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Investigations in annealing effects on structure and properties of β-isotactic polypropylene with X-ray synchrotron experiments

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Abstract

The influence of annealing on the microstructure and mechanical properties of β-form isotactic polypropylene (iPP) was investigated via in situ synchrotron small-angle X-ray scattering (SAXS), wide-angle X-ray diffraction (WAXD), and differential scanning calorimetry (DSC). Transition of β-iPP to α-iPP was investigated via recrystallization at high annealing temperatures (T a > 120 °C). And crystallinity, crystal sizes, and long period of ordered structure increased with increasing annealing temperature. Abrupt changes were found in both mechanical properties and structural features at the same T a range (∼120 °C). The in situ synchrotron SAXS and WAXD shows that the destruction of b phase at yielding and after yielding should account for the ductility of β-iPP. The thermodynamics and kinetics of annealing were investigated with DSC and X-ray synchrotron experiments. A characteristic annealing time was investigated, which measures the rate of phase evolution in annealing of β-iPP. Eventually, a hypothesized model can be used to describe the property/structure relations during this process.

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References

  1. Wu HY, Li XX, Wang YH et al (2011) Fracture behaviors of isotactic polypropylene/poly(ethylene oxide) blends: effect of annealing. Mater Sci Eng A 528:8013–8020

    Article  CAS  Google Scholar 

  2. Nitta KH, Odaka K (2009) Influence of structural organization on tensile properties in mesomorphic isotactic polypropylene. Polymer 50:4080–4088

    Article  CAS  Google Scholar 

  3. Colombe G, Gree S, Lhost O (2011) Correlation between mechanical properties and orientation of the crystalline and mesomorphic phases in isotactic polypropylene fibers. Polymer 52:5630–5643

    Article  CAS  Google Scholar 

  4. Zhao JC, Qiu J, Niu YH, Wang ZG (2009) Evolution of morphology and crystalline ordering upon annealing of quenched isotactic polypropylene. J Polym Sci B 47:1703–1712

    Article  CAS  Google Scholar 

  5. Ran SF, Zong XH, Fang DF (2001) Structural and morphological studies of isotactic polypropylene fibers during heat/draw deformation by in-situ synchrotron SAXS/WAXD. Macromolecules 34:2569–2578

    Article  CAS  Google Scholar 

  6. Coulon G, Castelein G, G’Sell C (1999) Scanning force microscopic investigation plasticity and damage mechanisms in polypropylene spherulites under simple shear. Polymer 40:95–110

    Article  CAS  Google Scholar 

  7. Aboulfaraj M, G’Sell C, Ulrich B, Dahoun A (1995) In situ observation of the plastic deformation of polypropylene spherulites under uniaxial tension and simple shear in the scanning electron microscope. Polymer 36:731–742

    Article  CAS  Google Scholar 

  8. Tordjeman P, Robert C, Marin G, Gerard P (2001) The effect of α, β crystalline structure on the mechanical properties of polypropylene. Eur Phys J E 4:459–465

    Article  CAS  Google Scholar 

  9. Henning S, Adhikari R, Michler GH, Balta- Calleja FJ, Karger-Kocsis J (2004) Macromechanical mechanisms for toughness enhancement in β-modified polypropylene. Macromol Symp 214:157–171

    Article  CAS  Google Scholar 

  10. Chen HB, Karger-kocsis J, Wu JS, Varga J (2002) Fracture toughness of α- and β- phase polypropylene homopolymers and random- and block-copolymers. Polymer 43:6505–6514

    Article  CAS  Google Scholar 

  11. Karger-Kocsis J, Varga J, Ehrenstein GW (1997) Comparison of the fracture and failure behavior of injection-molded α- and β-polypropylene in high-speed three-point bending tests. J Appl Polym Sci 64:2057–2066

    Article  CAS  Google Scholar 

  12. Luo F, Geng CZ, Wang K et al (2009) New understanding in tuning toughness of β-polypropylene: the role of β-nucleated crystalline morphology. Macromolecules 42:9325–9331

    Article  CAS  Google Scholar 

  13. Bai HW, Wang Y, Zhang ZJ et al (2009) Influence of annealing on microstructure and mechanical properties of isotactic polypropylene with β-phase nucleating agent. Macromolecules 42:6647–6655

    Article  CAS  Google Scholar 

  14. Bai HW, Luo F, Zhou TN et al (2011) New insight on the annealing induced microstructural changes and their roles in the toughening of β-form polypropylene. Polymer 52:2351–2360

    Article  CAS  Google Scholar 

  15. Ferrer-Balas D, ML M, Martinez AB, Santana OO (2001) Influence of annealing on the microstructural, tensile and fracture properties of polypropylene films. Polymer 42:1697–1705

    Article  CAS  Google Scholar 

  16. Vittoria V (1989) Effect of annealing on the structure of quenched isotactic polypropylene. J Macromol Sci, Part B; Physics 28:489–502

    Article  Google Scholar 

  17. Na B, Li Z J, Lv R H, Zou S F. (2012) Annealing-induced structural rearrangement and its tougheningeffect in injection-molded isotactic polypropylene. Polymer Engineering and Science, 52(4):893–900

  18. Li XX, Wu HY, Han L et al (2010) Annealing induced microstructure and fracture resistance changes in isotactic polypropylene/ethylene-octene copolymer blends with and without β-phase nucleating agent. J Polym Sci B 48:2108–2120

    Article  CAS  Google Scholar 

  19. Li J, Bao RY, Yang W et al (2012) Effect of annealing temperature on the mechanical properties, thermal behavior and morphology of β-iPP/PA6 blends. Mater Des 40:392–399

    Article  CAS  Google Scholar 

  20. Alberola N, Fugier M, Fetit D, Fillon B (1995) Microstructure of quenched and annealed films of isotactic polypropylene. J Mater Sci 30:1187–1195

    Article  CAS  Google Scholar 

  21. Poussin L, Bertin YA, Parisot J, Brassy C (1998) Influence of thermal treatment on the structure of an isotactic polypropylene. Polymer 39:4261–4265

    Article  CAS  Google Scholar 

  22. Martorana A, Piccarolo S, Sapoundjieva D (1999) SAXS/WAXD study of the annealing process in quenched samples of isotactic poly(propylene). Macromol Chem Phys 200:531–540

    Article  CAS  Google Scholar 

  23. Hedesiu C, Demco DE, Kleppinger R et al (2007) Effect of temperature and annealing on the phase composition, molecular mobility, and the thickness of domains in isotactic polypropylene studied by proton solid-state NMR, SAXS, and DSC. Macromolecules 40:3977–3989

    Article  CAS  Google Scholar 

  24. Wu HY, Li XX, Xiang FM et al (2012) Microstructure evolution of isotactic polypropylene during annealing: effect of poly(ethylene oxide). Chin J Polym Sci 30:199–208

    Article  CAS  Google Scholar 

  25. Drozdov AD, Christiansen JD (2003) The effect of annealing on the nonlinear viscoelastic response of isotactic polypropylene. Polym Eng Sci 43:946–958

    Article  CAS  Google Scholar 

  26. Varga J (1989) β-Modification of polypropylene and its two-component systems. J Therm Anal Calorim 35:1891–1912

    Article  CAS  Google Scholar 

  27. Cho K, Saheb DN, Yang H et al (2003) Memory effect of locally ordered α-phase in the melting and phase transformation behavior of β-isotactic polypropylene. Polymer 44:4053–4059

    Article  CAS  Google Scholar 

  28. Han L, Li XX, Li YL et al (2010) Influence of annealing on microstructure and physical properties of isotactic polypropylene/calcium carbonate composites with β-phase nucleating agent. Material Science and Engineering A 527:3176–3185

    Article  Google Scholar 

  29. Turner-Jones A, Aizlewood JM, Beckett DR (1964) Crystalline forms of isotactic polypropylene. Macromol Chem Phys 75:134–159

    Article  CAS  Google Scholar 

  30. Cai ZW, Zhang Y, Li JQ et al (2012) Real time synchrotron SAXS and WAXS investigations on temperature related deformation and transition of β-iPP with uniaxial stretching. Polymer 7:1593–1601

    Article  Google Scholar 

Download references

Acknowledgments

This work was supported by the National Natural Science Foundation of China (51173130, 20974077, 21204062).

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Correspondence to Yingrui Shang.

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Shang, Y., Zhao, J., Li, J. et al. Investigations in annealing effects on structure and properties of β-isotactic polypropylene with X-ray synchrotron experiments. Colloid Polym Sci 292, 3205–3221 (2014). https://doi.org/10.1007/s00396-014-3368-8

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  • DOI: https://doi.org/10.1007/s00396-014-3368-8

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