Nanoscale
PAPER
Ci e his: Nanoscale, 2023, 15, 5726
Recei ed 7 h Janua y 2023,
Accep ed 26 h Feb ua y 2023
DOI: 10.1039/d3n 00098b
sc.li/nanoscale
Ligh -powe ed swa ming pho e ic an imony
chalcogenide-based mic o obo s wi h “on- he-fly”
pho odeg ada ion abili ies†
Anna Jancik-P ochazko a
a
and Ma in Pume a *
a,b,c,d
Mic o obo s a e a he o e on o esea ch o biomedical and en i onmen al applica ions. Whe eas a
single mic o obo exhibi s qui e low pe o mance in he la ge-scale en i onmen , swa ms o mic o obo s
a e ep esen ing a powe ul ool in biomedical and en i onmen al applica ions. He e, we ab ica ed
pho e ic Sb
2
S
3
-based mic o obo s ha exhibi ed swa ming beha io unde ligh illumina ion wi hou any
addi ion o chemical uel. The mic o obo s we e p epa ed in an en i onmen ally iendly way by eac ing
he p ecu so s wi h bio-o igina ed empla es in aqueous solu ion in a mic owa e eac o . The c ys alline
Sb
2
S
3
ma e ial p o ided he mic o obo s wi h in e es ing op ical and semiconduc i e p ope ies. Because
o he o ma ion o eac i e oxygen species (ROS) upon ligh illumina ion, he mic o obo s possessed
pho oca aly ic p ope ies. To demons a e he pho oca aly ic abili ies, indus ially used dyes, quinoline
yellow and a azine we e deg aded using mic o obo s in he “on- he-fly”mode. O e all, his p oo -o -
concep wo k showed ha Sb
2
S
3
pho oac i e ma e ial is sui able o designing swa ming mic o obo s o
en i onmen al emedia ion applica ions.
In oduc ion
Mic o obo s a e au onomous mic o-scaled de ices ha a e
designed o accomplish a speci ic mission on mic oscale.
1–3
Mic o obo s a e chemically p og ammed o collec , anspo ,
and deli e ca go,
4–6
deg ade pollu an s
7,8
and bac e ial
con amina ion,
9,10
o sense desi ed subs ances,
11,12
e c.
Howe e , a single mic o obo exhibi s ela i ely poo efficiency
when s udied in he mac o-scale. Inspi ed by mo phogenesis
in biology, mic o obo ic sys ems we e p og ammed o commu-
nica e and coope a e wi h each o he by o ming swa ms o
mic o obo s.
13,14
The swa ming mic o obo s p omise a powe -
ul ool o medical and en i onmen al applica ions, as hey
can eac in esponse o en i onmen al s imuli, such as
change in mo phology, ca go loading and anspo , imaging,
e c.
15–17
Swa ming beha io can be induced by using a ious
ex e nal s imuli, i.e. magne ic ield, ligh , acous ic o elec ic
ield.
18
Ligh -induced swa m o ma ion is qui e a e sa ile
app oach conside ing i s low-cos ins umen a ion, p ecise
con ol, and biocompa ibili y. The mechanism o ligh -
induced swa ming lies in diffe en mechanisms, such as elec-
opho esis, diffusiopho esis, and he mopho esis.
19
A ypical
example o ligh -induced swa m o ma ion a e TiO
2
-based
swa ming pho opho e ic mic o obo s.
20
Upon ligh i adia ion,
TiO
2
mic o obo s show schooling beha io consis ing o he
expansion and con ac ion o he swa ms ha ac as a mic o-
i ewo k o mic opump sys em due o pho opho e ic p o-
pe ies.
21
E en ually, due o nega i e pho o axis, he swa ms
can mo e wi hin he sample and anspo desi ed sub-
s ances.
22
L. Wang e al.
23
used pho e ic in e ac ions among
TiO
2
-based mic o obo s o emo e mic oplas ics om aqueous
samples. In addi ion o TiO
2
, ligh -induced swa ming beha io
was obse ed in a ious ypes o semiconduc o s, o example
o ganic pho oac i e molecules
24
and polyme s,
25
sil e chlo -
ide,
26
sil e phospha e,
27
i on oxide,
28
o chalcogenide
semiconduc o s.
29,30
The la e is also known o good he mo-
dynamic s abili y, acile syn hesizabili y and dopabili y, and
unique op oelec ical p ope ies ha enable hei applica ion
in sola cells, hin ilm ansis o s, diodes, o wa e spli ing
pho oelec oca alys s.
31
Recen ly, chalcogenide semi-
conduc o s ha e been applied as sui able ma e ials o he ab-
ica ion o ligh -d i en mic o obo s; X. Zhan e al.
32
epo ed
on p epa a ion o Sb
2
Se
3
-based mic o obo s o aniso opic
c ys al s uc u e ha we e na iga ed unde pola ized ligh .
Simila ly, me al dichalcogenides, such as WS
2
and MoS
2
, we e
†Elec onic supplemen a y in o ma ion (ESI) a ailable. See DOI: h ps://doi.o g/
10.1039/d3n 00098b
a
Cen e o Ad anced Func ional Nano obo s, Depa men o Ino ganic Chemis y,
Uni e si y o Chemis y and Technology P ague, Technicka 5, 166 28 P ague, Czech
Republic. E-mail: pume [email p o ec ed]
b
Fu u e Ene gy and Inno a ion Labo a o y, Cen al Eu opean Ins i u e o Technology,
B no Uni e si y o Technology, Pu kyno a 656/123, 621 00, B no, Czech Republic
c
Facul y o Elec ical Enginee ing and Compu e Science, VSB –Technical Uni e si y
o Os a a, 17. lis opadu 2172/15, 70800 Os a a, Czech Republic
d
Depa men o Medical Resea ch, China Medical Uni e si y Hospi al, China
Medical Uni e si y, No. 91 Hsueh-Shih Road, Taichung, Taiwan 40402
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applied o he ab ica ion o pho opho e ic swa ming
mic o obo s.
29,30
He e, we ab ica ed swa ming pho e ic an imony(III) sul ide
(Sb
2
S
3
)-based mic o obo s ( u he e e ed as “mic o obo s”).
Sb
2
S
3
is an ea h-abundan semiconduc o wi h low oxici y
and good s abili y in ai .
33
I shows ema kable op oelec ical
p ope ies sui able o sola cells
34
and li hium ion ba e ies
ab ica ion,
35
pho oca aly ic wa e spli ing
36
and pho o-
ca aly ic pollu an deg ada ion.
37,38
Being awa e o cu en
“g een chemis y” ends,
39
ou objec i e was o apply he syn-
he ic app oach o mic o obo s manu ac u ing in an en i on-
men ally iendly way. The e o e, we employed bio-o igina ed
p ecu so s as capping agen s, ha is, p o eogenic α-amino acid
L-cys eine and a a ic acid, which occu s na u ally in many
ypes o ui s. The syn he ic ou e was hen ca ied ou in a
mic owa e eac o p o iding g ea ep oducibili y, low-ene gy
usage, and la ge-scale p oduc ion.
40,41
The esul ing mic o o-
bo s we e p opelled unde ul a iole (UV) ligh i adia ion due
o he elec opho e ic and diffusiopho e ic beha io o he
mic o obo s. Since he elec opho e ic and diffusiopho e ic-
induced p opulsion is caused by ions and ROS o ma ion and
edis ibu ion, we applied he mic o obo s o pho oca aly ical
deg ada ion o o ganic pollu an s. As model pollu an s, we
chose a azine and quinoline yellow ood dyes. Gi en hei
poo biodeg adabili y, syn he ic ood dyes can accumula e in
was ewa e and nega i ely in luence he en i onmen .
42–44
Anionic azo-dye a azine (E 102) and anionic quinoph halone
dye quinoline yellow (E 104) a e claimed o induce alle gic and
in ole ance eac ions, pa icula ly in as hma ics, and cause
hype ac i i y, especially in child en.
45–47
Resul s and discussion
Fab ica ion and cha ac e iza ion o mic o obo s
The Sb
2
S
3
mic o obo s we e p epa ed in a mic owa e eac o
(Fig. 1) by eac ing SbCl
3
(an imony(III) chlo ide) wi h bioma-
e ial-based empla es L-cys eine and a a ic acid. As
sugges ed in a p e ious epo ,
48
Sb
3+
o ms a complex wi h
a a ic acid and hus allows coupling ia hyd ogen bonds
wi h L-cys eine, which ac s as a sul u izing agen o allow he
o ma ion o Sb
2
S
3
. To pe o m he syn hesis in an en i on-
men ally iendly way, we p oceeded he eac ion in an
aqueous en i onmen . Al hough wa e is no conside ed he
mos efficien sol en o con e mic owa e i adia ion in o
hea , especially in compa ison o e hylene glycol, dime hyl
sul oxide, o me hanol,
49
his syn he ic app oach showed g ea
esul s and can be ega ded as en i onmen ally iendly.
To op imize he p ocedu e, diffe en eac ion condi ions
we e es ed. Fig. S1†shows he in luence o magne ic s i ing,
eac ion ime, empe a u e, and a a ic acid concen a ion on
he esul ing mo phology o he mic o obo s. B ie ly, s i ing
he eac ion mix u e du ing he syn hesis enabled o ma ion
o homogeneous size and mo phology dis ibu ion o mic o o-
bo s. I is wo h emphasizing ha s i ing is no ypically
allowed in con en ional hyd o he mal syn he ic me hods, bu
i can be applied and con olled in he case o using a mic o-
wa e eac o . Nex , he eac ion ime o 15 minu es caused he
o ma ion o sphe ical and od-like mic o obo s oge he . A e
30 minu es, only od-shaped mic o obo s we e ob ained,
sugges ing homogeneous shape and size con ol. No u he
effec was obse ed when p olonging he eac ion ime o
45 minu es. The mo phology was u he in luenced by he
eac ion empe a u e. The op imal empe a u e was e alua ed
a 180 °C as he lowe empe a u e o 160 °C led o a educ ion
o mic o obo size homogenei y; howe e , highe empe a u e
o 200 °C caused only a sligh inc ease in size homogenei y.
Fu he , a a ic acid concen a ion was obse ed o ha e a sig-
ni ican effec on he esul ing mo phology o he mic o obo s
as well. The op imal concen a ion o a a ic acid was e alu-
a ed as 8 mol. eq. wi h espec o SbCl
3
. When he concen-
a ion was educed o 6 mol. eq. wi h espec o SbCl
3
,
sponge-like mic opa icles we e o med, whe eas inc easing
he concen a ion o 10 mol. eq. wi h espec o SbCl
3
caused
he o ma ion o la ge ods. The p o ocol o he op imized
mic owa e-assis ed syn he ic p ocedu e is shown in Fig. S2.†
Namely, he empe a u e, p essu e, and powe p o iles a e p e-
sen ed. I is wo h no ing ha he p ecise hold o he empe a-
u e du ing he syn hesis enables high ep oducibili y o he
ma e ial p epa a ion. Mo eo e , he powe o he mic owa e
eac o is ∼20 W a e eaching he se empe a u e sugges ing
low-ene gy consump ion mode du ing he syn hesis.
A e op imizing he syn he ic p ocedu e, he mic o obo s
esembled ods wi h a e age leng h o 16 ± 5 μm and wid h o
Fig. 1 Schema ic illus a ion showing (A) he “one-po ”p epa a ion o Sb
2
S
3
mic o obo s using a mic owa e eac o and (B) hei pho e ic p ope ies
unde ligh i adia ion ha induce swa ming-like beha io . CB and VB s and o conduc ion and alence bands, espec i ely.
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3.0 ± 0.9 μm (Fig. 2A). EDX images e ealed a homogeneous
p esence o an imony and sul u wi hin he mic o obo s,
sugges ing ha no an imony- o sul u - ich domains we e
o med du ing he p epa a ion (Fig. 2A). The EDX spec a a e
p esen ed in Fig. S3.†The o ma ion o he Sb
2
S
3
phase was
p o ed by eco ding Raman spec a. Fig. 2B demons a es he
well- esol ed esul ing Raman spec um ha poin s o he c ys-
alline s uc u e.
50
The peaks localized a 303, 282, and
254 cm
−1
co espond o he Sb–S s e ching ib a ion, and he
peak a 190 cm
−1
co esponds o he S–Sb–S bending
ib a ion.
51
To con i m he c ys alline na u e o he mic o o-
bo s, powde X- ay diff ac ion (powde XRD) analysis was pe -
o med. The esul ing diff ac og ams (Fig. 2C) e eal a c ys al-
line s uc u e wi hou signs o impu i ies. The diff ac og am
co esponded o he o ho hombic s uc u e o s ibni e wi h
la ice pa ame e s a= 11.33, b= 3.84, and c= 11.24 which is in
ag eemen wi h epo ed da a.
48
In he nex s ep, we eco ded
abso p ion spec a o he powde ed ma e ial o cha ac e ize i s
op ical p ope ies. As seen in Fig. 2D, he abso p ion occu s
e en in isible ange, wi h he onse o abso p ion a a ound
750 nm. Assuming an indi ec ansi ion, he op ical bandgap
was es ima ed a 1.6 eV, which is in ag eemen wi h p e ious
epo s.
52
I should be no ed ha du ing he ypical hyd o he mal
p epa a ion o Sb
2
S
3
ma e ial, an amo phous phase is o med
and u he sin e ing is necessa y o ans o m he ma e ial
in o a c ys alline phase.
48,50
Based on he esul s discussed in
he la e pa ag aph, he mic owa e i adia ion ob iously acili-
a ed o ma ion o he c ys alline phase du ing he syn he ic
p ocedu e. The e o e, he esul ing ma e ial could be di ec ly
used o he desi ed applica ion wi hou any u he ene gy-
consuming and ime-demanding he mal ea men . This
obse a ion is in ag eemen wi h p e ious indings in which
mic owa e adia ion assis ed in he o ma ion o high-quali y
c ys alline s uc u es.
53
The mic o obo s we e u he cha ac e ized by measu ing
ze a po en ial in aqueous dispe sions. The alue o −40 ±
4 mV sugges ed he o ma ion o s able colloidal solu ions ha
do no equi e any u he s abiliza ion h ough he use o
su ac an s.
Fig. 2 S uc u al and op ical cha ac e iza ion o mic o obo s. (A) SEM image o he mic o obo s and EDX elemen al mapping images. Scale ba
25 μm. (B) Raman spec um wi h labelled cha ac e is ic s e ching (ν) and bending (δ) ib a ions. (C) Powde XRD pa e n o mic o obo s showing he
cha ac e is ic finge p in o he Sb
2
S
3
ma e ial in compa ison wi h he e e ence pa e n (JCPDS No. 01-075-4015). (D) Abso p ion spec um o
mic o obo s wi h Tauc plo in he inse o de e mine op ical bandgap.
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Ligh -induced locomo ion o mic o obo s
Ini ially, we es ed whe he he pho oca aly ic p ope ies o
Sb
2
S
3
would enable sel -p opulsion o mic o obo s unde UV
ligh i adia ion. As Fig. 3A and C demons a e, mode a e sel -
p opulsion induced by UV i adia ion was indeed obse ed
(Video S1†). The a e age eloci y o he mic o obo s unde UV
i adia ion was 0.3 ± 0.1 μms
−1
. On he con a y, only
B ownian mo ion was obse ed wi hou any UV i adia ion. To
explain his obse a ion, i should be no ed ha as a pho o-
ac i e ma e ial, Sb
2
S
3
is capable o ligh abso p ion; hence,
sui able ene gy o i adia ion can cause exci on o ma ion
whe e elec ons (e
−
) a e accumula ed in he conduc ion band
and can in e ac on he su ace o mic o obo s wi h p o ons
gene a ed om he in e ac ion o holes (h
+
) wi h wa e .
54
The
p ocess can be summa ized by he ollowing equa ions:
2H2Oþ4hþ!4HþþO2ð1Þ
4Hþþ4e!2H2ð2Þ
In addi ion o p o ons, oxygen, and hyd ogen, diffe en
pho ogene a ed species, such as O
2
−
,OH
•
, and OH
−
, can be
o med by u he in e ac ions. Due o he non-symme ical
shape o mic o obo s, he ion g adien a ound an indi idual
mic o obo is no homogeneous, hus, sel -elec opho e ic
mo ion is induced.
21,55
To in es iga e he o igin o he phenomenon deepe , we
de e mined he pho oelec ochemical p ope ies o mic o o-
bo s by plo ing Ta el cu es. As he Ta el cu es (Fig. 3B)
sugges , he e is a signi ican shi o abou 360 mV owa d
posi i e po en ial a e exposu e o he sample o UV
i adia ion. This obse a ion suppo s ou conclusions abou
pho ochemically d i en locomo ion.
Sel -p opulsion was u he enhanced by applying hyd ogen
pe oxide as a uel (Video S2†). The pho oca aly ic decompo-
si ion o hyd ogen pe oxide o ms eac i e oxygen species
(ROS) by he ollowing equa ions:
H2O2þ2hþ!2HþþO2ð3Þ
H2O2þ2e!2OHð4Þ
Combining he in e ac ions desc ibed in eqn (1)–(4), he
concen a ion o ionic species and adicals inc eases, he e o e
he sel -elec opho e ic phenomenon is enhanced.
55
The esul s o he eloci y calcula ions a e summa ized in
Fig. 3A. Ob iously, he a e age eloci y o he mic o obo s
inc eased wi h inc easing uel concen a ion s a ing om he
Fig. 3 Cha ac e iza ion o he locomo ion o he mic o obo s. (A) A e age eloci y o mic o obo s a diffe en uel concen a ions and he influence
o UV i adia ion. (B) Ta el plo s o s a ic mic o obo s o demons a e pho oca aly ic ac i i y. The Ta el cu es we e measu ed in pu e wa e unde
da k condi ions (a) and unde UV i adia ion (b). (C) Typical ajec o ies o mic o obo s a diffe en condi ions collec ed a e 20 s.
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concen a ion o 1 w % hyd ogen pe oxide. P opulsion was
also obse ed in he p esence o >1 w % hyd ogen pe oxide
unde da k condi ions. Howe e , in his case he a e age el-
oci y did no depend on he concen a ion o hyd ogen pe -
oxide and emained cons an in he ange 0.4–0.5 μms
−1
.
Obse ing mic o obo s in hei aqueous dispe sion, a
s ong in luence o UV i adia ion on mic o obo s o ganiza ion
wi hin he sample was obse ed. As Fig. 4 sugges s, UV
i adia ion induces collec i e beha io and he swa ms o
mic o obo s expand (o iginal mic og aphs wi hou any labels
a e shown in Fig. S4†). Con e sely, when UV ligh was swi ched
off, he swa ms s a ed sh inking, sugges ing a e e sible
p ocess (Video S3†). Same phenomenon was p e iously
obse ed in he case o i anium dioxide-based mic o obo s.
55
As men ioned abo e, Sb
2
S
3
ac s as a semiconduc i e pho o-
ca alys and upon UV i adia ion, ions and ROS a e o med
acco ding o eqn (1)–(4). In addi ion o elec opho esis, o he
phenomena, such as osmo ic p opulsion and su ace cha ge
in e ac ion, occu . Ions, adicals, and ROS a e gene a ed unde
UV i adia ion, which leads o he accumula ion o su ace
cha ge and elec os a ic epulsions ake place causing expan-
sion o he swa ms. Unde da k condi ions, he accumula ed
cha ged species induce elec o-osmosis du ing hei dis-
socia ion and diffusion, which ob iously causes clus e ing o
mic o obo s’swa ms.
21,22,55
As expec ed, he addi ion o
hyd ogen pe oxide inc eased he collec i e beha io due o
mo e in ensi e ions and ROS gene a ion. Compa ison o ligh -
induced swa ming beha io o ueled and non- ueled mic o o-
bo s is also demons a ed in Video S3.†To exclude pho o he -
mal ela ed effec s, such as he mal con ec ion ha is induced
when he sample is locally hea ed wi h UV ligh ,
28
non-pho o-
ca aly ic polyme mic opa icles we e s udied a he same
se ing while applying 5% hyd ogen pe oxide as a uel and i a-
dia ing he sample wi h UV ligh . As a esul , no p opulsion
was induced in ha expe imen (Video S4†) sugges ing ha
he swa ming beha io o he mic o obo s was no caused by
empe a u e g adien s.
Pho oca aly ic deg ada ion o ood dyes
Taking in o accoun he ema kable pho oca aly ic p ope ies
o Sb
2
S
3
, we employed mic o obo s o pho oca aly ic deg a-
da ion o ood dyes, i.e., quinoline yellow and a azine. I
was assumed ha he ac i e adicals, ions, and ROS
p oduced unde UV i adia ion would be able o deg ade he
ood dyes.
Quinoline yellow is an acid dye wi h a cha ac e is ic abso p-
ion spec um due o he a oma ic s uc u e, wi h i s
maximum a 412 nm. On he o he hand, a azine, as a
membe o azo-dye amily, shows a cha ac e is ic abso p ion
spec um, wi h i s maximum a 428 nm (Fig. S5†). In bo h
cases, deg ada ion is expec ed o cause a dec ease in abso p-
ion bands due o he dis up ion o he s uc u e.
56
The e o e,
he deg ada ion p ocess was moni o ed by eco ding UV-Vis
spec a o he samples. To pe o m he deg ada ion expe i-
men s, s ock solu ions o ood dyes we e p epa ed and exposed
o UV i adia ion o i s moni o s abili y wi hou he p esence
o mic o obo s. A e wo hou s o exposu e o UV i adia ion,
he dec ease in abso bance was ∼7 and ∼1% in he case o qui-
noline yellow and a azine, espec i ely, sugges ing ha bo h
ood dyes exhibi g ea s abili y when exposed o UV
i adia ion.
P io he pho oca aly ic expe imen s, he samples con ain-
ing mic o obo s alongside he ood dyes we e magne ically
s i ed o 20 minu es a da k condi ions and he UV-Vis
spec a we e eco ded o moni o he possible adso p ion o
dyes on he mic o obo s. Howe e , no d op in he abso bance
was de ec ed du ing hese equilib a ion expe imen s indica -
ing ha no adso p ion occu ed. In he nex s ep, he samples
we e exposed o UV i adia ion and he s abili y o ood dyes
was moni o ed using a spec opho ome e . Fig. 5 summa izes
he deg ada ion o ood dyes as obse ed in he p esence o
mic o obo s. In he case o quinoline yellow, he e was a 35%
dec ease in abso bance when mic o obo s we e applied. In he
case o a azine, he dec ease in abso bance was by 17%,
sugges ing i s be e s abili y owa d pho oca aly ic decompo-
si ion in his se up. The low deg ada ion efficiency o a a-
zine could be explained by diffe en endency owa d pho o-
ca aly ic deg ada ion a diffe en pH o solu ions. In ou s udy,
no pH con ol was applied by using buffe solu ions. The pH
o he quinoline yellow and a azine solu ions con aining he
mic o obo s we e 6.5 and 6.4, espec i ely be o e he pho o-
ca aly ic deg ada ion expe imen s. As desc ibed in a p e ious
s udy, pho odeg ada ion efficiency o a azine is highe a
acidic condi ions
57
whe eas pho odeg ada ion o quinoline
yellow showed o be he mos efficien wi hou any pH
con ol.
58
To in es iga e he deg ada ion p ocess o ood dyes deepe ,
con ol expe imen s o he pho odeg ada ion o quinoline
yellow we e pe o med wi h e hylenediamine e aace ic acid
(EDTA). EDTA is a commonly used sca enge ha in e ac s
wi h pho ogene a ed holes and hinde s he o ma ion o OH
•
adicals.
59
As clea ly demons a ed in Fig. S6,† he p esence o
he sca enge signi ican ly dec eased he efficiency o pho o-
Fig. 4 Collec i e swa ming beha io o mic o obo s as a unc ion o UV
i adia ion. Compa ison o ueled and non- ueled mic o obo s.
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ca aly ic deg ada ion o quinoline yellow; he abso bance
dec eased by 22% a e wo hou s This obse a ion suppo s
he assump ion ha he ROS, especially OH
•
adicals a e gen-
e a ed upon exposu e o he mic o obo s unde UV illumina-
ion p o iding he deg ada ion abili ies.
Conclusions
We employed a mic owa e-assis ed echnique o de elop a
ep oducible, low-cos , and “g een”manu ac u ing p ocess o
mic o obo s. I is wo h no ing ha he o iginal syn hesis o
he Sb
2
S
3
ma e ial was pe o med in an au ocla e a 180 °C o
12 hou s and u he annealing a 250 °C o 3 hou s was
necessa y o ob ain he c ys alline s uc u e.
48
He e, we pe -
o med he eac ion in a mic owa e eac o a 180 °C o
30 min wi hou any u he he mal ea men . Sb
2
S
3
was p e-
sen ed as pho oac i e ma e ial ha enables he sel -p opulsion
o he esul ing mic o obo s unde UV i adia ion. Sel -p opul-
sion was u he enhanced in he p esence o hyd ogen pe -
oxide as a uel. Due o hei pho oca aly ic p ope ies, mic o o-
bo s we e applied o he deg ada ion o ood dyes, namely,
a azine and quinoline yellow. I can be expec ed ha such
mic o obo s can ind applica ion in he emo al o esidual
ood dyes and beyond.
Expe imen al
Ma e ials
An imony(III) chlo ide (SbCl
3
,≥99.5%), L- a a ic acid
(≥99.5%), L-cys eine (97%), a azine (analy ical s anda d),
quinoline yellow (mix u e o he mono- and disul onic acids),
e hylenediamine e aace ic acid (EDTA, ≥98.5%), and hyd o-
gen pe oxide (30%) we e ob ained om Sigma Ald ich.
E hanol absolu e A.G. was pu chased om Pen a. All chemi-
cals we e used as ecei ed.
Syn hesis o Sb
2
S
3
mic o obo s
Fo a ypical mic owa e-assis ed syn hesis o Sb
2
S
3
mic o o-
bo s, SbCl
3
(0.46 mmol) was dissol ed in 20 mL o a a ic acid
s ock solu ion (0.17 mol dm
−3
) using a sonica ion ba h. In he
nex s ep, L-cys eine (0.65 mmol) was added and he solu ion
was magne ically s i ed o 10 minu es. The p ecu so solu-
ion was ans e ed o a eac ion ial and placed in he mic o-
wa e eac o (Monowa e 400, An on Paa ). The eac ion was
ca ied ou a 180 °C o 30 minu es while being magne ically
s i ed (600 pm). The c ude p oduc was collec ed by cen i u-
ga ion (4000 pm, 3 min) and washed wi h ul apu e wa e
wice and wi h e hanol h ee imes. The esul ing mic o obo s
we e acuum-d ied a 40 °C o e nigh .
Cha ac e iza ion
Mo phology was cha ac e ized using a MIRA 3 XMU (Tescan)
scanning elec on mic oscope equipped wi h an EDX de ec o
(Ox o d Ins umen s) o elemen al mapping. Powde samples
we e cha ac e ized on an adhesi e ca bon ape.
Powde XRD cha ac e iza ion was pe o med using a
Rigaku Sma Lab 3 kW X- ay powde diff ac ome e wi h Cu
Kα adia ion sou ce. Raman spec a we e measu ed wi h an
IR-Raman spec ome e (B uke RFS 100) using a 9394.4 cm
−1
lase o exci a ion. The abso p ion spec a o mic o obo s in
solid s a e we e eco ded by a Jasco V-750 UV-Vis spec ome e
equipped wi h an in eg a ing sphe e (ISV-922). The ze a po en-
ial was measu ed by Ze asize Ul a (Mal e n Panaly ical L d)
and an a e age o 5 measu emen s was calcula ed.
Ta el plo s we e ob ained by pe o ming linea sweep ol-
amme y on a PGSTAT 204 (Me ohm Au olab) equipped wi h
UV LED (365 nm, 700 mA, adian lux 3.3 W, LedEngin Inc.).
Fo his pu pose, mic o obo s’aqueous dispe sion was d op-
cas ed o e an ITO subs a e ha was hen d ied a ambien
condi ions. Ag/AgCl and pla inum elec odes we e employed as
e e ence and coun e elec odes, espec i ely. The measu e-
men s we e made in dis illed wa e unde da k condi ions and
unde UV i adia ion.
Fig. 5 Pho odeg ada ion o ood dyes de e mined by he change in abso bance. G aphs show deg ada ion o quinoline yellow (A) and a azine (B)
using pho oca aly ically ac i e mic o obo s and UV i adia ion alongside he con ol expe imen whe e no mic o obo s we e applied.
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Locomo ion analysis was pe o med using a Nicon Eclipse
Ts2R in e ed mic oscope equipped wi h a Basle ace acA1920-
155uc digi al came a. The mic oscope was also equipped wi h
a UV-LED sou ce (pE-100, 365 nm, 1670 W cm
−2
). The sample
o he locomo ion analysis was p epa ed by placing a d ople
o mic o obo s’solu ion (5 μl) on a glass slide. The concen-
a ion was adjus ed acco ding o he se ing o mic oscope o
ob ain ideos o a leas 60 acks. Al e na i ely, hyd ogen pe -
oxide was added o he mic o obo s in a speci ic amoun o
each i s desi ed concen a ion o ac as uel. The acks o he
mic o obo s we e analyzed using he T ackMa e plugin wi hin
ImageJ so wa e.
60
A Py hon code sub ac ing e en ual d i
was used o calcula e a e age eloci ies o each ideo.
61
The
esul ing eloci ies we e ob ained as an a e age and a s anda d
de ia ion o a leas h ee ideos. Finally, he ep esen a i e a-
jec o ies we e isualized using NIS so wa e.
Food dyes deg ada ion expe imen s
The sample con aining mic o obo s (0.2 mg mL
−1
) and ood
dye (quinoline yellow o a azine, bo h 0.01 mg mL
−1
)in
o al olume 20 mL was magne ically s i ed o 20 min in a
50 mL eac ion ial a da k condi ions be o e he expe imen .
The sample was exposed o UV i adia ion (365 nm, 700 mA,
adian lux 4.1 W, LedEngin Inc.) and aliquo s we e aken a
gi en ime in e als o moni o he deg ada ion p ocess. Fo
his pu pose, he sample was cen i uged (4000 pm, 3 min) o
emo e mic o obo s and he abso p ion spec um o he supe -
na an was eco ded in qua z cu e es (1 × 1 cm) using he
UV-Vis spec ome e . The abso bance o quinoline yellow and
a azine was ead a 412 and 428 nm, espec i ely. The
con ol expe imen wi h EDTA was pe o med a same con-
di ions wi h he modi ica ion ha EDTA was added o he eac-
ion mix u e (0.1 mM) be o e he pho oca aly ic eac ion.
Au ho con ibu ions
A.J.P. pe o med he expe imen s, ea ed he da a, and w o e
he manusc ip . M.P. supe ised he p ojec and e ised he
manusc ip .
Conflic s o in e es
The e a e no con lic s o decla e.
Acknowledgemen s
This wo k was suppo ed by he p ojec Ad anced Func ional
Nano obo s ( eg. no. CZ.02.1.01/0.0/0.0/15_003/0000444
inanced by he EFRR). CzechNanoLab p ojec LM2018110
unded by MEYS CR is g a e ully acknowledged o he inan-
cial suppo o he measu emen s a CEITEC Nano Resea ch
In as uc u e.
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