Name: The Effect of Ultraviolet Radiation on the Chemical Bath Deposition of Bis(thiourea) Cadmium Chloride Crystals and the Subsequent CdS Obtention (Video) | JoVE Journal
Uploaded: 2018-08-30T14:00:00.000+00:00
Duration: 5 min 21 s
Description: Learn chemical bath deposition to synthesize bis(thiourea) cadmium chloride crystals and study UV light effects on morphology. This protocol enables controlled crystal growth for material science research.

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5 minutes

L.E. Trujillo and F.J. Willars Rodr&#237;guez thank CONACYT for their scholarships. E.A. Chavez-Urbiola thanks CONACYT for the &#34;Catedras CONACYT&#34; program. Authors also acknowledge the technical assistance of C.A. Avila Herrera, M. A. Hern&#225;ndez Landaverde, J.E. Urbina Alv&#225;rez, and A. Jim&#233;nez Nieto.

CAUTION: The chemicals used in this protocol are toxic and carcinogenic; thus, the safety recommendations and procedures must be followed carefully. Wear proper protective equipment and consult any relevant materials safety data sheet (MSDS).
1. Synthesis of Bis(thiourea) Cadmium Chloride
<ol>
	<li>Preparation of the precursor solution
	<ol>
		<li>Pour 500 mL of deionized water into a 1 L beaker with constant agitation; add 0.3 mL of hydrochloric acid at a 36.5% concentration, making sure that the pH of the solution is as close as possible to 3, using a pH meter. 
		CAUTION: To avoid any health effects, performing this action inside a fume hood is highly recommended.</li>
		<li>Pour 50 mL of the precursor solution prepared as indicated in step 1.1.1 into each of two 100 mL beakers (hereafter, these beakers will be named A and B). 
		NOTE: Two experiments (A and B, dependent on the beaker used) are carried out simultaneously. Only experiment B will be exposed to UV light.</li>
	</ol>
	</li>
	<li>Weigh 2.29 g of CdCl2 for each beaker (A and B). 
	CAUTION: Perform this action inside the fume hood as the material used is identified as hazardous. Cadmium is highly toxic and identified as carcinogenic when inhaled; it must be handled carefully.</li>
	<li>Weigh 1.33 g of CS(NH2)2 for each beaker (A and B). 
	CAUTION: Perform this action inside the fume hood as the material used is dangerously unhealthy. Thiourea is highly toxic when inhaled and must be handled carefully.</li>
	<li>Add 2.29 g of CdCl2 and 1.33 g of CS(NH2)2 to each beaker (A and B) containing 50 mL of the precursor solution.</li>
</ol>
2. Comparative Synthesis of Bis(thiourea) Cadmium Chloride
<ol>
	<li>Experimental arrangement without UV light (A).
	<ol>
		<li>Place the beaker (A) on the stirring hot plate and heat it up to 343 K. Set the plate on a moderate stirring speed. 
		CAUTION: Perform this action inside the fume hood.</li>
		<li>Keep the solution in the beaker (A) moderately stirring for 2 h on the plate at 343 K.</li>
	</ol>
	</li>
	<li>Experimental arrangement with UV light (B).
	<ol>
		<li>Place the beaker B on the plate and heat it up to 343 K. Set the stirring speed on a moderate level and switch on the UV light source. 
		NOTE: The experimental arrangement is shown in Figure 1. 
		CAUTION: Perform this action inside the fume hood.</li>
		<li>Keep the temperature and stirring conditions as described in step 2.2.1 for 2 h.</li>
	</ol>
	</li>
</ol>
3. Obtaining Bis(thiourea) Cadmium Chloride Crystals
<ol>
	<li>Mount 2 glass funnels with filter paper (No. 40, &#216; = 125 mm), each one over a 100 mL volumetric flask, for A and B. To avoid the crystal formation at this stage; do not let the solution cool before filtering it.</li>
	<li>Filter the solutions A and B through the paper, each into their own 100 mL flask. 
	CAUTION: Perform this action inside the fume hood.</li>
	<li>Let both solutions inside the volumetric flasks cool to room temperature. 
	NOTE: The crystals begin to grow in the first minutes inside the volumetric flasks.</li>
	<li>Prepare the filtering assembly again (step 3.1) with a new filter paper.</li>
	<li>Filter the solutions with the crystals through the filter paper into separate volumetric flasks. 
	CAUTION: Perform this action inside the fume hood.</li>
	<li>Transfer the crystals on the filter paper to the respective watch glass. 
	NOTE: At this point, there are 2 watch glasses, 1 for A and 1 for B.</li>
	<li>Confirm the presence of bis(thiourea) cadmium chloride crystals by powder X-ray diffraction (XRD) and Raman spectroscopy, as reported in Trujillo et al.12.</li>
</ol>
4. Calcination of the Crystals to Obtain CdS
<ol>
	<li>Place the crystals obtained in step 3.7 into 2 different crucibles, 1 for A and 1 for B.</li>
	<li>Preheat an electric laboratory furnace and stabilize its temperature at 773 K or higher.</li>
	<li>Place the crucibles of step 4.1 inside the preheated furnace. 
	CAUTION: The released vapors during calcination are toxic. Make sure that the furnace is in a fume hood due to the toxic fumes that it will be exhausted.</li>
	<li>Let the material stand inside the furnace for 1 h at 773 K. Then, turn off the furnace and let it cool to room temperature. After that, remove the crucibles from the oven.</li>
</ol>

<ol><li>Venkataramanan, V., Maheswaran, S., Sherwood, J. N., Bhat, H. L. <a target="_blank" href="https://www.sciencedirect.com/science/article/pii/S0022024897001371">Crystal growth and physical characterization of the semiorganic bis(thiourea) cadmium chloride.</a> Journal of Crystal Growth. 179 (3-4), 605-610 (1997).</li>
<li>Ushasree, P. M., Muralidharan, R., Jayavel, R., Ramasamy, P. <a target="_blank" href="https://www.sciencedirect.com/science/article/pii/S0022024800005935">Growth of bis(thiourea) cadmium chloride single crystals a potential NLO material of organometallic complex.</a> Journal of Crystal Growth. 218 (2-4), 365-371 (2000).</li>
<li>Ushasree, P. M., Jayavel, R. <a target="_blank" href="https://www.sciencedirect.com/science/article/pii/S0925346702002082">Growth and micromorphology of as-grown and etched bis(thiourea) cadmium chloride (BTCC) single crystals.</a> Optical Materials. 21 (1-3), 569-604 (2002).</li>
<li>Pawar, S. M., Pawar, B. S., Kim, J. H., Joo, O., Lokhande, C. D. <a target="_blank" href="https://www.sciencedirect.com/science/article/pii/S1567173910002178">Recent status of chemical bath deposited metal chalcogenide and metal oxide thin films.</a> Current Applied Physics. 11 (2), 117-161 (2011).</li>
<li>Suriakarthick, R., Kumar, V. N., Shyju, T. S., Gopalakrishnan, R. <a target="_blank" href="https://www.sciencedirect.com/science/article/pii/S1369800114002200">Investigation on post annealed copper sulfide thin films from photochemical deposition technique.</a> Materials Science in Semiconductor Processing. 26 (1), 155-161 (2014).</li>
<li>Podder, J., Kobayashi, R., Ichimura, M. <a target="_blank" href="https://www.sciencedirect.com/science/article/pii/S0040609004008934">Photochemical deposition of Cu x S thin films from aqueous solutions.</a> Thin Solid Films. 472 (1-2), 71-75 (2005).</li>
<li>Gunasekaran, M., Gopalakrishnan, R., Ramasamy, P. <a target="_blank" href="https://www.sciencedirect.com/science/article/pii/S0167577X03004166">Deposition of ZnS thin films by photochemical deposition technique.</a> Materials Letters. 58 (1-2), 67-70 (2004).</li>
<li>Ichimura, M., Goto, F., Ono, Y., Arai, E. <a target="_blank" href="https://www.sciencedirect.com/science/article/pii/S0022024898009853">Deposition of CdS and ZnS from aqueous solutions by a new photochemical technique.</a> Journal of Crystal Growth. 198 (1), 308-312 (1999).</li>
<li>Kumaresan, R., Ichimura, M., Sato, N., Ramasamy, P. <a target="_blank" href="https://www.sciencedirect.com/science/article/pii/S0921510702003227">Application of novel photochemical deposition technique for the deposition of indium sulfide.</a> Materials Science Engineering: B. 96 (1), 37-42 (2002).</li>
<li>Rama, G., Jeevanandam, P. <a target="_blank" href="https://link.springer.com/article/10.1007/s11051-015-2961-1">Evolution of different morphologies of CdS nanoparticles by thermal decomposition of bis(thiourea)cadmium chloride in various solvents.</a> Journal of Nanoparticle Research. 17 (1), 1-13 (2015).</li>
<li>Pabitha, G., Dhanasekaran, R. Growth and characterization of a nonlinear optical crystal - bis thiourea cadmium chloride. International Journal of Innovative Research in Science, Engineering and Technology. 4 (1), 34-38 (2015).</li>
<li>Trujillo, L. E., et al. <a target="_blank" href="https://www.sciencedirect.com/science/article/pii/S0022024817305353">Di-thiourea cadmium chloride crystals synthesis under UV radiation influence.</a> Journal of Crystal Growth. 478 (1), 140-145 (2017).</li>
<li>Elilarassi, R., Maheshwari, S., Chandrasekaran, G. <a target="_blank" href="https://www.researchgate.net/publication/268365456_Structural_and_optical_characterization_of_CdS_nanoparticles_synthesized_using_a_simple_chemical_reaction_route">Structural and optical characterization of CdS nanoparticles synthesized using a simple chemical reaction route.</a> Optoelectronics and Advanced Materials - Rapid Communications. 4 (3), 309-312 (2010).</li>
<li>Selvasekarapandian, S., Vivekanandan, K., Kolandaivel, P., Gundurao, T. K. <a target="_blank" href="https://onlinelibrary.wiley.com/doi/abs/10.1002/crat.2170320214">Vibrational Studies of Bis(thiourea) Cadmium Chloride and Tris(thiourea) Zinc Sulphate Semiorganic Non-linear Optical Crystals.</a> Crystal Research & Technology. 32 (2), 299-309 (1997).</li>
</ol>

The authors have nothing to disclose.

The discussion presented in this section focuses only on the protocol and not on the results already shown in the representative results.
One of the most critical parts of the protocol is the preparation of the precursor solution. It is fundamental to maintain an acidic pH to avoid the Cd(OH)2 formation. If the pH is not acidic, it leads to the direct formation of CdS due to the thiourea dissociation and the Cd(OH)2 formation. 
The second most important step is step ...

An important area of research is single crystals; their growth is aimed at different applications. These can be used as non-linear optical materials applied in the areas of laser technology, in the field of optoelectronics, and for the storage of information1, which provides an area of opportunity for their investigation. Bis(thiourea) cadmium chloride is a metal-organic material and can be synthesized from two precursors, thiourea and cadmium chloride, obeying the following chemical formula: 2CS(NH2)2 + CdCl2 CdCl2-[CS(NH2)2]2. This metal-organic material has been prepared under different reaction conditions, such as temperature and pH, but never with the assistance of ultraviolet (UV) light.
The influence of pH on the structure of the crystal has been reported; at a pH &#60; 6, it is possible to obtain the formation of monocrystals. These, in turn, are modified depending on the pH range. At an interval of 6 to 4, it is possible to obtain hexagonal structures, for if pH is &#60; 4, an orthorhombic crystalline structure is obtained2. The ion dissociation is promoted by the acidic pH Cd2+ and Cl- since it prevents cadmium hydroxide formation [Cd(OH)2]. This stabilizes the cadmium: a cadmium atom joins with two sulfur-free radicals and two chlorines.
Here, the synthesis is carried out using the chemical bath deposition technique (CBD), controlling the different conditions that intervene at the time of the chemical reaction3. In CBD, the factors that control the chemical reaction are the following: the solution temperature, the precursor ions, the solution pH, the number of reagents, and the agitation speed, to name a few. On the other hand, the compared technique used here is called photochemical bath deposition (PCBD) because it uses UV light assistance. There have been reports in which UV light assistance has been used to synthesize films of CuSx4,5, ZnS6, CdS7, and InS8, among others. Ichimura and Gunasekaran9 present in their work that sulfate solutions have an absorption edge close to 300 nm. Due to this absorption range, ultraviolet radiation is applied, which results in a similar emission range to that of the absorbed solutions.
Another property of bis(thiourea) cadmium chloride is its degradation when heated. It exhibits an initial decomposition at temperatures of 512 K and above, forming cadmium sulfide (CdS). The degradation reaction is as follows: [Cd(CS[NH2])2]Cl2 &#8594; &#916; CdS + HNCS + NH3 + NH4SCN. This degradation generates thiocyanuric acid and various thiocyanates10,11. Also, in the research group, some effects caused by the UV radiation were studied12. Last, in this work, a comparative synthesis procedure for bis(thiourea) cadmium chloride crystals is described, as well as the effects of UV light.

<table><tbody><tr><td>&lt;strong&gt;Reagents&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>Cadmium chloride Anh. ACS, 99.4 %</td><td>Fermont</td><td>PQ24291</td><td>Highly toxic</td></tr><tr><td>Thiourea technical grade, 99.9 %</td><td>Reasol</td><td>R5913</td><td>Toxic</td></tr><tr><td>Hydrochloric acid, 36.5 &amp;ndash; 38.0 %</td><td>J.T.Baker</td><td>MFCD00011324</td><td>Highly corrosive liquid</td></tr><tr><td>&lt;strong&gt;Material&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>Filter paper</td><td>Whatman</td><td>1440 125</td><td>40, Ashless, Circles, 125 mm</td></tr><tr><td>Beaker</td><td>Kimax</td><td>1400</td><td>100 mL</td></tr><tr><td>Volumetric Flask</td><td>Kimax</td><td>28012-100</td><td>Class A 100 mL</td></tr><tr><td>Glass Funnel</td><td>Kimax</td><td>28980-150</td><td>Addition Funnel, Long Stem, 60&amp;deg; Angle, Wide Top. Type I, Class B.</td></tr><tr><td>Watch glasses</td><td>Pyrex</td><td>9985-150</td><td>Corning, 150&amp;nbsp;mm</td></tr><tr><td>Crucibles</td><td>Fisherbrand</td><td>FB-965-D</td><td>High-Form Porcelain</td></tr><tr><td>&lt;strong&gt;Equipment&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>Furnace</td><td>Briteg Instrumentos Cientificos S.A. de C.V.</td><td>1010</td><td></td></tr><tr><td>Fume Hood</td><td>Fisher Alders, S.A. de C.V.</td><td>F1124</td><td></td></tr><tr><td>Light surce</td><td>Philips</td><td>PL-S 9W UV-A/2P 1CT/6X 10 CC</td><td></td></tr><tr><td>pH meter</td><td>OAKTON</td><td>WD-35419-10</td><td></td></tr><tr><td>Hotplate whit magnetic stirrer</td><td>Cole-Parmer</td><td>JZ-04660-75</td><td></td></tr></tbody></table>

the effect of ultraviolet radiation on the chemical bath deposition of bis(thiourea) cadmium chloride crystals and the subsequent cds obtention

The Effect of Ultraviolet Radiation on the Chemical Bath Deposition of Bis(thiourea) Cadmium Chloride Crystals and the Subsequent CdS Obtention

In this work, the effects on the preparation of bis(thiourea) cadmium chloride crystals when illuminated with ultraviolet (UV) light at a wavelength of 367 nm using the chemical bath deposition technique are studied comparatively. Two experiments are performed to make a comparison: one without UV light and the other with the aid of UV light. Both experiments are performed under equal conditions, at a temperature of 343 K and with a pH of 3.2. The precursors used are cadmium chloride (CdCl2) and thiourea [CS(NH2)2], which are dissolved in 50 mL of deionized water with an acidic pH. In this experiment, the interaction of electromagnetic radiation is sought at the moment the chemical reaction is carried out. The results demonstrate the existence of an interaction between the crystals and the UV light; the UV light assistance causes crystal growths in an acicular shape. Also, the final product obtained is cadmium sulfide and shows no evident difference when synthesized with or without the use of UV light.

The UV-Vis diffusion's reflectance absorption spectra in both precursor solutions, A and B, show the existence of a bis(thiourea) cadmium chloride complex—CdCl2-(CS(NH2)2)2. This is evidenced by a broad absorption band within the range of 250 - 500 nm in Figure 2c. In turn, Figure 2c is the combination of the main absorption bands of the isolated CdCl2 and CS(NH2)<...

This article presents a protocol for the synthesis of bis(thiourea) cadmium chloride crystals by chemical bath deposition. Two experiments are described: one aided by ultraviolet light compared to one without ultraviolet light.

In this work, the effects on the preparation of bis(thiourea) cadmium chloride crystals when illuminated with ultraviolet (UV) light at a wavelength of ...

the-effect-ultraviolet-radiation-on-chemical-bath-deposition-bis

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Learn chemical bath deposition to synthesize bis(thiourea) cadmium chloride crystals and study UV light effects on morphology. This protocol enables controlled crystal growth for material science research.

The Effect of Ultraviolet Radiation on the Chemical Bath Deposition of Bis(thiourea) Cadmium Chloride Crystals and the Subsequent CdS Obtention (Video) | JoVE Journal

The Effect of Ultraviolet Radiation on the Chemical Bath Deposition of Bis(thiourea) Cadmium Chloride Crystals and the Subsequent CdS Obtention

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