Tailoring of structural, optical and electrical properties of anatase TiO2 via doping of cobalt and nitrogen ions

doi:10.1016/j.jmst.2021.09.014

Abstract

Abstract:

Pure (pristine) anatase and mono-doped and co-doped derivatives of TiO₂ having nitrogen (N) and cobalt (Co) as dopants with respective fixed doping concentrations of 0.7 mol.% and 1.0 mol.% were synthesized using auto-combustion sol-gel technique. The doping effects at corresponding non-metal and transition metal sites of TiO₂ on the basis of the structural, optical and electrical properties have been investigated. X-ray diffraction (XRD) measurement confirms the formation of pure anatase phase of TiO₂ for all samples having I4₁/amd space group of tetragonal structure which has been also verified by the Raman spectroscopy measurement. Various crystallographic parameters have been calculated by performing Rietveld refinement of XRD data including average crystallite size that has been observed in the range of 10-15 nm. Pure anatase phase indicates the incorporation of Co²⁺ into TiO₂ lattice which assists the substitution of N in place of oxygen in co-doped TiO₂. The band gap tuning towards the visible region from 3.2 to 2.1 eV has been achieved with mono-doping and co-doping of the N and Co in TiO₂ lattice. This can be described in terms of the formation of localized levels of N-2p and Co-3d states in mono-doping and an isolated intermediate band formation in co-doping case. Electrical properties have been investigated in details and explained as the synergetic effects of structural and inherent ionic characters of various dopants. The observed band gaps of all doped samples lie within the visible region which makes them pertinent as the solar energy harnessing materials for photocatalytic and photovoltaic applications.

Key words: TiO₂, Sol-Gel, X-ray diffraction, Electrical properties, Optical properties

Anchal Sharma, Puneet Negi, Ruhit Jyoti Konwar, Hemaunt Kumar, Yogita Verma, Shailja, Prakash Chandra Sati, Bhargav Rajyaguru, Himanshu Dadhich, N.A. Shah, P.S. Solanki. Tailoring of structural, optical and electrical properties of anatase TiO₂ via doping of cobalt and nitrogen ions[J]. J. Mater. Sci. Technol., 2022, 111: 287-297.

Figures/Tables 13

References 71

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Simulated /calculated crystallographic parameters			TiO₂	N-TiO₂	Co-TiO₂	N-Co-TiO₂
Lattice parameters	a = b (A^°) c (A^°)		3.784 (0) 9.507 (1)	3.784 (0) 9.504 (1)	3.786 (0) 9.502 (1)	3.785 (0) 9.501(1)
Atomic positions	X	Ti Co O N	0.000 (0) - 0.000 (0) -	0.000 (0) - 0.000 (0) 0.000 (0)	0.000 (0) 0.000 (0) 0.000 (0) -	0.000 (0) 0.000 (0) 0.000 (0) 0.000 (0)
	Y	Ti Co O N	0.750 (0) - 0.750 (0) -	0.750 (0) - 0.750 (0) 0.750 (0)	0.750 (0) 0.750 (0) 0.750 (0) -	0.750 (0) 0.750(0) 0.750 (0) 0.750 (0)
		Ti Co O N	0.125 (0) - 0.335 (0) -	0.125 (0) - 0.334 (0) 0.334 (0)	0.125 (0) 0.125 (0) 0.337 (0) -	0.125 (0) 0.125 (0) 0.335 (0) 0.335 (0)
Shape/FWHM parameters	U V W		1.399 (0) - 0.682 (0) 0.435 (0)	1.345 (0) - 0.676 (0) 0.503 (0)	1.541 (0) - 0.841 (0) 0.531 (0)	0.374 (0) 0.510 (0) 0.477 (0)
R-factors	R_p R_exp R_wp R_f R_bragg		18.0 21.3 23.0 3.01 4.81	16.7 20.8 22.0 2.89 4.04	19.5 22.3 23.7 3.45 5.38	18.1 22.1 23.5 3.15 4.33
GOF(χ²) Volume per unit cell (Å³)			1.16 136.178(7)	1.13 136.115(3)	1.13 136.196(4)	1.13 136.094(6)
Calculated corresponding to the most intense (101) peak
FWHM (deg.) Crystallite Size (nm) X-ray density (gcm^-3) Specific surface area (m²/g)			0.594(3) 14.20(1) 3.896(1) 109(6)	0.647(2) 12.82(3) 3.894(1) 119(5)	0.648(1) 12.92(5) 3.899(1) 119(6)	0.781(2) 10.12(8) 3.901(1) 152(6)
Calculated by W-H Plot
Crystallite size (nm) Lattice strain, ε			16.38(4) 12(2)×10^-4	14.16(2) 8(2)×10^-4	14.41(4) 9(2)×10^-4	10.80(2) 7(1) ×10^-4
Crystallographic structure parameters using VESTA software
Bond Angle (deg.)	O-Ti-O O-Ti-O O-Ti-O O-Ti-O O-Ti-O		78.75(1) 92.18(5) 101.25(5) 157.5(3) 180.00(0)	78.42(2) 92.31(5) 101.58(1) 156.8(3) 180.00(0)	79.23(4) 92.00(5) 100.77(2) 158.5(3) 180.00(0)	78.51(1) 92.28(5) 101.49(3) 157.0(3) 180.00(0)
Bond Length (Å)	Ti-O Ti-O		1.9294(8) 2.000(4)	1.9315(9) 1.988(4)	1.9269(8) 2.016(4)	1.9311(9) 1.990(4)

Simulated /calculated crystallographic parameters			TiO₂	N-TiO₂	Co-TiO₂	N-Co-TiO₂
Lattice parameters	a = b (A^°) c (A^°)		3.784 (0) 9.507 (1)	3.784 (0) 9.504 (1)	3.786 (0) 9.502 (1)	3.785 (0) 9.501(1)
Atomic positions	X	Ti Co O N	0.000 (0) - 0.000 (0) -	0.000 (0) - 0.000 (0) 0.000 (0)	0.000 (0) 0.000 (0) 0.000 (0) -	0.000 (0) 0.000 (0) 0.000 (0) 0.000 (0)
	Y	Ti Co O N	0.750 (0) - 0.750 (0) -	0.750 (0) - 0.750 (0) 0.750 (0)	0.750 (0) 0.750 (0) 0.750 (0) -	0.750 (0) 0.750(0) 0.750 (0) 0.750 (0)
		Ti Co O N	0.125 (0) - 0.335 (0) -	0.125 (0) - 0.334 (0) 0.334 (0)	0.125 (0) 0.125 (0) 0.337 (0) -	0.125 (0) 0.125 (0) 0.335 (0) 0.335 (0)
Shape/FWHM parameters	U V W		1.399 (0) - 0.682 (0) 0.435 (0)	1.345 (0) - 0.676 (0) 0.503 (0)	1.541 (0) - 0.841 (0) 0.531 (0)	0.374 (0) 0.510 (0) 0.477 (0)
R-factors	R_p R_exp R_wp R_f R_bragg		18.0 21.3 23.0 3.01 4.81	16.7 20.8 22.0 2.89 4.04	19.5 22.3 23.7 3.45 5.38	18.1 22.1 23.5 3.15 4.33
GOF(χ²) Volume per unit cell (Å³)			1.16 136.178(7)	1.13 136.115(3)	1.13 136.196(4)	1.13 136.094(6)
Calculated corresponding to the most intense (101) peak
FWHM (deg.) Crystallite Size (nm) X-ray density (gcm^-3) Specific surface area (m²/g)			0.594(3) 14.20(1) 3.896(1) 109(6)	0.647(2) 12.82(3) 3.894(1) 119(5)	0.648(1) 12.92(5) 3.899(1) 119(6)	0.781(2) 10.12(8) 3.901(1) 152(6)
Calculated by W-H Plot
Crystallite size (nm) Lattice strain, ε			16.38(4) 12(2)×10^-4	14.16(2) 8(2)×10^-4	14.41(4) 9(2)×10^-4	10.80(2) 7(1) ×10^-4
Crystallographic structure parameters using VESTA software
Bond Angle (deg.)	O-Ti-O O-Ti-O O-Ti-O O-Ti-O O-Ti-O		78.75(1) 92.18(5) 101.25(5) 157.5(3) 180.00(0)	78.42(2) 92.31(5) 101.58(1) 156.8(3) 180.00(0)	79.23(4) 92.00(5) 100.77(2) 158.5(3) 180.00(0)	78.51(1) 92.28(5) 101.49(3) 157.0(3) 180.00(0)
Bond Length (Å)	Ti-O Ti-O		1.9294(8) 2.000(4)	1.9315(9) 1.988(4)	1.9269(8) 2.016(4)	1.9311(9) 1.990(4)

Raman modes (cm^-1)	TiO₂	N-TiO₂	Co-TiO₂	N-Co-TiO₂
Symmetric stretching vibration of oxygen atoms in O-Ti-O bond, E_g1(1)	143	144	145	145
Symmetric stretching vibration of oxygen atoms in O-Ti-O bond, E_g(2)	196	195	197	192
Symmetric bending vibration of O-Ti-O bond B_1g	397	394	396	394
Vibration of O-Ti-O bond with fixed Ti atom (A_1g & B_1g)	515	514	513	515
Symmetric stretching vibration of oxygen atoms in O-Ti-O bond, E_g(3)	639	638	636	637

Raman modes (cm^-1)	TiO₂	N-TiO₂	Co-TiO₂	N-Co-TiO₂
Symmetric stretching vibration of oxygen atoms in O-Ti-O bond, E_g1(1)	143	144	145	145
Symmetric stretching vibration of oxygen atoms in O-Ti-O bond, E_g(2)	196	195	197	192
Symmetric bending vibration of O-Ti-O bond B_1g	397	394	396	394
Vibration of O-Ti-O bond with fixed Ti atom (A_1g & B_1g)	515	514	513	515
Symmetric stretching vibration of oxygen atoms in O-Ti-O bond, E_g(3)	639	638	636	637

Tailoring of structural, optical and electrical properties of anatase TiO₂ via doping of cobalt and nitrogen ions

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