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Facile decoration of CdS nanoparticles on TiO2: robust photocatalytic activity under LED illumination

  • Maryam Fatolah and Gholam Reza Khayati EMAIL logo
Published/Copyright: June 21, 2021
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Zeitschrift für Naturforschung B
From the journal Zeitschrift für Naturforschung B Volume 76 Issue 6-7

Abstract

A facile approach is presented to obtain visible-light-active TiO2/CdS nanocomposites with visible-light photocatalytic activity. Ordered nanospheres of TiO2 (with anatase as the main crystalline phase) were synthesized using evaporation-induced self-assembly (EIS) with P123 block polymer without any hazardous additives. Then, a rapid microwave (MW) protocol was used to obtain visible-light-absorbing nanocomposites between TiO2 and CdS in just 10 s. Based on Rietveld refinements of X-ray diffractrograms and elemental analysis it was found that nanoparticles of CdS are mainly decorated between the nanospheres of TiO2, which can simultaneously improve light absorption and suppress the unwanted photo-corrosion effects. The prepared nanocomposites were put to test for the removal of malachite green as a model pollutant from aqueous media under irradiation. The results revealed, that excessive loading results in unwanted surface covering and less than ideal activity, but for the sample with optimized loading, about 86 and 77% of the pollutant was degraded after 100 min of illumination at room temperature under the xenon short-arc and LED illumination, respectively.

Keywords: cadmium sulfide; functional applications; microwave processing; sol–gel processes; sulfide; titanium dioxide

1 Introduction

To mitigate the challenges imposed by environmental pollutions, considerable research efforts in various fields have been devoted to advanced oxidation techniques [1]. A major portion of solar irradiation consists of photons in the visible region. Therefore, the usage of semiconductors that can absorb and effectively utilize these photons is one of the most promising approaches [2]. Heterogeneous photocatalysts can effectively remove a wide variety of pollutants in ambient conditions without the need of harsh chemical reagents or producing hazardous by-products [3]. Amongst these, nanophotocatalysts occupy a significant place due to their high activity and size-dependent properties [4]. On the other hand, heterojunctions between semiconductors with suitable band structures can effectively increase both visible-light absorption and quantum efficiency simultaneously [5], [6].

As an n-type semiconductor, TiO2 is now considered as one of the most utilized photoactive materials for a wide variety of applications, e.g., hydrogen production water splitting, anti-fog and self-cleaning glasses, or air purification [7]. Notably, the first report regarding this material as photocatalyst dates back to 1972 [8]. TiO2 is abundant, non-toxic, economically viable and chemically stable, yet it can only absorb photons of the UV region [9] which is the major limitation when considering solar-based applications. Various approaches have been proposed to optimize the photo-activity of TiO2, such as phase and morphology engineering [10], metal or non-metal doping [11], [12], decoration with co-catalysts [13], [14] and most importantly for the current discussion, making heterojunctions with the other appropriate semiconductors [5].

As a II–VI semiconductor, cadmium sulfide (CdS) has a 2.4 eV direct band gap [15] and suitable band positions for making a variety of heterojunctions [16]. On its own term, CdS has found various photocatalytic applications [17] and is a great absorbent for visible photons. Unfortunately, it suffers from photo-corrosion and lacks the chemical stability needed for widespread utilization [18]. This phenomenon has been studied excessively [19] and efficient approaches have been proposed to mitigate its unwanted effects. These include shell-protective layers [20], [21], deposition of co-catalysts [22], masking in the pores of micro-/mesoporous supports [23] and also heterojunctions [24], [25], [26].

As we have seen so far, the band structures of TiO2 and CdS are suitable to form effective heterojunctions, which in turn leads to the special separation of photo-induced electron-hole pairs. On the other hand, the feasibility of inter-particle charge transfer can conceal CdS from the chemical reaction media and prohibit photo-corrosion. During the past decades, TiO2/CdS heterojunction photocatalysts have been used for a variety of applications including but not limited to solar cells [27], hydrogen evolution [28], [29], [30], degradation of organic compounds [31], [32] and dyes [33], [34], notably malachite green [32].

Several reports can be found in the literature regarding the microwave (MW) synthesis of CdS/TiO2 nanocomposites for photocatalytic as well as solar cell applications (see Table 1). N,N-dimethylformamide (DMF) has been used as a medium for the MW synthesis of pristine CdS nanoparticles and offers great control over the particle size and morphology in particular [35], [36], [37], [38], but the decoration of TiO2 has yet to be performed in DMF or DMF-containing media which can drastically change the synthesis conditions as well as the obtained nanocomposites. Our aim in the current study is to present a novel mixed-solvent approach to decorate TiO2 supports as a model large band gap support with CdS nanoparticles as photosensitizer. After loading optimization, the obtained heterostructured nanocomposites were investigated in terms of activity and robustness for visible-light removal of a model organic dye from aqueous medium.

Table 1:

Brief summary of the literature review for the microwave (MW) route for CdS/TiO- type heterojunctions.a

EntryComposition (TiO2 type)Cd and S precursorsSolventConditionsApplicationYear Ref.
1CdS/TiO2 (film)CdCl2 thioureaH2O100 W up to 40 minsolar cell2006 [39]
2CdS/TiO2/Au (P25)CdCl2H2O100 Wmethyl orange removal2007 [40]
Na2S10 min
3CdS/TiO2/RGO (P25)CdCl2H2O100 Wmethyl orange removal2010 [33]
Na2S10 min
4CdS/TiO2 (P25)Cd(NO3)2 thioureaH2O100 Wsolar cell2011 [27]
30 min
5CdS/TiO2 (P90)CdCl2H2O100 Wn/a2011 [41]
C3H6O2S30 min
6CdS/TiO2/Ag (in situ)Cd(NO3)2 thioacetamideethylene glycol600–900 Wmethyl orange and rhodamin B removal2012 [42]
6–8 min
7CdS/TiO2 (film)Cd(NO3)2 thioureaH2O100 WCr(VI) reduction2012 [43]
20 min
8CdS/TiO2 (P25)CdCl2 thioureaH2O180 Wmethylene blue removal2014 [44]
20 min
9CdS/TiO2(EIS)Cd(OAc)2thioacetamideDMF-H2O800 Wmalachite green removalthis study
10 s

  1. an/a = not available.

2 Experimental section

2.1 Materials and methods

All materials were of synthetic grade and used without further purification. Titanium isopropoxide Ti(O-iPr)4 (C12H28O4Ti, TTIP) was purchased from DaeJung® (South Korea); absolute ethanol (99.98%), EtOH; cadmium acetate Cd(CH3COO)2·2H2O, Cd(OAc)2; thioacetamide (C2H5NS); N,N-Dimethylmethanamide C3H7NO, DMF; and malachite green C23H25N2, were from Merck (Germany) while pluronic P123 block copolymer (PEO-PPO-PEO) was obtained from Sigma–Aldrich (United States). Doubly distilled di-ionized water was used in all experiments.

Powder X-ray diffraction patterns were recorded with a Philips (Holland) PW1730 instrument using CuKα irradiation (λ = 1.5418 Å) and Rietveld refinement was performed using the materials analysis diffraction program MAUD [45], [46], [47]. Scanning electron microscopy (SEM) as well as wavelength-dispersive X-ray spectroscopy (WDS) were performed on a Jeol (Japan) JXA-840 microscope. Field-emission scanning electron microscopy (FESEM) and energy-dispersive X-ray spectroscopy (EDS) were conducted using a TESCAN Mira 3 instrument (Czech Republic). Transmission electron microscopy (TEM) was performed using holey carbon copper grids with a Philips (Holland) CM120 apparatus working at 100 kV as acceleration voltage. Diffuse reflectance spectra (DRS) were measured with barium sulfate as blank standard on a Shimadzu (Japan) UV-2550 spectrophotometer.

2.2 Synthesis of pristine TiO2

TiO2 was obtained through the evaporation-induced self-assembly (EIS) method. In a typical run, 3 g of P123 (0.5 mmol) was added to 30 mL of absolute EtOH under vigorous magnetic stirring, then 4.5 mL of TTIP (15.2 mmol) was added drop-wise over the course of 5 min (if it’s added quickly, the sol would instantly become turbid). The obtained clear sol (Figure 1a) was transferred to a ceramic crucible (50 mL capacity) and kept at room temperature for one week; procure yellow xerogel (Figure 1b) was calcined at 500 °C in a static air muffle furnace for 6 h and annealed at room temperature overnight. The white powdery product was finely grounded and kept under vacuum until further use (Figure 1c) and characterization (Figure 1d).

Figure 1: Steps for obtaining TiO2/CdS nanocomposites; a) clear titanium sol in absolute ethanol; b) xerogel after going through evaporation for one week at room temperature; c) scanning electron micrograph of calcined and annealed TiO2 (d); e) TiO2/CdS nanocomposite obtained with MW approach (sample code “b”) after washing and drying for seven days at room temperature, along with a scanning electron micrograph (f).
Figure 1:

Steps for obtaining TiO2/CdS nanocomposites; a) clear titanium sol in absolute ethanol; b) xerogel after going through evaporation for one week at room temperature; c) scanning electron micrograph of calcined and annealed TiO2 (d); e) TiO2/CdS nanocomposite obtained with MW approach (sample code “b”) after washing and drying for seven days at room temperature, along with a scanning electron micrograph (f).

2.3 Decoration of CdS on TiO2

A mixed-solvent MW route is followed for obtaining the nanocomposite samples. In a typical run, 100 mg of Cd(OAc)2 (0.375 mmol) was dissolved in 10 mL of a 1:1 volumetric mixture of water and DMF, then 300 mg of thioacetamide (4 mmol) was added as the excess source of sulfur while being stirred. The solution turned yellow immediately, which is accounted for by the formation of complex clusters. 200 mg of TiO2 (2.5 mmol) was added to this solution and dispersed thoroughly by shaker and then in an ultrasonic bath. The mixture was then transferred to a Teflon® vessel (100 mL capacity) and placed at the center of a household MW oven (2.45 GHz, Panasonic, Japan and irradiated for 10 s at the maximum power [800 W]). The obtained orange mixture was centrifuged at 5000 rpm and washed twice with di-ionized water and once with absolute ethanol, then dried at room temperature and kept under vacuum (Figure 1e for sample “b”). To achieve other loadings of CdS on TiO2, the same 200 mg of pristine TiO2 was used in the above-mentioned procedure, only the amount of Cd and S precursors were respectively 50:150 mg for the sample “a” and 200:600 mg for the sample “c”, MW irradiation and washing protocols were the same.

2.4 Photocatalytic activity evaluation

In a typical run, 5 mg of the photocatalyst was added to 20 mL of 10 ppm malachite green solution in a 22 mL capacity capped Pyrex® tube, dispersed by shaker and ultrasonic bath, and then kept for 30 min in a dark environment with 30 °C to achieve adsorption equilibrium. The mixture was then placed 30 cm away from the light source (500 W short-arc Xe lamp, 50 W cool-white LED which gives 3750 lm light intensity with 6500 K color temperature) on top of a magnetic stirrer and cooled using an axial flow fan. On appropriate time intervals, 2 mL samples were taken from the reaction mixture and analyzed using a UV–Vis spectrophotometer (PG, T80+, U.K.). The samples were immediately injected back to the reactors. Each individual test was performed three times in order to achieve higher confidence in the results and reported as the mean ± standard error of the average; P < 0.05 was considered statistically different.

3 Results and discussion

3.1 Characterization

Powder X-ray diffraction patterns were recorded for phase identification, determination of the crystallite size and strain calculations. The spectra are presented in Figure 2 after smoothing and baseline correction. Indexed peaks along with Rietveld refinement results clearly reveal that the pristine TiO2 sample mainly consists of the anatase phase, with a minor contribution of rutile (compare the intensity of the (101) plane of anatase to that of the (110) plane of rutile – denoted R-110 – which contributes to about 3 wt% of the latter phase). The main anatase peak (101) shows a small discrepancy (at higher 2θ values) from the standard value (card no. 01-075-1537) which can be attributed to the morpholgical strain. This peak tends to shift to lower diffraction angles as more CdS is loaded. This strain can be attributed to the concealed nature of the secondary particles which has also been proved by TEM (Figure 3b). The characteristic peaks related to the extreme sample d (cubic and hexagonal phases of CdS) are extremely weak for either of the nanocomposite samples, thus leading to phase contribution values that are much smaller as compared to the results obtained from elemental analysis. Meanwhile, the (110) peak related to rutile starts to intensify which can be attributed to a reconstructive phase transition under MW irradiation, promoted by the presence of Cd as an “anatase to rutile transition” (ART) promoter [48]. Furthemore, the Williamson–Hall method [49] was used to calculate the crystallite sizes and strain of all samples. As can be seen from Table 2, the crystallite size tends to increase with CdS loading despite the TEM results (Figure 3b), This can be attributed to the discrete contribution of CdS peaks to the characteristic peaks of TiO2 and should be treated with caution and only used for comparative purposes. On the other hand, the crystalline strain tends to first increase and then to decrease with CdS loading. In sample “c” with the lowest strain, a significant intensity has been recorded for the (110) plane of rutile, which is probably due to the ART promotion. The above-mentioned properties along with a general summary of characterization results of the prepared samples are presented in Table 2.

Figure 2: Powder X-ray diffraction patterns of the samples. Indexing has been performed according to PDF cards of cubic CdS (00-001-0647), anatase (01-075-1537) and rutile (01-076-1939) along with Rietveld refinement results for each pattern.
Figure 2:

Powder X-ray diffraction patterns of the samples. Indexing has been performed according to PDF cards of cubic CdS (00-001-0647), anatase (01-075-1537) and rutile (01-076-1939) along with Rietveld refinement results for each pattern.

Figure 3: a) FESEM; b) and c) TEM micrographs for the sample “b” with 11 wt% CdS loading.
Figure 3:

a) FESEM; b) and c) TEM micrographs for the sample “b” with 11 wt% CdS loading.

Table 2:

Summary of the properties of prepared samples.

CodeOptical band gap (eV)Crystallite size (XRD) (nm)Crystalline strain (XRD) (%)Crystallite size (TEM) (nm)Elemental analysis (EDS) (wt%)
TiCdS
TiO23821055––
a2.393–5041
b2.214295283
c2.2161–50114
d2.11558–5918

To gain more insight into the micro/nano-structural features of the samples, SEM, FESEM and TEM were utilized, the first two equipped with WDS and EDS detectors, respectively. This has made elemental analysis and mapping possible. The results are presented in Figures S1–S5 (Supporting Information available online). The micron-sized spheres of pristine TiO2 (Figure 1d) are composed of much smaller crystallites (Figure S3a) and there is an abundance of empty space between them (Figure S1b), which is in agreement with the results of the above-mentioned XRD analysis regarding crystallite size.

The scanning electron micrograph of sample “b” with 11 wt% CdS (based on EDS elemental analysis) revealed the effect of the addition of smaller morphological features to the spheres of TiO2 (designated in Figure S2a). WDS mapping (Figure S2b–d) showed fairly even elemental distribution, which has also been proved with EDS for this and the other prepared composite samples (Figure S5). Essentially, every part of the sample is showing Ti, Cd and S simultaneously which may suggest that the CdS nanoparticles are not only placed at the surface of the TiO2 spheres, but also in the empty spaces between TiO2 crystallites. Indeed, XRD analysis confirmed this phenomenon, which also appears in the TEM micrographs (Figure 3b, c). The features of the FESEM micrograph (Figure 3a) can be related to the added smaller nanoparticles of CdS, apparent also in TEM.

DRS for the prepared samples are presented in Figure 4a. Kubelka–Munk (K–M) functions [50] were plotted and used to measure the optical band gaps with more confidence (Figure 4b and Table 2). According to this theory, the total diffuse reflectance of a material can be related to absorption and scattering [51]. The K–M function is defined as F(R∞) = (1 – R∞)2/2 R∞ where R∞ is the total reflectance measured for the material. When plotting the K–M function against the photon energy, the observed shoulder is related to the optical band gap of the material under study.

Figure 4: a) DRS absorption spectra and b) Kubelka–Munk (K–M) functions. The legend is the same for both parts.
Figure 4:

a) DRS absorption spectra and b) Kubelka–Munk (K–M) functions. The legend is the same for both parts.

In the case of pristine TiO2 and sample “d” (cubic CdS), optical band gaps are affected by anatase-rutile heterojunctions and oxygen doping, respectively. Decoration of CdS even in extremely small loads is proved to be profoundly effective upon optical absorption, making it possible to utilize a higher number of visible photons while reducing the use of hazardous species. Furthermore, the addition of CdS for heterojunction formation effectively enhances the special separation of photo-generated electron-hole pairs, which in turn leads to higher quantum efficiency.

3.2 Photocatalytic/adsorptive removal of malachite green

As mentioned above, all samples were thoroughly mixed with malachite green solution in the dark prior to illumination in order to achieve adsorption/desorption equilibrium. The results can be found in Figures 5, S6 and S7. The extreme samples of pristine TiO2 and sample “d” can remove 13 and 14% of the malachite green concentration after only 30 min of dark contact, which is justifiable with their small crystallite sizes and inter-particle empty spaces. Upon CdS loading, the adsorption capacity showed a maximum for the optimized “b sample” (11 wt%) which can be attributed to the simultaneous contribution of both CdS and TiO2. Upon further loading (e.g., 15 wt% for “c”), the absorption capacity shows a sudden decline. As is noted in Figure 5c, almost no empty space was left for sample “b” and further CdS loading would only add to the surface coverage and effectively inhibit TiO2 particles from contribution while masking most of the CdS nanoparticles leading to the lowest adsorption capacity in the present study (only about 2%).

Figure 5: a) Time-dependent photocatalytic activity of the nanocomposite samples under cool-white LED illumination at room temperature and b) Results of recycling experiments for the “b” sample.
Figure 5:

a) Time-dependent photocatalytic activity of the nanocomposite samples under cool-white LED illumination at room temperature and b) Results of recycling experiments for the “b” sample.

As can be seen from Figure 5a, malachite green itself undergoes a limited photo-degradation when illuminated with high-intensity light, but this phenomenon is negligible within the time frame of our tests and this dye is still a fairly good model pollutant. Both TiO2 and CdS can cause photo-degradation in pure form; the activity of the former is rather unsatisfactory while the latter is hazardous because it is corroded rapidly under standard conditions. Loading of TiO2 with extremely low quantities of CdS on the other hand significantly enhances the activity. The visible-light activity is high enough so that even cool-LED light can lead to photo-degradation reactions. Nonetheless, there still is an optimized region for this enhancement phenomenon (Figure 5a). Furthermore, for the prepared sample “b” there is a 9% difference between activities under Xe and LED lights, which seems a fair tradeoff when considering the 10-fold power consumption of the former. Furthermore, recycling experiments (four times) are presented in Figure 5b and prove that even without washing or activation protocols, the optimized sample retains a great portion of its activity in consecutive reaction runs. This is a vitally important feature for any robust environmental catalyst.

The well-known heterojunction mechanism can be utilized to explain the enhanced photocatalytic activity of the obtained nanocomposites. The band structures of CdS and TiO2 are suitable for special separation of photo-induced charge carriers. While CdS absorbs the lower-energy photons of the visible spectrum (up to 600 nm), TiO2 can only absorb photons close to the UV region (wavelengths slightly above 400 nm) [52]. Nonetheless, the conduction band of TiO2 has lower-energy compared to the conduction band of CdS, so the photo-induced electrons concentrating on CdS nanoparticles can easily migrate to the neighboring TiO2 particles. It should be noted that there is intimate contact between CdS and TiO2 in the obtained composites, hence the DRS spectra show an absorption edge between the two extremes rather than showing two distinct edges (the optical band gap decreases from the original 3 eV for TiO2 to 2.2 eV in the case of sample “c”). On the other hand, it can be postulated that loading excessive amounts of CdS nanoparticles (in the case of sample “c”) will lead to unwanted surface covering of the TiO2 particles. It should be noted that CdS can absorb all photons with the energies greater than its band gap (Figure 4a) and would not let TiO2 receive a considerable portion of higher-energy photons in the case of an excessively covered surface. On the other hand, photo-induced electrons are the active species in malachite green degradation (Figure 6) and special charge separation which concentrates electrons on TiO2 would deteriorate the total activity of the composite in the case of excessive CdS loading, especially at the surface of TiO2 particles.

Figure 6: Plausible mechanism for photocatalytic removal of malachite green from aqueous media under light irradiation.
Figure 6:

Plausible mechanism for photocatalytic removal of malachite green from aqueous media under light irradiation.

4 Conclusions

Photoactive nanocomposites of TiO2/CdS were synthesized in a straightforward route. The proposed MW approach for decorating pristine TiO2 can be used for other semiconductors and compositions. In the current study CdS was chosen as a model secondary semiconductor and successful decoration was performed in just 10 s offering a facile method with energy-saving merits for a wide range of environmentally active photocatalysts. Even only small loadings of the secondary phase were enough to enhance the visible-light activity considerably and the nanocomposites have shown fairly good photo-degradation activity for malachite green removal from aqueous media even under LED light which is both economically and environmentally viable. We will continue our efforts in developing this approach further and hope it will contribute to the broader quest for environmental photocatalysts.

5 Supporting information

SEM and TEM micrographs, WDS elemental maps, FESEM images and EDS maps for the materials in this study. Time-dependent visible absorption spectra for the photocatalysts and time-dependent photocatalytic activity of some of the samples. This material can be found as supplementary material available online (https://doi.org/10.1515/znb-2021-0036).

Corresponding author: Gholam Reza Khayati, Department of Materials Science and Engineering, Shahid Bahonar University of Kerman, P. O. Box No. 76135-133, Kerman, I. R. Iran, E-mail:

  1. Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.

  2. Research funding: None declared.

  3. Conflict of interest statement: The authors declare no conflicts of interest regarding this article.

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Supplementary Material

The online version of this article offers supplementary material (https://doi.org/10.1515/znb-2021-0036).

Received: 2021-03-06
Accepted: 2021-05-16
Published Online: 2021-06-21
Published in Print: 2021-07-27

© 2021 Walter de Gruyter GmbH, Berlin/Boston

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  2. In this issue
  3. Research Articles
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  5. Approximate estimation of the critical diameter in Koenen tests
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  10. A new N-oxide benzylisoquinoline alkaloid isolated from the leaves of atemoya (Annona cherimola × Annona squamosa)
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  13. Facile decoration of CdS nanoparticles on TiO2: robust photocatalytic activity under LED illumination
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  15. A. Sigel, E. Freisinger and R. K. O. Sigel (Editors and Series Editors): Metal Ions in Bio-Imaging Techniques: Volume 22 of the series Metal Ions in Life Sciences
https://doi.org/10.1515/znb-2021-0036
Keywords for this article
cadmium sulfide; functional applications; microwave processing; sol–gel processes; sulfide; titanium dioxide

Articles in the same Issue

  1. Frontmatter
  2. In this issue
  3. Research Articles
  4. Synthesis and structure of the λ6Si-silicate [Cs(18-crown-6)]2[Si(OSO2CH3)6]
  5. Approximate estimation of the critical diameter in Koenen tests
  6. Laves phases forming in the system ScCo2-“InCo2”-TaCo2
  7. Magnesium intermetallics: synthesis and structure of Eu2Pt2Mg and Sr2Pt2Mg
  8. Intermetallic phases in the Sc–Ir–In system – synthesis and structure of Sc1.024Ir2In0.976 and Sc3Ir1.467In4
  9. Crystal structure and physical properties of a new two-dimensional zinc coordination polymer based on 1,4-bis(4-(imidazole-1-yl)benzyl)piperazine and benzophenone-2,4′-dicarboxylate ligands
  10. A new N-oxide benzylisoquinoline alkaloid isolated from the leaves of atemoya (Annona cherimola × Annona squamosa)
  11. One-pot synthesis of 1-(benzothiazolylamino)aryl methyl-2-naphthols and 3-benzothiazolyl 2,3-dihydroquinazolinones using a magnetically recoverable core–shell nanocomposite as catalyst
  12. An efficient click synthesis of chalcones derivatized with two 1-(2-quinolon-4-yl)-1,2,3-triazoles
  13. Facile decoration of CdS nanoparticles on TiO2: robust photocatalytic activity under LED illumination
  14. Book Review
  15. A. Sigel, E. Freisinger and R. K. O. Sigel (Editors and Series Editors): Metal Ions in Bio-Imaging Techniques: Volume 22 of the series Metal Ions in Life Sciences
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