AU2023222862A1 - Polymer composite - Google Patents
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- AU2023222862A1 AU2023222862A1 AU2023222862A AU2023222862A AU2023222862A1 AU 2023222862 A1 AU2023222862 A1 AU 2023222862A1 AU 2023222862 A AU2023222862 A AU 2023222862A AU 2023222862 A AU2023222862 A AU 2023222862A AU 2023222862 A1 AU2023222862 A1 AU 2023222862A1
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- polypropylene
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- basalt fiber
- whisker
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- 239000002131 composite material Substances 0.000 title claims abstract description 178
- 229920000642 polymer Polymers 0.000 title claims abstract description 38
- 229920002748 Basalt fiber Polymers 0.000 claims abstract description 179
- 239000011777 magnesium Substances 0.000 claims abstract description 111
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 111
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 110
- 239000000835 fiber Substances 0.000 claims abstract description 71
- 239000000945 filler Substances 0.000 claims abstract description 19
- CENHPXAQKISCGD-UHFFFAOYSA-N trioxathietane 4,4-dioxide Chemical compound O=S1(=O)OOO1 CENHPXAQKISCGD-UHFFFAOYSA-N 0.000 claims abstract description 3
- -1 polypropylene Polymers 0.000 claims description 172
- 239000004743 Polypropylene Substances 0.000 claims description 171
- 229920001155 polypropylene Polymers 0.000 claims description 165
- 239000000203 mixture Substances 0.000 claims description 17
- 239000003963 antioxidant agent Substances 0.000 claims description 16
- 230000003078 antioxidant effect Effects 0.000 claims description 13
- 239000007822 coupling agent Substances 0.000 claims description 10
- 239000000654 additive Substances 0.000 claims description 9
- 239000002086 nanomaterial Substances 0.000 claims description 9
- 229920001577 copolymer Polymers 0.000 claims description 7
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 6
- 229910000077 silane Inorganic materials 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 5
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical group CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 4
- 239000004626 polylactic acid Substances 0.000 claims description 4
- WPMYUUITDBHVQZ-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoic acid Chemical compound CC(C)(C)C1=CC(CCC(O)=O)=CC(C(C)(C)C)=C1O WPMYUUITDBHVQZ-UHFFFAOYSA-N 0.000 claims description 3
- 229920001046 Nanocellulose Polymers 0.000 claims description 3
- 239000004952 Polyamide Substances 0.000 claims description 3
- 239000012963 UV stabilizer Substances 0.000 claims description 3
- 238000010306 acid treatment Methods 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 239000002041 carbon nanotube Substances 0.000 claims description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 3
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 3
- 239000003063 flame retardant Substances 0.000 claims description 3
- 238000007306 functionalization reaction Methods 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- MNEXIOKPOFUXLA-UHFFFAOYSA-N n'-(11-trimethoxysilylundecyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCCCCCCCCCNCCN MNEXIOKPOFUXLA-UHFFFAOYSA-N 0.000 claims description 3
- 239000002667 nucleating agent Substances 0.000 claims description 3
- 238000009832 plasma treatment Methods 0.000 claims description 3
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 3
- 229920002647 polyamide Polymers 0.000 claims description 3
- 229920001707 polybutylene terephthalate Polymers 0.000 claims description 3
- 238000007788 roughening Methods 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- JCGDCINCKDQXDX-UHFFFAOYSA-N trimethoxy(2-trimethoxysilylethyl)silane Chemical compound CO[Si](OC)(OC)CC[Si](OC)(OC)OC JCGDCINCKDQXDX-UHFFFAOYSA-N 0.000 claims description 3
- USYJXNNLQOTDLW-UHFFFAOYSA-L calcium;heptanedioate Chemical compound [Ca+2].[O-]C(=O)CCCCCC([O-])=O USYJXNNLQOTDLW-UHFFFAOYSA-L 0.000 claims description 2
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims 1
- 239000011159 matrix material Substances 0.000 abstract description 79
- 230000001747 exhibiting effect Effects 0.000 abstract 1
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- 230000016507 interphase Effects 0.000 description 23
- 230000015556 catabolic process Effects 0.000 description 20
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- 238000013016 damping Methods 0.000 description 5
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- 230000021715 photosynthesis, light harvesting Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229920000049 Carbon (fiber) Polymers 0.000 description 3
- 239000004917 carbon fiber Substances 0.000 description 3
- 239000011151 fibre-reinforced plastic Substances 0.000 description 3
- 230000017525 heat dissipation Effects 0.000 description 3
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- 230000004048 modification Effects 0.000 description 3
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- 238000001878 scanning electron micrograph Methods 0.000 description 3
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- 230000002195 synergetic effect Effects 0.000 description 3
- 238000002411 thermogravimetry Methods 0.000 description 3
- 241000220317 Rosa Species 0.000 description 2
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- 238000002360 preparation method Methods 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
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- 229920003002 synthetic resin Polymers 0.000 description 2
- PZJJKWKADRNWSW-UHFFFAOYSA-N trimethoxysilicon Chemical compound CO[Si](OC)OC PZJJKWKADRNWSW-UHFFFAOYSA-N 0.000 description 2
- RMSGQZDGSZOJMU-UHFFFAOYSA-N 1-butyl-2-phenylbenzene Chemical group CCCCC1=CC=CC=C1C1=CC=CC=C1 RMSGQZDGSZOJMU-UHFFFAOYSA-N 0.000 description 1
- 238000010146 3D printing Methods 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229920002430 Fibre-reinforced plastic Polymers 0.000 description 1
- 208000034530 PLAA-associated neurodevelopmental disease Diseases 0.000 description 1
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
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- 239000002557 mineral fiber Substances 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to a composite material, more particularly to a natural fiber reinforced and
sustainable polymeric composite comprising basalt fiber and magnesium oxysulfate filler in a
polymer matrix. The present invention thus provides a hybrid polymer composite material
exhibiting superior strength and stiffness whilst simultaneously reducing the toughness. Moreover,
the composite is recyclable, renewable and ecofriendly.
Description
[001] The invention relates to a composite material, more particularly to a polymeric composite material for lightweighting applications, specifically in automobiles.
[002] Polymer composites play an important role in the multi-material strategy used for light weighting auto systems. Typically, glass fiber reinforced thermoplastics are used for semi structural automotive applications. Glass fibers are hygroscopic in nature and have high manufacturing costs because of the addition of special additives in their manufacture. Another alternative is carbon fibers. Carbon fibers are also high performing fibers. However, the use of carbon fibers is also limited due to the high manufacturing costs.
[003] With increasing focus on sustainability, natural fibers are being explored in the field of fiber reinforced polymer composites. However, plant based natural fibers have reduced thermal stability and hence find restricted use in the field of mobility, especially in semi-structural or structural applications.
[004] Therefore, there exists a need for an ecofriendly, hybrid polymer composite material with adequate strength and stiffness without compromising on the toughness.
[005] In one aspect, the present invention provides a polymer composite comprising: at least one polymer, basalt fiber and magnesium oxysulphate (MOS) filler.
[006] In an embodiment, at least one polymer is present in a range of 55 - 95%, the basalt fiber is present in a range of 5 - 40% and magnesium oxysulfate filler is present in a range of 1 - 20%.
[007] In another embodiment, at least one polymer is selected from polypropylene, polyamide, polybutylene terephthalate, polylactic acid and copolymer thereof.
[008] In yet another embodiment, the basalt fiber has fiber length in range of 3 - 10mm.
[009] In another embodiment, the basalt fiber is treated by either roughening or by functionalization like silane treatment, acid treatment, alkali treatment, plasma treatment or nanomaterial deposition. The silane treatment is preferably carried out with a coupling agent selected from 3-(aminopropyl)triethoxysilane (APS), 3-(glycidoxypropyl)trimethoxysilane(GPS), (N-(2-aminoethyl)-11- aminoundecyltrimethoxysilane), 1,2- ethylenebis(trimethoxysilane) and vinyltriethoxysilane.
[010] In another embodiment, the composite is modified by adding compatibilizer or coupling agents. The compatibilizer is Polypropylene-graft-Maleic anhydride (PP-g-MA).
[011] In yet another embodiment, the composite further comprises additives selected from antioxidants, coupling agent, UV stabilizers, compatibilizers, nucleating agents, anti-static additives, nanomaterials, flame retardants and mixture thereof. The nanomaterial is selected from carbon nanotubes, graphene, nano-silica, nano-calcium carbonate, nano-calcium pimelate, nanocellulose and mixture thereof. The antioxidant is selected from tris(2,4-ditert butylphenyl)phosphite, pentaerythritol tetrakris(3-(3,5-di-tert-butyl-4-hydroxphenyl)propionate, Pentaerythritoltetrakis(3,5-di-tert-butyl-4-hydroxyhydrocinnamate andmixturethereof.
Figure 1 illustrates DSC graphs of 5% MOS filled, and basalt fiber reinforced polypropylene composites. Figure 2 illustrates melting point and degree of crystallinity of 5% MOS filled, and basalt fiber reinforced polypropylene composites. Figure 3 illustrates DSC graphs of 10% MOS filled, and basalt fiber reinforced polypropylene composites. Figure 4 illustrates melting point and degree of crystallinity of 10% MOS filled, and basalt fiber reinforced polypropylene composites.
Figure 5 illustrates TGA graphs of 5% MOS filled, and basalt fiber reinforced polypropylene composites. Figure 6 illustrates TGA graphs of 10% MOS filled, and basalt fiber reinforced polypropylene composites. Figure 7 illustrates storage modulus plots of 5% MOS filled, and basalt fiber reinforced polypropylene composites. Figure 8 illustrates loss modulus plots of5% MOS filled, and basalt fiber reinforced polypropylene composites. Figure 9 illustrates tan delta plots of 5% MOS filled, and basalt fiber reinforced polypropylene composites. Figure 10 illustrates Peak of tan 6 (a - transition) of 5% MOS filled, and basalt fiber reinforced polypropylene composites. Figure 11 illustrates Storage modulus plots of 10% MOS filled, and basalt fiber reinforced polypropylene composites. Figure 12 illustrates Loss modulus of 10% MOS filled, and basaltfiber reinforced polypropylene composites. Figure 13 illustrates tan 6 plots of 10% MOSfilled, and basalt fiber reinforced polypropylene composites. Figure 14 illustrates Peak of tan delta of 10% MOS filled, and basalt fiber reinforced polypropylene composites. Figure 15 illustrates Tensile strength and tensile modulus of 5% MOS filled, and basalt fiber reinforced polypropylene composites. Figure 16 illustrates Tensile properties of 10% MOS filled, and basalt fiber reinforced polypropylene composites. Figure 17 illustrates Flexural properties of 5% MOS filled, and basalt fiber reinforced polypropylene composites. Figure 18 illustrates Flexural properties of 10% MOS filled, and basalt fiber reinforced polypropylene composites. Figure 19 illustrates Izod impact properties of 5% MOS filled, and basalt fiber reinforced polypropylene composites. Figure 20 illustrates Izod impact properties of 10% MOS filled, and basalt fiber reinforced polypropylene composites. Figure 21 illustrates SEM images of (a) 5% MOS filled polypropylene without PP-g-MA and (b) with PP-g-MA.
Figure 22 illustrates SEM images of tensile fracture surfaces of (a) 10% MOS filled matrix modified polypropylene composite and (b) 10% MOS filled, and 20% basalt fiber reinforced matrix modified polypropylene composite.
[012] The present invention is directed towards a composite polymer material and process of production thereof, wherein the eco-friendly composite polymer material exhibits good strength and stiffness with improved toughness and improved near - isotropic mechanical properties.
[013] In one aspect, the present invention provides a polymer composite comprising: At least one polymer resin, basalt fiber, and magnesium oxysulphate (MOS).
[014] In an embodiment, the polymer composite comprises basalt fiber in a range of 5 - 40% and magnesium oxysulphate (MOS) filler in a range of 1 - 20% in a polymer resin matrix present in the range of 55 - 95%. In this regards, reinforcing the at least one polymer selected from polypropylene, polyamide, polybutylene terephthalate, polylactic acid (PLA) and copolymer thereof, with basalt fiber helps in improving the strength, stiffness and toughness and the resulting composite finds huge potential in lightweighting applications. Basalt fiber reinforced polymer systems have been found to be sustainable and have lower environmental impact. The use of biodegradable resins like PLA leads to green, environment friendly composites that are fully sustainable.
[015] In an embodiment, the basalt fiber is selected from short basalt fiber and long basalt fiber with fiber length in range of 3 - 10 mm. Basalt fibers are sustainable and natural mineral fibers that are derived from basalt rocks. Their manufacture does not involve any expensive manufacturing process or addition of additives.
[016] The fiber-polymer matrix interphase can be improved by matrix modification to couple the non-polar polymer matrix to the polar basalt fiber. Fiber surface treatment by either roughening the fiber through either a chemical treatment that etches the fiber surface or through mechanical milling or by functionalization like silane treatment, acid treatment, alkali treatment, plasma treatment or nanomaterial deposition, can also couple the fiber to the polymer matrix thereby contributing to an improvement in the fiber-matrix interphase. In this regards, the silane treatment is preferred and is carried out with a coupling agent selected from 3-(aminopropyl)triethoxysilane (APS), 3-(glycidoxypropyl)trimethoxysilane (GPS), (N-(2-aminoethyl)-11 aminoundecyltrimethoxysilane), 1,2- ethylenebis(trimethoxysilane), vinyltriethoxysilane.
[017] The basalt fiber addition results in improved thermal stability of the polymer matrix. The maximum degradation temperature saw an increasing trend with the addition of basalt fibers. This is attributed to the ability of the basalt fibers to reduce the heat transfer rate and subsequently the degradation of the polymer.
[018] The polymer matrix can be modified by adding compatibilizer or coupling agents, preferably Polypropylene-graft-Maleic anhydride (PP-g-MA) composite. This PP-g-MA addition to basalt fiber reinforced polymer increased the degradation temperature thereby delaying the degradation of the polymer. PP-g-MA addition caused further increase in strength and modulus owing to the fiber - matrix interfacial bonding improvement. Increasing the fiber content and length works towards improving the impact strength of the composites. Basalt fiber addition reduces the notched Izod impact strength of the composites due to insufficient fiber length.
[019] In an embodiment, the addition of magnesium oxysulphate fillers to the polymer composite obstructed matrix crystallinity resulting in drop in the degree of crystallinity. The degradation temperature of the composite increases as a result of the magnesium oxysulphate addition. Addition of PP-g-MA to the magnesium oxysulphate - polymer blend resulted in improved dispersion of the magnesium oxysulphate in the polymer matrix. This improved the filler - matrix interphase resulting in superior tensile strength, tensile modulus and reduced notched Izod impact strength. Magnesium oxysulphate fillers aid in improving the strength and stiffness of the composites whilst also improving the dimensional stability.
[020] In an embodiment, the composite may further comprise additives, wherein these additives are selected from, but not limited to, antioxidants, coupling agents, UV stabilizers, compatibilizers, nucleating agents, anti-static additives, nanomaterials, flame retardants and mixture thereof. The nanomaterial is selected from carbon nanotubes, graphene, nano-silica, nano-calcium carbonate, nano calcium pimelate, nanocellulose and mixture thereof. The antioxidant is selected from tris(2,4-ditert-butylphenyl)phosphite, pentaerythritol tetrakris(3-(3,5-di-tert-butyl-4- hydroxphenyl)propionate, Pentaerythritol tetrakis(3,5-di-tert-butyl-4-hydroxyhydrocinnamate and mixture thereof.
[021] In another aspect, the invention relates to a process for preparation of a composite polymer material. The process comprises the steps of melt compounding magnesium oxysulphate fillers and basalt fibers in polymer matrix.
[022] In an embodiment, the process comprises the steps of compounding basalt fibers of varying fiber contents (10, 20 and 30%) with polypropylene resin, magnesium oxysulphate fillers at varying filler loadings (5% and 10%) and with PP-g-MA in a co-rotating twin screw compounding extruder to give basalt fiber reinforced polypropylene composites and basalt fiber reinforced matrix modified polypropylene composites.
[023] In an embodiment, the composite material exhibits superior strength and stiffness whilst simultaneously reducing the toughness. Moreover, the composite is recyclable, renewable and becomes biodegradable with the use of resins like PLA and thus an ecofriendly option.
[024] In an embodiment, this composite polymer material is useful in lightweight applications as well as applications that require strength, stiffness, and toughness including, not limited to, bumper beams, front end modules, seat bracket and other structural applications in automobile, Instrument panel carrier, battery top/bottom cover, control arm, 3D printing etc. The composite material helps in reducing overall weight of the automotive vehicles and is applicable to a whole range of automotives including electric vehicles and hybrid vehicles.
[025] The following experimental examples are illustrative of the invention but not limitative of the scope thereof:
Material:
[026] A heterophasic polypropylene impact copolymer (BD265MO grade from M/s Borealis) was selected as the polymer matrix. Such heterophasic polypropylene impact copolymers offer significant improvements over the conventional isotactic polypropylene in terms of toughness.
They are usually the starting material used in compounding for further property enhancements. The selected grade had a typical tensile modulus of around 1200MPa with a no break impact strength.
[027] Chopped basalt fiber with 13pm diameter and 6.4mm length was commercially obtained. The chopped basalt fiber had been pre-sized with a sizing agent suitable for bonding with polypropylene and polyethylene matrices.
[028] To protect the polymer from thermal degradation effects, a synergistic processing and long term heat stabilizer consisting of a blend of 67% tris(2,4-ditert-butylphenyl) phosphite and 33% pentaerythritol tetrakris(3-(3,5-di-tert-butyl-4-hydroxphenyl)propionate) with the trade name Irganox B215 from BASF was used.
[029] A commercial grade of PP-g-MA coupling agent was used.
[030] Magnesium oxysulphate whiskers (MOSw) fillers were commercially obtained.
Composite preparation, characterization, and test methods
[031] For understanding the possible synergy due to a combination of basalt fiber and magnesium oxysulphate (MOSw) on the mechanical properties of basalt fiber reinforced and magnesium oxysulphate filled polypropylene composites, a sampling plan was arrived as detailed in tables 1 and 2.
Table 1: Samples and formulations based on 5% MOSw
Sr. Sample ID Experiment / Formulation No. 1 PP Polypropylene (99.8%) + Antioxidant (0.2%) 2 PP5M Polypropylene (94.8%) + MOSw (5%) + Antioxidant (0.2%) 3 PP5MC Polypropylene (89.8%) + MOSw (5%) + PP-g-MA (5%) +
Antioxidant (0.2%)
4 PP5M20BC Polypropylene (69.8%)+ MOSw (5%)+ 6.4mm as received basalt fiber (20%) + PP-g-MA (5%) + Antioxidant (0.2%) PP5M30BC Polypropylene (59.8%)+ MOSw (5%)+ 6.4mm as received basalt fiber (30%) + PP-g-MA (5%) + Antioxidant (0.2%)
Table 2: Samples and formulations based on 10% MOSw Sr. Sample ID Experiment / Formulation No. 1 PP Polypropylene (99.8%) + Antioxidant (0.2%) 2 PP1OM Polypropylene (89.8%) + MOSw (10%) + Antioxidant (0.2%) 3 PP1OMC Polypropylene (84.8%)+ MOSw (10%)+ PP-g-MA (5%) + Antioxidant (0.2%) 4 PP1OM20BC Polypropylene (64.8%) + MOSw (10%) + 6.4mm as received basalt fiber (20%) + PP-g-MA (5%)
+ Antioxidant (0.2%)
Differential scanning calorimetry (DSC)
[032] The prepared composites were characterized using DSC to determine the degree of crystallinity. A comparison of the DSC graphs of the 5% MOS filled polypropylene composites with 6.4mm basalt fibers is given in figure 1. A comparison of the melting point and degree of crystallinity of the 5% MOS filled and 6.4mm basalt fiber reinforced polypropylene composites is given in figure 2.
[033] A comparison of the DSC graphs of the 10% MOS filled polypropylene composites with 6.4mm basalt fibers is given in figure 3.
[034] A comparison of the melting point and degree of crystallinity of the 10% MOS filled polypropylene composites with 6.4mm basalt fibers is given in figure 4. Addition of 5% Magnesium oxysulphate whisker to polypropylene obstructed matrix crystallinity as could be seen from the drop in the degree of crystallinity.
[035] The addition of PP-g-MA slightly reduced it further. Basalt fiber addition obstructed polypropylene matrix crystallinity in the case of 20% and 30% fiber dosage levels as could be inferred from the drop in the degree of crystallinity. Basalt fibers induced matrix amorphousness. This is attributed to two reasons. The first reason being the presence of more fibers that obstructed the crystallite formation. The second reason is the increase in interfacial interaction between the matrix and the basalt fiber that had a default sizing amenable to polypropylene matrix. 10% Magnesium oxysulphate whisker addition to polypropylene obstructed matrix crystallinity as could be seen from the drop in the degree of crystallinity. The addition of PP-g-MA slightly reduced it further. Basalt fiber addition obstructed polypropylene matrix crystallinity in case of % fiber dosage levels as could be inferred from the drop in the degree of crystallinity. Basalt fibers induced matrix amorphousness. This is attributed to two reasons. The first reason being the presence of more fibers that obstructed the crystallite formation. The second reason is the increase in interfacial interaction between the matrix and the basalt fiber that had a default sizing amenable to polypropylene matrix. Increased whisker content did not have any effect on the degree of crystallinity as could be evidenced from the identical values.
Thermogravimetric analysis
[036] The 5% magnesium oxysulphate whisker filled and basalt fiber reinforced polypropylene granules were analyzed using a thermogravimetric analyzer. The samples were loaded in a TGA furnace, and the mass loss was captured over a temperature range of ambient to 600°C with a °C/ minute ramp-rate. The degradation temperatures at 5%, 50% and maximum mass loss and the residue content have been captured in table 3.
Table 3. TGA analysis of 5% MOS filled, and basalt fiber reinforced polypropylene composites.
Sr. Sample Description T-5 (°C) T-5 o Residue (%) No. (0C) 1 PP - BD265MO 296 360 -
2 PP5M 395 441 4 3 PP5MC 390 439 4 4 PP5M20BC 391 445 24 PP5M30BC 396 448 27
[037] The TGA graph is given in figure 5.
[038] The degradation temperature of basalt fiber reinforced composites increased with the addition of 5% magnesium oxysulphate whisker. The onset of degradation denoted by T-5 °C rose from 296°C for neat polypropylene to 395°C with 5% magnesium oxysulphate whisker addition. Addition of PP-g-MA caused a slight reduction in the degradation onset temperature to 390°C that was still higher than neat polypropylene. Addition of 20% basalt fibers to the 5% magnesium oxysulphate filled polypropylene composite slightly increased the degradation onset temperature to 391°C and 30% basalt fiber addition increased it further to 396 C. The temperature at 50% degradation rose with addition of both magnesium oxysulphate whisker addition and basalt fiber addition. Addition of basalt fibers to polypropylene served to increase the degradation temperature of the composite. This is attributed to the ability of the basalt fibers to reduce the heat transfer rate and subsequently the degradation of polypropylene.
[039] The 10% magnesium oxysulphate whisker filled and basalt fiber reinforced polypropylene granules were analyzed using a thermogravimetric analyzer. The samples were loaded in a TGA furnace, and the mass loss was captured over a temperature range of ambient to 600°C with a10°C / minute ramp-rate. The degradation temperatures at 5%, 50% and maximum mass loss and the residue content have been captured in table 4.
[040] Table 4: TGA analysis of 10% MOS filled, and basalt fiber reinforced polypropylene composites Sr. Sample Description T-5 (°C) T-5o Residue(%) No. ( 0C) 1 PP - BD265MO 296 360 -
2 PP1OM 385 440 4 3 PP1OMC 389 442 8 4 PP1OM20BC 384 447 24
[041] The TGA graph is given in figure 6.
[042] Interestingly, addition of 10% magnesium oxysulphate whisker addition increased the degradation onset temperature. However, addition of PP-g-MA further increased the degradation onset temperature of the composite. Again, 20% basalt fiber addition did not cause any increase to the degradation onset temperature of the 10% magnesium oxysulphate whisker filled polypropylene composite. This trend was different from that of the temperature at which 50% degradation took place. Addition of both magnesium oxysulphate whisker and basalt fibers progressively increased the temperature at which 50% degradation (T-50 C) occurred. This is attributed to the ability of both magnesium oxysulphate and basalt fibers to transfer the heat and dissipate it effectively.
Dynamic mechanical analysis
[043] Dynamic mechanical analysis of the basalt fiber reinforced polypropylene composites was run in a TA Q800 DMA equipment. The samples were run in the three-point bending mode and were subjected to a temperature sweep from ambient to 135 °C at 2 °C / minute ramp rate. The frequency was set as 1Hz and the strain amplitude as 20pm. The storage modulus, loss modulus and tan delta values of the composites were plotted as a function of temperature. The storage modulus plot of the 5% Magnesium oxysulphate whisker filled and basalt fiber reinforced polypropylene composites with 6.4mm initial fiber length is given in figure 7.
[044] Storage modulus is a measure of elasticity of the composite. At 40 °C, neat polypropylene had a storage modulus of 905MPa. 5% addition of magnesium oxysulphate whiskers increased the storage modulus of the Magnesium oxysulphate whisker filled polypropylene to 1506MPa. This is due to the reinforcing effect of the whiskers. This was due to the effective load transfer from the polypropylene resin to whisker through the establishment of an interphase as evidenced from the drop in the degree of crystallinity of the polypropylene resin. Addition of PP-g-MA further increased the storage modulus to 1950MPa. This signified the whisker - matrix interphase improvement through PP-g-MA addition. 20% addition of basalt fibers further increased the storage modulus to 3098MPa. 30% addition of basalt fibers increased the storage modulus to 4202Mpa. The improvement in storage modulus upon increasing basalt fiber dosage is due to the reinforcing efficiency of the basalt fiber that served to increase the elasticity of the magnesium oxysulphate whisker filled and basalt fiber reinforced polypropylene composites. The loss modulus plot of the 5% Magnesium oxysulphate whisker filled and basalt fiber reinforced polypropylene composites with 6.4mm initial fiber length is given in figure 8.
[045] Loss modulus is a measure of the energy lost due to heat dissipation within the composite. At 40°C, the loss modulus ofneat polypropylene was 48MPa. 5% magnesium oxysulphate whisker addition increased the loss modulus to 69MPa. PP-g-MA addition increased the loss modulus further to 82MPa. 20% basalt fiber addition further increased the storage modulus to 120MPa. % basalt fiber addition increased the storage modulus to 146MPa. This signified the ability of both magnesium oxysulphate whiskers and basalt fibers to dissipate the heat thereby increasing the loss modulus. Tan 6 is the damping factor and is the ratio of the loss modulus to the storage modulus of the material. The tan 6 plot of the magnesium oxysulphate whisker filled and basalt fiber reinforced polypropylene composites with 6.4mm initial fiber length is given in figure 9.
[046] Neat polypropylene had the highest tan 6 signifying that the material had the highest damping. 5% magnesium oxysulphate whisker addition reduced the tan 6 at temperatures up to ~85 °C post which, the tan 6 kept increasing signifying the viscous nature of the 5% magnesium oxysulphate whisker filled composites. The polypropylene composite with 5% whisker had the highest damping especially at temperatures around 100 C. PP-g-MA addition served to further lower the tan 6 of the composites that proved that matrix modification served to further improve the filler - matrix interphase. 20% and 30% basalt fiber dosage served to further lower the tan 6 of the whisker filled and basalt fiber reinforced polypropylene composites due to the reinforcing behavior of basalt fibers at increasing dosage levels through the establishment of the fiber-matrix interphase. Also, the tan 6 plots pointed to a single a - transition that happened between 70 - 85 °C.
[047] The plot of peak of tan 6 curve (a - transition) of the 5% magnesium oxysulphate filled basalt fiber reinforced polypropylene composites with 6.4mm initial fiber length is given in figure 10.
[048] 5% magnesium oxysulphate whisker addition served to slightly increase the a - transition temperature from 79 °C to 80 C. This further rose to 83 °C upon PP-g-MA addition thereby signifying the establishment of a whisker - matrix interphase. 20% basalt fiber addition slightly lowered the a - transition temperature to 83 C. This shift in the a - transition temperature peak points to the reinforcing nature of the basalt fiber that served in increasing the modulus through the establishment of an adequate fiber - matrix interphase. However, reduction in fiber length especially in case of 30% basalt fiber reinforced polypropylene composite points to the reduced fiber reinforcing efficiency at 30% fiber dosage as compared to 20% fiber dosage. The shift in the a - transition temperature was significant for the 20% basalt fiber reinforced matrix modified composite that saw the temperature to increase from 79 °C to 84 C.
[049] The storage modulus plot of the 10% Magnesium oxysulphate whisker filled and basalt fiber reinforced polypropylene composites with 6.4mm initial fiber length is given in figure 11.
[050] At 40 °C, neat polypropylene had a storage modulus of 905MPa. 10% addition of magnesium oxysulphate whiskers increased the storage modulus of the Magnesium oxysulphate whisker filled polypropylene to 1621MPa. This is due to the reinforcing effect of the whiskers. Addition of PP-g-MA further increased the storage modulus to 2028MPa. This signified the whisker - matrix interphase improvement through PP-g-MA addition. 20% addition of basalt fibers further increased the storage modulus increased the storage modulus to 2616MPa. The improvement in storage modulus upon increasing basalt fiber dosage is due to the reinforcing efficiency of the basalt fiber that served to increase the elasticity of the magnesium oxysulphate whisker filled and basalt fiber reinforced polypropylene composites. However, it is noted that whilst 20% addition of basalt fibers to 5% magnesium oxysulphate whisker filled polypropylene composite increased the storage modulus to 3098MPa, 20% basalt fiber addition to 10% magnesium oxysulphate whisker filled polypropylene composite caused a reduction in the storage modulus. Basalt fiber addition to 10% magnesium oxysulphate whiskerfilled composite increased the storage modulus of the resultant composites at 80°C. The storage modulus of 20% basalt fiber reinforced and 10% magnesium oxysulphate whisker filled polypropylene composite rose to 1723MPa as compared to 389MPa for neat polypropylene and 994MPa for whisker filled matrix modified PP composite. The loss modulus plot of the 10% Magnesium oxysulphate whisker filled and basalt fiber reinforced polypropylene composites with 6.4mm initial fiber length is given in figure 12.
[051] At 40 °C, the loss modulus of neat polypropylene was 48MPa. This rose to 63MPa upon % magnesium oxysulphate whisker addition. The addition of whiskers reinforced the polypropylene as was evident from the enhanced heat dissipation. PP-g-MA addition further increased the loss modulus to 90MPa. This increase is attributed to the establishment of a fiber matrix interphase. Interestingly, addition of 20% basalt fibers to the 10% magnesium oxysulphate whisker filled matrix modified polypropylene composite caused a reduction in the loss modulus value at temperatures till -80 C. However, at 80 °C, the loss modulus of the 20% basalt fiber reinforced and 10% magnesium oxysulphate whisker filled polypropylene composite was the highest at 104MPa signifying maximum heat dissipation upon basalt fiber addition through the establishment of a fiber - matrix interphase. The tan 6 plot of the 10% magnesium oxysulphate whisker filled and basalt fiber reinforced polypropylene composites with 6.4mm initial fiber length is given in figure 13.
[052] Neat polypropylene had the highest tan 6 signifying that the material had the highest damping. 10% magnesium oxysulphate whisker addition reduced the tan 6. PP-g-Ma addition decreased the tan 6 at temperatures up to -85 °C post which, the tan6 kept increasing signifying the viscous nature of the 10% magnesium oxysulphate whisker filled and matrix modified polypropylene composites. The matrix modified polypropylene composite with 10% whisker had the highest damping especially at temperatures around 100 C. 20% basalt fiber dosage served to lower the tan 6 of the whisker filled and basaltfiber reinforced polypropylene composites due to the reinforcing behavior of basalt fibers at increasing dosage levels through the establishment of the fiber-matrix interphase. Also, the tan 6plots pointed to a single a - transition that happened between 70 - 85 C.
[053] The plot of peak of tan 6 curve (a - transition) of the 10% magnesium oxysulphate filled basalt fiber reinforced polypropylene composites with 6.4mm initial fiber length is given in figure 14.
[054] 10% magnesium oxysulphate whisker addition did not alter the a- transition temperature of the polypropylene. Interestingly PP-g-MA addition also did not alter the a - transition temperature of the polypropylene. 20% basalt fiber addition increased the a - transition temperature to 81 C. This shift in the a - transition temperature peak points to the reinforcing nature of the basalt fiber that served in increasing the modulus through the establishment of an adequate fiber - matrix interphase.
Tensile properties
[055] A graph comparing the tensile strength and tensile modulus of 5% MOS filled polypropylene composites is given in figure 15. Neat polypropylene had a tensile strength of MPa. This did not increase upon 5% magnesium oxysulphate whisker addition. This could possibly be due to agglomeration arising out of a lack of adequate surface treatment of the whisker for adhesion to polypropylene. PP-g-MA addition increased the tensile strength of the 5% magnesium oxysulphate whisker filled polypropylene composite to 30MPa. This is attributed to the establishment of a whisker - polypropylene interphase through PP-g-MA addition.
[056] The addition of 20% basalt fibers to the 5% magnesium oxysulphate whisker filled polypropylene composite increased the tensile strength to 57MPa which was a 90% improvement over that of the composite without basalt fibers. Basalt fibers reinforced the polypropylene and served to synergistically increase the tensile strength of the composites. This behavior was evident in case of 30% basalt fiber addition that resulted in increasing the tensile strength further to 63MPa which was a 110% increment over the composite without basalt fibers. As compared to neat polypropylene, both the 30% basalt fiber and 5% magnesium oxysulphate whisker addition synergistically improved the tensile strength by 215% as compared to neat polypropylene. Interestingly, the tensile strength of 30% basalt fiber reinforced and 5% magnesium oxysulphate whisker filled and matrix modified polypropylene was not significant as compared to that of the composite having 20% basalt fibers. This could be due to the reduction in meanfiber length arising due to increased fiber loading (30% as compared to 20%). Increased fiber loading leads to higher fiber - fiber and fiber - machine interactions thereby lowering the fiber reinforcing efficiency as the fiber length becomes lower than the critical fiber length. Again, this could also be attributed to fiber packing and increased stress concentration. The improvement in tensile strength of the basalt fiber reinforced composites was accompanied with a drop in the elongation at yield. As compared to neat polypropylene resin, the elongation at yield of 5% magnesium oxysulphate whisker filled polypropylene composite reduced slightly from 5% to 4%. This dropped further to 3% upon PP g-MA addition thereby signifying the reinforcement upon establishment of a fiber-matrix interphase. The elongation at yield was restored to 5% upon both 20% and 30% basalt fiber addition. Neat polypropylene had a tensile modulus of 904MPa. This rose to 1333MPa upon 5% magnesium oxysulphate whisker filling. PP-g-MA addition further increased it to 1671MPa. 20% basalt fiber addition to the 5% magnesium oxysulphate whisker filled matrix modified polypropylene composite further increased the tensile modulus to 4236MPa which was a 154% increment as compared to the composite without basalt fibers. 30% basalt fiber addition to 5% magnesium oxysulphate whisker filled matrix modified composite increased the tensile modulus of the resultant composite by 60%. However, as compared to the 20% basalt fiber reinforced and % magnesium oxysulphate whisker filled matrix modified composite, the tensile modulus of the % basalt fiber reinforced and 5% magnesium oxysulphate whisker filled matrix modified composite was lower by 37%. Low mean fiber length, high fiber content and increased fiber packing could be attributed to the reasons behind the drop in the tensile modulus of the 30% basalt fiber reinforced polypropylene.
[057] A graph comparing the tensile properties of 10% MOS filled, and basalt fiber reinforced polypropylene composite is given in figure 16.
[058] Neat polypropylene had a tensile strength of 20MPa. This rose to 32MPa upon addition of % magnesium oxysulphate whisker. This is attributed to the reinforcing nature of the magnesium oxysulphate whisker. Interestingly, PP-g-MA addition caused a drop in the tensile strength of the resultant composite to 22MPa. 20% basalt fiber addition to the 10% magnesium oxysulphate whisker filled polypropylene composite increased the tensile strength to 55MPa which was a 150% improvement as compared to the composite without basalt fibers. The elongation at yield of neat polypropylene was 5%. This dropped to 3% upon addition of 10% magnesium oxysulphate whisker. PP-g-MA addition did not cause any change to the elongation at yield values. 20% basalt fiber addition to the 10% magnesium oxysulphate whisker filled polypropylene composite increased the elongation at yield and brought it back to that of the neat polypropylene (5%). This is attributed to the reinforcing nature of the basalt fibers.
[059] The tensile modulus rose concomitantly with the addition of 10% magnesium oxysulphate whisker by 72%. PP-g-MA addition further increased the modulus by 85% as compared to neat polypropylene. 20% basalt fiber addition to the 10% magnesium oxysulphate whisker filled and matrix modified polypropylene composite further increased the tensile modulus by 157% as compared to neat polypropylene. 20% basalt fiber addition accounted for 40% improvement in modulus as compared to that of the matrix modified and 10% magnesium oxysulphate whisker filled polypropylene composite without basalt fiber. This was a significant reduction (45%) from the modulus values obtained for 20% basalt fiber reinforced and 5% magnesium oxysulphate whisker filled matrix modified polypropylene composite.
[060] The reinforcing efficiency of basalt fibers and whiskers were reduced at 20% and 10% loading levels respectively. In all, the 20% basalt fiber reinforced and 5% magnesium oxysulphate filled matrix modified polypropylene composite relatively had better tensile properties as compared to other composites.
Flexural properties
[061] A graph comparing the flexural strength and flexural modulus of 5% MOS filled, and basalt fiber reinforced polypropylene composites is given in figure 17. Neat polypropylene had a flexural strength of 22MPa. This rose to 26MPa upon addition of 5% magnesium oxysulphate whisker. PP- g-MA addition enhanced the flexural strength to 26MPa through the establishment of a filler matrix interphase. 20% addition of basalt fibers led to an enhancement of the flexural strength of the composites by 78% as compared to the magnesium oxysulphate whisker filled matrix modified polypropylene composite. This was a 191% improvement as compared to neat polypropylene. Similarly, 30% addition of basalt fibers led to further enhancement of the flexural strength of the resultant composites by 106%. This was a 236% improvement as compared to neat polypropylene. This is attributed for the better interphase between the polypropylene matrix, magnesium oxysulphate whisker filled and the basalt fiber. The flexural modulus of the basalt fiber reinforced polypropylene composites increased with the 5% magnesium oxysulphate whisker filler loading. Addition of PP-g-MA further improved the flexural modulus further. Basalt fiber addition increased the flexural modulus further. The flexural modulus of a fiber reinforced composite depended on the fiber volume fraction, fiber orientation, resin and fiber modulus and to a lesser extent on the fiber length. Hence, with increasing fiber volume fraction, the flexural modulus continued to improve. The 30% basalt fiber reinforced and 5% magnesium oxysulphate whisker filled polypropylene composite had the highest flexural modulus of 4008MPa which was a 343% improvement as compared to neat polypropylene. This signified the synergistic role played by both magnesium oxysulphate whisker and basalt fiber in enhancing the flexural properties of the composites. A graph comparing the flexural properties of 10% magnesium oxysulphate whisker filled and basalt fiber reinforced polypropylene composites is given in figure 18.
[062] Neat polypropylene had a flexural strength of 22MPa. This rose to 33MPa upon addition of 10% magnesium oxysulphate whisker. Interestingly, PP-g-MA addition lowered the flexural strength to 27MPa. This might be due to agglomeration issues with the 10% magnesium oxysulphate filled matrix modified polypropylene composite. 20% addition of basalt fibers led to an enhancement of the flexural strength of the composites by 119% as compared to the magnesium oxysulphate whisker filled matrix modified polypropylene composite. This was a 168% improvement as compared to neat polypropylene. This is attributed for the better interphase between the polypropylene matrix, magnesium oxysulphate whisker filled and the basalt fiber. The flexural modulus of the basalt fiber reinforced polypropylene composites increased with the 10% magnesium oxysulphate whisker filler loading. Addition of PP-g-MA further improved the flexural modulus further. Basalt fiber addition increased the flexural modulus further. Flexural modulus of a fiber reinforced composite depended on the fiber volume fraction, fiber orientation, resin and fiber modulus and to a lesser extent on the fiber length. Hence, with increasing fiber volume fraction, the flexural modulus continued to improve.
[063] The 20% basalt fiber reinforced and 10% magnesium oxysulphate whisker filled polypropylene composite had the highest flexural modulus of 2555MPa which was a 183% improvement as compared to neat polypropylene. This signified the synergistic role played by both magnesium oxysulphate whisker and basalt fiber in enhancing the flexural properties of the composites. However, the flexural modulus of the 20% basalt fiber reinforced and 10% magnesium oxysulphate whisker filled polypropylene composite was low than the 20% basalt fiber reinforced and 5% magnesium oxysulphate whisker filled polypropylene composite. This is attributed mainly due to the agglomeration and dispersion issues associated with 10% whisker loading as compared to 5% whisker loading.
Impact properties
[064] A graph comparing the Izod impact properties of the 5% magnesium oxysulphate whisker filled and basalt fiber reinforced polypropylene composites with 6.4mm initial fiber length is given in figure 19.
[065] Notched impact strength captures the energy required for crack propagation through the sample. The room temperature notched Izod impact strength of polypropylene was retained upon addition of 5% magnesium oxysulphate whisker filler. This dropped by 84% upon PP-g-MA signifying an improved whisker - matrix interphase. Basalt fiber presence increased the energy dissipation by absorbing the impact energy. 20% basalt fiber addition increased the notched Izod impact strength by 157% as compared to the matrix modified whisker filled polypropylene composite without basalt fiber. 30% basalt fiber addition increased it further by 11% thereby resulting in 186% increase as compared to the matrix modified whiskerfilled polypropylene composite without basalt fiber. Fiber content in the composite governs the notched impact strength of the composite. Increasing the fiber content works towards improving the impact strength of the composites. Typically, the chief failure mechanisms during impact include deformation and matrix crack in the area before the crack tip and transfer of the load to the fiber that exceeds the interfacial shear strength between the fiber and matrix thereby resulting in matrix debonding. Addition of basalt fibers to polypropylene matrix reduced the room temperature Izod impact strength of the composites.
[066] The presence of an adequate fiber - matrix interphase is the cause for the reduction in impact strength. Another cause is insufficient fibre length. The addition of PP-g-MA as a matrix modifier to the basalt fiber reinforced composites effected an improvement in the Izod impact strength and hence the toughness of the composites. The improvement in impact strength in has been attributed to energy dissipation through fiber pull-out. 5% magnesium oxysulphate whisker addition to polypropylene served to reduce the low temperature notched Izod impact strength of the resultant composite. The addition of PP-g-MA increased the Izod impact strength at -30°C. The Izod impact strength of both 20% and 30% basalt fiber reinforced matrix modified composite exceeded that of pure polypropylene. 30% basalt fiber reinforced and 5% magnesium oxysulphate whisker filled matrix modified polypropylene composite had the highest low temperature impact strength at 12KJ/m 2 . This improvement in the -30 °C notched Izod impact performance is attributed to the reduced contribution of the matrix and more contribution from the fiber. A graph comparing the impact properties of 10% magnesium oxysulphate whisker filled and 6.4mm basalt fiber reinforced polypropylene composites is given in figure 20.
[067] The room temperature notched Izod impact strength of polypropylene reduced upon addition of 10% magnesium oxysulphate whisker filler. This could be mainly attributed to the agglomeration of whiskers. Addition of PP-g-MA increased whisker dispersion. This resulted in restoring the notched Izod impact strength of the whiskerfilled matrix modified polypropylene composite. Basalt fiber presence increased the energy dissipation by absorbing the impact energy. The energy dissipation happened through fiber pull-out. 10% magnesium oxysulphate whisker addition to polypropylene served to reduce the low temperature notched Izod impact strength of the resultant composite. Addition of PP-g-MA further reduced the Izod impact strength at -30°C. The Izod impact strength of both 20% and 30% basalt fiber reinforced matrix modified composite exceeded that of pure polypropylene. 30% basalt fiber reinforced and 5% magnesium oxysulphate whisker filled matrix modified polypropylene composite had the highest low temperature impact strength at 12KJ/m 2 . This improvement in the -30 °C notched Izod impact performance is attributed to the reduced contribution of the matrix and more contribution from the fiber.
Tensile fracture surface characterization using scanning electron microscopy (SEM)
[068] The tensile fractured surfaces of 5% magnesium oxysulphate whisker filled polypropylene was observed under a scanning electron microscope (SEM) 5% Magnesium oxysulphate whisker reinforced the whisker and upon tensile loading, the composite exhibited ductile behavior (Figure 21a). Agglomeration of magnesium oxysulphate whiskers were also observed in the SEM images. PP-g-MA addition ensured better dispersion of the whiskers and led to a composite without much agglomeration. This resulted in a composite that failed in a ductile manner upon tensile loading (Figure 21b).
[069] Heavy agglomeration of the whisker was observed in the tensile fractured surface of 10% magnesium oxysulphate whisker filled polypropylene composites as given below (Figure 22a). This was coupled with inadequate fiber - matrix interphase. Inadequate fiber - matrix interphase was observed in the 20% basalt fiber reinforced and 10% magnesium oxysulphate whisker filled matrix modified polypropylene composite as could be seen from the image below (Figure 22b). This could be the reason for the poor tensile properties of the composite.
[070] The following composite formulations were prepared according to the invention:
Table 6 Formulation Chemical Component (%) '40. Heterophasic Antioxidant Polypropylene- Magnesium Basalt nucleated (Blend of 67% tris(2,4- graft-Maleic Oxysulphate Fiber polypropylene ditert- Anhydride 6.4 mm impact copolymer butylphenyl)phosphite and 33% pentaerythritol tetrakris(3-(3,5-di-tert butyl-4 hydroxphenyl)propionate) 1. 99.8 0.2 2. 94.8 0.2 5 3. 89.8 0.2 5 5 4. 69.8 0.2 5 5 20 5. 59.8 0.2 5 5 30 6. 99.8 0.2 7. 89.8 0.2 10 8. 84.8 0.2 5 10 9. 64.8 0.2 5 10 20
[071] The formulation No. 4 was tested for the thermo-mechanical properties and exhibited the following properties:
Table 7
Property Unit Hybrid 20% basalt fiber reinforced and 5% magnesium oxysulphate filled polypropylene impact copolymer
Tensile strength MPa 57
Tensile modulus MPa 4236
Flexural strength MPa 64
Flexural modulus MPa 3322
Izod impact strength at KJ/m 2 18 23 0 C Izod impact strength at - KJ/m 2 9 300 C
[072] Advantageously, the present invention provides a composite polymer material, the composite comprising basalt fiber and magnesium oxysulphate in polymer. These composite exhibits good strength and stiffness without compromising on the toughness, improved low temperature impact strength and is eco-friendly as it is derived from natural rocks.
[073] The foregoing description of the invention has been set merely to illustrate the invention and is not intended to be limiting. While the present invention has been described with respect to certain embodiments, it will be apparent to those skilled in the art that various changes and modification may be made without departing from the scope of the invention as defined in the following claims.
[074] It will be understood that the terms "comprise" and "include" and any of their derivatives (e.g. comprises, comprising, includes, including) as used in this specification, and the claims that follow, is to be taken to be inclusive of features to which the term refers, and is not meant to exclude the presence of any additional features unless otherwise stated or implied.
Claims (10)
- The claims defining the invention are as follows: 1. A polymer composite comprising: At least one polymer, basalt fiber and magnesium oxysulphate filler.
- 2. The polymer composite as claimed in claim 1, wherein at least one polymer is present in a range of 55 - 95%, the basalt fiber is present in a range of 5 - 40% and magnesium oxysulfate filler is present in a range of 1 - 20%.
- 3. The polymer composite as claimed in claim 1 or 2, wherein at least one polymer is selected from polypropylene, polyamide, polybutylene terephthalate, polylactic acid and copolymer thereof.
- 4. The polymer composite as claimed in any one of claims I to 3, wherein the basalt fiber has fiber length in range of 3 - 10mm.
- 5. The polymer composite as claimed in any one of claims 1 to 4, wherein the basalt fiber is treated by either roughening through a chemical treatment or by functionalization like silane treatment, acid treatment, alkali treatment, plasma treatment or nanomaterial deposition.
- 6. The polymer composite as claimed in claim 5, wherein the silane treatment is carried out with a coupling agent selected from 3-(aminopropyl)triethoxysilane (APS) 3 (glycidoxypropyl)trimethoxysilane (GPS), (N-(2-aminoethyl)-11 aminoundecyltrimethoxysilane), 1,2- ethylenebis(trimethoxysilane) and vinyltriethoxysilane.
- 7. The polymer composite as claimed in any one of claims 1 to 6, wherein the composite is modified either by adding compatibilizer or coupling agents, wherein the compatibilizer is Polypropylene-graft-Maleic anhydride (PP-g-MA).
- 8. The polymer composite as claimed in any one of claims 1 to 7, wherein the composite further comprises an additive selected from antioxidants, coupling agent, UV stabilizers, compatibilizers, nucleating agents, anti-static additives, nanomaterials, flame retardants and mixture thereof.
- 9. The polymer composite as claimed in claim 8, wherein the nanomaterial is selected from carbon nanotubes, graphene, nano-silica, nano-calcium carbonate, nano calcium pimelate, nanocellulose and mixture thereof.
- 10. The polymer composite as claimed in claim 8, wherein the antioxidant is selected from tris(2,4-ditert-butylphenyl) phosphite, pentaerythritol tetrakris(3-(3,5-di-tert-butyl-4- hydroxphenyl)propionate, Pentaerythritol tetrakis(3,5-di-tert-butyl-4 hydroxyhydrocinnamate and mixture thereof.
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