Characterization

of ZnO powders

by

X-Ray Diffraction

Prof. M.Abrudeanu

Asist.drd. G.Plaiasu

Nanocrystalline ceramic and composite materials present a set of highly improved and novel mechanical, electronic, optical, catalytic or bioactive properties over the traditional materials.

New processes for the synthesis and sintering are required to be developed to control and optimize the chemical composition, component distribution, crystalline and grain sizes

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Department for International Relations & European Integration Department for Strategy and Curricula MarketingEducation’s Quality Assurance DepartmentDepartment of Scientific and Educational ResearchMUNTENIA Center for Vocational Education & TrainingDepartment for Teaching Staff TrainingOpen & Distance Learning Department“Eudoxiu Hurmuzachi” Department for the Romanians of DiasporaUniversity of Pitesti Publishing HouseUniversity Library

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Master Master francofranco ––roumainroumainSCIENCE ET TECHNOLOGIE DES SCIENCE ET TECHNOLOGIE DES

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a la l’’UniversitUniversitéé de Pitestide Pitesti ):):

INP Toulouse Pr. Alain GLEIZES , Pr. Bernard VIGUIR INP Toulouse Pr. Alain GLEIZES , Pr. Bernard VIGUIR ––responsables responsables franfranççaisaisECP ECP ––Pr. Claude PETOTPr. Claude PETOTINSA Lyon INSA Lyon –– Pr. Jean Pierre MILLETPr. Jean Pierre MILLETUniversitUniversitéé de Metz de Metz –– Pr. GPr. Géérard FERRONrard FERRONEcole de Mines de Nancy Ecole de Mines de Nancy –– Pr. Elisabeth GAUTIERPr. Elisabeth GAUTIERENI Tarbes ENI Tarbes –– Pr. Jacques Alain PETIT Pr. Jacques Alain PETIT

Enseignants roumains:Enseignants roumains:Pr. Pr. MarioaraMarioara ABRUDEANUABRUDEANU–– UPITUPIT-- responsable roumain responsable roumain Pr. Pr. RaduRadu Nicolae DOBRESCU Nicolae DOBRESCU ––UPITUPITPr. Maria PETRESCU Pr. Maria PETRESCU ––UPBUPB-- membre de lmembre de l’’AcadAcadéémie Roumaniemie RoumaniePr. Pr. NicoaleNicoale PETRESCU PETRESCU -- UPBUPB-- membre de lmembre de l’’AcadAcadéémie Roumaniemie RoumanieCp.ICp.I dr. dr. RaduRadu Robert PITICESCU Robert PITICESCU ––IMNR BucurestiIMNR Bucuresti

Master Master francofranco ––roumainroumainSCIENCE ET TECHNOLOGIE DES SCIENCE ET TECHNOLOGIE DES

MATERIAUXMATERIAUXDirecteursDirecteurs de stages de de stages de rechercherecherche: :

ProfesseursProfesseurs participants a participants a ll’’enseignementenseignement des universities des universities partenairespartenaires au au mastermasterPr. Claude MONTY Pr. Claude MONTY -- SOLFACE SOLFACE Pr. Marc GABRIEL Pr. Marc GABRIEL ––Univ. Nancy Univ. Nancy

ResultatsResultats107 107 diplomesdiplomes

En 2004/2005 En 2004/2005 sursur le le classemntclassemnt de de ll’’INPTINPT les les etudiantsetudiants dede PitestiPitesti ontont occupeoccupeles positions 2, 3, 6les positions 2, 3, 6……

ActuellementActuellement les les diplomesdiplomes ::EnseignantsEnseignants a a ll’’UPITUPITResponsablesResponsables de de projetsprojets chez chez DaciaDacia Renault Renault DrecteursDrecteurs dansdans les les entreprisesentreprises avec participation avec participation francaisefrancaiseDocteursDocteurs et et doctorandsdoctorands des des universitesuniversites francaisesfrancaises et et roumainesroumaines..

DoctoratDoctorat en en SCIENCE ET GENIE DES MATERIAUXSCIENCE ET GENIE DES MATERIAUX

THESES EN COTUTELLE THESES EN COTUTELLE ––FRANCO ROUMAINE FRANCO ROUMAINE En En deroulementderoulement en 2005en 2005--2006: 2006:

•• UPITUPIT-- INSA Lyon INSA Lyon –– Pr.JPPr.JP MILLETMILLET --2 theses2 theses•• UPITUPIT-- INSA Lyon INSA Lyon –– MC MC HassanHassan IDRISSIIDRISSI•• UPIT UPIT –– UniversitieUniversitie de Metz de Metz ––Pr Gerard FERRON Pr Gerard FERRON --2 theses 2 theses •• UPITUPIT--UTBM UTBM --2 theses 2 theses

•Different techniques were reported in the literature for the preparation of thin ZnO films: chemical vapour deposition, pulse laser deposition, sputtering, spray pyrolysis, sol-gel methods.

•The high potential of the vaporisation-condensation process in solar reactor (Solar PVD) to grow nanocrystalline doped ZnO as whiskers (10 to 50 nm large and several microns long) or as small particles with mean crystallite sizes of 5 nm has been demonstrated [1,2] ; recent experiments have shown that Zn or ZnO coatings can be obtained on glass with the same method [C. Monty, Private communication]

•That opens the way for important fundamental results on the electronic, magnetic and optical properties of nanopowders, nanocrystalline dense ZnO ceramics or thin films.

ZnOZnO based nanomaterialsbased nanomaterials

Preparation of ZnO powders andAl-doped ZnO powders by hydrothermal process at IMNR

Obtaining of large quantities of ZnO and Al-doped ZnOnanophases using the vaporisation-condensation process in the solar furnace at PROMES starting from powders obteined by hydrothermal process(INCDMNR) and plasma(Inst.Solid State Physics Riga)

Characterization of ZnO powders by X-Ray diffraction and study evolution of XRD characteristic peaks vs. synthesis parameters

Main objectivesMain objectives

ZnO nanomaterialsSemi-conducting transparent oxide with a large band gap (3.4eV). Doping with impurities such as Al and In can increase the conductivity of ZnO

Piezoelectric properties of zinc oxide thin films can be used in various transducers, acoustic wave and acoustic-optical devices.

Combination of high visible transparency and low electrical resistivity is very useful in applications such as transparent electrodes in solar cells, luminescence display screens, ultraviolet diodes .

When ZnO is in polycrystalline form, luminescence depends on the grain size;

ZnO nanomaterials offer from this point of view a new and promisingfield of investigations.

Nanophase ZnO synthesis in solar reactor

Hydrothermal synthesis

NANOSOL reactor (30.06.2006), pressed pellet 1tf, p=20 torrWo=916W/m2

Vc[Hy2.5AlZnO]2_f

NANOSOL reactor (29.06.2006), pressed pellet 1tf,p=20 torr

Wo=937W/m2

Vc[Hy1AlZnO]_f

NANOSOL reactor (29.06.20060pressed pellet 1tf,p=20 torrWo=910W/m2

Vc[Hy0.05AlZnO]_f

NANOSOL reactor(27.06.2006) pressed pellet 1tf, p=20 torr Wo=750W/m2

Vc[Hy2ZnO]_f

ConditionsSample

Synthesis parameters

Experimental results

VC[Hy2ZnO]_f VC[Hy0.05AlZnO]_f

VC[Hy1AlZnO]2_f VC[Hy2,5AlZnO]3_f

VC[Hy2ZnO]_f VC[Hy0.05AlZnO]_f

VC[Hy1AlZnO]2_f VC[Hy2,5AlZnO]3_f

Experimental resultsZnO hexagonal

XRD results

D=376.3Å100%a=3.252ÅC=5.211Å

ZnO, hexagonalType B4

Simbol Pearson: hP4

Vc[Hy2.5AlZnO]2_f

D=414.7Å100%a=3.255ÅC=5.216Å

ZnO, hexagonalType B4

Simbol Pearson: hP4

Vc[Hy1AlZnO]_f

D=367Å100%a=3.252ÅC=5.210Å

ZnO, hexagonalType B4

Simbol Pearson: hP4

Vc[Hy0.05AlZnO]_f

D=349.7Å100%a=3.254ÅC=5.214Å

ZnO, hexagonalType B4

Simbol Pearson: hP4

Vc[Hy2ZnO]_f

Main grain sizeQuantitative Analyze Qualitative analyze Sample

5.2

5.21

5.22

0 1 2 3

Al content(%weight)c[

A]

3.2

3.3

3.4

3.5

0 0.5 1 1.5 2 2.5 3

Al content (%weight)

a[A

]

NANOSOL 07.07.2006, pressed pellet 1tfp=20 torr

Wo=914W/m2

Vc[PL5,1AlZnO]_f

NANOSOL 05.07.2006, pressed pellet 1tf,p=20 torr

Wo=750W/m2

Vc[PL1,9AlZnO]_f

NANOSOL 29.06.2006, pressed pellet 1tfp=20 torr

Wo=864W/m2

Vc[PlG2_3ZnO]_f

ConditionsSample

Synthesis parameters

Vc[PLG2_3ZnO]-fVc[PL1,9AlZnO]-f

Vc[PL5.1AlZnO]-f

Experimental results

Vc[PLG2_3ZnO]-f Vc[PL1,9AlZnO]-f

Vc[PL5.1AlZnO]-f

Experimental resultsZnO hexagonal

D=387.5Å100%a=3.252ÅC=5.2111Å

ZnO, hexagonalType B4

Simbol Pearson: hP4

Vc[PL5,1AlZnO]_f

D=427.8Å100%a=3.252ÅC=5.210Å

ZnO, hexagonalType B4

Simbol Pearson: hP4

Vc[PL1,9AlZnO]_f

D=362.9Å100%a=3.253ÅC=5.212Å

ZnO, hexagonalType B4

Simbol Pearson: hP4

Vc[PlG2_3ZnO]_f

Main grain sizeQuantitative Analyze Qualitative analyze

Sample

5

5.5

6

0 1 2 3 4 5 6

Al content(%weight)

c[A

]

3.2508

3.2529

3.255

0 2 4 6

Al content (%Weight)

a[A

]

XRD results

ConclusionsHydrothermal synthesis and plasma synthesis was used for

the preparation of nanostructured ZnO and Al doped ZnOpowders with controlled Al content

large quantities of Al-doped ZnO nanophases can be produced using the vaporisation-condensation process in the solar furnace at PROMES starting from powders obteined at IMNR and at Inst.Solid State Physics Riga

solar PVD method is a powerful method to obtain Al-doped ZnO nanophases

X ray diffraction phase analysis relieved that all the samplesindependent of alumina content, present only the corresponding zinc oxide peaks

AcknowledgementsAcknowledgementsAcknowledgements

Dr. Claude Monty –Olalde CNRS /PROMES France

Nanostructured Materials Laboratory – INCDMNR Pantelimon

Dr. Larisa Grjgorieva and Dr. D.Millers– Inst.

Solid State Physics Riga

Dr. Viorel Malinovki and Dr. Catalin Ducu - CCMA-University of Pitesti