph showing Crack and Filler Dispersion in PA 66 - 11 nm Ca3(PO4)2 Nanocomposite
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 107
Results and Discussion
Fig 4.37 AFM 3D Photograph showing Crack and Filler Dispersion in PA 66 – 11 nm Ca3(PO4)2 Nanocomposite
Fig 4.38: Tensile strength of PA filled with different fillers Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 108
Results and Discussion
4.4.3.2 Young’s modulus of nano Ca3(PO4)2: PA composites A relation between weight percentage of filler loading (nano and commercial Ca3 (PO4)2) and Young’s modulus of polyamide composites is shown in fig 4.39. It is observed that Young’s modulus of nano Ca3(PO4)2 filled polyamide nanocomposites was higher than that of commercial Ca3 (PO4)2 filled polyamide composites. Also, the Young’s modulus of 11 nm Ca3 (PO4)2 is found to be more than that of 23 and 17 nm sizes of Ca3 (PO4)2. 1 wt % loading of, 11 nm Ca3 (PO4)2 shows Young’s modulus 3806 Mpa, while the same wt % of loading of commercial Ca3 (PO4)2 Yields 3652 Mpa. Whereas, 4 wt % loadings of 11 nm Ca3 (PO4)2 and commercial Ca3 (PO4)2 show Young’s modulus 4006 Mpa and 3727 Mpa.
Fig-4.39: Young’s Modulus of PA filled with different fillers Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 109
Results and Discussion
4.4.3.3 Elongation at break of nano Ca3(PO4)2: PA composites Fig 4.40 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 a continuous decrement in elongation at break with increase in amount of filler loading for all compositions. 11 nm Ca3(PO4)2 filled polyamide composite showed more decrement in elongation at break compared to other nano sizes of Ca3 (PO4)2. This might be due to hard nature of polyamide as well as nano inorganic filler. 1 % loading of nano Ca3 (PO4)2 showed elongation at break 20, 18, 16 and 14 % for commercial, 23,17and 11 nm Ca3 (PO4)2 respectively. Whereas, 4 wt % loadings of commercial, 23,17, and 11 nm Ca3 (PO4)2 showed elongation at break 15,13, 10 and 8 % 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, and thus decreases the extensibility of the composite [13].
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 110
Results and Discussion
Fig 4.40 Elongation at break of PA filled with different fillers
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 111
4.4 Nano Ca3(PO4)2: PA Composites 4.4.1 Physical properties of nano Ca3(PO4)2: PA composites 4.4.1.1 Hardness of nano Ca3(PO4)2: PA composites Fig 4.30 The effect of weight percentage of filler loading (nano and commercial Ca3(PO4)2 on hardness of polyamide composites. It is observed that hardness of nano Ca3(PO4)2 filled polyamide nanocomposites is higher than that of commercial Ca3(PO4)2 filled polyamide composites. Also the hardness of 11 nm Ca 3(PO4)2 found to be more improved than that of 23 and 17 nm sizes of Ca 3(PO4)2. The hardness is recorded as 86 and 77 for 1 wt % loading of 11 nm and commercial Ca3(PO4)2 respectively, while 4 wt % loadings of 11 nm and commercial Ca3(PO4)2 showed hardness 98 and 82 respectively. This might be due to uniform dispersion of nano Ca3(PO4)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 [8-13].
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 98
Results and Discussion
Fig 4.30: Hardness of PA filled with different fillers 4.4.2 Thermal properties of nano Ca3(PO4)2: PA composites 4.4.2.1 Thermal gravimetric analysis of nano Ca3(PO4)2: PA composites Fig 4.31 to 4.33 shows thermal properties of pristine, commercial Ca3(PO4)2 and nano Ca3(PO4)2
(23, 17, and 11 nm) filled polyamide composites. The
incorporation of, nano Ca3(PO4)2 into polyamide composites with reduced particle size shows better thermal stability than that of commercial Ca3(PO4)2 filled polyamide composite. 23, 17, 11 nm Ca3(PO4)2 shows decomposition temperature at 500, 520, and 542 oC at 1 wt % loading, while 4 wt % loading shows decomposition temperatures 543, 557 and 570o C respectively. The enhancement in thermal stability is due to uniform dispersion and reduced particle size of nano Ca3(PO4)2, which is responsible for the uniform absorption of heat and prevent out diffusion of volatile decomposition products. It can be summarized from the results Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 99
Results and Discussion
that the reduced nanosizes of Ca3(PO4)2 provides better thermal, and mechanical properties than that of commercial Ca3(PO4)2 in polyamide- 6, 6. It can also be observed from a morphological study that the nanoparticles dispersed uniformly throughout the matrix up to a 4-wt % loading. As the uniform dispersion of nanoCa3(PO4)2 brings the chains closer and keeps them intact with nanoparticles and provides more strength and toughness to composites than commercial Ca3(PO4)2 , whereas reduced nanosizes showed more enhancement in the hardness in comparison to commercial Ca3(PO4)2. This is also due to the uniform dispersion of the nanoparticles in the polymer chains [10-11]. As the nanoparticles are so small that they dispersed 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- Ca3(PO4)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.
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 100
Results and Discussion
Fig 4.31 TGA of 11 nm Ca3(PO4)2 polyamide filled with various sizes of CaSO4
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 101
Results and Discussion
Fig 4.32 TGA of 17 nm Ca3(PO4)2 polyamide filled with various sizes of CaSO4
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 102
Results and Discussion
Fig 4.33 TGA of 21 nm Ca3(PO4)2 polyamide filled with various sizes of CaSO4
4.4.2.2 Flammability of nano Ca3(PO4)2: PA composites The rates of flame retardency of different filler compositions are shown in fig 4.34. The nanosize Ca3(PO4)2 filled in polyamide shows significant improvement flammability compared to that of commercial Ca3(PO4)2 filled polyamide. The flammability values are 3.4 and 2.5 sec/mm for 1 wt % of 11 nm size Ca3(PO4)2 and commercial Ca3(PO4)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, Ca3(PO4)2 can delay the time before ignition
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 103
Results and Discussion
and suppress the release of smoke. Ca3(PO4)2 with high activity can also absorb many substances, including free radical and carbon[8-11].
Fig 4.34: Rate of flame retardancy of PA filled with different fillers
4.4.2.3 Vicat softening temperature of nano Ca3(PO4)2: PA composites The nano size Ca3(PO4)2 filled in polyamide shows significant improvement in vicat softening temperature compared to that of commercial Ca3(PO4)2 filled polyamide composite shown in fig 4.35. The vicat softening temperatures are 304 and 247o C for 1 wt % of 11 nm size Ca3(PO4)2 and commercial Ca3(PO4)2 respectively. It means that reduction in nano sizes shows better enhancement in vicat softening temperature of polyamide composites [11]. it absorbs
heat
uniformly. Uniform transfer of heat throughout the polymer matrix that makes the surface hard and
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 104
Results and Discussion
rigid.
Fig 4.35 VST of PA filled with different Nanofillers
4.4.3 Mechanical properties of nano Ca3(PO4)2: PA composites 4.4.3.1 Tensile strength of nano Ca3(PO4)2: PA composites A relation between weight percentage of filler loading (nano and commercial Ca3(PO4)2 and tensile strength of polyamide composites is shown in fig 4.38. It is observed that tensile strength of nano Ca3(PO4)2 filled polyamide nanocomposites is higher than that of commercial Ca3 (PO4)2 filled polyamide composites [13]. Also the tensile strength of 11 nm Ca3 (PO4)2 is found to be more improved than that of 23 and 17 nm sizes of Ca3(PO4)2 . The tensile strength is recorded as 109 MPa and 96 MPa for 1 wt % loading of 11 nm and
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 105
Results and Discussion
commercial Ca3(PO4)2 respectively. Whereas, 4 wt % loading of 11 nm and commercial Ca3(PO4)2 shows tensile strength 102 MPa and 139 MPa respectively. It means nano filler provides higher tensile strength compared to commercial Ca3(PO4)2. This increment in tensile strength is due to uniform dispersion of nano filler throughout the matrix [8, 10, and 11]. Also due to reduction in particles size of Ca3 (PO4)2, that forms smaller spherullits for shorter period of time. Moreover, during processing, rate of transfer of heat is uniform from particle to particle due to fine sizes of nano Ca3(PO4)2 , which leads in formation of composite without any failure .The uniform dispersion of nano Ca3 (PO4)2 is evidenced from AFM images as shown in fig10 (a-b). During tensile test the fine cracks are developed on specimen shown in AFM photograph (fig 4.36 and 4.37).
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 106
Results and Discussion
Fig 4.36 AFM Photograph showing Crack and Filler Dispersion in PA 66 - 11 nm Ca3(PO4)2 Nanocomposite
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 107
Results and Discussion
Fig 4.37 AFM 3D Photograph showing Crack and Filler Dispersion in PA 66 – 11 nm Ca3(PO4)2 Nanocomposite
Fig 4.38: Tensile strength of PA filled with different fillers Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 108
Results and Discussion
4.4.3.2 Young’s modulus of nano Ca3(PO4)2: PA composites A relation between weight percentage of filler loading (nano and commercial Ca3 (PO4)2) and Young’s modulus of polyamide composites is shown in fig 4.39. It is observed that Young’s modulus of nano Ca3(PO4)2 filled polyamide nanocomposites was higher than that of commercial Ca3 (PO4)2 filled polyamide composites. Also, the Young’s modulus of 11 nm Ca3 (PO4)2 is found to be more than that of 23 and 17 nm sizes of Ca3 (PO4)2. 1 wt % loading of, 11 nm Ca3 (PO4)2 shows Young’s modulus 3806 Mpa, while the same wt % of loading of commercial Ca3 (PO4)2 Yields 3652 Mpa. Whereas, 4 wt % loadings of 11 nm Ca3 (PO4)2 and commercial Ca3 (PO4)2 show Young’s modulus 4006 Mpa and 3727 Mpa.
Fig-4.39: Young’s Modulus of PA filled with different fillers Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 109
Results and Discussion
4.4.3.3 Elongation at break of nano Ca3(PO4)2: PA composites Fig 4.40 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 a continuous decrement in elongation at break with increase in amount of filler loading for all compositions. 11 nm Ca3(PO4)2 filled polyamide composite showed more decrement in elongation at break compared to other nano sizes of Ca3 (PO4)2. This might be due to hard nature of polyamide as well as nano inorganic filler. 1 % loading of nano Ca3 (PO4)2 showed elongation at break 20, 18, 16 and 14 % for commercial, 23,17and 11 nm Ca3 (PO4)2 respectively. Whereas, 4 wt % loadings of commercial, 23,17, and 11 nm Ca3 (PO4)2 showed elongation at break 15,13, 10 and 8 % 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, and thus decreases the extensibility of the composite [13].
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 110
Results and Discussion
Fig 4.40 Elongation at break of PA filled with different fillers
Ph.D Thesis, Mr. Shriram S. Sonawane, UDCT, North Maharashtra University, Jalgaon
Page 111
Related Documents
Chapter 4b
July 2020 1
Chapter 4b(modern Cpu)
November 2019 2
4b
May 2020 17
4b
April 2020 37
4b
April 2020 22