Advertisement

Journal of Sol-Gel Science and Technology

, Volume 86, Issue 2, pp 410–422 | Cite as

High-temperature stable transition aluminas nanoparticles recovered from sol–gel processed chitosan-AlOx organic–inorganic hybrid films

  • Fakhreia Al Sagheer
  • Shamsun Nahar
  • Ahmed Abdel Nazeer
  • Ali Bumajdad
  • Mohamed I. Zaki
Original Paper: Nano-structured materials (particles, fibers, colloids, composites, etc.)
  • 90 Downloads

Abstract

Five and ten weight percent-alumina-containing chitosan-AlOx films were prepared via sol–gel processing. The films were AlOx-agglomerate-free. These organic–inorganic films were degraded by heating at 500 °C. The solid powder residues were found by means of thermogravimetry, X-ray diffractometry, infrared spectroscopy, and electron microscopy to consist of alumina (Al2O3) nanoparticles entraping volatile components, whose thermal removal encouraged ambient oxygen uptake. The surface microstructure and morphology of the recovered alumina nanoparticle were inspected by high-resolution transmission and scanning electron microscopy. Also, the surface chemistry and texture were evaluated by X-ray photoelectron spectroscopy and N2 sorptiometry. Coalescences of globular nanoparticles of γ-/η-Al2O3 were the dominant composition of the 800 °C calcination product of the recovered alumina, irrespective of the alumina-content of the film. Upon increasing the calcination temperature up to 1100 °C, an enhanced polymorphic transition into agglomerated nanoparticles of the seldom encountered Iota-(ι-)Al2O3 took place. The high thermal stability of the otherwise unstable transition aluminas (at ≥950 °C) may suggestively owe to its polymorphic interdependence and/or persistent nanoscopic nature (average particle size = ca. 3–4 nm; specific surface area = ca. 80–60 m2/g). The surface chemical composition for the recovered transition aluminas nanopowders promises versatile acid–base properties for catalysis applications. Accordingly, the highly abundant bio-waste, chitosan, was successfully utilized as a novel synthesis medium for catalytic-grade alumina nanoparticles.

The highly abundant bio-waste material, chitosan, is successfully employed as a synthetic medium for catalytic-grade alumina nanoparticles. This novel sol–gel synthesis process resulted in nearly 100%-recovery of nanoparticle transition γ-/η- and ι-Al2O3 and may be utilized in fabricating other materials/metal oxides

Keywords

Alumina Sol–gel synthesis Nanoparticle Chitosan Organic–inorganic composite Bio-waste materials 

Notes

Acknowledgements

The authors gratefully acknowledge the support provided by the Research Administration of Kuwait University, under Grant Number’s SC06/13 and GS 03/01, GS01/01, GS01/03, GS01/05 and GE03/08. They also appreciate help given by the Nanoscopy Science Center at Kuwait University in performing AFM, TEM and HRTEM measurements.

Funding

This work was supported by Kuwait University [grant number SC06/13].

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.

Supplementary material

10971_2018_4617_MOESM1_ESM.docx (203 kb)
Supplementary Materials

References

  1. 1.
    Storozhev VB, Yermakov AN (2015) Combustion of nano-sized aluminum particles in steam: numerical modeling. Combust Flame 162(11):4129–4137CrossRefGoogle Scholar
  2. 2.
    Nayar P, Khanna A, Kabiraj D, Abhilash SR, Beake BD, Losset Y, Chen B (2014) Structural, optical and mechanical properties of amorphous and crystalline alumina thin films. Thin Solid Films 568:19–24CrossRefGoogle Scholar
  3. 3.
    Vinogradov VV, Agafonov AV, Vinogradov AV, Pillai KT, Pai RV, Mukerjee SK, Aggarwal SK (2011) Synthesis of organized mesoporous γ-alumina templated with polymer–colloidal complex. J Sol–Gel Sci Technol 60:6–10CrossRefGoogle Scholar
  4. 4.
    Singh IB, Gupta A, Dubey S, Shafeeq M, Banerjee P, Sinha ASK (2016) Sol–gel synthesis of nanoparticles of gamma alumina and their application in defluoridation of water. J Sol–Gel Sci Technol 77:416–422CrossRefGoogle Scholar
  5. 5.
    Dubey S, Singh A, Nim B, Singh IB (2017) Optimization of molar concentration of AlCl3 salt in the sol–gel synthesis of nanoparticles of gamma alumina and their application in the removal of fluoride of water. J Sol–Gel Sci Technol 82(2):468–477CrossRefGoogle Scholar
  6. 6.
    Zhang Z, Pinnavaia TJ (2002) Mesostructured-Al2O3 with a lathlike framework morphology. J Am Chem Soc 124:12294–12301CrossRefGoogle Scholar
  7. 7.
    Shirai T, Watanabe H, Fuji M, Takahashi M (2009) Structural properties and surface characteristics on aluminum oxide powders. Ann Rep Ceram Res 9:23–31Google Scholar
  8. 8.
    Levin I, Brandon D (1998) Metastable alumina polymorphs: crystal structures and transition sequences. J Am Ceram Soc 81(8):1995–2012CrossRefGoogle Scholar
  9. 9.
    Macedo MIF, Osawa CC, Bertran CA (2004) Sol–gel synthesis of transparent alumina gel and pure gamma alumina by urea hydrolysis of aluminum nitrate. J Sol–Gel Sci Technol 30(3):135–140CrossRefGoogle Scholar
  10. 10.
    Aryal S, Rulis P, Ouyang L, Ching WY (2011) Structure and properties of the low-density phase ι- Al2O3 from first principles. Phys Rev B 84(17):174123CrossRefGoogle Scholar
  11. 11.
    Cava S, Tebcherani SM, Souza IA, Pianaro SA, Paskocimas CA, Longo E, Varela JA (2007) Structural characterization of phase transition of Al2O3 nanopowders obtained by polymeric precursor method. Mater Chem Phys 103(2-3):394–399CrossRefGoogle Scholar
  12. 12.
    Karim MR, Rahman MA, Miah MAJ, Ahmad H, Yanagisawa M, Ito M (2011) Synthesis of γ-alumina particles and surface characterization. Open Colloid Sci J 4:32–36CrossRefGoogle Scholar
  13. 13.
    Schüth F, Unger K (1997) In: Ertl G, Knözinger H, Weitkamp J (eds) Handbook of heterogeneous catalysis. Wiley, Weinheim, pp 72–86Google Scholar
  14. 14.
    Ertl G, Knözinger H, Weitkamp J (eds) (1997) Handbook of heterogeneous catalysis. Wiley, Weinheim, pp 1–5Google Scholar
  15. 15.
    Lippens BC, De Boer JH (1964) Study of phase transformations during calcination of aluminum hydroxides by selected area electron diffraction. Acta Crystallogr 17:1312–1321CrossRefGoogle Scholar
  16. 16.
    Wilson SJ (1979) Phase transformations and development in microstructure in boehmite-derived transition aluminas. Proc Br Ceram Soc 28:281–294Google Scholar
  17. 17.
    Knözinger H, Ratnasamy P (1979) Catalytic aluminas: surface models and characterization of surface sites. Cat Rev Sci Eng 17:31–70CrossRefGoogle Scholar
  18. 18.
    Tsygenenko AA, Filimonov VN (1973) Infrared spectra of surface hydroxyl groups and crystalline structure of oxides. J Mol Struct 19:579–589CrossRefGoogle Scholar
  19. 19.
    Busca G, Lorenzelli V, Ramis G, Willey RJ (1993) Surface sites on spinel-type and corundum-type metal oxide powders. Langmuir 9(6):1492–1499CrossRefGoogle Scholar
  20. 20.
    Morterra C, Bolis V, Magnacca G (1994) IR spectroscopic and microcalorimetric characterization of lewis acid sites on (transition phase) Al2O3 using adsorbed CO. Langmuir 10:1812–1824CrossRefGoogle Scholar
  21. 21.
    Yamaguchi G, Yasui I, Chiu WCA (1970) New method of preparing θ-alumina and the interpretation of its x-ray powder diffraction pattern and electron diffraction pattern. Bull Chem Soc Jpn 43:2487–2491CrossRefGoogle Scholar
  22. 22.
    Boudart M (1997) In: Ertl G, Knözinger H, Weitkamp J (eds) Handbook of heterogeneous catalysis. Wiely, Weinheim, pp 1–11Google Scholar
  23. 23.
    Zaki MI, Fouad NE, Mekhemer GAH, Oga SB (2011) TiO2 nanoparticle size dependence of porosity, adsorption and catalytic activity. Colloids Surf A 385:195–200CrossRefGoogle Scholar
  24. 24.
    Ali AAM, Zaki MI (2011) Thermal and spectroscopic studies of polymorphic transitions of zirconia during calcination of sulfated and phosphate Zr(OH)4 precursors of solid acid catalysts. Thermochim Acta 36(1–2):17–25Google Scholar
  25. 25.
    Wong P, Robinson M (1970) Chemical vapour deposition of polycrystalline alumina. J Am Ceram Soc 53(11):617–621CrossRefGoogle Scholar
  26. 26.
    Uchida Y, Sawabe Y, Mohri M, Shiraga N, Matsui Y (1995) Nearly monodispersed single crystal particles of α-alumina. in Adair JH, Casey JA, Clive A Randall, Venigalla S (eds) Handbook on Science, Technology, and Applications of Colloidal Suspensions,Ceramic Transactions, Vol. 54, The American Ceramic Society, pp 159–165Google Scholar
  27. 27.
    Kadokura H, Umezaki H, Higuchi Y (1987) Process for producing high purity metallic compound. US. Patent, No. 4, 650, 895,1987Google Scholar
  28. 28.
    Al-Omani SJ, Bumajdad A, Al Sagheer FA, Zaki MI (2012) Surface and related bulk properties of Titania nanoparticles recovered from aramid–titania hybrid films: a novel attempt. Mater Res Bull 47(11):3308–3316CrossRefGoogle Scholar
  29. 29.
    Rahim M, Mas Haris MRH (2015) Application of biopolymer composites in arsenic removal from aqueous medium: a review. J Radiat Res Appl Sci 8(2):255–263CrossRefGoogle Scholar
  30. 30.
    Chauhan VS, Yunus M, Sankararamakrishnan N (2010) Preparation, characterization and application studies of inorganic–organic novel polymer composite. Adv Mater Lett 1(3):225–231CrossRefGoogle Scholar
  31. 31.
    Al-Sagheer F, Muslim S (2010) Thermal and mechanical properties of chitosan/SiO2 hybrid composites. J Nanomater 2010:1–7CrossRefGoogle Scholar
  32. 32.
    Suciu C, Gagea L, Hoffmann AC, Mocean M (2006) Sol–gel production of zirconia nanoparticles with a new organic precursor. Chem Eng Sci 61(24):7831–7835CrossRefGoogle Scholar
  33. 33.
    Al-Sagheer FA, Merchant S (2011) Visco-elastic properties of chitosan-titania nano-composites. Carbohydr Polym 85(2):356–362CrossRefGoogle Scholar
  34. 34.
    Al-Sagheer FAA, Al-Sughayer MA, Muslim S, Elsabee MZ (2009) Extraction and characterization of chitin and chitosan from marine sources in Arabian Gulf. Carbohydr Polym 77(2):410–419CrossRefGoogle Scholar
  35. 35.
    Kumirska J, Czerwicka M, Kaczynski Z, Bychowska A, Brzozowski K, Thoming J, Stepnowski P (2010) Application of spectroscopic methods for structural analysis of chitin and chitosan. Mar Drugs 8:1567–1636CrossRefGoogle Scholar
  36. 36.
    Muzzarelli RAA (1977) Chitin. Pergamon Press, OxfordGoogle Scholar
  37. 37.
    Tonny W, Tuhin MO, Islam R, Khan RA (2014) Fabrication and characterization of biodegradable packaging films using starch and chitosan: effect of glycerol. J Chem Eng Chem Res 1(5):343–352Google Scholar
  38. 38.
    Ahmad Z, Sarwar MI, Wang S, Mark JE (1997) Preparation and properties of hybrid organic–inorganic composites prepared from poly(phenylene terephthalamide) and titania. Polymer 38(17):4523–4529CrossRefGoogle Scholar
  39. 39.
    Xiao G, Su H, Tan T (2015) Synthesis of core-shell bioaffinity chitosan-TiO2 composite and its environmental applications. J Hazard Mater 283:888–896CrossRefGoogle Scholar
  40. 40.
    Viswanathan N, Meenakshi S (2010) Enriched fluoride sorption using alumina/chitosan composite. J Hazard Mater 178(1–3):226–232CrossRefGoogle Scholar
  41. 41.
    Steenkamp GC, Keizer K, Neomagus HWJP, Krieg HM (2002) Copper(II) removal from polluted water with alumina/chitosan composite membranes. J Memb Sci 197(1–2):147–156CrossRefGoogle Scholar
  42. 42.
    Boddu VM, Abburi K, Talbott JL, Smith ED (2003) Removal of hexavalent chromium from wastewater using a new composite chitosan biosorbent. Environ Sci Technol 37(19):4449–4456CrossRefGoogle Scholar
  43. 43.
    Gandhi MR, Viswanathan N, Meenakshi S (2010) Preparation and application of alumina/chitosan biocomposite. Int J Biol Macromol 47(2):146–154CrossRefGoogle Scholar
  44. 44.
    Zhang J, Zhou Q, Ou L (2012) Kinetic, isotherm, and thermodynamic studies of the adsorption of methyl orange from aqueous solution by chitosan/alumina composite. J Chem Eng Data 57(2):412–419CrossRefGoogle Scholar
  45. 45.
    International Center for Diffraction Data, 12 Campus Boulevard, Newtown Square, PA 19073-3273, USAGoogle Scholar
  46. 46.
    Snyder RL (1999) In: Lifshin E (ed) X-ray characterization of materials. Wiley, Weinheim, Toronto, 4–103Google Scholar
  47. 47.
    Brunauer S, Emmett PH, Teller E (1938) Adsorption of gases in multimolecular layers. J Am Chem Soc 60:309CrossRefGoogle Scholar
  48. 48.
    Barrett EP, Joyner LS, Halenda PP (1951) The determination of pore volume and area distrbitutions in porous substances. I. Computations from nitrogen isotherm. J Am Chem Soc 73:373–380CrossRefGoogle Scholar
  49. 49.
    Gadsden JA (1975) Infrared spectra of minerals and related inorganic compounds. Butterworths, LondonGoogle Scholar
  50. 50.
    Wefers K, Mirsa C (1987) Oxides and hydroxides of aluminum. ALCOA Laboratories, PennsilvaniaGoogle Scholar
  51. 51.
    Santos PS, Santos HS, Toledo SP (2000) Standard transition aluminas. Electr Microsc Stud Mater Res 3:104–114Google Scholar
  52. 52.
    Foster PA (1959) The nature of alumina in quenched cryolite-alumina melts. J Electrochem Soc 106:971–975CrossRefGoogle Scholar
  53. 53.
    Fischer RX, Schneider H, Schmuecker M (1994) Crystal structure of Al-rich mullite. Am Miner 79(9–10):983–990Google Scholar
  54. 54.
    Lecloux AJ (1981) Texture of catalysts. Catal Sci Eng 2:171–229Google Scholar
  55. 55.
    Rouquerol F, Rouquerol J, Sing K (1999) Adsorption by powders & porous solids principles, methodology and applications. Academic Press, San Diego, pp 440–441Google Scholar
  56. 56.
    Gregg SJ (1982) Adsorption of gases—tool for the study of the texture of solids. In: Rouquerol J, Sing KSW (eds) Adsorption at the gas–solid and liquid–solid interface. Elsevier, AmsterdamGoogle Scholar
  57. 57.
    Gregg SJ, Sing KSW (1967) Adsorption, surface area and porosity. Academic Press, London, p 153–164Google Scholar
  58. 58.
    Wagner CD, Riggs WM, Davis LE, Moulder JF (1979) In: GE Muilenberg (ed) Handbook of X-ray photoelectron spectroscopy. Perkin-Elmer Corp., Minnesota 55344Google Scholar
  59. 59.
    Sohlberg K, Pantelides ST, Pennycook SJ (2001) Surface reconstruction and the difference in surface acidity between γ- and η-alumina. J Am Chem Soc 123:26–29CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media, LLC, part of Springer Nature 2018

Authors and Affiliations

  1. 1.Chemistry Department, Faculty of ScienceKuwait UniversitySafatKuwait
  2. 2.Chemistry Department, Faculty of ScienceMinia UniversityEl-MiniaEgypt

Personalised recommendations