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Requirement
Write a paper on Synthesis of copper-1-selenide nanoroid.
Requirements:
1. Chemicals required:
Cupric Chloride (CuCl2), Na2SeO3, cyclohexane, Sodium borohydride NaBH4, CTAB, ethanol and water. All the chemicals including Cupric Chloride (CuCl2), Na2SeO3, Se powder. Cyclohexane, Sodium borohydride NaBH4 were from the Sigma-Aldrich company.
2. Apparatus and equipment required:
Refluxing system, beaker, centrifugation, test tubes.
Solution
Preparation Procedure:
The Na2SeSO3 solution was first prepared by refluxing the five mM of selenium powder and five mM of Na2SO3 in 200 ml distilled water under the nitrogen atmosphere for 24 h.10 mL of DI water, five mL cyclohexane and 0.0.1 CTAB were mixed together thoroughly. The obtained mixture was then stirred continuously for 24 hours at nitrogen temperature until a homogenous mixture was obtained. In the typical preparation process, ten mL of 25 mM Cupric Chloride or CuCl2 was mixed along with the homogenous mixture with a vigorous stirring at the room temperature( 25 C). The prepared solution was kept at static under the nitrogen temperature for 2 hours. The prepared solution was kept undisturbed during this period. After keeping it undisturbed for 2 hours, ten mL of 25 mM of Na2SeO3 was added to the mixture. Following that five mL of NaBH4 was added to the solution. It was observed that the colour of the mixture instantly turned to black after adding of Na2SeO3 and NaBH4. Following that the mixture was stirred again in a vigorous manner for at least an hour. The mixture was then kept static for 5-6 hours at ambient temperature and was then stirred vigorously again. The mixed solution so obtained was then kept static at the ambient temperature for 24 hours. An accumulation of black coloured particle on the bottom of the beaker was expected. It was observed that the black particles had settled down at the bottom of the beaker. The so obtained mixture and the sample were then send to the autoclave. The mixture was then separated using the technique of centrifugation. For that, the centrifugation was set at the speed of 15,000 rpm and the mixture was then centrifugated. The collected sampled were then washed thoroughly with the double distilled water for two to three times. The washed samples were then again washed using ethanol mixture for five to six times.
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Finally, when the phase where the nanoroid were expected to grow, four replicas of the experiment samples were made to run in parallel. But the replica of the single experiment was terminated at different temperatures of 24 hours, 36 hours, 48 hours and 72 hours.
These synthesized Copper selenide nanoroids were then characterized using the UNICAM UV300 spectrophotometer from the Thermo Spectronic, USA. The high-resolution transmission electron microscopy i.e. the HR-TEM, Hitachi H-700H from Hitachi, Japan, energy dispersive spectroscopy, a PerkinElmer LS55 spectrofluorimeter, Laser Raman spectroscopy and the Fourier transform infrared (FT-IR) spectroscopy. (Dhasade et al., 2015)
The chemical equation involved in this reaction:
A detailed procedure has been depicted in the tabular form below.
Raman spectroscopy is used for investigating the changes occurring in the of nanomaterials’ electronic properties via the special electron–phonon coupling. This electron–phonon coupling occurs only under the strong resonant situations. Hence, the Raman spectra can be quite effective in a case of detecting the new chemical bonds.
Hence, the copper-1-selenide nanorods were effectively prepared at the ambient temperature. Photochemical Properties: These nanoroids were seen to be readily dispersed in water and were seen to exhibit NIR along with a high value of molar extinction coefficient observed at 980 nm. Further, on excitation at 800 nm of light, the nanoroids were seen to produce a considerable photothermal heating that was accompanied by a moderate photothermal transduction efficiency. (Zhang et al., 2015)
This efficiency was observed to be around 22% when it was directly compared with the nanorods as well as the nanoshells of gold (Au). Further, it was observed that the in-vitro photothermal heating of selenide copper nanorods led to the destruction of cell exactly after 5 min of laser irradiation at 33 W/cm in the presence of human colorectal cancer cell (HCT-116. This demonstrated the viability of selenide copper nanorods for the application in the photothermal therapy. (Hessel et al., 2011)
Optical Properties: The investigation of the optical band gap energy in case of the irradiated copper selenide thin films was done. The crystal size of the deposited copper one selenide was found to be around 11 nm along with the band gap energy of 2.57 eV. The crystal sizes of the irradiated copper selenide were examined to be around approximately of 83, 64, 42 and 21 nm. The band gap energies were found out to be approximately around 2.39, 2.43, 2.48, 2.51 eV when to treat with the doses of 10, 20, 35 and 45 kGy, respectively. It was seen that the increase in the copper one selenide nanoroids resulted in a decrease in band gap energy. This decrease in band gap energy that was inversely proportional to the crystal size of the copper selenide was found to be attributed to the quantum confinement effect.
Additionally, it was observed that with the dose of around 50 kGy the crystallite size of copper selenide was found to be around 6 nm. This nanoroid size was less than that of the deposited copper selenide thin film when compared, and the band gap energy was found out to be around 2.62 eV, which was observed to be more than as the deposited CuSe thin film.
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Dhasade, S., Thombare, J., Gaikwad, R., Gaikwad, S., Kumbhare, S., & Patil, S. (2015). Copper selenide nanorods grown at room temperature by electrodeposition. Materials Science In Semiconductor Processing, 30, 48-55. http://dx.doi.org/10.1016/j.mssp.2014.09.021
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Hessel, C., Pattani, V., Rasch, M., Panthani, M., Koo, B., Tunnell, J., & Korgel, B. (2011). Copper Selenide Nanocrystals for Photothermal Therapy. Nano Letters, 11(6), 2560-2566. http://dx.doi.org/10.1021/nl201400z
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Zhang, L., Zhao, S., Li, Y., Lan, Y., Han, M., Dai, Z., & Bao, J. (2015). Monoclinic Copper(I) Selenide Nanocrystals and Copper(I) Selenide/Palladium Heterostructures: Synthesis, Characterization, and Surface-Enhanced Raman Scattering Performance. Eur. J. Inorg. Chem., 2015(13), 2229-2236. http://dx.doi.org/10.1002/ejic.201500008
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