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New BImetallic nanoparticles with applications in

Physical Chemistry Institute “Ilie Murgulescu. New BImetallic nanoparticles with applications in water CLEANing of chlorinated compounds and BIOSensors Type : PCCA-1 / 46/2012 Project duration : 36 months Project director: Dr . Balint Ioan Contact details : ibalint@icf.ro

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New BImetallic nanoparticles with applications in

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  1. Physical Chemistry Institute “Ilie Murgulescu New BImetallic nanoparticles with applications in water CLEANing of chlorinated compounds and BIOSensors Type: PCCA-1/ 46/2012 Project duration: 36 months Project director:Dr. Balint Ioan Contact details: ibalint@icf.ro Total budget: 1 850 000 Contracting Authority: UEFISCDI Program: Partnerships BICLEANBIOS

  2. Participants CO-(IPC) Institute of Physical Chemstry “Ilie Murgulescu” belongs to Romanian Academy. Director: Dr Ioan Balint P1 (NIRDMP): National Institute of Research and Development of Material Physics Scientific Responsible P1: Dr. Mihai Lazarescu P2 (NIBS) National Institute of Research and Development for Biological Science Scientific Responsible P2: Dr. Ioana Vasilescu

  3. Project Summary • The project proposes the use eco-friendly bimetallic nanoparticles with controlled composition, morphology (size and shape), structure and oxidation state in catalytic and photocatalytic abatement of toxic chlorinated compounds in Water via dehydrochlorination reaction. • The fine tuning of nanoparticle structure prepared by alkaline polyol method is expected to bring crucial improvements by increasing the catalytic activity and resistance against poisoning compared to already existing materials. A strategy of improving the catalytic performances is proposed by using ordered mesostructured Al2O3 as supporting material which will be synthesized by combined microemulsion-hydrothermal techniques. In addition, the photocatalytic hydrodechlorination reaction over bimetallic nanoparticles assembled in a controlled manner with TiO2 will be investigated.All catalytic materials will be characterized by a bunch of physico chemical techniques (XRD, XPS, fractal analysis, gas titration TPO, TPR, Cyclic Voltammetry). • The targeted technical goal is to develop a laboratory technology for catalytic and photocatalytic degradation of chlorinated compounds in polluted waters. Sensitive and stable biosensors devoted to TCE assessment and based on bimetallic nanoparticles use are also planned to be developed at prototype level. • In order to achieve these ambitious objectives, in the three years proposed, a well-balanced and multidisciplinary consortium of three partners has been created. All the participant Members have a well-established reputation in catalysis, material science, bio-chemistry and physicochemical characterization techniques

  4. Project objectives • The main concepts of the project are to use bimetallic nanoparticles (NPs) with controlled composition, morphology (size and shape), structure and oxidation state in catalytic dehydrochlorination reaction and biosensors. • The fine tuning of nanoparticle structure in colloidal synthesis stage is expected to bring crucial improvements by increasing the catalytic activity and resistance against poisoning in hydrodechlorination reaction compared to already existing materials. • The use of the materials that we are proposing in this project is enhanced by the fact that they will provide low genotoxicity, being highly eco-friendly. • The core objective is to to develop new eco-friendly catalytic materials based on bimetallic NPs with a well defined morphology and structure and low genotoxic impact, to be applied in water de-contamination technologies, based on catalytic dehydrochlorination reaction. A very important application field of the NPs is to play as immobilization support (enhancing sensitivity) and/or redox mediators in sensors/biosensors development.

  5. Phase list

  6. Research team

  7. Etapa I 2012 • Sinteza si caracterizarea nanoparticulelor bimetalice Pt-M, Pd-M, Rh-M (M=Ag, Cu, Au) • Buget etapa I : 460 000

  8. Rezumat etapa I 2012 • Raportul stiintific descrie prepararea nanoparticulelor bimetalice bimetalice Pt-M, Pd-M,Rh-M (M=Ag, Cu, Au) prin metoda poliol alcalina precum si caracterizarea complexa a acestora. Sinteza nanoparticulelor bimetalice in faza organica de etilen glicol s-a realizat in prezenta polivinil pirolidonei care a jucat atat rol de agent de directionare a structurii cat si de prevenire a aglomerarii.Prin ajustarea parametrilor de sinteza s-a incercat obtinerea Nanoparticulelor bimetalice cu structuri core-shell, core-shell invers sau de aliaj. Nanoparticulele obtinute au fost caracterizate prin microscopie electronica (TEM), XPS, TPR (termoreducere programata), TPO (termooxidare programata), chemosorptie si voltametrie ciclica. Din imaginile TEM s-au determinat histogramele de dimensiuni ale nanoparticulelor bimetalice folosind programe de analiza a imaginii. TEM, porozimetrie (distributie de pori si suprafata specifica) si difractie de raze X. Caracterizarea electrochimica a nanoparticulelor bimetalice s-a facut indeosebi prin tehnici de voltametrie ciclica, deoarece caracterizarea riguroasa a bimetalelor sintetizate poate conduce la imbunatatirea proprietatilor catalitice prin ajustarea unora dintre parametrii de sinteza.

  9. Obiectivele generale ale etapei I • Prepararea nanoparticulele bimetalice cu o morfologie controlata de Pt-M, Pd-M, si Rh-M (M=Cu, Ag, Au) protejate cu PVP (polivinil pirolidon) prin metoda poliol alcalina, activitate realizata exclusiv de catre coordonator, ICF Bucuresti (CO); • Caracterizarea complexa a nanoparticulelor bimetalice prin metode fizico-chimice, activitate realizata de intregul consortiu (CO, P1, P2): • Stabilirea citotoxicitatii si genotoxicitatii nanoparticulelor bimetalice, activitate realizata de Institutul National De Cercetare-Dezvoltare pentru Stiinte Biologice Bucuresti (P2).

  10. Rezultate estimate etapa I 2012 • Raport stiintific care sa contina rezultatele obtinute • O comunicare prezentata la o conferinta internationala

  11. Rezultate obtinute in etapa I • S-a realizat sintetiza nanoparticulelor bimetalice de Pt, Pd, Rh-M (M=Cu, Ag, Au) prin metoda poliol alcalina. Metoda de preparare a fost variata astfel incat sa se obtina nanoparticule cu morfologii si structuri diferite. • Nanoparticulele bimetalice au fost caracterizate extensiv prin metodele fizico-chimice propuse in planul de lucru: TEM, XRD, XPS, chemosorptie, TPR, TPO, voltametrie ciclica. Pe baza datelor de caracterizare s-au tras concluzii importante privind morfologia (dimensiune medie, forma), structura (core-shell, aliaj sau core-shell invers), structura cristalina, stare de oxidare, activitate pentru reactia de evolutie a hidrogenului. • Din rezultatele obtinute la caracterizarea fizico-chimica si morfologica a nanoparticulelor bimetalice pe baza de platina, paladiu si rodiu aliate cu argin , cupru si aur se poate concluziona ca acestia pot fi folositi cu succes ca si potentiali catalizatori. • Datele de caracterizare electrochimica a NP Cu-Rh, recomanda utilizarea acestora ca si potential mediator redox in constructia viitoare de biosenzori.

  12. Rezultate obtinute in etapa I • La o prima analiza microscopica se pare ca NP de tip Pt, Pd, Rh-M nu afecteazamorfologia celulelor fibroblast-like (NCTC) in timp ce NP de tip M-Pt, Pd, Rhdeterminao apoptoza celulara chiar la concentratii foarte reduse. • S-a demonstrat ca un numar de 7 probe din cele 15 testate prezinta genotoxicitate prin generare de SRO de tip lipoperoxid, dar rezultatele nu trebuie privite ca alarmante intrucat s-a lucrat cu concentratii destul de ridicate de nanoparticule, de 50 mg/mL, astfel incat este necesar ca, dupa ce vor fi definite intervalele de concentratii la care NP sintetizate vor fi utilizate in reactia de dehidroclorurare, pe baza protocolului stabilit in aceasta etapa sa fie re-testate NP de interes. • S-a demonstrat de asemenea ca majoritatea NP bimetalice au o buna eficacitate de descompunere a apei oxigenate.

  13. Indicatori de rezultat • Obiectivele au fost realizate in totalitate, planul de realizare fiind urmarit si respectat cu rigurozitate; • 25 studii experimentale; • 1 conferinta • 4 seminarii comune coordonator-parteneri pentru a urmari progresul cercetarii in vederea realizarii obiectivelor Etapei I-a; • 1 publicatie ISI • 2 articole in faza de pregatire.

  14. Diseminarea rezultatelor Lucrari publicate 1.Platinum-modified SiO2 with tubular morphology as efficient membrane type microreactors for mineralization of formic acid“ Crina Anastasescu, Mihai Anastasescu, Maria Zaharescu, Ioan Balint Journal of Nanoparticle Research 14(10), 1198-1209, 2012) Conferinte si prezentari orale 1.Synthesis and characterization of bimetallic nanoparticles Au-M (M = Pd, Pt,Rh) byalkaline Polyol method , Autori: Răzvan State, F. Papa, A. Miyazaki, M.Scurtu,G. Dobrescu, I.Balint, ICOSECS 8 ,Belgrad, 27-29 iunie 2013 2. Synthesis and characterization of Cu-M (M = Pd, Pt, Rh) bimetallic nanoparticles, Autori: Răzvan State, Florica Papa, Akane Miyazaki, Mariana Scurtu, Gianina, Dobrescu, Ioan Balint,ROMPHYSCHEM XV-2013, 11-13 september, Bucharest 3.The effect of surface basicity on the C2+ formation yield over an equimolecular mixture of M2O3-MgO (M= Fe, La, Nd, Sm, Gd),Autori: Florica Papa, Georgeta Postole, Aline Auroux, Dana Gingasu, Luminita,Patron,Gianina Dobrescu, Ioan Balint ROMPHYSCHEM XV-2013, 11-13 september, Bucharest

  15. Conferinte si prezentari orale 4. Comparative study on the catalytic and photocatalytic reduction of NO3- over Pd-Cu nanoparticles supported on Al2O3 and TiO2, Autori: Mariana Scurtu, Florica Papa, Răzvan State, Cornel Munteanu, Cătălin Negrilă, Ioan Balint, ROMPHYSCHEM XV-2013, 11-13 september, Bucharest 5. Catalytic denitration over simple and alumina-supported Pt-Cu bimetallic nanoparticles, Autori: Ioan Balint, Kahori Matsuda, Akane,Miyazaki, Florica Papa, Catalin Negrila, Iuliana Pasuk, ROMPHYSCHEM XV-2013, 11-13 september Bucharest 6. Fractal Analysis of Pt-Cu Nanoparticles, Autori: Gianina Dobrescu, Florica Papa, Iudit Fangli, Ioan Balint ROMPHYSCHEM XV-2013, 11-13 september Bucharest 7. Fractal Analysis and Morphology of Pd-Cu and Pd-Au Nanoparticles Autori: Gianina Dobrescu, Florica Papa, Iudith Fangli,Ioan Balint, Corina Bradu Europacat XI, 1-6 september, 2013, Lyon, France

  16. Etapa II 2013 • Sinteza alumimei mesoporoase ; Asamblarea materialelor support (Al2O3, TiO2 , folie titan) cu nanoparticule bimetalice .Caracterizarea sistemelor realizate • Buget etapa II : 414 000

  17. Obiectivele generale ale etapei II • Sinteza si caracterizarea aluminei mezoporoase (CO) • Caracterizarea aluminei mezoporoase prin XPS, XRD si TEM ( P1) • Asamblarea controlata a nanoparticulelor bimetalice cu alumina mesoporoasa, TiO2 (Degusa) si Titan folie (CO) • Testarea citotoxicitatii si genotoxicitatii materialelor asamblate (P2) • Evaluarea si diseminarea rezultatelor experimentale • Publicare articole si participare la conferinte internationale si vizite de lucru

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