dean Technol., Vol. 24, No.3, 동ptember 2018, pp. 206-211

협정핀정기솔

Photocatalytic Decomposition of Rhoclamine B on PbMo04

Using a Sur힘ctant-assisted Hydrothermal Method

Seong-Soo Hong*

Depattment of Chemical Engineering, Pukyon용 N양ional University 45YoI핑so-ro， Nam-gu, Busan, 48513 Korea

(Rec터ved for revíew May 1, 2018; Revision receivedJune 5, 2018)

Abs1ract

Leadmol'야쳐ate αbMo04)were 없ccess찌lly synthesized using a fa다le surfactant←as혀없dhyl따uthermal process 뻐d때aracterized

by XRD, Raman, PL, BET and DRS. We a1so investigated the photocata1ytic activity ofthese materi떠s for the decomposition of Rhodamine B under UV-light irradiation. From XRD 뻐d Raman res'띠，ts， well-cry뼈Jlized PbMo04 crys'뻐ls have been 뻐ccessfully synthesized with a facile sur훨짜ant웰sisted hydrothermal process a끄d 뼈d 52-69 nm 뼈rticle 혀ze. ’I'he PbM004 ca뻐lysts 야epared at 160 t: showed the highest photoca뼈lytic activity. The PL P않k was appeared at about 540 nm at a11 ca뼈lysts

and it was also shown that the excitonic PL sigI퍼1 was π'Oportional to the photoca삐lytic activity for the decomposition of Rh때와피neB.

K빼vord&: 1없dmoly벼ate αbMo04)， Sur옮C빼t-as뾰뼈dhydroth없mal process, Photoc뼈lytic decomposition of Rh여amineB

1. Intrc영uction

Semiconductor photocatalysts on a nanometer-scale have

become more and more attraιtive because of their difl하'Cnt

physi뼈 and chem뼈lprφerties from b띠kmateri외s [1,2]. The

su빼ce structure of photocatalysts play an important role to

th링r photocatalytic activities because the photocata1ytic reaction

or photoelectron conversion 빼:es p빼ce on1y when photoinduced

electrons 뻐dholes 없'C av히뻐ble on the 잉nface [3]. For exau껴plκ

both theoretical and experimen뼈1 studies have demonstrated

that the {001} facets of anatase Ti02 are much more reactive

than the therm여y뼈mi앓lly more stable {1O 1} fa않ts [4]. There­

fore, the sur옮ce controll혀 fabrication of nanocry용빼18 is not

on1y a rational route to study the relations between the surface

structures and the photocatalytic prop뼈es but also a f농잃뻐，le

행proaιh for developing hi뱅ly active photoc뼈lys빼.

Me없1 molybdate and me뻐ltungs뻐，te ma:않d왜s as a scheelite

struc따e have wide potenti왜 and practical appli앓tions in many

fields, e.g. photoluminescence (PL), solid-state opti명1 maser, optical fi밟s， scintillator ma없뻐18， 뻐midity sensor, magnetic

materi허s and ca뻐lysts [5,6]. PbMo04 뼈d SrMo04 σys뻐뻐zein

this s양-called scheelite structur"C, which belong to the tetragOl뻐I

뼈ce group 14./a [5]. 돼ey have bc빼 합lO11ed due to 벼g 와>ove

* Towhom ∞Irte빼ondence 뼈ould be addr앵8쩌. E빼피: sshong@pknu.ac.kr; 감1: +82-51 -629-6433; Fax: +82-51-629-6429

doi: 10.7464!lcsct.2018.24.3.206 plSSN 1598-9712 elSSN 2288-0690

mentioned applications. PbMo04 has also been 11한>orted as a

φotoca빼lyst for the spli빼g ofwater [꺼. Unf뼈mately， 에mo8t

려1 of the PbM004 α%해18 synthes없d by tr뼈itiOl뻐1 solid s뼈te

뼈ctions 없ui solution P뼈se meth여s are dor피m뼈d by irregular

shape 없ld large crystal size due to its rapid crystal growth

feaαre [8]. Recent1y, Zheng 때d co-workers have 빼orted "(­

BhMo06 sheets with preferent빼y exposed (010) crysta1 facets

t뼈ibiting great1y 빼뼈nced photo뼈vity in com뼈rison with "(

-Bi2Mo06 nanopartlcles and sheets with preferentiaI1y e씩>08ed

(131) cry빼lfa짧， and fourul that the exposed (010) fa없 ∞<0-

뼈ining much more oxygen d영ècts 없'C benefi떠alforsu함m:ss피g

the photogenera때 않me엉 recombination 뼈d promoting the

gen하ation of OH radical [9]. The above investigations remind

us that the photocata양tic activity of 빼otoca없lysts 않n be 뻐ilored

by controlling their exposed crystal facet and morphology.

Therefore, the controllable preparation of photoca뻐lysts with

different morphologies and exposed crys뻐1 facets is still very

impor뼈nt and challe:맹ng. Shen 뻐d co-work!하s have repo:πed

that the 뻐뼈ctant on the pr맹휠ation of PbM004 played an 피1-

portant role in the formation of preferentially exposed crys뼈l

fac앙sto 해hance the photocata1ytic acti찌ty [10]. ’Iherefore, the

preparation of u피form， high-purity PbMo04 n뻐ocrys뻐ls with

돼뼈is an 야!eIl-Access article벼뾰h뼈d under the tcrms of1he α'ca며e Com따ms Attri뼈anNa바::ommcn:뻐l μcense (http :μ'crcativecommons.or빙i야:nc뼈

by-.마/3.0) which permits unrestrict혀 non-commercial use, dis떠，bution， and πproduction in any medium, pm찌ded the ori믿nal work 색 properly cìted

206

207

Figure 1 shows the XRD patt않lS of PbMo04 cata1ysts prepared

using hydrothermal process at different preparation temperature.

πle temperature was changed from 100 to 180 oc. πleir XRD

pattems revea1ed that the products can be indexed as the tetra­

gona1 structure with space group I41/a regardless of the prep따ation

temperature, in agreement with the respective JCPDS No. 08-

0475 for PbMo04.

πle exp앉imental lattice par없net앉s were calculated using the

equation of plane spacing for the tetragona1 structure and Bragg’s

law for diffraction [11]. πley are a = 5.4070 Å and c = 12.0388

Å for PbMo04. The approximate crystallite sizes of PbM04

were calcu1ated from (112) peak of XRD patt않lS with Sch없Ter’s

equation [11].

D = 0.9λ / βcosB

where D is the crystallite size in nm, λ is the radiation wave­

len야1 (0.15405 nm for CuKa), ß is corrected half-width, and

Photocatalytic Decomposition ofRhodamine B on PbMo04 Using a Surfactant-assisted Hydrothermal Method

3. Results and discussion

(204) (303) 180 0 C (101)

l A

160 0 C l

130 0 C

100 0 C 一iF ‘

80

Figure 1. X-ray diffraction pattems ofPbMo04 catalysts prepared using hydrothermal process at different preparation tem­perature.

Table 1. The physical properties and photocatalytic activity of PbMo04 catalysts prepared at di:fferent preparation tem­perature

tem Pprecpraamrarhco (n℃) Partic1e size S따face area e) (nm) (m2g-1 ( X 10-3 min-1

100 52 3.0 50.3

130 56 2.8 67.1

160 59 2.6 121.8

180 59 2.6 71.4

a) apparent first-order constant (kapp) of photocata1ytic degradation of RhodamineB

controllable 따ystallographic facets can be obtained using a facile

surfactant-assisted hydrothermal process.

In this paper, we prepared nanosized PbMo04 partic1es using

a facile surfactant-assisted hydrothermal process. πle synthesized

materials were characterized using XRD, DRS, PL, BET and

Raman. Their activity as photocatalysts for the decomposition

of Rhodamine B was investigated. In addition, the optimal ex­

periment conditions for the preparation were investigated to get

the high photocatalytic activity.

In a facile surfactant-assisted hydrothermal process, (NH4)6

MOyO찌'4H20 (5.3 g), Pb(N03)2'4H20 (9.94 g) and cetyl띠methyl

ammonium bromide (CTAB) were used as the starting materials

without further purification. The appropriate amounts of starting

materia1s were dissolved in distiUed water (120 mL) and added

into a Teflon-lined steel autoc1ave of 150 mL. Then 24 g of

ethylene glycol was added. Under stirring, 4 mol L-1 of NaOH

solution was used to a예ust that the pH value is 9, and the auto­

c1ave was heated under autogenous pressure at from 100 to 180

OC for 12 h. The resulting solid powders were collected, and

washed with deionized water and e깐laIlol， and then 삼ley were dried

at the 120 oc for 12 h. In order to investigate the effect of ca1-

cination temperature on the morph이ogy and the crystal facets

of PbMo04, the temperature was changed from 200 to 500 oc. The crystal structures of the prepared PbMo04 materials

were examined by powder X-ray diffraction 0않D) with Cu-Ka

radiation (Rigaku Co. Model DMax). The BET surface area of

the prepared p따tic1es was determined by nitrogen physisorption

data at 77 K using a Q뻐ntachrome NOVA 1000. UV-vis di짧lSe

reflectance spectroscopy (DRS) was p앙formed on a Varian Cary

100 using PTFE (polytetrafluoroethylene) as a standard. The

micro-Raman (MR) spectra of the products were obtained with

a Raman spectrometer (Dimension-pl-Raman, USA) with a ra­

diation of 532 nm from 뻐 argon ion laser. Photoluminescence

(PL) spectra were examined using a fluorescence spectrophoto­

meter κIMMON KOHA, Japan) with Xe lamp (power: 350 w)

as the light source at room temperature.

The photocatalytic reactions were performed with a 300 W

Xe-따C 빼Iψ (Oriel). Li맹lt was passed through a 10 cm IR water

filter and then focused onto a 100 mL pyrex with a quartz

window. The reactor was filled with 100 mL of an aqueous

dispersion in which the concentrations of the photocatalyst and

Rhodamine B were 1 g L-1 and 10 mg L-\ respectively. This

solution was magnetically stirred that the concentration and

temperature remained uniform. The s없nples were immediately

centrifuged and the quantitative determination of Rhodamine B

was performed using a UV -vis spectrophotometer (Mecasys

Optizen Pop).

2. Experimental

60 40

2 까leta (degree)

20

(}-E

.

S』@)를일필=-

#·=3

.a』m)〉느mZφ#z-

Seong-Soo Hong

500 0 C l

400 0 C

300 0 C

200 0 C

No calcination

208

(를그

.

S』삐) 효m=일드

1200 1000 800 600 400 200 80 60 40 20

Wavelength (cm-1)

Figure 3. Ram없1 spectra ofPbMo04 catalysts prepared using hydro­thermal process at diff농rent preparation temperature.

2 까leta (degree)

Figure 2. X-ray di짧action pattems ofPbMo04 catalysts prepared using hydrothermal process at diff농rent calcination tem­perature.

preted as the weaker V4 (Bg) and stronger V2 (A라 of the regular

[M004t tetrahedrons. πle Ag mode at 166.5 cm-1 for PbMo04

is much weaker than other modes. πlese resu1ts were consistent

with other reports about PbMo04 [6,12]. No peaks in the XRD

or R없nan spectra from other impurities were detected. Therefore, it is reasonable to conclude that we11-crystallized PbMo04 αys때S

have be없1 successfully synthesized with the hydroth앙mal method

regardless of the preparation temperature.

The light absorption properties of the photocatalysts were

examined by diffuse reflectance UV-Vis spectroscopy. Figure

4 shows the UV-Vis diffuse reflectance spectra of PbMo04

catalysts prepared using hydrothermal process at different pre­

paration temp앉ature. As shown in Figure 4, a11 the catalysts dis­

played similar absorption spectrum in the UV light region re-

Table 2. The physical properties and photocatalytic activity of PbMo04 catalysts calcined at different temperature

Calcination Particle size Surface area k a)

temperature (OC) (nm) (m2gJ ( X 10-3 min-1

No calcination 52 2.6 121.8

200 56 2.5 90.3

300 59 2.4 19.4

400 63 2.4 10.1

500 69 2.2 5.2

려 apparent first-order constant (kapp) ofphotocatalytic degradation of RhodamineB

500

Figure 4. UV-Vis diffuse reflectance spectra ofPbMo04 catalysts prepared using hydrothermal process at different prepa­ratlOn temperature.

450 400

Wavelength (nm)

350 300 250 200

m m<

() is the diffraction peak angle. The average crysta11ite sizes of

a11 samples are calculated by Scherrer’s equation as shown in

Table 1. The crysta11ite size increased 당om 52 to 59 nm with

an increase of preparation temperature.

Figure 2 shows the XRD patterns of PbM어)4 catalysts prepared

using hydrothermal process at different calcination temperature.

Their XRD pattems also revealed that the products can be

indexed as the tetragonal structure with space group I4da

regardless of the calcination temperature. As shown in Table 2, the crystallite size increased from 52 to 69 nm with an increase

of calcination temperature.

Figure 3 shows the Raman spectra in the range from 150 to

1000 cm-1 of PbMo04 catalysts prepared using hydrothermal

process at different preparation temperature. The Raman peak

at 869.5 cm-1 was assigned to the symmetric stretching vibration

mode V1 (Ag) of the [Mo04] clusters in the PbMo04 crystal

[12]. The peaks at 767.0 때d 741.2 cm-1 corresponded to the

anti-symmetric stretching V3 (Bg) and V3 (E값 vibration modes, respectively. Two modes at 347.6 and 317.2 cm-1 were inter-

Photocata1ytic Decomposition ofRhodamine B on PbMo04 Using a Surfactant-assisted Hydrothermal Method 209

gardless of the preparation temperature. However, the absorption

edge of the sample moved slightly to higher wavelength with

an increase of preparation temperature, which can be ascribed

to the increase of grain size. From the onset of the absorption

edge in Figure 4, the band gap is estimated at about 3.20 eV, which can be ascribed to the characteristic absorption of PbMo04

[13]. The band structure of PbMo04 was suggested to be com­

posed of M04d (conduction band, CB) and hybridization of 02p

and Pb6s (va1ence band, VB) according to other research [13,14].

It is well known that photocatalytic oxidation of organic

pollutants follows Langmuir-Hinshelwood kinetics [15], where

the rate is proportional to the coverage 8:

KC r = - -: = kB = k dt .V~ .v 1 + KC

where k is the true rate constant which is dep앙ldent upon 쩌rious

P따æneters such as mass of the cata1yst, the flux efficiency, oxygen

coverage, etc., K is the adsorption coefficient of the reactant, and C is the reactant concentration. When C is very small, the

product KC is negligible with respect to unity and under these

conditions Equation (1) describes a first-order kinetic reaction.

Setting the parameters in Equation (1) to the initial conditions

of the photocatalytic procedure, t=O, the concentration can be

given as C=Co, which results in Equation (2).

-/n (승) = kappt

where k app is the apparent first-order reaction constant.

πle photocata1ytic acti찌ty for the decomposition of Rhodamine

B over PbMo04 c따alysts prepared using hydrothermal process

1.0

0.8

0.6

-Qu-。-0.4

0.2

0.0 0

-톨>- 100 0C ----T- 130 Oc -톨←- 160 0 C -+- 180 0C

10 20 30 40

Time (min)

50

Figure 5. Photocatalytic decomposition of Rhodamine B over PbMo04 catalysts prepared using hydrothermal method at different preparation temperature.

160 0 C

m m<

350 400 450 500 550 600

n / / l

·、

Wavelength (nm)

Figure 6. PL spectra of PbMo04 catalysts prepared using hydro­thermal method at different preparation temperature.

(2)

at different preparation temperature is shown in Figure 5 and

Table 1. When a blank test was carried out in the absence of

the photocatalyst, about 2% of the Rhodamine B was decom­

posed after 2 h by the photolysis reaction. As ShOWll in Figure 5, the photocatalytic activity increased with increasing preparation

t없lperature and Rhodamin B was completely decomposed within

30 min on the PbMo04 catalysts prepared at 160 oc. However, the acti"찌ty of PbMo04 cata1yst prepared at 180 oc was decreased.

Figure 6 shows the PL spectra of PbMo04 catalysts prepared

using hydrothermal process at different preparation temperature.

It is shown that the PbMo04 samples can obvious excitonic PL

signa1s with similar shape regardless of preparation temperature.

In addition, the excitonic PL signal shows the hi양lest intensity

in the case of PbMo04 catalyst prepared at 160 oc. It is well

known that PbMo04 materials exhibit the strong and wide PL

signals at the range from 500 to 600 nm with the excited wave­

length of 300 nm. For the PbMo04 catalysts, one obvious PL

peak is appeared at about 540 nm. It is known that the emission

spectrum of the metal molybdates might be ascribed to the

charge-transfer transitions within the [Mo04] c1usters [16]. The

stronger the excitonic PL signal, the hi양ler the content of surface

oxygen vacancy and defect. In addition, during the process of

the photocata1ytic reaction, oxygen vacancy and defect 때n become

the c없lters to capture photo-induced electrons so that the recom­

bination of photo-induced electrons and holes can be inhibited.

Moreover, oxygen vacancies 대n promote the adsorption of oxygen

and then the strong interaction between the photo-induced elec­

trons bound by oxygen vacancies and adsorbed oxygen can be

formed. This result indicates that the binding for the photo­

induced electrons of oxygen vacancies can make the capture

for photo-induced electrons of adsorbed oxygen and oxygen

radical group was produced at the same 바ne. Therefore, oxygen

60

21 0 Seong-Soo Hong

1.0

0.8

----- No Calcination ----T- 200 0C _ 300 0C

--+-- 400 0C

-흩- 500 0C

0.6

u‘u‘。0.4

0.2

0.0 0 10 15

Time (min)

20 25 5

Figure 7. Photocatalytic decomposition of Rhodamine B over PbMo04 catalysts prepared using hydrothermal method at different calcination temperature.

vacancy and defect are in favor of photocatalytic reactions in

that oxygen is active to promote the oxidation of organic sub­

stances. This sugges잉 that the stronger the PL intensity, the

larger the amount of oxygεn vacancy and defect, the hi양1er the

photocatalytic acti띠ty. As shown in Figure 6, the photocatalytic

actψity on the decomposition of Rhodamine B shows the same

order with the intensity of PL peaks of PbMo04 catalysts.

Figure 7 shows the photocatalytic activity for the decom­

position of Rhodamine B over PbMo04 catalysts prepared by

different calcination temperature. As shown in Figure 7 and

Table 2, the photocatalytic acti띠ty was deα.eased with an increase

of calcination temperature and the PbMo04 catalyst prepared

without a calcination process showed the highest activity.

Figure 8 shows the PL spectra of PbMo04 catalysts prepared

m m<

No calcination 200 0 C 300 0 C 400 0 C

500 0 C

350 400 450 500 550 600

Wavelength (nm)

Figure 8. PL spectra of PbMo04 catalysts prepared using hydro­thermal method at different calcination temperature.

using differ없lt calcination 없nperatures. PbMo04 s없nples showed

one obvious excitonic PL signals at 540 nm regard1ess of the

calcination temperature. The excitonic PL signal increased with

decreasing calcination t않lperature. Furth앉more， the photocatalytic

activity for the decomposition of Rhodamin B also showed the

same order with the intensity of PL peaks of PbMo04 catalysts

prepared at diffi많앉1t calcination ter때않atures. As afore-m얹ltioned，

this resu1t also verified that the stronger the PL intensity, the

higher the photocatalytic activity.

4. Conclusions 30

In this study, we have investigated the photocatalytic activity

of lead molybdate (PbMo04) scheelite-type oxides prepared using

a facile surfactant-assisted hydrothermal process on the decom­

position of Rhodamine B. From the XRD and Raman results, the formation of the well-crystallized PbMo04 phase was con­

firmed for all catalysts regardless of preparation temperature.

The photocatalytic activity increased with increasing prepara­

tion temperature and Rhodamine B was completely decomposed

within 30 min on the PbMo04 catalysts prepared at 160 oC. In

때dition， the photocatalytic acti띠tywasdeσ'eased wi삼1 an incrl없se

of calcination temperature and the PbMo04 catalyst prepared

without a calcination process showed the highest activity. The

PL peak was appeared at about 540 nm at all catalysts and it was

also shown that the excitonic PL signal was proportional to the

photocatalytic activity for the decomposition of Rhodamine B.

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