Effects of Calcination Holding Time on Properties of Wide Band Gap Willemite Semiconductor Nanoparticles by the Polymer Thermal Treatment Method
Abstract
:1. Introduction
2. Results and Discussion
2.1. Thermogravimetric Analysis
2.2. Raman Analysis
2.3. FT–IR Analysis
2.4. X-ray Diffraction Analysis
2.5. HR-TEM Analysis
2.6. FESEM-EDX Analysis
2.7. UV–Vis Analysis
2.8. Photoluminescence Analysis
3. Material and Methods
Characterization
4. Conclusions
Acknowledgments
Author Contributions
Conflicts of Interest
References
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Sample Availability: Samples of the compounds are available from the authors. |
Wave Number (cm–1) | Assignment of Vibration Mode | Reference |
---|---|---|
800–1100 | Stretching vibration of SiO4 group | [47,48] |
859–866 | Crystalline Zn2SiO4 vibration peak | [48,49] |
758 | Ring C–C vibration | [45] |
885 | C–C stretching vibration | [45] |
934 | C–C Ring breathing | [45,46] |
1233 | C–C Back bone | [45] |
1370 | C–H Deformation | [45,46] |
1494 | CH2 Scissors | [45] |
1665 | C=O (amide) | [45] |
Wave Number (cm–1) | Assignment of Vibration Mode | Reference |
---|---|---|
379–441 | Zn–O asymmetric stretching vibration | [26] |
580 | Zn–O symmetric stretching vibration | [26] |
884–884 | Si–O stretching vibration | [26] |
639–641 | C–N=O bending vibration | [52] |
838 | C–C ring vibration | [51,52] |
1277 | C–N stretching vibration | [41,50,51] |
1402–1429 | –C–H– bending vibration of methylene group | [42] |
1648 | N–H stretching vibration | [50] |
2945 | C–H vibration | [41,50,51] |
3414 | N–H bending vibration | [41,50,51] |
Calcination Holding Time (h) | Peak Position (2θ) | FWHM | DXRD (nm) | DTEM (nm) | Experimental Eg (eV) |
---|---|---|---|---|---|
1 | 33.86 | 0.476 | 18.23 | 19.74 | 5.39 ± 0.04 |
2 | 33.90 | 0.388 | 21.70 | 23.03 | 5.35 ± 0.04 |
3 | 33.96 | 0.351 | 22.29 | 26.34 | 5.34 ± 0.04 |
4 | 33.98 | 0.308 | 27.40 | 29.71 | 5.27 ± 0.04 |
Method | Precursors | Synthesis Conditions | Particle Size (nm) | Morphology | References |
---|---|---|---|---|---|
Solid–state | Zinc oxide, silicon oxide powder | calcination: 1330 °C, 4 h | 1000–5000 | Larger grain size | [22] |
Hydrothermal | zinc nitrate, silicon oxide | 700 °C, 10 h | 300–1000 | Non–uniform distribution | [39] |
Super critical water | zinc hydroxide, Amorphous silica | 30 MPa, 1 h, 400 °C | 1000–2000 | Non–uniform nanorods, distribution | [55] |
Sol–gel method | Tetraethylorthosilicate, and zinc acetate dihydrate | 1200 °C, 2 h, | 70–80 | Non–uniform particle distribution | [18] |
Spray pyrolysis | zinc acetate, tetraethyl orthosilicate, sulpuric acid | 1000 °C, 10 h | 200–1000 | Spherical particles, aggregate morphology | [29] |
Sonochemical | Tetraethylorthosilicate, and zinc acetate dihydrate | 950, 2h | 50 | Uniform distribution | [26] |
Polymer thermal treatment | zinc acetate dihydrate Silicon tetraacetate | 900 °C 3 h | 26 | Uniform Nanoparticle | This Paper |
Optical Bandmgap (eV) | Eg (Experimental) | Direct Allowed Transition n = 1/2 | Direct Forbidden Transition n = 3/2 | Indirect Allowed Transition n = 2 | Indirect Forbidden Transition n = 3 |
---|---|---|---|---|---|
1 h | 5.39 ± 0.04 | 5.38 ± 0.04 | 5.32 ± 0.04 | 5.23 ± 0.04 | 5.43 ± 0.04 |
2 h | 5.36 ± 0.04 | 5.35 ± 0.04 | 5.27 ± 0.04 | 5.17 ± 0.04 | 5.38 ± 0.04 |
3 h | 5.34 ± 0.04 | 5.33 ± 0.04 | 5.21 ± 0.04 | 5.07 ± 0.04 | 5.27 ± 0.04 |
4 h | 5.27 ± 0.04 | 5.25 ± 0.04 | 5.16 ± 0.04 | 4.72 ± 0.04 | 5.10 ± 0.04 |
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Alibe, I.M.; Matori, K.A.; Sidek, H.A.A.; Yaakob, Y.; Rashid, U.; Alibe, A.M.; Mohd Zaid, M.H.; Ahmad Khiri, M.Z. Effects of Calcination Holding Time on Properties of Wide Band Gap Willemite Semiconductor Nanoparticles by the Polymer Thermal Treatment Method. Molecules 2018, 23, 873. https://doi.org/10.3390/molecules23040873
Alibe IM, Matori KA, Sidek HAA, Yaakob Y, Rashid U, Alibe AM, Mohd Zaid MH, Ahmad Khiri MZ. Effects of Calcination Holding Time on Properties of Wide Band Gap Willemite Semiconductor Nanoparticles by the Polymer Thermal Treatment Method. Molecules. 2018; 23(4):873. https://doi.org/10.3390/molecules23040873
Chicago/Turabian StyleAlibe, Ibrahim Mustapha, Khamirul Amin Matori, Hj Abdul Aziz Sidek, Yazid Yaakob, Umer Rashid, Ali Mustapha Alibe, Mohd Hafiz Mohd Zaid, and Mohammad Zulhasif Ahmad Khiri. 2018. "Effects of Calcination Holding Time on Properties of Wide Band Gap Willemite Semiconductor Nanoparticles by the Polymer Thermal Treatment Method" Molecules 23, no. 4: 873. https://doi.org/10.3390/molecules23040873