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Atransparenttellurite ceramic fornear infrared applications
MorganeDOLHENE-mail:[email protected]
A.Bertrand,J.Carreaud,S.Chenu,M.Allix,J.Cornette,M.Colas,E.Véron,V.Couderc,T.Hayakawa,F.Célarié,C.Genevois,P.Thomas,J.-R.Duclère,G.Delaizir
Transparent ceramics
2
MgAl2O4 Transparentarmor[2]
Nd:YAGLaserceramic[3]
Mechanical
Dielectric
Thermal
OPTICAL
PROPERTIES
ALONInfraredwindowsopticallenses[1]
Transparent ceramics
2
Light scattering sources [4]:• 1: Grain boundary• 2: residual pores• 3: secondary phase(s)• 4: double refraction• 5: inclusions• 6: surface roughness
MgAl2O4 Transparentarmor[2]
Nd:YAGLaserceramic[3]
Mechanical
Dielectric
Thermal
OPTICAL
PROPERTIES
[1]http://www.surmet.com/technology/alon-optical-ceramics/[2]A.Goldstein,etal.,JournaloftheEuropeanCeramicSociety2012,32,2869-2886.[3]W.Liu,etal.,CeramicsInternational2012,38,259-264[4]L.B.Kong,etal.,TransparentCeramics.Editor,SpringerInternationalPublishing,2015.
ALONInfraredwindowsopticallenses[1]
Transparent crystalline material elaboration
3
[5]H.Li,etal.,OpticalMaterials2013,35,1071-1076[6]R.Boulesteix,etal.,Materials Letters 2010,64,1854-1857[7]K.Morita,etal.,JournaloftheEuropeanCeramicSociety2016,36,2961-2968[8]R.Boulesteix,etal.,ScriptaMaterialia 2014,75,54-57[9]J.Akiyama,etal.,inBookFirstdemonstrationofrare-earth-dopedanisotropicceramiclaser,ed.byEditor,City,2011,Chap.,pp.1-1.
SapphirecrystalsConventionalsingle-crystalgrowthby
Czochralski [5]
TRANSPARENT
3
Nd:YAG Vacuumreaction-sintering[6]
SapphirecrystalsConventionalsingle-crystalgrowthby
Czochralski [5]
TRANSPARENT
Transparent crystalline material elaboration
[5]H.Li,etal.,OpticalMaterials2013,35,1071-1076[6]R.Boulesteix,etal.,Materials Letters 2010,64,1854-1857[7]K.Morita,etal.,JournaloftheEuropeanCeramicSociety2016,36,2961-2968[8]R.Boulesteix,etal.,ScriptaMaterialia 2014,75,54-57[9]J.Akiyama,etal.,inBookFirstdemonstrationofrare-earth-dopedanisotropicceramiclaser,ed.byEditor,City,2011,Chap.,pp.1-1.
Transparent crystalline material elaboration
3
Nd:YAG Vacuumreaction-sintering[6]
SapphirecrystalsConventionalsingle-crystalgrowthby
Czochralski [5]
MgAl2O4 SparkPlasmaSintering[7]
TRANSPARENT Nd:Lu2O3 Slip-castingcoupledwithSparkPlasmaSintering (SPS)[8]
[5]H.Li,etal.,OpticalMaterials2013,35,1071-1076[6]R.Boulesteix,etal.,Materials Letters 2010,64,1854-1857[7]K.Morita,etal.,JournaloftheEuropeanCeramicSociety2016,36,2961-2968[8]R.Boulesteix,etal.,ScriptaMaterialia 2014,75,54-57[9]J.Akiyama,etal.,inBookFirstdemonstrationofrare-earth-dopedanisotropicceramiclaser,ed.byEditor,City,2011,Chap.,pp.1-1.
3
Nd:YAG Vacuumreaction-sintering[6]
SapphirecrystalsConventionalsingle-crystalgrowthby
Czochralski [5]
MgAl2O4 SparkPlasmaSintering[7]
TRANSPARENT Nd:Lu2O3 Slip-castingcoupledwithSparkPlasmaSintering (SPS)[8]
AnisotropicNd:FAP(Fluorapatite)ceramic[9]
Transparent crystalline material elaboration
[5]H.Li,etal.,OpticalMaterials2013,35,1071-1076[6]R.Boulesteix,etal.,Materials Letters 2010,64,1854-1857[7]K.Morita,etal.,JournaloftheEuropeanCeramicSociety2016,36,2961-2968[8]R.Boulesteix,etal.,ScriptaMaterialia 2014,75,54-57[9]J.Akiyama,etal.,inBookFirstdemonstrationofrare-earth-dopedanisotropicceramiclaser,ed.byEditor,City,2011,Chap.,pp.1-1.
3
Nd:YAG Vacuumreaction-sintering[6]
SapphirecrystalsConventionalsingle-crystalgrowthby
Czochralski [5]
MgAl2O4 SparkPlasmaSintering[7]
TRANSPARENT Nd:Lu2O3 Slip-castingcoupledwithSparkPlasmaSintering (SPS)[8]
AnisotropicNd:FAP(Fluorapatite)ceramic [9]
Presenceofporosity
Timeconsuming
Carboncontamination
Post-treatment
Transparent crystalline material elaboration
[5]H.Li,etal.,OpticalMaterials2013,35,1071-1076[6]R.Boulesteix,etal.,Materials Letters 2010,64,1854-1857[7]K.Morita,etal.,JournaloftheEuropeanCeramicSociety2016,36,2961-2968[8]R.Boulesteix,etal.,ScriptaMaterialia 2014,75,54-57[9]J.Akiyama,etal.,inBookFirstdemonstrationofrare-earth-dopedanisotropicceramiclaser,ed.byEditor,City,2011,Chap.,pp.1-1.
Full crystallization from glass technique
4
Mixprecursors
MeltingandAnnealing
GLASS
Congruentandfull
crystallization
TransparentCeramics
Full crystallization from glass technique
4
Mixprecursors
MeltingandAnnealing
GLASS
Congruentandfull
crystallization
TransparentCeramics
Easyglassshaping
Ceramicproperties
Cost-effectivenessAbsenceofporosityNocontamination
Full crystallization from glass technique
4
Aluminate[10]Mixprecursors
MeltingandAnnealing
GLASS
Congruentandfull
crystallization
TransparentCeramics
Easyglassshaping
Ceramicproperties
Cost-effectivenessAbsenceofporosityNocontamination
Silico-aluminate[12]
Aluminateetgallate [11]
[10]M.Allix,etal.,AdvancedMaterials2012,24,5570-5575[11]S.Alahraché,etal.,ChemistryofMaterials2013,25,4017-4024[12]K.AlSaghir,etal.,ChemistryofMaterials2015,27,508-514
1st Transparent tellurite ceramic
5
75TeO2 - 12.5Nb2O5 - 12.5Bi2O3
25μm
[13]A.Bertrand,etal.,AdvancedOpticalMaterials2016,4,1482-1486
1st Transparent tellurite ceramic
5
75TeO2 - 12.5Nb2O5 - 12.5Bi2O3
25μm
[13]A.Bertrand,etal.,AdvancedOpticalMaterials2016,4,1482-1486
Outline
6
Ø CharacteristicoftheTNBglass
• Glasscomposition
• DSCcurves
Ø StudyofthecrystallizationbyX-raydiffraction
Ø CharacteristicoftheTNBceramic
• Opticalproperties
• Microstructureandthermo-mechanicalproperties
Glass composition
7
Telluriteglassesvssilicaglasses[14]
• Highertransparency
• Lowermeltingpoint(800-900°C)
• Highrefractiveindex
• Goodnonlinearopticalproperties
[14]R.A.El-Mallawany,inBookTelluriteGlassesHandbook:PhysicalPropertiesandData,ed.byEditor,CRCpress,City,2011,Chapter.
Tellurite
Glass composition
7
75TeO2 - 12.5Nb2O5 - 12.5Bi2O3
Non-linearopticalproperties
Thermomechanicalproperties
(Eliaison Nb-O-Te >Eliaison Te-O-Te )
Homogeneousnucleation leadto
crystallization involume
[14]R.A.El-Mallawany,inBookTelluriteGlassesHandbook:PhysicalPropertiesandData,ed.byEditor,CRCpress,City,2011,Chapter
Congruentcrystallizationwithacubicsymmetry
Telluriteglassesvssilicaglasses[14]
• Highertransparency
• Lowermeltingpoint(800-900°C)
• Highrefractiveindex
• Goodnonlinearopticalproperties
Tellurite
Glasssystem
Characteristic of the TNB glass
8
• SimilarDSCcurvesbetweenpowderandbulkglass
• Stabilityoftheglass≈60°C
Homogeneouscrystallization
350 400 450 500 550
Temperature (°C)
Hea
t flo
w (m
W)
Exo
Bulk
Powder
Tg = 390°C
Mixprecursors(TeO2,Nb2O5,
Bi2O3)
Meltingatrelativelylowtemperature:
850°CPARENTGLASS
Tc1 =450°C Tc2 =500°C
Study of the crystallization
9
T<400°C:Glass
In-situX-raydiffraction
Study of the crystallization
9
400°C:CubicphaseBi0,8Nb0,8Te2,4O8(anti-glassβ-Bi2Te4O11)
T<400°C:Glass
In-situX-raydiffraction
Study of the crystallization
9
In-situX-raydiffraction
480°C:TransformationintoanotherpolymorphofBi0,8Nb0,8Te2,4O8(isostructuraltoSnTe3O8)400°C:CubicphaseBi0,8Nb0,8Te2,4O8(anti-glassβ-Bi2Te4O11)
T<400°C:Glass
Study of the crystallization
9
Temperaturerange400°C<T< 520°C
In-situX-raydiffraction
T>520°C:Secondary phases(BiNbTe2O8)
480°C:TransformationintoanotherpolymorphofBi0,8Nb0,8Te2,4O8(isostructuraltoSnTe3O8)400°C:CubicphaseBi0,8Nb0,8Te2,4O8(anti-glassβ-Bi2Te4O11)
T<400°C:Glass
Study of the crystallization
9[15]M.Trömel,etal.,JournalofTheLess-CommonMetals1985,110,421-424[16]O.Masson,etal.,JournalofSolidStateChemistry2004,177,2168-2176.[17]O.Durand,“Propriétés structurales etvibrationnelles desphasesdésordonnées dans lesystème TeO2-Bi2O3”,Université deLimoges,2006.
Anti-glass:concept introduce by Trömel [15] in 1983in tellurite-based glasses. Structure: acationic periodic order at long rangeorder and a disorder of the anions [16]
In-situX-raydiffraction
Raman spectra of β-Bi2Te4O11 [17]
T>520°C:Secondary phases(BiNbTe2O8)
480°C:TransformationintoanotherpolymorphofBi0,8Nb0,8Te2,4O8(isostructuraltoSnTe3O8)400°C:CubicphaseBi0,8Nb0,8Te2,4O8(anti-glassβ-Bi2Te4O11)
T<400°C:Glass
Optical characterization
10
200 400 600 800 1000 1200 1400 1600 18002,1
2,2
2,3
2,4
2,5
2,6
2,7
2,8
2,9
Refra
ctive
inde
x n
Wavelength (nm)
glass antiglass ceramic
RefractiveindexSlight difference between glass,antiglass and ceramic
Optical characterization
10
200 400 600 800 1000 1200 1400 1600 18002,1
2,2
2,3
2,4
2,5
2,6
2,7
2,8
2,9
Refra
ctive
inde
x n
Wavelength (nm)
glass antiglass ceramic
RefractiveindexSlight difference between glass,antiglass and ceramic
510°C– 1h30
T < 510°C: light scattering (residual
glass and/or antiglass with a different n)
T > 510°C: translucent and opaque
ceramics (cubic phase decomposition
and cracks at grain boundaries)
Transparent ceramic
11
ParentglassCrystallization(510°C– 1h30)
TRANSPARENTCERAMIC
§ High transparency up to 74%(15 cm between ceramic and text)
§ Transparent in the MIR (3 - 5 μm)
Properties of the ceramic
12
EDSanalysisCongruent crystallization
Properties of the ceramic
12
EBSD-SEMmap(F.Brisset,ICMMO)
EDSanalysisCongruent crystallization
AbsenceofporosityNoresidualanti-glassphase
Thingrainboundaries
20µm
SEMimage(Y.Launay,SPCTS)
Properties of the ceramic
12
EDSanalysisCongruent crystallization
AbsenceofporosityNoresidualanti-glassphase
Thingrainboundaries
TNBglass TNBceramicYoung’smodulus,E
[GPa] 59.4 79.5
Thermalconductivity[Wm-1 K-1] 0.75 1.1
EBSD-SEMmap(F.Brisset,ICMMO)
20µm
SEMimage(Y.Launay,SPCTS)
Conclusion
13
Fullandcongruentcrystallization
Parentglass Ceramic
Intricateshape(bulk,fibers,…)
Cost-effectiveprocess
Highrefractiveindexgoodthermo-
mechanicalpropertiesNoresidualporositynocontamination
Application:infraredlensesforthermalimagingcameras
Hightransparency(upto5.5μm)
14
Thankyou
for
yourattention
A.Bertrand,etal.,AdvancedOpticalMaterials2016,4,1482-1486
E-mail: [email protected]
15
15
amorphous
crystallized
Raman spectra of amorphous and crystallized phase
16
Raman spectra of glass, anti-glass and ceramic
17
Transmission Electron Microscopy
TEMimageofaceramic(thermallytreatedat510°C– 1h30)
18
LaserEmission?
J.Carreaud,A.Labruyère,H.Dardar,F.Moisy,J.R.Duclère,V.Couderc,A.Bertrand,M.Dutreilh-Colas,G.Delaizir,T.Hayakawa,A.Crunteanu,P.Thomas,OpticalMaterials2015,47,99-107