Diamond materials for detection Jean-Charles ARNAULT - PowerPoint PPT Presentation

09 juin 2015 Diamond materials for detection Jean-Charles ARNAULT jean-charles.arnault@cea.fr Workshop Diamant et détecteurs, LPSC, June 9, 2015

Diamond Sensors Laboratory from Chemical Vapour Deposition of diamond… … to sensors MEMS Electrodes Implants Photonic crystals Workshop Diamant et détecteurs, LPSC, June 9, 2015

Diamond structure Fd3m structure 1.8 10 23 atoms /cm 3 density C-C distance 0.154 nm Bond energy 360 kJ / mol a 0 = 0.357 nm Properties Si Young modulus (GPa) 1050 150 Sound velocity (km.s -1 ) 18 8 Thermal conductivity 20 2 (W.cm -1 .K -1 ) Workshop Diamant et détecteurs, LPSC, June 9, 2015

Fonctionnal coatings Mechanical coating (resistance & tribology) Thermal spreading Surfaces et specific properties First submicronic device on SOD High speed AFM Large surfaces & low temperature Workshop Diamant et détecteurs, LPSC, June 9, 2015

Health applications Materials process & MEA Porous 3D Diamond Proof of concept Cochlear Cortical implants Implant Retinal Implants Partners Workshop Diamant et détecteurs, LPSC, June 9, 2015

Sensors applications Diamond micro-cantilevers Mechanical performances sensitivity Biomimetic approach – electronic noise Surface acoustic waves sensors (SAW) covered with a layer of Functionalized diamond nanoparticles

Diamond electronic properties Applications in power electronics GREENDIAMOND (2015-2019) 7.3 eV 5.45 eV Si Breakdown voltage (V.cm -1 ) 10 7 3. 10 6 Indirect bandgap Ω .cm) 10 13 – 10 16 Resistivity ( Ω Ω Ω 3. 10 5 semiconductor Electron mobility (cm 2 .V -1 .s -1 ) 4000 1450 Hole mobility (cm 2 .V -1 .s -1 ) 3500 500 Temperature ( ° ° C) ° ° 700 120 Workshop Diamant et détecteurs, LPSC, June 9, 2015

Detectors applications Smart windows for X-ray tubes Positionning of micro/nano beams Workshop Diamant et détecteurs, LPSC, June 9, 2015

Diamond synthesis Carbon thermodynamics Chemical Vapour Deposition High Pressure High Temperature Workshop Diamant et détecteurs, LPSC, June 9, 2015

HPHT synthesis huge hydraulic press T > 1700 K P = 5-7 GPa Burns et al. J. Crystal Growth 104 (1990) Workshop Diamant et détecteurs, LPSC, June 9, 2015

HPHT synthesis (113) (100) (111) (110) (111) (111) (110) (113) (100) X-ray topography Substrates for homoepitaxy J. Härtwig, J. Morse (ESRF) Workshop Diamant et détecteurs, LPSC, June 9, 2015

HPHT synthesis I b II a different grades Workshop Diamant et détecteurs, LPSC, June 9, 2015

CVD synthesis Hot Filament Micro-waves 2400 K 500-1000W H 2 + CH 4 (0.5-10 %) Plasma: Molecules, Ions, Radicals H • H 2 2 H Exothermic - 104 kcal/mole 1 • • • • CH 3 CH 4 + H T plasma ~ 3000-3500 K CH 3 + H 2 CH 3 + H CH 4 1 W. A. Yarbrough et al, Appl. Phys. Lett. 60, 2068 1992. Workshop Diamant et détecteurs, LPSC, June 9, 2015

CVD synthesis Activation of methyl radicals CH 4 + H CH 3 + H 2 Recombination of atomic hydrogen 2 H H 2 H • During diamond growth Surface passivation creation of free sites sp 2 carbon etching • CH 3 Diamond growth www.chm.bris.ac.uk/pt/diamond/growthmodel.htm Workshop Diamant et détecteurs, LPSC, June 9, 2015

Microwave Plasma CVD Micro-waves H 2 /CH 4 Plasma Substrate Substrate holder Pumping T surface ~ 770-1200 K Pressure 20 – 300 mBar Workshop Diamant et détecteurs, LPSC, June 9, 2015

MPCVD facilities at CEA 8 MPCVD reactors 1 for intrinsic single crystals (SC) 2 for boron doping (p- / p+) SC 1 connected to UHV set-up for fundamental studies 2 for prospective studies 2 semi-industrial reactors (intrinsic or B-doped) Substrate area: 2 à 4 inches Workshop Diamant et détecteurs, LPSC, June 9, 2015

MPCVD reactor - UHV set-up Sequential investigations by surface analysis Workshop Diamant et détecteurs, LPSC, June 9, 2015

Diamond homoepitaxy H 2 + CH 4 (<10%) Micro-waves 5-100 W/cm 3 e-, D H 2 2 H 3x3mm 2 (300€) CH 4 + H CH 3 + H 2 Plasma T~ 3000 - 3500 K Epitaxial film T~1100 K Ib HPHT substrate holder substrate Growth parameters • High pressure (240 - 340 mBar) • Low power (500 – 700 W) • Surface temperature (880 - 940 ° C) •Growth rate 1.5 µ m / h Workshop Diamant et détecteurs, LPSC, June 9, 2015

SC diamond for detection Radiation X-ray, γ γ , … γ γ Energy range keV-15 MeV electrode diamond + - + - + - Radiation detector - + - + - + Electric field + - + - + - electrode -1 ) electron mobility 3000 hole mobility -1 ,s 2800 2 ,V 2600 2400 Mobility (cm N. Tranchant et al., MRS Symp. Proc. 2200 1039, Warrendale, PA, 2008. 2000 1800 Applications 1600 Beam monitoring, 0 2 4 6 8 10 12 14 16 18 Methane concentration (%) dosimeter for radiotherapy Workshop Diamant et détecteurs, LPSC, June 9, 2015

SC diamond: recent advances High power density and pressure 1000 W / cm 3 300-400 Torr IIa CVD diamond grown on a 7 x7 mm 2 HPHT Muehle et al. Reuse of seeds and cloning DRM 42 (2014) 8 Yamada et al. DRM 24 (2012) 29 M. Schreck, J. Asmussen, S. Shikata, J. C. Arnault, N. Fujimori, MRS Bulletin 39 (2014) 504 Workshop Diamant et détecteurs, LPSC, June 9, 2015

Diamond on heterosubstrates Growth Nucleation Coalescence Columnar growth Workshop Diamant et détecteurs, LPSC, June 9, 2015

Nucleation vs Seeding Workshop Diamant et détecteurs, LPSC, June 9, 2015

Diamond nanoparticles Surface modifications Colloidal properties Surface analysis FTIR, XPS, AES Biofunctionalisation and Nanotechnologies Workshop Diamant et détecteurs, LPSC, June 9, 2015

Nucleation and seeding

Bias Enhanced Nucleation (BEN) + CH x H + + CH x C C C Substrate Workshop Diamant et détecteurs, LPSC, June 9, 2015

Bias Enhanced Nucleation (BEN) Diamond / Si S. Saada et al. , pss(a) 205 (2008) 2121 . 129 nm 139 nm Diamond / Ir A. Chavanne et al, DRM 22 (2012) 52. XRD Heteroepitaxial 0.69 ° ° ° ° diamond 0.27 ° ° ° ° 100 nm Workshop Diamant et détecteurs, LPSC, June 9, 2015

Polycrystalline diamond films Microcrystalline Textured (100) Textured (111) Grain size Nanocrystalline | PAGE 27 Workshop Diamant et détecteurs, LPSC, June 9, 2015

Diamond films From few mm 2 to 4 inches… 10 cm Workshop Diamant et détecteurs, LPSC, June 9, 2015

Heteroepitaxial diamond Up-scale substrate / Reproductibility HIRIS Heteroepitaxy Mono Poly potential Crystalline quality Workshop Diamant et détecteurs, LPSC, June 9, 2015

The best substrate: iridium BEN Silicon 1 11 (values from {111} Pole figures) 3C-SiC 2 10 ∆χ 111 ∆ϕ 111 9 ∆ϕ rot FWHM ( ° ) 8 Iridium 1, 3 7 1.2 6 ∆ω ∆ϕ 311 1.0 5 ∆ϕ rot 4 0.8 3 0.6 0 10 20 30 40 THICKNESS (µm) 0.4 1 M. Schreck et al., New Diam. Front. XRD diamond (111) 0.2 Carbon Technol. 11 (2001) 189 . FWHM 1.5 ° ° ° ° 0.0 2 H. Kawarada et al., thickness 20 µ µ µ m µ 0 10 20 30 40 J. Appl. Phys. 81 (1997) 3490. SCHICHTDICKE ( µ µ m) µ µ THICKNESS (µm) 3 A. Sawabe et al., New Diam. Front. Carbon Technol. 12 (2002) 343. . Workshop Diamant et détecteurs, LPSC, June 9, 2015

Diamond heteroepitaxy on the same nanometric area 100nm 100nm After BEN After growth N. Vaissière et al, DRM 36 (2013) 16. Workshop Diamant et détecteurs, LPSC, June 9, 2015

Growth of heteroepitaxial films C. Wild et al., DRM 1993 N. Vaissière, PhD 2014 Workshop Diamant et détecteurs, LPSC, June 9, 2015

Heteroepitaxial area 2013 2015 Thicknesses (ellipsometry) 1 131nm 1 2 128nm 2 3 130nm 3 4 127nm 4 4 x 4 mm 2 7 x 7 mm 2 K. H. Lee, PhD N. Vaissière, PhD Workshop Diamant et détecteurs, LPSC, June 9, 2015

Heteroepitaxial diamond HRTEM Diamond film grown on Ir / SrTiO3 / Si (001) Presented at Spring MRS 2015 Workshop Diamant et détecteurs, LPSC, June 9, 2015

Cross-section studied by Raman and CL H. Bensalah et al., ICDCM conference 2014 Material quality comparable to the state of art Workshop Diamant et détecteurs, LPSC, June 9, 2015

Charge Collection properties Heteroepitaxial diamond (M. Shreck et al.) E. Berdermann, ADAMAS collaboration, Dec 2013 Workshop Diamant et détecteurs, LPSC, June 9, 2015

Conclusions and perspectives CVD Diamond Single Crystal: excellent performances for detection limited size (< 7 x7 mm 2 ), substrate dependent Polycrystalline: size up to 4 inches deteriorated performances vs single crystal Heteroepitaxial: not commercially available size 7 x 7 mm 2 (towards 10 x10 mm 2 ) performances for detection under testing HIRIS 2013-2015 Workshop Diamant et détecteurs, LPSC, June 9, 2015

Acknowledgements K. H. Lee, N. Vaissière, A. Chavanne, F. Marsolat N. Tranchant, D. Tromson, H. A. Girard, M. Pomorski, P. Bergonzo, S. Saada R. Bachelet, B. Vilquin A. Tallaire, O. Brinza, J. Achard H. Bensala, I.Stenger, J. Barjon Workshop Diamant et détecteurs, LPSC, June 9, 2015

Diamond Sensors Laboratory Thank you for your attention! Workshop Diamant et détecteurs, LPSC, June 9, 2015