Skip to main content
SpringerLink
Log in

Hydrothermal precipitation of β-FeOOH nanostructure(s) in mixed solvent: study of their morphological and structural evolution

  • Research Paper
  • Published:
Journal of Nanoparticle Research Aims and scope Submit manuscript

Abstract

This paper describes the homogeneous precipitation of β-FeOOH nanorods (±5 nm dia.) in alcohol—water mixed solvents. Four alcohols, butanol (BuOH), propanol (PrOH), ethanol (EtOH) and methanol (MeOH), were mixed with water as the solvents to evaluate the effect of alcohols on the β-FeOOH particle characteristics under different hydrothermal process parameters. Crystal splitting was achieved at 0.7 M [FeCl3] in BuOH, and β-FeOOH nanoribbons were obtained in MeOH. Replacing Cl− with SO4 2− in a controlled pH (2) environment results a 98 % reduction in the synthesis time of hydronium iron jarosite, H3O.Fe3(SO4)2(OH)6, regardless of the nature of the alcohol. Single phase hydronium iron jarosite could not be synthesised without the presence of alcohol. Alcohol-to-water ratio played a critical role in controlling particle nucleation and growth. Spherical α-Fe2O3 (haematite) was obtained in pure alcohol, whereas an addition of 2 % (v/v) alcohol resulted in the precipitation of β-FeOOH nanofibrillar. Nanosize spherical α-Fe2O3 (average dia. 95 ± 19 nm) was achieved by altering solution pH in selective solvent. Required temperature for β-FeOOH to α-Fe2O3 transformation is solvent dependent and increases with the increasing carbon chain length in the linear alkyl chain of the solvent. The choice of solvent did not affect the Raman spectrum of the synthesised sample when compared to the standard Raman peaks. The synthesised β-FeOOH nanorods do not show ferromagnetism at any temperature down to 4 K and have a magnetic moment per unit mass of 1–1.5 Am2/kg at 5T.

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

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8
Fig. 9

Similar content being viewed by others

References

  • Amine K, Yasuda H, Yamachi M (1999) β-FeOOH, a new positive electrode material for lithium secondary batteries. J Power Sour 81–82:221–223

    Article  Google Scholar 

  • Bashir S, McCabe RW, Boxall C et al (2009) Synthesis of α- and β-FeOOH iron oxide nanoparticles in non-ionic surfactant medium. J Nanopart Res 11:701–706

    Article  Google Scholar 

  • Brayner R, Yepremian C, Djediat C et al (2009) Photosynthetic microorganism-mediated synthesis of akaganeite (β-FeOOH) nanorods. Langmuir 25:10062–10067

    Article  Google Scholar 

  • Chen HI, Chang HY (2004) Homogeneous precipitation of cerium dioxide nanoparticles in alcohol/water mixed solvents. Colloids Surf A 242:61–69

    Article  Google Scholar 

  • Chen M, Jiang J, Zhou X et al (2008) Preparation of akaganeite nanorods and their transformation to sphere shape hematite. J Nanosci Nanotechnol 8:3942–3948

    Article  Google Scholar 

  • Chen L, Yang X, Chen J et al (2010) Continuous shape and spectroscopy tuning of hematite nanocrystals. Inorg Chem 49:8411–8420

    Article  Google Scholar 

  • Chowdhury MR, Fester VG, Kale GM (2014) Growth kinetics evaluation of hydrothermally synthesised β-FeOOH nanorods. J Crys Gro 387:57–65

    Article  Google Scholar 

  • Cornell RM, Schwertmann U (2003) The iron oxides: structure, properties, reactions, occurrences and uses. Wiley, New York

    Book  Google Scholar 

  • Earle SA, Ramirez AP, Cava RJ (1999) The effect of gallium substitution for iron on the magnetic properties of hydronium iron jarosite. Phys B 262:199–204

    Article  Google Scholar 

  • Fester VG, Slatter PT, Biggs S et al (2008) Significance of alcohols in the synthesis of iron oxide nanorods. In: Azhar Uddin M (ed) Green chemistry & engineering, process intensification & nanotechnology conference. Albany, New York, pp 231–236

    Google Scholar 

  • Guo X, Xiao P (2006) Effects of solvents on properties of nanocrystalline hydroxyapatite produced from hydrothermal process. J Eur Chem Soc 26:3383–3391

    Google Scholar 

  • Khan Y, Durrani SK, Siddique M et al (2011) Hydrothermal synthesis of α-Fe2O3 nanoparticles capped by Tween-80. Mater Lett 65:2224–2227

    Article  Google Scholar 

  • Kumar A, Gupta SK (2013a) Synthesis of adenine mediated superparamagnetic colloidal β-FeOOH nanostructure(s): study of their morphological changes and magnetic behavior. J Nanopart Res 15:1466

    Article  Google Scholar 

  • Kumar A, Gupta SK (2013b) Synthesis of 5′-GMP-mediated porous hydrogel containing β-FeOOH nanostructures: optimization of its morphology, optical and magnetic properties. J Mater Chem B 1:5818–5830

    Article  Google Scholar 

  • Liang MT, Wang SH, Chang YL et al (2010) Iron oxide synthesis using a continuous hydrothermal and solvothermal system. Ceram Int 36:1131–1135

    Article  Google Scholar 

  • Liu L, Kou HZ, Mo W et al (2006) Surfactant-assisted synthesis of α-Fe2O3 nanotubes and nanorods with shape dependent magnetic properties. J Phys Chem B 110:15218–15223

    Article  Google Scholar 

  • Manna L, Milliron DJ, Meilsel A et al (2003) Controlled growth of tetrapod branched inorganic nanocrystal. Nat Mater 2:382–385

    Article  Google Scholar 

  • Millan A, Urtizberea A, Natividad E et al (2009) Akaganeite polymer nanocomposites. Polymer 50:1088–1094

    Article  Google Scholar 

  • Pu Z, Cao M, Yang J et al (2006) Controlled synthesis and growth mechanism of hematite nanorhombohedra, nanorods and nanocubes. Nanotechnol 17:799–804

    Article  Google Scholar 

  • Reguer S, Neff D, Gurlet B et al (2007) Deterioration of iron archaeological artefacts: micro-Raman investigation on Cl− containing corrosion products. J Raman Spectrosc 38:389

    Article  Google Scholar 

  • Shao HF, Qian XF, Yin et al (2005) Controlled morphology synthesis of β-FeOOH and the phase transition to Fe2O3. J Solid State Chem 178:3130–3136

    Article  Google Scholar 

  • Tang J, Alivisatos AP (2006) Crystal splitting in the growth of Bi2S3. Nano Lett 6:2701–2706

    Article  Google Scholar 

  • Wei C, Nan Z (2011) Effects of experimental conditions on One-dimensional single-crystal nanostructure of b-FeOOH. Mat Chem Phys 127:220–226

    Article  Google Scholar 

  • White AF (1990) Heterogeneous electrochemical reactions associated with oxidation of ferrous oxide and silicate surfaces. Rev Mineral Geochem 23:467–505

    Google Scholar 

  • Xiong YJ, Xie Y, Chen SW et al (2003) Fabrication of self-supported patterns of aligned β-FeOOH nanowires by a low-temperature solution reaction. Chem Eur J 9:4991–4996

    Article  Google Scholar 

  • Yue J, Jiang X, Yu A (2011) Experimental and theoretical study on the β-FeOOH nanorods: growth and conversion. J Nanopart Res 13:3961–3974

    Article  Google Scholar 

  • Zhang LY, Xue DS, Fen J (2006) Magnetic properties of amorphous β-FeOOH nanowire arrays. J Magn Magn Mater 305:228–232

    Article  Google Scholar 

Download references

Acknowledgments

The authors acknowledge the National Research Foundation, South Africa and Cape Peninsula University of Technology for funding the study.

Author information

Authors and Affiliations

  1. Cape Peninsula University of Technology, P.O. Box 652, Cape Town, 8000, South Africa

    Mahabubur Rahman Chowdhury & Veruscha Fester

  2. Institute for Materials Research, SPEME, University of Leeds, Leeds, LS2 9JT, UK

    Girish Kale

  3. School of Physics & Astronomy, University of Leeds, Leeds, LS2 9JT, UK

    Oscar Cespedes

Authors
  1. Mahabubur Rahman Chowdhury
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Veruscha Fester
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Girish Kale
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Oscar Cespedes
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Mahabubur Rahman Chowdhury.

Electronic supplementary material

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Chowdhury, M.R., Fester, V., Kale, G. et al. Hydrothermal precipitation of β-FeOOH nanostructure(s) in mixed solvent: study of their morphological and structural evolution. J Nanopart Res 16, 2412 (2014). https://doi.org/10.1007/s11051-014-2412-4

Download citation

  • Received:

  • Accepted:

  • Published:

  • DOI: https://doi.org/10.1007/s11051-014-2412-4

Keywords

Search

Navigation