石墨烯/聚酰胺6纤维的混合熔融纺丝工艺及性能
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摘要
采用溶液混合冷冻干燥法制备了质量分数0.004%的石墨烯/聚酰胺6(PA6)粒料,再用2种工艺制备石墨烯/PA6纤维——石墨烯/PA6粒料直接熔融纺丝;石墨烯/PA6粒料加入双螺杆挤出机熔融混合、挤出、造粒、熔融纺丝。用万能试验机测试了纤维的拉伸性能;用差示扫描量热分析测试了纤维的熔融行为并计算了结晶度;用扫描电镜(SEM)观察了石墨烯/PA6纤维的微观形态。研究结果表明,微量石墨烯的加入能够显著改善PA6纤维的拉伸性能,制备的石墨烯/PA6纤维的拉伸强度和拉伸模量分别可达到270 MPa和9.4GPa;工艺一制备的石墨烯/PA6纤维的热力学性能优于工艺二;较高的熔融纺丝温度可提高纤维的拉伸强度、拉伸模量、熔点和结晶度;SEM分析表明,石墨烯较均匀地分散在PA6基体中,纤维表面均匀,无明显瑕疵。
Solution mixing and freeze-drying method were used to prepare graphene/polyamide 6(PA 6)pellets with 0.004% graphene.Then,graphene/PA6 fibers were prepared by the following two processes respectively:one process is that graphene/PA6 pellets were directly used into melt spinning;the second process includes twin screw extrusion for the melting and remixing of graphene/PA6 pellets,granulation and melt spinning.Electronic universal testing machine was used to test the tensile properties of the graphene/PA6 fiber,DSC was used to analyze the melting behavior of graphene/PA6 fibers and calculate the crystallinity,and SEM was used to observe the morphology of graphene/PA6 fiber.Results show that the tensile properties of the fiber are improved by incorporating with a small amount of graphene,the tensile strength and modulus of the graphene/PA6 fiber could rise up to 270 MPa and 9.4 GPa respectively;graphene/PA6 fibers prepared by process one have better mechanical and thermodynamic performance than those prepared by process two;increasing the melt spinning temperature can improve the tensile strength,tensile modulus,melting point and crystallinity of the graphene/PA6 fibers;SEM images show that graphene is uniformly dispersed in the PA6 matrix and the surface of fiber does not present obvious defects.
Solution mixing and freeze-drying method were used to prepare graphene/polyamide 6(PA 6)pellets with 0.004% graphene.Then,graphene/PA6 fibers were prepared by the following two processes respectively:one process is that graphene/PA6 pellets were directly used into melt spinning;the second process includes twin screw extrusion for the melting and remixing of graphene/PA6 pellets,granulation and melt spinning.Electronic universal testing machine was used to test the tensile properties of the graphene/PA6 fiber,DSC was used to analyze the melting behavior of graphene/PA6 fibers and calculate the crystallinity,and SEM was used to observe the morphology of graphene/PA6 fiber.Results show that the tensile properties of the fiber are improved by incorporating with a small amount of graphene,the tensile strength and modulus of the graphene/PA6 fiber could rise up to 270 MPa and 9.4 GPa respectively;graphene/PA6 fibers prepared by process one have better mechanical and thermodynamic performance than those prepared by process two;increasing the melt spinning temperature can improve the tensile strength,tensile modulus,melting point and crystallinity of the graphene/PA6 fibers;SEM images show that graphene is uniformly dispersed in the PA6 matrix and the surface of fiber does not present obvious defects.
引文
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[2]Nilsson E,Oxfall H,Wandelt W,et al.Melt spinning of conductive textile fibers with hybridized graphite nanoplatelets and carbon black filler[J].J.Appl.Polym.Sci.,2013,130:2579-2587.
[3]Khan U,Young K,O'Neill A,et al.High strength composite fibres from polyester filled with nanotubes and graphene[J].J.Mater.Chem.,2012,22:12907-12914.
[4]Chatterjee S,Nüesch F,Chu B.Crystalline and tensile properties of carbon nanotube and graphene reinforced polyamide-12fibers[J].Chem.Phys.Lett.,2012,557:92-96.
[5]Mack J J,Viculis L M,Ali A,et al.Graphite nanoplatelet reinforcement of electrospun polyacrylonitrile nanofibers[J].Adv.Mater.,2005,17:77-80.
[6]Wang B,Chen Z,Zhang J,et al.Fabrication of PVA/graphene oxide/TiO2composite nanofibers through electrospinning and interface sol-gel reaction:effect of graphene oxide on PVA nanofibers and growth of TiO2[J].Colloids Surf.,A,2014,457:318-325.
[7]Rafiee M A,Rafiee J,Wang Z,et al.Enhanced mechanical properties of nanocomposites at low graphene content[J].ACS Nano,2009,3:3884-3890.
[8]Fu X,Yao C,Yang G.Recent advances in graphene/polyamide 6composites:a review[J].RSC Adv.,2015,5:61688-61702.
[9]Liu H H,Peng W W,Hou L C,et al.The production of a meltspun functionalized graphene/poly(e-caprolactam)nanocomposite fiber[J].Compos.Sci.Technol.,2013,81:61-68.
[10]Hwang S H,Kim B J,Baek J B,et al.Effects of process parameters and surface treatments of graphene nanoplatelets on the crystallinity and thermomechanical properties of polyamide 6composite fibers[J].Composites Part B,2016,100:220-227.
[11]Hou W,Tang B,Lu L,et al.Preparation and physico-mechanical properties of amine-functionalized graphene/polyamide 6nanocomposite fiber as a high performance material[J].RSC Adv.,2014,4:4848-4855.
[12]Medellin-Rodriguez F J,Larios-Lopez L,Zapata-Espinoza A,et al.Melting behavior of polymorphics:molecular weight dependence and steplike mechanisms in nylon-6[J].Macromolecules,2004,37:1799-1809.