Skip to main content
SpringerLink
Log in

Crystalline behaviors and phase transition during the manufacture of fine denier PA6 fibers

  • Published:
Science in China Series B: Chemistry Aims and scope Submit manuscript

Abstract

Recently we have successfully produced fine denier PA6 fibers by using additives containing lanthanide compounds. Meanwhile, crystallization and phase transition of PA6 fibers during spinning and drawing processes were investigated. During the spinning process, β phase crystal could be obtained in as-spun PA6 fibers which were produced with relatively high melt draw ratio, while γ phase crystal predominated when the melt draw ratio was relatively low. β phase crystal, whose behaviors are similar with those of γ phase by FT-IR and XRD characterization, could be transformed to α form easily when PA6 fibers are immersed in boiling water. However, γ phase crystal of PA6 remains unchanged in boiling water. Thus, β and γ phase crystals of PA6 can be differentiated by the crystalline behaviors of PA6 fibers after treatment in boiling water. Further experiments demonstrate that the β phase can also be produced during a drawing process where a phase transformation from γ to α occurs. In other words, β phase may act as an intermediate state during the phase transformation.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Similar content being viewed by others

References

  1. Acierno D, Lamantia F P, Polizzotti G, Ciferri A. Bulk properties of synthetic polymer inorganic salt systems 5. Mechanical-properties of oriented poly(caproamide). J Poly Sci Part B-Poly Phys, 1979, 17(11): 1903–1912

    CAS  Google Scholar 

  2. Acierno D, Lamantia F P, Polizzotti G, Alfonso G C, Ciferri A. Increasing elastic-modulus of polyamides. J Poly Sci Part C-Poly Lett, 1977, 15(6): 323–327

    CAS  Google Scholar 

  3. Roberts M F, Jenekhe S A. Lewis acid complexation of polymers: Gallium chloride complex of PA6. Chem Mater, 1990, 2(3): 224–226

    Article  CAS  Google Scholar 

  4. Roberts M F, Jenekhe S A. Site-specific reversible scission of hydrogen bonds in polymers: An investigation of polyamides and their Lewis acid-base complexes by infrared spectroscopy. Macromolecules, 1991, 24(11): 3142–3146

    Article  CAS  Google Scholar 

  5. Vasanthan N, Kotek R, Jung D W, Shin D, Tonellia E, Salem D R. Lewis acid-base complexation of polyamide 66 to control hydrogen bonding, extensibility and crystallinity. Polymer, 2004, 45(12): 4077–4085

    Article  CAS  Google Scholar 

  6. Kotek R, Jung D, Tonelli A E, Vasanthan N. Novel methods for obtaining high modulus aliphatic polyamide fibers. J Macromol Sci-Poly Rev, 2005, C45(3): 201–230

    Article  Google Scholar 

  7. Afshari M, Gupta A, Jung D, Kotek R, Tonelli A E, Vasanthan N. Properties of films and fibers obtained from Lewis acid-base complexed nylon 6,6. Polymer, 2008, 49(5): 1297–1304

    Article  CAS  Google Scholar 

  8. Xu Y Z, Sun W X, Li W H, Hu X B, Zhou H B, Weng S F, Zhang F, Zhang X X, Wu J G, Xu D F, Xu G X. Investigation on the interaction between polyamide and lithium salts. J Appl Poly Sci, 2000, 77(12): 2685–2690

    Article  CAS  Google Scholar 

  9. Xie A F, Tao D L, Zhang Z B, Xu Y Z, Wu Y J, Hu T D, Gu B Y, Wu J G, Yang G Z, Xu D F. The coordination and phase separation in nylon-copper chloride system. J Mol Struct, 2002, 613(1–3): 67–71

    Article  CAS  Google Scholar 

  10. Wu Y J, Xu Y Z, Wang D J, Zhao Y, Weng S F, Xu D F, Wu J G. FT-IR spectroscopic investigation on the interaction between nylon 66 and lithium salts. J Appl Poly Sci, 2004, 91(5): 2869–2875

    Article  CAS  Google Scholar 

  11. Li H Z, Wu Y J, Sato H, Kong L, Zhang C F, Huang K, Tao D L, Chen J, Liu X X, Zhao Y, Xu Y Z, Wu J G, Ozaki Y. A new facile method for preparation of nylon-6 with high crystallinity and special morphology. Macromolecules, 2009, 42(4): 1175–1179

    Article  CAS  Google Scholar 

  12. Holmes D R, Bunn C W, Smith D J. The crystal structure of polycaproamide—nylon-6. J Poly Sci, 1955, 17(83): 159–177

    Article  CAS  Google Scholar 

  13. Kinoshita Y. An investigation of the structures of polyamide series. Makromol Chem, 1959, 33(1): 1–20

    Article  CAS  Google Scholar 

  14. Ziabicki V A. Mesomorphe β-form von polycapronamid und ihre umwandlung in kristalline form α. Kolloid-Z, 1959, 2, 132–141

    Article  Google Scholar 

  15. Roldan L G, Kaufman H S. Crystallization of nylon 6. J Poly Sci Part B-Poly Lett, 1963, 1(11): 603–608

    Article  CAS  Google Scholar 

  16. Vogelsong D C. Crystal structure studies on polymorphic forms of nylons 6 and 8 and other even nylons. J Poly Sci Part A-Gen Pap, 1963, 1(3): 1055

    Article  CAS  Google Scholar 

  17. Arimoto H. α-γ Transition of nylon 6. J Poly Sci Part A-Gen Pap, 1964, 2(5): 2283–2294

    Article  CAS  Google Scholar 

  18. Arimoto H, Ishibash. M, Hirai M, Chatani Y. Crystal structure of gamma-form of nylon 6. J Poly Sci Part A -Gen Pap, 1965, 3(1): 317–326

    Article  CAS  Google Scholar 

  19. Miyasaka K, Makishim. K. transition of nylon 6 gamma-phase crystals by stretching in chain direction. J Poly Sci Part A-1: Poly Chem, 1967, 5(12): 3017–3027

    Article  CAS  Google Scholar 

  20. Ismat a-I. α-γ Transition in nylon 6. J Poly Sci Part A-1: Poly Chem, 1971, 9(1): 199–216

    Article  Google Scholar 

  21. Parker J P, Lindenmeyer P H. Crystal structure of nylon-6. J Appl Poly Sci, 1977, 21(3): 821–837

    Article  CAS  Google Scholar 

  22. Stepaniak R F, Garton A, Carlsson D J, Wiles D M. Examination of the crystal structures present in nylon-6 fibers. J Poly Sci Part B-Poly Phy, 1979, 17(6): 987–999

    CAS  Google Scholar 

  23. Heuvel H M, Huisman R. Effects of winding speed, drawing and heating on the crystalline-structure of nylon-6 yarns. J Appl Poly Sci, 1981, 26(2): 713–732

    Article  CAS  Google Scholar 

  24. Gianchandani J, Spruiell J E, Clark E S. Polymorphism and orientation development in melt spinning, drawing, and annealing of nylon-6 filaments. J Appl Poly Sci, 1982, 27(9): 3527–3551

    Article  CAS  Google Scholar 

  25. Murthy N S, Minor H, Latif R A. Effect of annealing on the structure and morphology of nylon 6 fibers. J Macromol Sci, Part B, 1987, 26(4): 427–446

    Article  Google Scholar 

  26. Salem D R, Moore R A F, Weigmann H D. Macromolecular order in spin-oriented nylon-6 (polycaproamide) fibers. J Poly Sci Part B-Poly Phys, 1987, 25(3): 567–589

    Article  CAS  Google Scholar 

  27. Murthy N S. Metastable crystalline phases in nylon-6. Poly Commun, 1991, 32(10): 301–305

    CAS  Google Scholar 

  28. Murthy N S, Bray R G, Correale S T, Moore R A F. Drawing and annealing of nylon-6 fibers: studies of crystal growth, orientation of amorphous and crystalline domains and their influence on properties. Polymer, 1995, 36(20): 3863–3873

    Article  CAS  Google Scholar 

  29. Murthy N S, Aharoni S M, Szollosi A B. Stability of the γ-form and the development of the α-form in nylon-6. J Poly Sci Part B-Poly Phys, 1985, 23(12): 2549–2565

    CAS  Google Scholar 

  30. Vasanthan N, Salem D R. FTIR spectroscopic characterization of structural changes in polyamide-6 fibers during annealing and drawing. J Poly Sci Part B-Poly Phys, 2001, 39(5): 536–547

    Article  CAS  Google Scholar 

  31. Penel-Pierron L, Depecker C, Seguela R, Lefebvre J M. Structural and mechanical behavior of nylon 6 films part I. Identification and stability of the crystalline phases. J Poly Sci Part B-Poly Phys, 2001, 39(5): 484–495

    Article  CAS  Google Scholar 

  32. Li Y Y, Goddard W A. Nylon 6 crystal structures, folds, and lamellae from theory. Macromolecules, 2002, 35(22): 8440–8455

    Article  CAS  Google Scholar 

  33. Auriemma F, Petraccone V, Parravicini L, Corradini P. Mesomorphic form (β) of nylon 6. Macromolecules, 1997, 30(24): 7554–7559

    Article  CAS  Google Scholar 

  34. Persyn O, Miri V, Lefebvre J M, Depecker C, Gors C, Stroeks A. Structural organization and drawability in polyamide blends. Poly Eng Sci, 2004, 44(2): 261–271

    Article  CAS  Google Scholar 

  35. Avramova N. Effect of the structure on sorption and diffusion processes in polyamide 6, part 1: Activation energy and thermodynamic parameters of water desorption in oriented and unoriented polyamide 6. J Appl Poly Sci, 2007, 106(1): 122–129

    Article  CAS  Google Scholar 

  36. Ramesh C, Gowd E B. High-temperature X-ray diffraction studies on the crystalline transitions in the α- and γ-forms of nylon-6. Macromolecules, 2001, 34(10), 3308–3313

    Article  CAS  Google Scholar 

  37. Murthy N S, Minor H. Analysis of poorly crystallized polymers using resolution enhanced X-ray-diffraction scans. Polymer, 1995, 36(13): 2499–2504

    Article  CAS  Google Scholar 

  38. Murthy N S, Bednarczyk C, Moore R A F, Grubb D T. Analysis of small-angle X-ray scattering from fibers: Structural changes in nylon 6 upon drawing and annealing. J Poly Sci Part B-Poly Phys, 1996, 34(5): 821–835

    Article  CAS  Google Scholar 

Download references

Author information

Authors and Affiliations

  1. Beijing National Laboratory for Molecular Sciences, CAS Key Laboratory of Engineering Plastics, Joint Laboratory for Polymer Science and Materials, Institute of Chemistry, Chinese Academy of Sciences, Beijing, 100190, China

    ChengFeng Zhang, YuHai Liu, Ying Zhao & DuJin Wang

  2. Beijing National Laboratory for Molecular Sciences, College of Chemistry and Molecular Engineering, Peking University, Beijing, 100871, China

    ShaoXuan Liu, HuiZhen Li, Kun Huang, QingHua Pan, XiaoHui Hua, WeiHong Li, ZhanLan Yang, YiZhuang Xu & JinGuang Wu

  3. Key Laboratory of Organosilicon Chemistry and Material Technology Ministry of Education, Hangzhou Normal University, Hangzhou, 310012, China

    QingHua Pan, ChaoWei Hao, QingFang Ma, ChangYou Lv, GuoQiao Lai & JianXiong Jiang

  4. College of Chemistry and Environmental Science, Henan Normal University, Xinxiang, 453007, China

    HuiZhen Li

  5. Graduate University of Chinese Academy of Sciences, Beijing, 100190, China

    ChengFeng Zhang & YuHai Liu

Authors
  1. ChengFeng Zhang
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. YuHai Liu
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. ShaoXuan Liu
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. HuiZhen Li
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Kun Huang
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. QingHua Pan
    View author publications

    You can also search for this author in PubMed Google Scholar

  7. XiaoHui Hua
    View author publications

    You can also search for this author in PubMed Google Scholar

  8. ChaoWei Hao
    View author publications

    You can also search for this author in PubMed Google Scholar

  9. QingFang Ma
    View author publications

    You can also search for this author in PubMed Google Scholar

  10. ChangYou Lv
    View author publications

    You can also search for this author in PubMed Google Scholar

  11. WeiHong Li
    View author publications

    You can also search for this author in PubMed Google Scholar

  12. ZhanLan Yang
    View author publications

    You can also search for this author in PubMed Google Scholar

  13. Ying Zhao
    View author publications

    You can also search for this author in PubMed Google Scholar

  14. DuJin Wang
    View author publications

    You can also search for this author in PubMed Google Scholar

  15. GuoQiao Lai
    View author publications

    You can also search for this author in PubMed Google Scholar

  16. JianXiong Jiang
    View author publications

    You can also search for this author in PubMed Google Scholar

  17. YiZhuang Xu
    View author publications

    You can also search for this author in PubMed Google Scholar

  18. JinGuang Wu
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to YiZhuang Xu.

Additional information

Supported by the National Natural Science Foundation of China (Grant Nos. 50673005, 50973003 & 20671007) and a program of Advanced Technology Institute, Peking University

Rights and permissions

Reprints and permissions

About this article

Cite this article

Zhang, C., Liu, Y., Liu, S. et al. Crystalline behaviors and phase transition during the manufacture of fine denier PA6 fibers. Sci. China Ser. B-Chem. 52, 1835–1842 (2009). https://doi.org/10.1007/s11426-009-0242-5

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s11426-009-0242-5

Keywords

Search

Navigation