Skip to main content
Log in

Insight into the Structural and Physical Properties of Semiorganic KHOOD Single Crystal

  • Original Article
  • Published:
Chemistry Africa Aims and scope Submit manuscript

Abstract

A metal–organic hybrid compound named potassium hydrogen oxalate oxalic acid dihydrate (KH3(C4O8)·2H2O) single crystal (KHOOD) is synthesized using a facile and different approach. The obtained crystals are thoroughly investigated using single crystal XRD (SCXRD), powder XRD (PXRD), UV–Vis absorption, photoluminescence, TGA-DTA and dielectric measurements. The crystal system is confirmed and the structure of the crystal is solved using single crystal X-ray diffraction (SCXRD) analysis to the R value of 0.024. The PXRD measurements are employed to evaluate the structural properties of the crystal. Absorption measurements are carried out in the UV–visible region, and photoluminescence measurements show strong blue emission at 427 nm. Thermal stability and degradation in the crystal is explored using TGA-DTA analysis. Frequency dependent electrical response of the crystal is investigated and parameters such as frequency dependent complex dielectric constant, complex impedance, loss factor, ac conductivity and Cole–Cole plots are determined. These results demonstrate the feasibility of facile synthesis of KH3(C4O8)·2H2O single crystal used in modern optoelectronic applications.

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

Access this article

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

Instant access to the full article PDF.

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8
Fig. 9
Fig. 10

Similar content being viewed by others

References

  1. Igoa F, Peinado G, Suescun L, Kremer C, Torres J (2019) Design of a white-light emitting material based on a mixed-lanthanide metal organic framework. J Solid State Chem 279:120925. https://doi.org/10.1016/j.jssc.2019.120925

    Article  CAS  Google Scholar 

  2. Vimal G, Mani KP, Jose G, Biju PR, Joseph C, Unnikrishnan NV, Ittyachen MA (2014) Growth and spectroscopic properties of samarium oxalate single crystals. J Cryst Growth 404:20–25. https://doi.org/10.1016/j.jcrysgro.2014.06.041

    Article  CAS  Google Scholar 

  3. Neto JGO, Neto OCS, Pedrochi F, Steimacher A, Filho JGS, de Sousa FF, Silva LM, Santos AO (2022) Structural, vibrational, thermal, and optical properties of l-threonine crystals containing Ce3+ ions. J Mol Struct 1254:132316. https://doi.org/10.1016/j.molstruc.2021.132316

    Article  CAS  Google Scholar 

  4. Ramki C, Ezhil Vizhi R (2017) Growth, optical, electrical and mechanical properties of sodium hydrogen oxalate hydrate (NaHC2O4·H2O) single crystal for NLO applications. Mater Chem Phys 197:70–78. https://doi.org/10.1016/j.matchemphys.2017.04.066

    Article  CAS  Google Scholar 

  5. Rajasekaran R, Ushasree PM, Jayavel R, Ramasamy P (2001) Growth and characterization of zinc thiourea chloride (ZTC): a semiorganic nonlinear optical crystal. J Cryst Growth 229:563–567. https://doi.org/10.1016/S0022-0248(01)01229-5

    Article  CAS  Google Scholar 

  6. Senthil Pandian M, Ramasamy P (2010) Conventional slow evaporation and Sankaranarayanan–Ramasamy (SR) method grown diglycine zinc chloride (DGZC) single crystal and its comparative study. J Cryst Growth 312:413–419. https://doi.org/10.1016/j.jcrysgro.2009.11.011

    Article  CAS  Google Scholar 

  7. Mahendra K, Fernandes JM, Udayashankar NK (2021) A novel approach to the synthesis of semiorganic ammonium hydrogen oxalate oxalic acid dihydrate single crystal and its characterization. J Therm Anal Calorim 146:93–102. https://doi.org/10.1007/s10973-020-09965-5

    Article  CAS  Google Scholar 

  8. Ramajothi J, Dhanuskodi S (2007) Crystal growth, thermal and optical studies on a semiorganic nonlinear optical material for blue-green laser generation. Spectrochim Acta Part A Mol Biomol Spectrosc 68:1213–1219. https://doi.org/10.1016/j.saa.2007.01.030

    Article  CAS  Google Scholar 

  9. Mahendra K, D’Souza A, Udayashankar NK (2017) Effect of Zn doping on the structural, optical, photoluminescence and mechanical properties of thiourea barium chloride (TBC) crystal. Mater Today Commun 13:178–185. https://doi.org/10.1016/j.mtcomm.2017.09.010

    Article  CAS  Google Scholar 

  10. Haas DJ (1964) The crystal structure of potassium tetraoxalate, K(HC2O4)(H2C2O4)·2H2O. Acta Cryst Acta Crystallogr 17:1511–1516. https://doi.org/10.1107/S0365110X64003784

    Article  CAS  Google Scholar 

  11. Sheldrick GM (2008) A short history of SHELX. Acta Crystallogr Sect A Found Crystallogr 64:112–122. https://doi.org/10.1107/S0108767307043930

    Article  CAS  Google Scholar 

  12. Fernandes JM, Mahendra K, Udayashankar NK (2020) Effect of erioglaucine dye dopant on the structural, optical, mechanical, electrical and nonlinear properties of ammonium dihydrogen phosphate single crystal. Opt Mater 110:110528. https://doi.org/10.1016/j.optmat.2020.110528

    Article  CAS  Google Scholar 

  13. Mahendra K, Kumar HKT, Udayashankar NK (2019) Enhanced structural, optical, thermal, mechanical and electrical properties by a noval approach (nanoparticle doping) on ferroelectric triglycine sulphate single crystal. Appl Phys A 125:228. https://doi.org/10.1007/s00339-019-2499-7

    Article  CAS  Google Scholar 

  14. Rajagopalan NR, Krishnamoorthy P (2017) A systematic approach to physico-chemical analysis of tris (thiourea) zinc selenite—a semi-organic nonlinear optical crystal. Optik 129:118–129. https://doi.org/10.1016/j.ijleo.2016.10.039

    Article  CAS  Google Scholar 

  15. Weber MJ (2018) Handbook of optical materials. CRC Press, Boca Raton. https://doi.org/10.1201/9781315219615

    Book  Google Scholar 

  16. Mahalakshmi V, Lincy A, Thomas J, Saban KV (2012) Crystal growth and characterization of a new co-ordination complex—barium tetrakis (maleate) dihydrate. J Phys Chem Solids 73:584–588. https://doi.org/10.1016/j.jpcs.2011.12.012

    Article  CAS  Google Scholar 

  17. Ezhil Raj AM, Jayanthi DD, Jothy VB (2008) Optimized growth and characterization of cadmium oxalate single crystals in silica gel. Solid State Sci 10:557–562. https://doi.org/10.1016/j.solidstatesciences.2007.10.019

    Article  CAS  Google Scholar 

  18. Sagadevan S (2016) Optical and electrical studies of non-linear optical crystal: potassium boro-oxalate. Opt Int J Light Electron Opt 127:5613–5621. https://doi.org/10.1016/j.ijleo.2016.03.067

    Article  CAS  Google Scholar 

  19. Minu MC, Vimal G, Mani KP, Jose G, Biju PR, Joseph C, Unnikrishnan NV, Ittyachen MA (2016) Growth and characterization of Sm3+ doped cerium oxalate single crystals. J Mater Res Technol 5:268–274. https://doi.org/10.1016/j.jmrt.2016.01.001

    Article  CAS  Google Scholar 

  20. Chandran S, Paulraj R, Ramasamy P (2017) Crystal growth, structural, optical, thermal and dielectric properties of lithium hydrogen oxalate monohydrate single crystal. Opt Mater 73:154–162. https://doi.org/10.1016/j.optmat.2017.07.051

    Article  CAS  Google Scholar 

  21. Dinnebier RE, Vensky S, Jansen M, Hanson JC (2005) Crystal structures and topological aspects of the high-temperature phases and decomposition products of the alkali-metal oxalates M2[C2O4] (M = K, Rb, Cs). Chem Eur J 11:1119–1129. https://doi.org/10.1002/chem.200400616

    Article  CAS  PubMed  Google Scholar 

  22. Higashiyama T, Hasegawa S (1971) The differential thermal analysis of potassium oxalate. BCSJ 44:1727–1730. https://doi.org/10.1246/bcsj.44.1727

    Article  CAS  Google Scholar 

  23. Sasi S, Robert R, Arumugam S, Inmozhi C (2016) Growth, optical and spectroscopic studies of l-cysteine doped KDP single crystals. Optik 127:2366–2369. https://doi.org/10.1016/j.ijleo.2015.10.195

    Article  CAS  Google Scholar 

  24. Dalal J, Kumar B (2016) Bulk crystal growth, optical, mechanical and ferroelectric properties of new semiorganic nonlinear optical and piezoelectric Lithium nitrate monohydrate oxalate single crystal. Opt Mater 51:139–147. https://doi.org/10.1016/j.optmat.2015.11.033

    Article  CAS  Google Scholar 

  25. Bindu K, Ajith KM, Nagaraja HS (2018) Electrical, dielectric and magnetic properties of Sn-doped hematite (α-SnxFe2-xO3) nanoplates synthesized by microwave-assisted method. J Alloy Compd 735:847–854. https://doi.org/10.1016/j.jallcom.2017.11.180

    Article  CAS  Google Scholar 

  26. Madhusudhan CK, Mahendra K, Madhukar BS, Somesh TE, Faisal M (2020) Incorporation of graphite into iron decorated polypyrrole for dielectric and EMI shielding applications. Synth Met 267:116450. https://doi.org/10.1016/j.synthmet.2020.116450

    Article  CAS  Google Scholar 

  27. Madhusudhan CK, Mahendra K, Raghavendra N, Revanasiddappa M, Faisal M (2021) Corrosion-resistant polypyrrole-banana carbon (PPy-BC) nanocomposites for protection against electromagnetic interference: a green approach. J Mater Sci: Mater Electron. https://doi.org/10.1007/s10854-021-07466-1

    Article  Google Scholar 

  28. Madhusudhan CK, Mahendra K, Madhukar BS, Somesh TE, Faisal M (2021) Multifunctional polypyrrole/multi-walled carbon nanotube composite material: dielectric, humidity sensing and broadband EMI shielding properties. Polym Sci Ser B 63:280–290. https://doi.org/10.1134/S156009042103009X

    Article  CAS  Google Scholar 

  29. De A, Rao KV (1988) Dielectric properties of synthetic quartz crystals. J Mater Sci 23:661–664. https://doi.org/10.1007/BF01174702

    Article  CAS  Google Scholar 

  30. Elwej R, Hlel F (2016) Hydrothermal synthesis, characterization by single crystal XRD, structural discussion and electric, dielectrical properties of (C6H9N2)2(Hg0.12Zn0.88)Cl4 hybrid compound. Phys E Low-Dimens Syst Nanostruct 84:498–504. https://doi.org/10.1016/j.physe.2016.07.009

    Article  CAS  Google Scholar 

  31. Anand S, Amaliya AP, Janifer MA, Pauline S (2017) Structural, morphological and dielectric studies of zirconium substituted CoFe2O4 nanoparticles. Mod Electron Mater 3:168–173. https://doi.org/10.1016/j.moem.2017.10.001

    Article  Google Scholar 

  32. Chand P, Vaish S, Kumar P (2017) Structural, optical and dielectric properties of transition metal (MFe2O4; M = Co, Ni and Zn) nanoferrites. Phys B 524:53–63. https://doi.org/10.1016/j.physb.2017.08.060

    Article  CAS  Google Scholar 

  33. Lahlali S, Essaleh L, Belaqziz M, Chehouani H, Alimoussa A, Djessas K, Viallet B, Gauffier JL, Cayez S (2017) Dielectric and modulus analysis of the photoabsorber Cu2SnS3. Phys B 526:54–58. https://doi.org/10.1016/j.physb.2017.09.069

    Article  CAS  Google Scholar 

  34. Chouaib H, Elfaleh N, Karoui S, Kamoun S, Graça MPF (2016) Synthesis, crystal structure, thermal analysis and dielectric properties of (C8H12N)3SnCl6·Cl compound. Synth Met 217:129–137. https://doi.org/10.1016/j.synthmet.2016.03.029

    Article  CAS  Google Scholar 

  35. Thukral K, Vijayan Sonia N, Haranath D, Maurya KK, Philip J, Jayaramakrishnan V (2019) Comprehensive study on l-proline lithium chloride monohydrate single crystal: a semiorganic material for nonlinear optical applications. Arab J Chem 12:3193–3201. https://doi.org/10.1016/j.arabjc.2015.08.022

    Article  CAS  Google Scholar 

  36. Dizaji HR, Rousta A (2016) Directional growth of KCl added KDP crystal from aqueous solution by S–R method and investigation on its physical properties. Optik 127:11336–11341. https://doi.org/10.1016/j.ijleo.2016.09.066

    Article  CAS  Google Scholar 

  37. Ma Y, Teng B, Cao L, Zhong D, Ji S, Teng F, Liu J, Yao Y, Tang J, Tong J (2018) Growth, structural, thermal, dielectric and optical studies on HBST crystal: a potential THz emitter. Spectrochim Acta Part A Mol Biomol Spectrosc 190:274–282. https://doi.org/10.1016/j.saa.2017.08.035

    Article  CAS  Google Scholar 

  38. Subhashini R, Sathya D, Sivashankar V, Mageshwari PSL, Arjunan S (2016) Growth and characterization of bis(l-threonine) copper (II) monohydrate single crystals: a semiorganic second order nonlinear optical material. Opt Mater C. https://doi.org/10.1016/j.optmat.2016.09.041

    Article  Google Scholar 

  39. Hatton BD, Landskron K, Hunks WJ, Bennett MR, Shukaris D, Perovic DD, Ozin GA (2006) Materials chemistry for low-k materials. Mater Today 9:22–31. https://doi.org/10.1016/S1369-7021(06)71387-6

    Article  CAS  Google Scholar 

  40. Aravind G, Raghasudha M, Ravinder D (2015) Electrical transport properties of nano crystalline Li–Ni ferrites. J Materiomics 1:348–356. https://doi.org/10.1016/j.jmat.2015.09.003

    Article  Google Scholar 

  41. Srinivasan P, Kanagasekaran T, Gopalakrishnan R, Bhagavannarayana G, Ramasamy P (2006) Studies on the growth and characterization of l-asparaginium picrate (LASP) a novel nonlinear optical crystal. Cryst Growth Des. https://doi.org/10.1021/cg060094

    Article  Google Scholar 

  42. Hamdi M, Karoui S, Oueslati A, Kamoun S, Hlel F (2018) Synthesis, crystal structure and dielectric properties of the new organic -inorganic hybrid compound [C6H10N2]7[Bi2Cl11]2.4[Cl]. J Mol Struct 1154:516–523. https://doi.org/10.1016/j.molstruc.2017.10.063

    Article  CAS  Google Scholar 

  43. Devan RS, Kolekar YD, Chougule BK (2006) Effect of cobalt substitution on the properties of nickel–copper ferrite. J Phys Condens Matter 18:9809. https://doi.org/10.1088/0953-8984/18/43/004

    Article  CAS  Google Scholar 

  44. Chouaib H, Kamoun S, Costa LC, Graça MPF (2015) Synthesis, crystal structure and electrical properties of N,N-dimethylanilinium trichloridostannate (II): (C8H12N)SnCl3. J Mol Struct 1102:71–80. https://doi.org/10.1016/j.molstruc.2015.08.041

    Article  CAS  Google Scholar 

  45. Macdonald JR (1992) Impedance spectroscopy. Ann Biomed Eng 20:289–305

    Article  CAS  Google Scholar 

  46. Helen F, Kanchana G (2015) Growth, mechanical, dielectric, thermal and optical studies of a nonlinear optical crystal: l-histidinium dipicrate dihydrate. Mater Chem Phys 151:5–13. https://doi.org/10.1016/j.matchemphys.2014.11.064

    Article  CAS  Google Scholar 

  47. Haque SU, Saikia KK, Murugesan G, Kalainathan S (2017) A study on dielectric and magnetic properties of lanthanum substituted cobalt ferrite. J Alloy Compd 701:612–618. https://doi.org/10.1016/j.jallcom.2016.11.309

    Article  CAS  Google Scholar 

Download references

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to K. Mahendra.

Supplementary Information

Below is the link to the electronic supplementary material.

Supplementary file1 (DOCX 15 KB)

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Mahendra, K., Fernandes, J.M. & Udayashankar, N.K. Insight into the Structural and Physical Properties of Semiorganic KHOOD Single Crystal. Chemistry Africa 5, 617–626 (2022). https://doi.org/10.1007/s42250-022-00360-1

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s42250-022-00360-1

Keywords

Navigation