article characterization and visible light photocatalytic

CHINESE JOURNAL OF CHEMICAL PHYSICS MARCH 31, 2021

ARTICLE

Characterization and Visible Light Photocatalytic Activity of

Cucurbit[n]urils/CdS-MoS2

Juan-juan Shi, An-ting Zhao∗, Zhang-mei Peng, Li-xia Yang, Chun-tao Zhou

College of Chemistry and Chemical Engineering, Guizhou University, Guiyang 550025, China

(Dated: Received on December 11, 2020; Accepted on March 15, 2021)

In order to reduce the impact of CdS photogenerated electron-hole recombination on its

photocatalytic performance, a narrow band gap semiconductor MoS2 and organic macro-

molecular cucurbit[n]urils (Q[n]) were used to modify CdS. Q[n]/CdS-MoS2 (n=6, 7, 8)

composite photocatalysts were synthesized by hydrothermal method. Infrared spectroscopy,

X-ray diffraction, X-ray photoelectron spectroscopy, field emission scanning electron mi-

croscopy, ultraviolet-visible and photoluminescence spectrum were used to characterize the

structure, morphology and optical properties of the products, and the catalytic degrada-

tion of the solutions of methylene blue, rhodamine B and crystal violet by Q[n]/CdS-MoS2composite catalyst was investigated. The results showed that the Q[n] played a regulatory

role on the growth and crystallization of CdS-MoS2 particles, Q[n]/CdS-MoS2 (n=6, 7, 8)

formed flower clusters with petal-like leaves, the flower clusters of petal-like leaves increased

the surface area and active sites of the catalyst, the Q[n]/CdS-MoS2 barrier width decreased,

the electron-hole pair separation efficiency was improved in the Q[6]/Cds-MoS2. Q[n] makes

the electron-hole pair to obtain better separation and migration. The Q[6]/CdS-MoS2 and

Q[7]/CdS-MoS2 have good photocatalytic activity for methylene blue, and the catalytic

process is based on hydroxyl radical principle.

Key words: Hydrothermal method, Cadmium sulfide, Narrow band gap, Cucurbit[n]uril,

Coordination

I. INTRODUCTION

CdS has a low direct band gap value and is sensi-

tive to visible light, so it is widely used in the study of

photocatalyst research [1, 2]. However, under illumina-

tion, electron holes generated by cadmium sulfide pho-

toelectricity are easy to recombine, affecting its photo-

catalytic efficiency [3–5]]. Therefore, in order to inhibit

the photoelectron-hole pair recombination in the photo-

catalytic process, the introduction of narrow band gap

semiconductors or organic compound recombination in

CdS is an effective way to improve its photocatalytic

performance [6–10]. Narrow band gap semiconductor

molybdenum disulfide has an adjustable energy band

gap, and the band gap width is 1.2−1.9 eV [11–16].

∗Author to whom correspondence should be addressed. E-mail:

[email protected]

Cao’s group [17] used CdS@MoS2 to produce hydrogen

efficiently under visible light. Hydrogen produced under

the condition of 0.30 mmol benzodiazepine substrate

was about 53 times higher than the pure CdS nanorod.

The pumpkin-shaped macromolecular cucurbit[n]urils

(Q[n], [C6H6O2N4]n, n=5−15) has a polar port. Non-

polar cavities and positively charged outer wall struc-

ture features, can coordinate with metal ions, inclusion

and hydrogen bonding [18–27]. Karami and his collab-

orators [28] synthesized a new dimer nano-palladium

(Q[6]-Pd NPs) catalyst dispersed on the surface of Q[6],

which was used for the coupling reaction between aryl-

halides and arylboric acid in water-ethanol (1:1), and

showed good reactivity and stability. Cucurbit[n]urils

is considered as a suitable carrier for the preparation

of nanostructured catalysts [29]. In view of this, a

series of Q[n]/CdS-MoS2 composite catalysts were de-

signed and synthesized by a hydrothermal method using

MoS2 with narrow band gap and organic macromolec-

DOI:10.1063/1674-0068/cjcp2012214 c⃝2021 Chinese Physical Society

Chin. J. Chem. Phys. Juan-juan Shi et al.

ular cucurbit[n]urils. The effects of MoS2 and differ-

ent cucurbit[n]urils on the morphology, structure and

catalytic degradation performance of CdS-MoS2 were

studied so as to obtain the composite catalyst with high

catalytic activity.

II. EXPERIMENTS

A. Materials

Cadmium chloride and thiourea were purchased from

Chengdu Jinshan Chemical Reagent Co., Ltd. Sodium

molybdate was purchased from Tianjin kemio Chemi-

cal Reagent Co., Ltd. Anhydrous ethanol and sodium

hydroxide were purchased from Chongqing Chuan-

dong chemical (Group) Co., Ltd. Hypomethyl-blue,

rhodamine B and crystal violet were obtained from

Tianjin kemeo chemical reagent development center.

Cucurbit[n]urils were prepared by the key laboratory of

macrocyclic and supramolecular chemistry of Guizhou

province. All chemicals are analytical grade.

B. Instrument

UV-Vis tests were conducted on Tu-1901 UV-

visible spectrophotometer (wavelength range 200−800

nm, Beijing general analysis general instrument Co.,

Ltd.). Functional group structure was observed by us-

ing VERTEX70 infrared spectrometer (scanning range

400−400 cm−1). The structure phase of products

was observed by using D8 ADVANCE X-ray powder

diffractometer (maximum output 3000 W, Cu target;

Brock, Germany). XPS spectra were taken on thermo

ESCALAB 250XI X-ray photoelectron spectroscopy

(Thermo Feiser Technologies, USA, monochrome Al

Kα, hν=1486.6 eV, binding energy calibrated with C1s

284.8). The morphology features were obtained by S-

4800 cold field emission scanning electron microscope

(SEM, Hitachi Co., Japan). Photoluminescence (PL)

spectra were taken on Cary Eclipse fluorescence spec-

trophotometer (R928 detector, Varian Inc).

C. Preparation of Q[n]/CdS-MoS2

With cadmium chloride (1.0002 g, 4 mmol), sodium

molybdate (1.0602 g, 4 mmol) and thiourea as raw ma-

terials, Q[n] as the compound agent (the amount of Q[n]

was 0.00 mmol or 0.15 mmol, Q[n], n=6−8) was added

into 30 mL of distilled water, followed by stirring. Then,

the mixture was transferred to 50 mL teflon-sealed au-

toclave and heated at 200 ◦C for 24 h, after natural

cooling to room temperature. The suspension was cen-

trifuged and washed with ethanol and distilled water

for 2−3 times, and dried at 60 ◦C oven to obtain the

product.

D. Visible light catalytic reaction

The photocatalytic reaction used a 300 W halogen

tungsten lamp as the experimental light source. Af-

ter filtering, only visible light with wavelength of more

than 420 nm was allowed to pass through. The dis-

tance between the light source and the reaction liq-

uid level was 25 cm, and the temperature of the re-

action solution was 298 K. The catalyst CdS-MoS2 and

Q[n]/CdS-MoS2 (n=6, 7, 8) dosage was 5 mg, 10 mg,

15 mg and 20 mg, respectively. The dyes were 100 mL

of 6 mg/L solutions of hymethylene blue, 6 mg/L rho-

damine B, and 28 mg/L crystal violet. Before photo-

catalysis, the dark reaction was performed for 30 min

to reach adsorption-desorption equilibrium. The illu-

mination time was 200 min. During the catalytic pro-

cess, the sampling interval was 20 min, and the ab-

sorbance of the supernatant after centrifugation were

measured by UV-Vis spectrophotometer at the maxi-

mum absorption wavelength of the dyes solution (664

nm, 554 nm, and 583 nm). According to the formula

D(%)=(A0−A)/A0×100%, the degradation rate D was

calculated, here A0 and A are the absorbance of the dye

solution at the beginning and after any time of reaction.

E. Determination of radicals on the surface of samples

The hydroxyl radicals on the surface of composite cat-

alyst Q[6]/CdS MoS2 were determined by using tereph-

thalic acid as a fluorescent probe. 20 mg Q[6]/CdS-

MoS2 was added into 5×10−4 mol/L terephthalic acid

solutions, and an ultrasonic dispersion, the experimen-

tal conditions of adsorption and catalysis was the same

as the visible light catalytic reaction in the above sub-

section D. The emission peak was excited at 320 nm

and generated at 428 nm. The hydroxyl radicals on the

surface of composite catalyst Q[6]/CdS MoS2 were de-

termined by using p-benzoquinone as superoxide radical

capture agent to confirm the effect of superoxide radi-

cals on the photo degradation process.


Chin. J. Chem. Phys. Photocatalytic Activity of Cucurbit[n]urils/CdS-MoS2

FIG. 1 XRD patterns of CdS, CdS-MoS2, and Q[6]/CdS-MoS2.

III. RESULTS AND DISCUSSION

A. The X-ray powder diffraction of Q[n]/CdS-MoS2

The XRD spectra are presented in FIG. 1. Products

have a hexagonal zinc fiber CdS structure (PDF# 41-

1049) as compared to standard card. In addition to the

diffraction peak of hexagonal CdS, the CdS-MoS2 and

Q[6]/CdS-MoS2 also gave the weak diffraction peaks

of (002) and (101) crystal surface of MoS2 (PDF#37-

1492). The preferred growth crystal surface of hexago-

nal CdS was (101), while the preferred growth crystal

surface of CdS-MoS2 and Q[6]/CdS-MoS2 was (002),

and the diffraction peak slightly shifted to a lower an-

gle. The grain size of the product was about 36 nm and

had a crystallinity of greater than 90%. It can be seen

from XRD that cucurbit[n]urils and MoS2 had an effect

on the preferential growth of the crystal surface.

B. Scanning electron microscope and energy spectrum

analysis

Morphology of the products CdS-MoS2, Q[6]/CdS-

MoS2 and Q[7]/CdS-MoS2 were flower clusters with a

combination of petals (FIG. 2), the thickness of the

petals was about 15 nm and the diameter was about

200 nm, the cluster of galaxies had a large surface area.

But morphology of Q[8]/CdS-MoS2 was multilateral

shape, particles size was about 210 nm. The EDS spec-

tra of CdS-MoS2 and Q[6]/CdS-MoS2 show that the

products all contain Cd, Mo, S, C and O. The peaks of

C and O elements may be caused by the adsorption of

organic matter in the air on the particle surface. The

N peak comes from the cucurbit[n]urils in Q[n]/CdS-

MoS2. It can be viewed on EDS that the products were

loaded with Cd, Mo and S elements, CdS and MoS2

FIG. 2 SEM spectra and EDS analysis of CdS-MoS2 andQ[n]/CdS-MoS2.

were the main components in the crystal grains.

C. FT-IR analysis

The infrared spectrum analysis of Q[n], CdS-MoS2and Q[n]/CdS-MoS2 is shown in FIG. 3. The FT-IR

peaks of the functional groups of cucurbit[n]urils with

different sizes had the same repeat unit structure, the

carbonyl stretching vibration peak of cucurbit[n]urils

appeared at about 1730 cm−1, and moved to low

wavenumber with the increase of n value (1738−1722

cm−1). In addition, the characteristic peak of

cucurbit[n]urils skeleton also appeared below 1500

cm−1 (-CH group: 1474 cm−1, 1421 cm−1, 968 cm−1,

806 cm−1, 734 cm−1; C−N: 1360 cm−1; C−C: 1176

cm−1). After Q[n]/CdS-MoS2 complex were formed by

Q[n] and CdS-MoS2, the stretching vibration intensity

of carboxyl peak (1727 cm−1) and the characteristic

peak of Q[n] (below 1500 cm−1) was significantly weak-



FIG. 3 FT-IR spectra of CdS-MoS2, Q[n], and Q[n]/CdS-MoS2 (n=6, 7, 8).

ened, which may be due to the fact that carbonyl of

port and outer wall of Q[n] were covered by CdS-MoS2.

It also reported the existence of Q[n] in Q[n]/CdS-MoS2complex catalyst.

D. X-ray photoelectron spectroscopy analysis

The X-ray photoelectron energy spectra (FIG. 4) of

CdS-MoS2 and Q[6]/CdS-MoS2 all show Cd, Mo, S,

C and O elements. Among them, the N peak (N

1s1/2, 403.2 eV) of Q[6]/CdS-MoS2 came from cucur-

bit[6]urils, which was consistent with the conclusion

in EDS. The characteristic peaks of binding energy

of 412.0 eV and 405.2 eV in CdS-MoS2 corresponded

to Cd 3d3/2 and Cd 3d5/2 in cadmium sulfide, the

characteristic peaks of binding energy at 163.0 eV and

161.8 eV were 2p1/2 and 2p3/2 of sulfur characteristic

peak, the characteristic peaks with binding energy of

232.2 eV and 229.0 eV corresponded to 3d3/2 and 3d5/2of tetravalent molybdenum, indicating that Mo element

exists in the product in the form of Mo4+, The char-

acteristic peak of binding energy of 531.9 eV may be

caused by the adsorption of organic oxygen from the

air on the particle surface. The binding energy of each

element in Q[6]/CdS-MoS2 moves slightly towards the

direction of low binding energy relative to CdS-MoS2,

it indicates that the electrons around Q[6]/CdS-MoS2were enriched and the shielding effect was increased [30].

E. Fluorescence spectrum analysis

The change of fluorescence intensity in the PL spec-

trum can reflect the recombination and separation

of electron-hole pairs. Therefore, solid-state fluores-

cence of CdS-MoS2 and Q[n]/CdS-MoS2 was tested.

The excitation was at the wavelength of 325 nm,

and a fluorescence emission peak appeared at 375 nm

(FIG. 5). It can be seen that the fluorescence inten-

sity of Q[8]/CdS-MoS2 has no change relative to CdS-

MoS2, while Q[6]/CdS-MoS2 and Q[7]/CdS-MoS2 have

fluorescence quenching and the fluorescence intensity is

weakened, the phenomenon indicates that the probabil-

ity of electron-hole pair recombination in the substance

was decreased. Among them, Q[6]/CdS-MoS2 has the

highest fluorescence intensity reduction and the highest

electron-hole pair separation efficiency, which may be

related to the heterostructure of CdS-MoS2 and the size

of the cucurbit[6]urils, Q[6] has better matching with

CdS-MoS2, and can better transfer electrons on CdS-

MoS2. The effective electron-hole separation and life

span increase as well as the increase of optical quantum

yield which was conducive to the activity of the cata-

lyst. The combination of Q[6] and Q[7] was expected

to improve the catalytic performance of the composite

catalyst, which was also consistent with the subsequent

results.

F. Ultraviolet visible diffuse reflection analysis

The corresponding energy gaps obtained by the solid

ultraviolet-visible diffuse reflectance test of the CdS-

MoS2 and Q[n]/CdS-MoS2 composite catalysts are

shown in FIG. 6. The ultraviolet absorption edge and

band gap were determined by extrapolating the point

where the line intersects the starting point (or baseline)

of the curve. The ultraviolet absorption edge of CdS-

MoS2, Q[6]/CdS-MoS2, Q[7]/CdS-MoS2 and Q[8]/CdS-

MoS2 appeared at 555.9 nm, 552.9 nm, 555.9 nm and

552.9 nm, respectively, so the band gap of CdS-MoS2and Q[7]/CdS-MoS2 was 2.24 eV, and that of Q[6]/CdS-

MoS2 and Q[8]/CdS-MoS2 was 2.23 eV. Their band

gaps were comparable and less than 2.42 eV of CdS.

The results showed that both MoS2 and Q[6] were favor-

able for an electron transition in the composite, and the

photoelectron-hole separation efficiency of Q[6]/CdS-

MoS2 was the highest.

G. CdS-MoS2 and Q[n]/CdS-MoS2 photocatalysis results

and analysis

As can be seen from the catalytic data, when the

amount of composite catalyst increases from 5 mg to

20 mg, the absorbance value of the dye decreases more,

the catalytic degradation efficiency of the catalyst in-



FIG. 4 X-ray photoelectron spectroscopy analyses of CdS-MoS2 and Q[6]/CdS-MoS2.

FIG. 5 Solid fluorescence spectra of products CdS-MoS2

and Q[n]/CdS-MoS2 (n=6, 7, 8).

creases in turn, and the catalytic reaction rate was ac-

celerated (as shown in FIG. 7). When 20 mg composite

catalyst was used for the photoreaction for 200 min, the

photocatalytic degradation efficiency of methylene blue

reached the maximum values of CdS-MoS2, Q[6]/CdS-

MoS2, Q[7]/CdS-MoS2 and Q[8]/CdS-MoS2 which were

85.9%, 92.2%, 91.8%, and 89.5%, respectively (FIG. 8).

Cucurbit[n]urils improved the degradation rate of CdS-

MoS2 photocatalytic degradation of methine blue, and

FIG. 6 UV-visible diffuse reflectance spectra of CdS-MoS2

and Q[n]/CdS-MoS2 (n=6, 7, 8).

the compound of ucurbit[n]urils was beneficial for the

improvement of CdS-MoS2 photocatalysis. The differ-

ence of degradation efficiency of methylene blue was

mainly related to the use of Q[n]. Content of CdS and

MoS2 decreased with the introduction of Q[n], but the

catalytic effect of Q[n]/CdS-MoS2 was still greater than

or equal to CdS-MoS2. This may be because Q[n] ad-

justed the energy band structure of CdS-MoS2, making

the band gap width of Q[n]/CdS-MoS2 narrow and the



FIG. 7 Photocatalytic performances of methylene blue by CdS-MoS2 and Q[n]/CdS-MoS2.

FIG. 8 Photocatalytic degradation of Rhodamine B, methy-lene blue, and crystal violet by 20 mg Q[6]/CdS-MoS2.

electrons on CdS-MoS2 surface migration of Q[n], which

can promote the separation of electrons and holes, in-

crease the separation efficiency of the photogenerated

carriers, and improve the visible light catalytic activity

of the catalyst.

Then, 20 mg Q[6]/CdS-MoS2 was used to photocat-

alytically degrade 100 mL of 6 mg/L rhodamine B, me-

thine blue, and 28 mg/L crystal violet, respectively.

The catalytic effect is shown in FIG. 8. After 200 min of

photocatalysis, the degradation rates of the three dyes

reached 72.3%, 92.2% and 72.9%, respectively. The re-

sults show that Q[6]/CdS-MoS2 has photocatalytic ef-

fect on three different structural dyes, and the photocat-

alytic degradation efficiency of methylene blue solution

is the best.

H. Catalytic mechanism speculation

The mechanism was speculated that terephthalic

acid reacted with hydroxyl radicals to generate 2-

hydroxyterephthalic acid with good fluorescence prop-

erties. In visible light, using terephthalic acid as a

fluorescence probe, production of ·OH by photocata-

lyst Q[6]/CdS-MoS2 was determined. The concentra-

tion of hydroxyl radical was indirectly indicated ac-

cording to the fluorescence intensity of the emission

peak. The stronger the fluorescence intensity was,

more 2-hydroxyterephthalic acid was generated, that

is, the higher the concentration of hydroxyl radical was

generated. As can be seen from FIG 9, the fluores-

cence intensity of the reaction solution increases with

the increase of time, indicating that with the increase

of time, the concentration of ·OH produced by the

composite catalyst increases continuously, and the 2-

hydroxyterephthalic acid was gradually increased. It

was reflected from the side that the composite catalyst



FIG. 9 Determination of hydroxyl radicals produced byQ[6]/CdS-MoS2.

FIG. 10 Effect of p-benzoquinone inhibitor on catalyticdegradation MB by Q[6]/CdS-MoS2.

produced ·OH in the photocatalytic degradation exper-

iment, which has strong oxidability ·OH to degrade the

dye.

In addition, p-benzoquinone was added as superox-

ide radical capture agent to confirm the effect of super-

oxide radicals on the photo degradation process. And

the catalytic data obtained before and after adding p-

benzoquinone were compared. The results are shown in

FIG. 10. After the addition of BQ, the photocatalytic

degradation efficiency of methylene blue by Q[6]/CdS-

MoS2 decreased from 92.2% to 72.2%, indicating that

superoxide radicals were involved in the photocatalytic

degradation of methylene blue. The photocatalytic

degradation process was based on the principle of free

radical.

Through the above experiments, characterization and

analysis, the mechanism of Q[6]/CdS-MoS2 composite

catalysts photocatalytic degradation of dyes was spec-

ulated, as shown in FIG. 11. Due to the difference in

FIG. 11 Mechanism of photocatalytic degradation of dyesby Q[6]/CdS-MoS2.

energy level positions of CdS and MoS2, the e− on the

valence band of CdS and MoS2 can easily transit to the

conduction band under the action of the built-in elec-

tric field when illuminated, and form h+ on the valence

band, the role of light makes the electrons on the con-

duction band of CdS transfer to the conduction band of

MoS2, and the holes were transferred from high to low.

The cucurbit[n]urils also plays a role in the transmis-

sion and separation of photo-generated carriers in CdS-

MoS2, promoting photo-generated electrons to migrate

from center to surface, so that electron-hole pairs on

CdS-MoS2 can be effectively separated. The electrons

can be trapped by O2 to generate superoxide radicals

(·O2−). The holes and water react to produce highly

active ·OH, ·O2−, and ·OH catalyze the degradation of

dyes. Q[n]/CdS-MoS2 has good photocatalytic activity.

IV. CONCLUSION

In summary, the compounds CdS-MoS2 and

Q[n]/CdS-MoS2 were synthesized by hydrothermal

method using thiourea as the sulfur source, the prod-

uct has flower cluster morphology, petals and leaves in-

crease the specific surface area and active sites of the

composite catalyst Q[n]/CdS-MoS2 (n=6, 7, 8). The

heterojunction of CdS-MoS2 and the cucurbit[n]urils

make the CdS valence band shift, and broaden the visi-

ble light absorption range of Q[n]/CdS-MoS2; the elec-

trons on the surface of CdS-MoS2 can quickly migrate

to the Q[n] layer, which can promote the separation

of electrons and holes, accelerate the utilization rate

of photogenerated electrons. The results showed that



Q[n]/CdS-MoS2 composite catalyst had better photo-

catalysis, and the best photocatalytic degradation ef-

fect of methylene blue was Q[6]/CdS-MoS2, the photo-

catalytic degradation rate of Q[6]/CdS-MoS2 to 100 mL

of 6 mg/L methyl blue reached 92.2% after 200 min of

photocatalysis. The catalytic process is based on the

radical principle. This study provides a useful reference

for the design of functional cucurbit[n]urils composite

catalyst.

V. ACKNOWLEDGMENTS

This work was supported by the National Natural

Science Foundation of China (No.21871064), the Na-

tional College Students’ Innovative Training Program

of China (No.2020053), the “Undergraduate Teaching

Project” of Guizhou University (No.201936), and the

Student Research Training Foundation of Guizhou Uni-

versity, China (No.(2019)106).

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article characterization and visible light photocatalytic

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