Light-powered swarming phoretic antimony chalcogenide-based microrobots with "on-the-fly" photodegradation abilities

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 5726 |Nanoscale,2023,15, 5726–5734 This jou nal is © The Royal Socie y o Chemis y 2023 Open Access A icle. Published on 03 Ma ch 2023. Downloaded on 7/28/2023 8:31:37 AM. This a icle is licensed unde a C ea i e Commons A ibu ion 3.0 Unpo ed Licence. View A icle Online View Jou nal | View Issue 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. Nanoscale Pape This jou nal is © The Royal Socie y o Chemis y 2023 Nanoscale,2023,15, 5726–5734 | 5727 Open Access A icle. Published on 03 Ma ch 2023. Downloaded on 7/28/2023 8:31:37 AM. This a icle is licensed unde a C ea i e Commons A ibu ion 3.0 Unpo ed Licence. View A icle Online 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. Pape Nanoscale 5728 |Nanoscale,2023,15, 5726–5734 This jou nal is © The Royal Socie y o Chemis y 2023 Open Access A icle. Published on 03 Ma ch 2023. Downloaded on 7/28/2023 8:31:37 AM. This a icle is licensed unde a C ea i e Commons A ibu ion 3.0 Unpo ed Licence. View A icle Online 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. Nanoscale Pape This jou nal is © The Royal Socie y o Chemis y 2023 Nanoscale,2023,15, 5726–5734 | 5729 Open Access A icle. Published on 03 Ma ch 2023. Downloaded on 7/28/2023 8:31:37 AM. This a icle is licensed unde a C ea i e Commons A ibu ion 3.0 Unpo ed Licence. View A icle Online 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. Pape Nanoscale 5730 |Nanoscale,2023,15, 5726–5734 This jou nal is © The Royal Socie y o Chemis y 2023 Open Access A icle. Published on 03 Ma ch 2023. Downloaded on 7/28/2023 8:31:37 AM. This a icle is licensed unde a C ea i e Commons A ibu ion 3.0 Unpo ed Licence. View A icle Online 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. Nanoscale Pape This jou nal is © The Royal Socie y o Chemis y 2023 Nanoscale,2023,15,5726–5734 | 5731 Open Access A icle. Published on 03 Ma ch 2023. Downloaded on 7/28/2023 8:31:37 AM. This a icle is licensed unde a C ea i e Commons A ibu ion 3.0 Unpo ed Licence. View A icle Online 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. 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