Progress in extruded fluoroindate glass fibers for mid-ir applications

Transcription

1 Progress in extruded fluoroindate glass fibers for mid-ir applications Heike Ebendorff-Heidepriem 1,2,3 and Jiafang Bei 1 1) Institute for Photonics and Advanced Sensing (IPAS) 2) ARC Centre of Excellence for Nanoscale BioPhotonics (CNBP) 3) Australian National Fabrication Facility (ANFF) The University of Adelaide, Australia

2 Institute for Photonics and Advanced Sensing (IPAS) 1 of 5 institutes at Univ. Adelaide Launched Nov 2009 Transdisciplinary approach create new measurement tools for research and industry 195 research members across physics, chemistry, biology, engineering, mathematics 6 overlapping science themes Director: Andre Luiten new building in 2013 founded by Tanya Monro

3 Optofab Adelaide Capabilities more than glass and optics. Surfaces and Molecules - surface functionalization - customized molecules Glass Processing - melting - MCVD - extrusion - drawing Advanced Manufacturing - milling - drilling - 3D printing Optical Fibre Sensors Optical Glasses and Fibres Structured Glass Products for non-optical applications (e.g. microfluidics capillaries) Implants & Prosthetics Intricate Metal Products Prototyping

4 Glass and Fibre Glass Preform Fibre Bulk Macroscopic Structure Nano/Micro Structure open air & controlled atm melting facilities: fluoride, tellurite, germanate extrusion: soft and hard glass MCVD: doped silica u/sonic drilling: all glasses drawing towers (incl. caning, pressurization and spinning): soft glass & silica commercial glasses: silica, F2,

5 noninear refractive index linear refractive index Glass Properties Overview As 2 Se 3 As 2 S 3 TeO 2 Bi-B 2 O 3 /SiO 2 Pb-GeO 2 ZrF 4 : ZBLAN InF 3 : IZSB TeO 2 : Tellurite Pb-GeO 2 : Lead-Germanate Pb-SiO 2 : F2, SF57 SAL: La-Al-silicate SiO 2 : silica high nonlinearity 1.5 Pb-SiO 2 SAL ZrF 4 InF 3 BK7 SiO glass transition temperature Tg ( o C) therm. / mech. / corrosion stability NC in glass melting temperature MIR transmission sensing IR lasers high power H. Ebendorff-Heidepriem, ECOC, London, Sep2013

6 Extrusion glass billet 1.) heating of billet to softening point 2.) forcing soft material through die die geometry preform geometry steel die glass preform Single step: all holes formed simultaneously Automated: highly reproducible Versatile: used for many glass types and large variety of structures possible ~180mm used for drawing H. Ebendorff-Heidepriem, T.M. Monro, Opt. Express 15, (2007) OD=16mm

7 Customized Extrusion machines extremely precise control of extrusion speed Soft Glass Extrusion ( o C) Hard Glass Extrusion ( o C)

8 Extrusion - Materials PMMA polymer TOPAS polymer fluoride-phosphate (FK51A) fluoroborosilicate (FK5) ZBLAN fluoride glass InF 3 -based fluoride glass (IZSB) GeSbSe (IG5) lead silicates (LLF1, F2, SF57) bismuth lead germanate tellurite borosilicate (BK7) Ba-Zn-germanate La-Al-silicate polymer <200 o C fluoride o C chalcogenide o C heavy metal oxide o C high temp. oxide o C

9 Extrusion recent progress / research almost unlimited range of structures modelling of extrusion flow reduce/counterbalance structure deformation use of 3D printed dies new die materials and designs M. Trabelsii, et al., J. Am. Ceram. Soc. 97, 1572 (2014) H. Ebendorff-Heidepriem, T.M. Monro, Opt. Mater. Express 2, 304 (2012) H. Ebendorff-Heidepriem, T.M. Monro, Opt. Express 15, (2007) H. Ebendorff-Heidepriem, et al., Opt. Lett. 33, 2861 (2008) S. Warren-Smith, et al., Opt. Express 17, (2009) S. Atakamarians, et al., Opt. Express 17, (2009)

10 5-axis CNC mill DMG DMU-20 Ultrasonic Hard materials (glass, ceramic) and Metals Simultaneous 5-axis machining Surface finish: Ra <0.1µm (material dependent) Work piece size: 200 X Ø 200mm Latest ultrasonic technology High positioning accuracy

11 Doped silica Preforms via MCVD facility is the first to produce on-line hydrogen, oxygen and nitrogen generation Ge, P, B, Al, rare earth doping different doping concentrations range of index profiles (step-index, W, pedestal)

12 Silica, Soft Glass, Polymer Nano/Microstructured Fibres

13 3D metals & ceramics printer Phenix PXM selective laser melting Build volume: 140mm X 140mm X 100mm Detail size: ~150µm High density parts (>99%) Build materials: stainless steel, tool steel, titanium alloy, cobaltchromium alloy, aluminium alloy, inconel, alumina, cermet

14 Surface Functionalization and Sensor Molecules suite of equipment for surface functionalization of fibres and other substrates synthesis of tailored sensor molecules Photoswitchable sensor molecules Silanisation

15 NANOSCALE BIOPHOTONICS, A WINDOW INTO THE BODY Prof Mark Hutchinson Director

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17 Centre for Nanoscale BioPhotonics $38M 7 years funding $11M in-kind

18 Fibre Sensor Platforms Suspended core fibres Exposed core fibres dip sensors small sample volume (nl) variable core and hole size no filling required easy access to the core real-time & distributed sensing Hollow core fibres large light-matter overlap particularly suited for Raman Sensing Methods fluorescence-based label-free: - whispery gallery modes in microspheres - grating based - Raman-based surface functionalization to achieve specificitiy and selectivity

19 Optical Fibre Sensors What can be detected? metal ions (e.g. Al 3+, Zn 2+, Pb 2+ ) anions (e.g. F -, PO 3-4 ) ph small molecules (e.g. H 2 O 2, SO 2, O 2 ) large molecules (e.g. protein, cancer marker) virus physical parameters (temperature, pressure) ionisation radiation and more

20 Glass Platforms Nanoparticles in Glass (CNBP) new method of direct doping NP: nanodiamond, upconversion nanocrystals, gold, palladium, tellurite glasses: visible transmission + low melting temperature other glasses in the future Mid-Infrared Glasses & Fibres fluoride glasses: ZBLAN, fluoroindate lead-germanate see David Lancaster s talk Ho 3+ doped germanate glass ZBLAN glass

21 Nanodiamond in Tellurite Glass Yinlan Ruan, Tanya Monro Nanodiamond with NV = Single Photon Emitter 2-step melting key to ND survival and low glass loss: 1. higher temperature to obtain clear glass melt 2. low temperature (<650 o C) to disperse and survive ND Andrew Greentree, Brant Gibson 1 st temp = 900 o C preservation of ND emission properties emission of embedded diamond single-photon emission 1 st temp = 690 o C M. Henderson, et al., Advanced Mater. 23, 2806 (2011) H. Ebendorff-Heidepriem, et al., Opt. Mater. Express 4, 2608 (2014) Y. Ruan, et al. Opt. Mater. Express 5, 73 (2015)

22 Mid-Infrared Applications in the mid-infrared region ( 2µm) countermeasures (defence) 2-5μm gas sensing (CO 2, CH 4 ) 3-5μm organic compounds fingerprint 2-20μm medicine 3-10μm astronomy >2μm telecom 2µm

23 Mid-IR Glass Types chalcogenide tellurite & germanate fluoride very high refractive index detrimental for high power applications high index low index desired for high power applications

24 Fluoride Glasses wide transmission range (UV to mid-infrared) 4cm low nonlinearity high power transmission in the mid-infrared 5cm lasers in the mid-infrared two fluoride glass types ZrF 4 -based ZBLAN (53 ZrF 4 20 BaF 2 3 LaF 3 4 AlF 3 20 NaF): established composition bulk glass up to 150g 3 different device platforms InF 3 -based IZSB (32 InF 3 20 ZnF 2 20 SrF 2 18 BaF 2 8 GaF 3 2 CaF 2 ): new composition explore fibre fabrication and durability H. Ebendorff-Heidepriem, et al., Opt. Lett. 33, 2861 (2008) H. Ebendorff-Heidepriem, et al., IQEC/CLEO-PR, Sydney, 2011

25 ZBLAN fibres (1) Commercial fibres made using casting methods step-index fibres double-clad fibres for cladding pumping available db/m at 2-4µm active and passive fibres large and small core fibres casting of long preforms: manual operation that requires skilled operator M. Saad, SPIE 7313, paper 73160N (2009)

26 ZBLAN fibres (2) Our microstructured fibres made using extrusion technique large core AND good beam profile microstructured fibre design extrusion of fluoride glass for the first time ~1dB/m at 4µm good beam quality in the mid-infrared extrusion of long preforms from billets: - automatic operation with high reproducibility - versatility in structure H. Ebendorff-Heidepriem, et al., Opt. Lett. 33, 2861 (2008)

27 ZBLAN extrusion ZBLAN stainless steel: extrusion in crystallization region graphite: extrusion below onset of crystallization!! H. Ebendorff-Heidepriem, et al., Opt. Lett. 33, 2861 (2008)

28 Fluoroindate glass & fibre 32 InF 3 20 ZnF 2 20 SrF 2 18 BaF 2 8 GaF 3 2 CaF 2 Controlled Atmosphere Glass Melting Facility Glass Preform Extrusion Machine Chemical etching and polishing Soft Glass Fibre Drawing Tower Bulk Preform Preform after surface treatment unstructured Fibre

29 Fluoroindate Glass Melting Impact of raw material type (e.g. * InF 3 x 3H 2 O, ** InF 3 anhydrous) fluorination method melting temperature DSC measurement Sample Melting Conditions T g ( C) DT ( C) A* N B* N 2 + SF C* N 2 + NH 4 HF D** N 2 + NH 4 HF J. Bei, et al., Opt. Mater. Express 3, 318 (2013) J. Bei, et al., Opt. Mater. Express 3, 1285 (2013)

30 IR edge and Tg ZBLAN ZrF 4 IZSB high upconversion/ visible fluorescence! T g =260 o C InF 3 T g =308 o C low phonon energy IR edge shifted by ~1µm! enhanced thermomech. stability enhanced corrosion stability J. Bei, et al., Opt. Mater. Express 3, 318 (2013) J. Bei, et al., Opt. Mater. Express 3, 1285 (2013)

31 Fluoroindate Extrusion as for ZBLAN graphite dies for extrusion impact of die design and extrusion temperature viscosity determination via extrusion J. Bei, et al., Opt. Mater. Express 3, 1285 (2013)

32 surface roughness decreases fiber loss decreases Fluoroindate Fibres surface roughness of fibre affects fibre loss and strength surface treatment of preform using etching and polishing is critical! 1.8dB/m at 4.7µm loss for first extruded fluoroindate fibre (using commercial raw materials) compare: 4.0dB/m at 4.7µm for extruded ZBLAN fibre surface roughness decreases fiber strength inreases J. Bei, et al., Opt. Mater. Express 3, 1285 (2013)

33 Chemical Durability in Water ZBLAN ZrF 4 IZSB InF 3 enhanced stability in water

34 of hydrated layer Chemical Durability in Water 20% NaF ZBLAN: NaF required to achieve sufficient crystallisation stability for fibre drawing no NaF no NaF Fluoroindate glass: enhanced stability in water due to lack of NaF nevertheless sufficient crystallization stability for fibre drawing!

35 Conclusions InF 3 - based glass offers advantages over ZBLAN glass enhanced IR transmission up to ~5-6µm for meter-long fibres enhanced thermomechanical stability (e.g. easier polishing) enhanced chemical durability fluoride glass extrusion route to new structures and automation future: step-index fluoroindate fibre fabrication using extrusion future: rare-earth doped fluoroindate fibres

36 Acknowledgment Alastair Dowler for fibre drawing Alexander Hemming from DSTO for helpful discussions Defence Science and Technology Organisation Australian Research Council Australian National Fabrication Facility SA State Government