Production(?) of chalcogenide glass optics : Xiang-Hua ZHANG, Laurent CALVEZ Hongli MA and Jacques LUCAS

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1 Production(?) of chalcogenide glass optics : motivation, current status and future development Xiang-Hua ZHANG, Laurent CALVEZ Hongli MA and Jacques LUCAS Laboratory of glasses and ceramics, UMR CNRS Sciences chimiques de Rennes, Université de Rennes I, Rennes cedex, France

2 Outline Background and motivations Current technique for chalcogenide glass fabrication Challenges and future trends for chalcogenide glass and lens fabrication Summary

3 Thermal imaging was developed for defense application with more and more commercial applications

4 Why infrared is interesting for driving assistance Visible camera Infrared camera

5 Thermal Imaging A growing market 350 Millio ons US dollars Driver's vision enhancement Maintenance Process control Fire fighting Surveillance Other commercial applications Weapon guidance Civil and military ground applications Other civil and military applications Year Great progress achieved in uncooled infrared detectors Constant need for cheaper, more efficient materials

6 Thermal Imaging : how it works Based on the detection of the radiations emitted by hot bodies Atmospheric transmission Monochromatic luminescence ence energy (W.m -2.sr -1.m -1 ) K Visible range 3000K 1000K 3-5µm 500K µm 300K 200K 100K ,1 1 Wavelength (µm) nd atmospheric window (MWIR) : 3-5 µm 3 rd atmospheric window (LWIR) : 8-12 µm Need for materials transparent in these windows

7 Cost of Infrared detectors Defense consumer Cost of detector + cooler (euros)

8 Typical IR Optics

9 Materials for thermal imaging optics Single Crystalline Germanium Expensive Single point diamond turning Polycrystalline Zinc Selenide (ZnSe) Synthesized by CVD Single point diamond turning

10 Chalcogenide glasses - Definition S Se Te Ga Ge As Sb

11 Chalcogenide glasses - Properties Silica Fluorides Large transparency in the Infrared Sulfides Selenides Tellurides Wavelength (µm) moldable Low dn/dt Bulk / Fibers Lenses

12 Chalcogenide glass samples

13 Chalcogenide glass synthesis Vacuum pump Sealing Liquid Nitrogen Starting raw elements quenching

14 Industrial fabrication of chalcogenide glass Ge-As-Se Dr. A. Ray Hilton, Sr. Amorphous Materials, Inc. Garland, Texas

15 Industrial fabrication of chalcogenide glass Ge-As-Se Dr. A. Ray Hilton, Sr. Amorphous Materials, Inc. Garland, Texas

16 Casting of chalcogenide glass Dr. A. Ray Hilton, Sr. Amorphous Materials, Inc.

17 Casting of chalcogenide glass

18 Different steps of Chalcogenide glass production Maximum size : 200 mm Raw materials, sealed under vacuum Reaction et distillation Homogenisation, cooling and annealing

19 Homogeneity control CCD Camera Glass to be controlled

20 Homogeneity control

21 Fabrication of optical lenses Grinding/polishing : spherical surfaces Single point diamond turning Molding Molding of chalcogenid glass lenses

22 Examples of molded chalcogenide glass optics

23 Challenges for chalcogenide glass molding Sumitomo patent upper mold glass In inert gas or in vacuum to avoid oxidation vapor pressure non negligible at Ts Necessity to prepare preform before molding lower mold

24 Toshiba patented molding machine

25 Amorphous Materials Inc molding machine

26 Challenges and future trends for chalcogenide glass and lens fabrication

27 Synthesis of chalcogenide glasses Important difference in vapor pressures for the different elements Vapor Pressure (Pa) Closed systems 1 10 S As Se Te Sb Ga Ge Temperature ( C) Highly sensitive to contamination by oxygen Controlled atmosphere

28 Set-up for chalcogenide glass synthesis in argon

29 Vapor pressure of As and Se Vapor pres ssure (Pa) Temperature ( C)

30 Photos of good sample λ=3-5 µm Example of glass obtained with sealed silica tube

31 Index reproducibility 3 glasses tested Index precision : Index at 1.55 µm glasses Lower Upper difference Technique samplecan sample not be used for synthesizing A Germanium containing glass B C Difference B-C

32 Continuous production line Umicore patent For IR optics

33 New approach for chalcogenide glass production

34 Mechanosynthesis using mechanical energy instead of thermal energy to induce chemical reaction Starting elements Mechanosynthesis Glass powder Milling jar Milling balls Melting in reusable silica chamber Hot Uniaxial Pressing Spark Plasma Sintering Consolidation Bulk material

35 Mechanosynthesis 80GeSe 2-20Ga 2 Se 3 Evolution of powder coloration with milling duration 0h 3h 5h 8h 10h 20h 40h 80h Progressive reaction between the elements and lowering of particle size Frequency (%/µm) Particle size distribution 10h 3h 40h 80h counts (arb. units) XRD Spectra 80h 40h 20h 10h 8h 5h 3h 0, Particle size (µm) Angle ( 2 θ) Ge

36 Mechanosynthesis Synthesis of micrometric glass powder Thermal properties close to that of glasses prepared in sealed silica ampoule To produce bulk glasses or optics Melting and casting Sintering

37 Melting of the powders/casting experimental set-up In closed silica chamber under argon atmosphere Argon exit Agitation system Argon entrance The powders already possess the desired composition Reduced risks of evaporation of selenium Rotating Helix Furnace Glass

38 Bulk glass/lenses fabrication by hot pressing Principle: sintering of the powder at a temperature above the glass transition temperature (Tg) but below the melting temperature (Tm) Hot Uniaxial Pressing (HUP) Pressure control P Spark Plasma Sintering (SPS) Pressure control P die furnace Vacuum chamber powder protective plate pistons powder Power supply P P Faster temperature ramps reached with SPS

39 Conventional hot pressing needs stable glasses 80GeSe 2-20Ga 2 Se 3 composition: T<100 C Materials obtained: Inhomogeneous sintering (thermal profile of the press) Uncontrolled crystallization No optical transmission 1µm Crystallization due to prolonged stages at T>Tg Need to reduce sintering process duration => SPS

40 Fast sintering of 80GeSe 2-20Ga 2 Se 3 powder with SPS Dr Synter 505 Syntex SPS machine Experimental conditions Under vacuum Thermal treatment min, 390 C Densification > 99% Temperature ( C) Time (min) Sample surface area x 16 Total duration: 10 min (more than 2h for HUP)

41 glass bulks sintered at different dwell temperatures (50 MPa, 2-min ) 250 C 350 C 390 C G. Delaizir et al J. Am. Ceram. Soc., 95 [7] (2012)

42 Fast sintered 80GeSe 2-20Ga 2 Se 3 glass discs Powder sintered 2 minutes at 390 C (Tg+40 C), 50MPa visible Thermal camera 8-12µm Densification > 99% Transparent bulk samples Ø = 8 mm, 20 mm et 36 mm Maximum diameter obtained using silica tubes = 9 mm

43 Fast sintered 80GeSe2-20Ga2Se3 Glass-Ceramics Sintering at 390 C for longer durations 15 min 2 min 30 min Progressive controllable crystallization (crystals < 100 nm) 70 Transmission (%) 60 2 min min Ge-O 30 min critical load (N). Glass prepared in silica tube and ground 0.2 Glass-ceramics transparent in the 0.1 infrared range 0 60 min 10 Important pollution by oxygen (transmission cut-off at µm) Ceramisation time (hours) Wavelength (µm) min Cooperation with LARMAUR 140

44 Summary Chalcogenide glasses are fabricated batch by batch in sealed silica tube Discontinued process Expensive single use silica ampoules Only for highly stable glasses Fabrication in controlled atmosphere Highly homogenous glasses Only for Ge-free glasses Mechano-synthesis + Spark plasma Sintering Possibility of continuous process Wide choice of glass composition Large size glass ceramic optics We need process revolution

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