READ ME File For Dataset to support the article "Effects of the reaction temperature and Ba/Ti precursor ratio on the crystallite size of BaTiO3 in hydrothermal synthesis"

Dataset DOI: https://doi.org/10.5258/SOTON/D2382

Date that the file was created: September, 2022

Authors: Min Zhang,a Joseph Falvey,a Andrew L. Hector *a and Nuria Garcia-Araez a,b
a School of Chemistry, University of Southampton, Highfield, Southampton SO17 1BJ, UK
E-mail: A.L.Hector@soton.ac.uk
b The Faraday Institution, Quad One, Harwell Campus, Didcot OX11 0RA, UK

Licenses/restrictions placed on the data, or limitations of reuse:CC BY

This dataset supports the publication:
AUTHORS:Min Zhang,a Joseph Falvey,a Andrew L. Hector *a and Nuria Garcia-Araez a,b
TITLE:Effects of the reaction temperature and Ba/Ti precursor ratio on the crystallite size of BaTiO3 in hydrothermal synthesis
JOURNAL:RSC Advances
PAPER DOI IF KNOWN: 10.1039/d2ra03707f

This dataset contains:

Original data used to produce the following figures are provided in Microsoft Excel format, with column titles explaining their content.

Fig. 1 (a) XRD patterns of BaTiO3 samples hydrothermally synthesised with Ba/Ti precursor ratios of 4:1, 2:1 and 1:1, at various reaction temperatures of 80, 120, 150, 180 and 220 °C; (b) crystallite size and (c) tetragonality (c/a) of BaTiO3 samples plotted against reaction temperature in hydrothermal synthesis using Ba/Ti precursor ratios of 4:1, 2:1 and 1:1, obtained from the Rietveld fits to the XRD patterns (sample labels explained in Table 1).

Fig. 2 (a) Raman spectra of BaTiO3 samples hydrothermally synthesised with Ba/Ti precursor ratios of 4:1, 2:1 and 1:1, at various reaction temperatures of 80, 120, 150, 180 and 220 °C (peaks at ~307 cm-1 being marked as shaded); (b) relative integrated intensities of the Raman peak at 307 cm-1 for BaTiO3 samples plotted against reaction temperature in hydrothermal synthesis using Ba/Ti precursor ratios of 4:1, 2:1 and 1:1 (sample labels explained in Table 1).

Fig. 3 SEM images of BaTiO3 samples hydrothermally synthesised using a 4:1 Ba/Ti precursor ratio with reaction temperatures of (a) 80 °C, (b) 150 °C and (c) 220 °C; the patterns below to show the grain sizes of the samples determined using the ImageJ software, and the size distributions analysed with a Gaussian function.

Fig. 4 DLS patterns (above) and TEM images (below) of BaTiO3 samples hydrothermally synthesised using a 4:1 Ba/Ti precursor ratio with reaction temperatures of (a) 80 °C, (b) 150 °C and (c) 220 °C.

Fig. 5 (a) TGA curves and (b) mass losses against crystallite sizes of BaTiO3 samples hydrothermally synthesised using a 4:1 Ba/Ti precursor ratio with reaction temperatures of 80, 120, 150, 180 and 220 °C, examined by heating in Ar with a heating process of at 1 °C/min from 25 to 200 °C, then at 10 °C/min from 200 to 1000 °C (sample labels explained in Table 1).

Fig. 6 SEM images of BaTiO3 samples hydrothermally synthesised at 220 °C using Ba/Ti precursor ratios of (a) 4:1, (b) 2:1 and (c) 1:1; the patterns below to show the grain sizes of the samples determined using the ImageJ software, and the size distributions analysed with a Gaussian function.

Fig. 7 DLS patterns (above) and TEM images (below) of BaTiO3 samples hydrothermally synthesised at 220 °C using Ba/Ti precursor ratios of (a) 4:1, (b) 2:1 and (c) 1:1.

Fig. 8 Fit of the WDS spectra peaks for the Ba-Lα and Ti-Kα peaks of (a) the standard BaTiO3 and BaTiO3 samples hydrothermally synthesised at 220 °C using Ba/Ti precursor ratios of (b) 4:1, (c) 2:1 and (d) 1:1 (sample labels explained in Table 1).

Fig. 9 (a) XRD patterns of BaTiO3 samples hydrothermally synthesised using Ba/Ti precursor ratios of 4:1, 2:1 and 1:1 with Ba precursor concentration kept constant at 0.09 mol/L, and reacted at various synthesis temperatures of 120, 150, 180 and 220 °C; (b) crystallite size and (c) tetragonality (c/a) of BaTiO3 samples plotted against reaction temperature in hydrothermal synthesis using Ba/Ti precursor ratios of 4:1, 2:1 and 1:1, obtained from the Rietveld fits to the XRD patterns (sample labels explained in Table 4).

Fig. 10 (a) Raman spectra of BaTiO3 samples hydrothermally synthesised using Ba/Ti precursor ratios of 4:1, 2:1 and 1:1 with Ba precursor concentration kept constant at 0.09 mol/L, and reacted at various synthesis temperatures of 120, 150, 180 and 220 °C (peaks at ~307 cm-1 being marked as shaded); (b) relative integrated intensities of the Raman peak at 307 cm-1 for BaTiO3 samples plotted against reaction temperature in hydrothermal synthesis using Ba/Ti precursor ratios of 4:1, 2:1 and 1:1 (sample labels explained in Table 4).

Fig. S1 XRD pattern of amorphous TiO2 powder precipitated when using Ti(OCH(CH3)2)4 as the Ti precursor in hydrothermal synthesis of BaTiO3.

Fig. S2 Rietveld fits to the XRD patterns of (a) BTO 4:1-80 °C, (b) BTO 4:1-120 °C, (c) BTO 4:1-150 °C, (d) BTO 4:1-180 °C, (e) BTO 4:1-220 °C, (f) BTO 2:1-120 °C, (g) BTO 2:1-150 °C, (h) BTO 2:1-180 °C, (i) BTO 2:1-220 °C, (j) BTO 1:1-180 °C and (k) BTO 1:1-220 °C samples (sample labels explained in Table 1). The data points and Rietveld fits are overlaid as black crosses and red lines, respectively. The difference plots and background are shown in blue and green, respectively. The pink tick marks represent the allowed reflection positions for tetragonal BaTiO3 structure with space group P4mm.
 
Fig. S3 WDS spectra of the standard BaTiO3 and BaTiO3 samples hydrothermally synthesised at 220 °C using Ba/Ti precursor ratios of 4:1, 2:1 and 1:1 (sample labels explained in Table 1).

Fig. S4 Rietveld fits to the XRD patterns of (a) BTO* 4:1-120 °C, (b) BTO* 4:1-150 °C, (c) BTO* 4:1-180 °C, (d) BTO* 4:1-220 °C, (e) BTO* 2:1-120 °C, (f) BTO* 2:1-150 °C, (g) BTO* 2:1-180 °C, (h) BTO* 2:1-220 °C, (i) BTO* 1:1-150 °C, (j) BTO* 1:1-180 °C and (k) BTO* 1:1-220 °C samples (sample labels explained in Table 4). The data points and Rietveld fits are overlaid as black crosses and red lines, respectively. The difference plots and background are shown in blue and green, respectively. The pink tick marks represent the allowed reflection positions for tetragonal BaTiO3 structure with space group P4mm.

Fig. S5 Crystallite size of BaTiO3 samples plotted against reaction temperature in hydrothermal synthesis using Ba/Ti precursor ratios of (a) 4:1 and (b) 1:1, obtained from the Rietveld fits to the XRD patterns, for the reaction conditions of (a) 0.18 M Ba : 0.045 M Ti and 0.09 M Ba : 0.0225 M Ti, (b) 0.045 M Ba : 0.045 M Ti and 0.09 M Ba : 0.09 M Ti. Sample labels explained in Table 1 and Table 4.