Skip to main content
SpringerLink
Log in

Zinc–diethanolamine complex: synthesis, characterization, and formation mechanism of zinc oxide via thermal decomposition

  • Original Paper: Sol–gel, hybrids, and solution chemistries
  • Published:
Journal of Sol-Gel Science and Technology Aims and scope Submit manuscript

Abstract

Zn(OAc)2(H2DEA) was synthesized by the reaction of zinc acetate dihydrate (Zn(OAc)2•2H2O) with diethanolamine (H2DEA), and was characterized using single-crystal X-ray structural analysis, nuclear magnetic resonance spectroscopy, Fourier-transform infrared (FT-IR) spectroscopy, and elemental analysis. Zn(OAc)2(H2DEA) had a trigonal bipyramidal geometry comprised of one zinc atom, two acetate groups, and one H2DEA as a neutral tridentate ligand to form two five-membered rings. The states of Zn(OAc)2(H2DEA) heated at various temperatures were determined by FT-IR spectroscopy. At 270 °C, the H2DEA ligand dissociated and was removed. The absorption bands assigned to Zn–O stretching vibration of Zn4O core such as the zinc-oxo cluster appeared. When heated at 500 °C, the absorption bands of μ4-oxozincate and the acetate group disappeared completely and hexagonal wurtzite structural ZnO was formed at 550 °C. A possible thermal decomposition pathway from Zn(OAc)2(H2DEA) to ZnO was proposed. The ZnO film was highly transparent and formed by the deposition of ZnO nanoparticles with size ~40 nm.

Zn(OAc)2(H2DEA) was synthesized and characterized. The states of Zn(OAc)2(H2DEA) heated at various temperatures were determined by FT-IR spectroscopy, and the formation mechanism of ZnO was estimated.

Highlights

  • Zinc–diethanolamine complex was synthesized by the reaction of zinc acetate with diethanolamine.

  • Zinc–diethanolamine complex was isolated and characterized.

  • The formation mechanism of ZnO was estimated by FT-IR spectra.

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

Scheme 1
Fig. 1
Fig. 2
Fig. 3
Scheme 2
Fig. 4

Similar content being viewed by others

References

  1. Fortunato E, Barquinha P, Martins R (2012) Oxide semiconductor thin-film transistors: a review of recent advances. Adv Mater 24:2945–2986

    Article  Google Scholar 

  2. Tari O, Aronne A, Addonizio ML, Daliento S, Fanelli E, Pernice P (2012) Sol–gel synthesis of ZnO transparent and conductive films: a critical approach. Sol Energy Mater Sol Cells 105:179–186

    Article  Google Scholar 

  3. Sirelkhatim A, Mahmud S, Seeni A, Haida N, Kaus M, Ann LC, Bakhori SKM, Hasan H, Mohamad D (2015) Review on zinc oxide nanoparticles: antibacterial activity and toxicity mechanism. Nano-Micro Lett 7:219–242

    Article  Google Scholar 

  4. Hussain M, Tahir MN, Mansoor MA, Arifin Z, Mazhar M (2013) Heptanuclear zinc cluster for growth of zincite and manganese-doped zincite thin films for sensor applications. Mon Chem 144:285–294

    Article  Google Scholar 

  5. Liu Y, Li Y, Zeng H (2013) ZnO-based transparent conductive thin films: doping, performance, and processing. J Nanomater 2013:196521

    Google Scholar 

  6. Rodnyi PA, Khodyuk IV (2011) Optical and luminescence properties of zinc oxide. Opt Spectrosc 111:776–785

    Article  Google Scholar 

  7. Adl AH, Kar P, Farsinezhad S, Sharma H, Shankar K (2015) Effect of sol stabilizer on the structure and electronic properties of solution-processed ZnO thin films. RSC Adv 5:87007–87018

    Article  Google Scholar 

  8. Stadler A (2012) Transparent conducting oxides—an up-to-date overview. Materials 5:661–683

    Article  Google Scholar 

  9. Kolodziejczk-Radzimska A, Jesionowski T (2014) Zinc oxide—from synthesis to application: a review. Materials 7:2833–2881

    Article  Google Scholar 

  10. Khatibani AB, Abbasi M (2018) Effect of Fe and Co doping on ethanol sensing property of powder-based ZnO nanostructures prepared by the sol–gel method. J Sol–Gel Sci Technol 86:255–265

    Article  Google Scholar 

  11. Li H, Wang J, Liu H, Yang C, Xu H, Li X, Cui H (2004) Sol–gel preparation of transparent zinc oxide films with highly preferential crystal orientation. Vacuum 77:57–62

    Article  Google Scholar 

  12. Znaidi L, GJAAS Illia, Benyahia S, Sanchez C, Kanaev AV (2003) Oriented ZnO thin films synthesis by sol–gel process for laser application. Thin Solid Films 428:257–262

    Article  Google Scholar 

  13. Znaidi L, GJAAS Illia, Guennic RL, Sanchez C, Kanaev A (2003) Elaboration of ZnO thin films with preferential orientation by a soft chemistry route. J Sol–Gel Sci Technol 26:817–821

    Article  Google Scholar 

  14. Chen WJ, Liu WL, Hsieh SH, Hsu YG (2012) Synthesis of ZnO:Al transparent conductive thin films using the sol–gel method. Proc Eng 36:54–61

    Article  Google Scholar 

  15. Salam S, Islam M, Akram A (2013) Sol–gel synthesis of intrinsic and aluminum-doped zinc oxide thin films as transparent conducting oxides for thin film solar cells. Thin Solid Films 529:242–247

    Article  Google Scholar 

  16. Ohya Y, Saiki H, Takahashi Y (1994) Preparation of transparent, electrically conducting ZnO film from zinc acetate and alkoxide. J Mater Sci 29:4099–4103

    Article  Google Scholar 

  17. Znaidi L (2010) Sol–gel-deposited ZnO thin films: a review. Mat Sci Eng B-Solid 174:18–30

    Article  Google Scholar 

  18. Nehmann JB, Ehrmann N, Reineke-Koch R, Bahnemann DW (2014) Aluminum-doped zinc oxide sol–gel thin films: influence of the sol’s water content on the resistivity. Thin Solid Films 556:168–173

    Article  Google Scholar 

  19. Conterosito E, Croce G, Palin L, Boccaleri E, van Beekab W, Milanesio M (2012) Crystal structure and solid-state transformations of Zn–triethanolamine–acetate complexes to ZnO. Cryst Eng Comm 14:4472–4477

    Article  Google Scholar 

  20. Gordon RM, Silver HB (1982) Preparation and properties of tetrazinc μ4-oxohexa-μ-carboxylates (basic zinc carboxylates). Can J Chem 61:1218–1221

    Article  Google Scholar 

  21. Sheldrick GM (1996) SADABS, Program for Simens area detector absorption correction, University of Göttingen, Germany

  22. Sheldrick GM (1997) SHELXS-97, Program for crystal structure solution, University of Göttingen, Germany

  23. Sheldrick GM (1997) SHELXL-97, Program for crystal structure refinement, University of Göttingen, Germany

  24. Johnson MK, Powell DB, Cannon RD (1981) Vibrational spectra of carboxylato complexes—I. Infrared and Raman spectra of beryllium(II) acetate and formate and of zinc(II) acetate and zinc(II) acetate dihydrate. Spectrochim Acta A Mol Spectrosc 37:899–904

    Article  Google Scholar 

  25. Zhang Y, Zhu F, Zhang J, Xia L (2008) Converting layered zinc acetate nanobelts to one-dimensional structured ZnO nanoparticle aggregates and their photocatalytic activity. Nanoscale Res Lett 3:201–204

    Article  Google Scholar 

  26. Masoud MS, El-Enein SAA, Abed IM, Ali AE (2002) Synthesis and characterization of aminoalcohol complexes. J Coord Chem 55:153–178

    Article  Google Scholar 

  27. Brannon DG, Morrison RH, Hall JL, Humphrey GL, Zimmerman DN (1971) Spectra and bonding for copper(II)-aminoalcohol complexes—I: the I.R. spectra of complexes of mono-, di- and triethanolamine. J Inorg Nucl Chem 33:981–990

    Article  Google Scholar 

  28. Berkesi O, Dreveni I, Andor JA, Goggin PL (1991) Formation and mid-FT-IR investigation of short (C2–C5) straight chain tetrazinc μ4-oxohexa-μ-carboxylates. Inorg Chim Acta 181:285–289

    Article  Google Scholar 

  29. Spanhel L (2006) Colloidal ZnO nanostructures and functional coatings: a survey. J Sol–Gel Sci Technol 39:7–24

    Article  Google Scholar 

  30. Meulenkamp EA (1998) Synthesis and growth of ZnO nanoparticles. J Phys Chem B 102:5566–5572

    Article  Google Scholar 

  31. Tokumoto MS, Pulcinelli SH, Santilli CV, Briois V (2003) Catalysis and temperature dependence on the formation of ZnO nanoparticles and of zinc acetate derivatives prepared by the sol–gel route. J Phys Chem B 107:568–574

    Article  Google Scholar 

  32. Schmidt T, Müller G, Spanhel L (1998) Activation of 1.54 μm Er3+ fluorescence in concentrated II–VI semiconductor cluster environments. Chem Mater 10:65–71

    Article  Google Scholar 

  33. Viart N, Richard-Plouet M, Muller D, Pourroy G (2003) Synthesis and characterization of Co/ZnO nanocomposites: toward new perspectives offered by metal/piezoelectric composite materials. Thin Solid Films 437:1–9

    Article  Google Scholar 

  34. O’Brien S, Nolan MG, Çopuroglu M, Hamilton JA, Povey I, Pereira L, Martins R, Fortunato E, Pemble M (2010) Zinc oxide thin films: characterization and potential applications. Thin Solid Films 518:4515–4519

    Article  Google Scholar 

Download references

Acknowledgments

This work was supported by a Grant-in-Aid for Scientific Research on Innovative Areas “New Polymeric Materials Based on Element-Blocks” (No. 2401) (JSPS KAKENHI Grant Number JP24102008). This work was also supported by JSPS KAKENHI Grant Number JP16K17951.

Author information

Authors and Affiliations

  1. Department of Pure and Applied Chemistry, Faculty of Science and Technology, Tokyo University of Science, 2641 Yamazaki, Noda, Chiba, 278-8510, Japan

    Ryohei Hayami, Nagato Endo, Takayuki Abe, Yuta Miyase, Takuya Sagawa, Kazuki Yamamoto & Takahiro Gunji

  2. Advanced Automotive Research Collaborative Laboratory, Graduate School of Engineering, Hiroshima University, 1-4-1 Kagamiyama, Higashi-Hiroshima City, Hiroshima, 739-8527, Japan

    Satoru Tsukada

Authors
  1. Ryohei Hayami
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Nagato Endo
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Takayuki Abe
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Yuta Miyase
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Takuya Sagawa
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. Kazuki Yamamoto
    View author publications

    You can also search for this author in PubMed Google Scholar

  7. Satoru Tsukada
    View author publications

    You can also search for this author in PubMed Google Scholar

  8. Takahiro Gunji
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Takahiro Gunji.

Ethics declarations

Conflict of interest

The authors declare that they have no conflict of interest.

Electronic supplementary material

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Hayami, R., Endo, N., Abe, T. et al. Zinc–diethanolamine complex: synthesis, characterization, and formation mechanism of zinc oxide via thermal decomposition. J Sol-Gel Sci Technol 87, 743–748 (2018). https://doi.org/10.1007/s10971-018-4768-x

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10971-018-4768-x

Keywords

Search

Navigation