a transparent tellurite ceramicfor nearinfraredapplications · 2016. 11. 24. · tellurite glasses...

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]


Czochralski [5]

TRANSPARENT




3



Czochralski [5]

MgAl2O4 SparkPlasmaSintering[7]

TRANSPARENT Nd:Lu2O3 Slip-castingcoupledwithSparkPlasmaSintering (SPS)[8]


3



Czochralski [5]



AnisotropicNd:FAP(Fluorapatite)ceramic[9]



3



Czochralski [5]



AnisotropicNd:FAP(Fluorapatite)ceramic [9]

Presenceofporosity

Timeconsuming

Carboncontamination

Post-treatment



Full crystallization from glass technique

4

Mixprecursors

MeltingandAnnealing

GLASS

Congruentandfull

crystallization

TransparentCeramics


4

Mixprecursors

MeltingandAnnealing

GLASS

Congruentandfull

crystallization

TransparentCeramics

Easyglassshaping

Ceramicproperties

Cost-effectivenessAbsenceofporosityNocontamination


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

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


9

400°C:CubicphaseBi0,8Nb0,8Te2,4O8(anti-glassβ-Bi2Te4O11)

T<400°C:Glass



9


480°C:TransformationintoanotherpolymorphofBi0,8Nb0,8Te2,4O8(isostructuraltoSnTe3O8)400°C:CubicphaseBi0,8Nb0,8Te2,4O8(anti-glassβ-Bi2Te4O11)

T<400°C:Glass


9

Temperaturerange400°C<T< 520°C


T>520°C:Secondary phases(BiNbTe2O8)


T<400°C:Glass


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]


Raman spectra of β-Bi2Te4O11 [17]

T>520°C:Secondary phases(BiNbTe2O8)


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


12

EBSD-SEMmap(F.Brisset,ICMMO)


AbsenceofporosityNoresidualanti-glassphase

Thingrainboundaries

20µm

SEMimage(Y.Launay,SPCTS)


12


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

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

a transparent tellurite ceramicfor nearinfraredapplications · 2016. 11. 24. · tellurite glasses...

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