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09 juin 2015 Diamond materials for detection Jean-Charles ARNAULT jean-charles.arnault@cea.fr Workshop Diamant et dtecteurs, LPSC, June 9, 2015 Diamond Sensors Laboratory from Chemical Vapour Deposition of diamond to sensors MEMS

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09 juin 2015 Jean-Charles ARNAULT jean-charles.arnault@cea.fr

Diamond materials for detection

Workshop Diamant et détecteurs, LPSC, June 9, 2015

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MEMS Photonic crystals Implants Electrodes

from Chemical Vapour Deposition of diamond…

… to sensors

Diamond Sensors Laboratory

Workshop Diamant et détecteurs, LPSC, June 9, 2015

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a0 = 0.357 nm

density 1.8 1023 atoms /cm3 C-C distance 0.154 nm Bond energy 360 kJ / mol Young modulus (GPa) 1050 150 Sound velocity (km.s-1) 18 8 Thermal conductivity 20 2

(W.cm-1.K-1)

Fd3m structure Properties

Diamond structure

Workshop Diamant et détecteurs, LPSC, June 9, 2015

Si

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Mechanical coating (resistance & tribology) Thermal spreading Surfaces et specific properties

First submicronic device on SOD

Large surfaces & low temperature

Fonctionnal coatings

High speed AFM

Workshop Diamant et détecteurs, LPSC, June 9, 2015

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Proof of concept Partners

MEA Retinal Implants Cochlear implants Cortical Implant Porous 3D Diamond

Materials & process

Health applications

Workshop Diamant et détecteurs, LPSC, June 9, 2015

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Diamond micro-cantilevers

Mechanical performances sensitivity

Biomimetic approach – electronic noise

Surface acoustic waves sensors (SAW) covered with a layer of Functionalized diamond nanoparticles

Sensors applications

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Indirect bandgap semiconductor

Breakdown voltage (V.cm-1) 107

  • 3. 106

Resistivity (Ω

Ω Ω Ω.cm) 1013 – 1016

  • 3. 105

Electron mobility (cm2.V-1.s-1) 4000 1450 Hole mobility (cm2.V-1.s-1) 3500 500 Temperature (°

° ° °C)

700 120

Si

5.45 eV 7.3 eV

Diamond electronic properties

Applications in power electronics GREENDIAMOND (2015-2019)

Workshop Diamant et détecteurs, LPSC, June 9, 2015

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Positionning of micro/nano beams Smart windows for X-ray tubes

Detectors applications

Workshop Diamant et détecteurs, LPSC, June 9, 2015

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Carbon thermodynamics

High Pressure High Temperature Chemical Vapour Deposition

Diamond synthesis

Workshop Diamant et détecteurs, LPSC, June 9, 2015

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huge hydraulic press T > 1700 K P = 5-7 GPa

Workshop Diamant et détecteurs, LPSC, June 9, 2015

HPHT synthesis

Burns et al. J. Crystal Growth 104 (1990)

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Workshop Diamant et détecteurs, LPSC, June 9, 2015

HPHT synthesis

(113) (110) (100) (111) (100) (110) (113) (111) (111)

  • J. Härtwig, J. Morse (ESRF)

Substrates for homoepitaxy

X-ray topography

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HPHT synthesis

Workshop Diamant et détecteurs, LPSC, June 9, 2015

I b II a different grades

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Workshop Diamant et détecteurs, LPSC, June 9, 2015

CVD synthesis

H2 + CH4 (0.5-10 %) Micro-waves 500-1000W Hot Filament 2400 K Tplasma~ 3000-3500 K Plasma: Molecules, Ions, Radicals CH4 + H CH3 + H2 CH3 + H CH4 CH3

  • H2

2 H H•

Exothermic - 104 kcal/mole 1

1 W. A. Yarbrough et al,

  • Appl. Phys. Lett. 60, 2068 1992.
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Workshop Diamant et détecteurs, LPSC, June 9, 2015

CVD synthesis

H• Activation of methyl radicals Recombination of atomic hydrogen

CH4 + H CH3 + H2

CH3

  • Diamond growth

www.chm.bris.ac.uk/pt/diamond/growthmodel.htm

During diamond growth Surface passivation creation of free sites sp2 carbon etching H2 2 H

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Micro-waves

Plasma H2/CH4 Pumping Substrate holder Substrate

Microwave Plasma CVD

Workshop Diamant et détecteurs, LPSC, June 9, 2015

Tsurface~ 770-1200 K Pressure 20 – 300 mBar

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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

MPCVD facilities at CEA

Workshop Diamant et détecteurs, LPSC, June 9, 2015

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MPCVD reactor - UHV set-up

Workshop Diamant et détecteurs, LPSC, June 9, 2015

Sequential investigations by surface analysis

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substrate holder Ib HPHT substrate H2 + CH4 (<10%) Micro-waves 5-100 W/cm3 T~1100 K Plasma T~ 3000 - 3500 K CH4 + H CH3 + H2 H2 2 H e-, D Epitaxial film

Growth parameters

  • High pressure (240 - 340 mBar)
  • Low power (500 – 700 W)
  • Surface temperature (880 - 940°C)
  • Growth rate 1.5 µm / h

3x3mm2 (300€)

Diamond homoepitaxy

Workshop Diamant et détecteurs, LPSC, June 9, 2015

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SC diamond for detection

Workshop Diamant et détecteurs, LPSC, June 9, 2015

Radiation X-ray, γ γ γ γ, … Energy range keV-15 MeV Electric field

+ - + - + -

  • + - + - +

+ - + - + -

electrode diamond electrode Radiation detector

Applications Beam monitoring, dosimeter for radiotherapy

  • N. Tranchant et al., MRS Symp. Proc.

1039, Warrendale, PA, 2008.

2 4 6 8 10 12 14 16 18 1600 1800 2000 2200 2400 2600 2800 3000

electron mobility hole mobility

Mobility (cm

2,V

  • 1,s
  • 1)

Methane concentration (%)

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SC diamond: recent advances

Workshop Diamant et détecteurs, LPSC, June 9, 2015

  • M. Schreck, J. Asmussen, S. Shikata, J. C. Arnault, N. Fujimori, MRS Bulletin 39 (2014) 504

IIa CVD diamond grown on a 7 x7 mm2 HPHT

Muehle et al. DRM 42 (2014) 8

High power density and pressure

1000 W / cm3 300-400 Torr

Reuse of seeds and cloning

Yamada et al. DRM 24 (2012) 29

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Columnar growth Nucleation Coalescence Growth

Workshop Diamant et détecteurs, LPSC, June 9, 2015

Diamond on heterosubstrates

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Nucleation vs Seeding

Workshop Diamant et détecteurs, LPSC, June 9, 2015

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Biofunctionalisation Nanotechnologies Surface analysis FTIR, XPS, AES and Colloidal properties Surface modifications

Diamond nanoparticles

Workshop Diamant et détecteurs, LPSC, June 9, 2015

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Nucleation and seeding

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Substrate

CHx

+

H+ C C C CHx

+

Bias Enhanced Nucleation (BEN)

Workshop Diamant et détecteurs, LPSC, June 9, 2015

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Bias Enhanced Nucleation (BEN)

  • S. Saada et al. , pss(a) 205 (2008) 2121 .

Diamond / Si

129 nm 139 nm

Workshop Diamant et détecteurs, LPSC, June 9, 2015

  • A. Chavanne et al, DRM 22 (2012) 52.

100 nm

Diamond / Ir

0.27° ° ° ° 0.69° ° ° °

XRD Heteroepitaxial diamond

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| PAGE 27

Microcrystalline Nanocrystalline Textured (100) Textured (111)

Polycrystalline diamond films

Workshop Diamant et détecteurs, LPSC, June 9, 2015

Grain size

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10 cm

Diamond films

Workshop Diamant et détecteurs, LPSC, June 9, 2015

From few mm2 to 4 inches…

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Poly Mono Up-scale substrate / Reproductibility Crystalline quality

Heteroepitaxy potential

Heteroepitaxial diamond

Workshop Diamant et détecteurs, LPSC, June 9, 2015

HIRIS

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The best substrate: iridium

3C-SiC 2

2 H. Kawarada et al.,

  • J. Appl. Phys. 81 (1997) 3490.

XRD diamond (111) FWHM 1.5° ° ° ° thickness 20 µ µ µ µm

10 20 30 40 3 4 5 6 7 8 9 10 11

∆χ111 ∆ϕ111 ∆ϕrot

(values from {111} Pole figures)

THICKNESS (µm) FWHM (° )

Silicon 1

1 M. Schreck et al., New Diam. Front.

Carbon Technol. 11 (2001) 189.

BEN

Iridium 1, 3

SCHICHTDICKE (µ µ µ µm)

10 20 30 40 0.0 0.2 0.4 0.6 0.8 1.0 1.2 ∆ϕ311 ∆ϕrot ∆ω

THICKNESS (µm)

3 A. Sawabe et al.,

New Diam. Front. Carbon Technol. 12 (2002) 343.. Workshop Diamant et détecteurs, LPSC, June 9, 2015

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Diamond heteroepitaxy

Workshop Diamant et détecteurs, LPSC, June 9, 2015

  • n the same nanometric area

100nm 100nm After BEN After growth

  • N. Vaissière et al, DRM 36 (2013) 16.
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Growth of heteroepitaxial films

  • C. Wild et al., DRM 1993

Workshop Diamant et détecteurs, LPSC, June 9, 2015

  • N. Vaissière,

PhD 2014

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3 4 1 2

4 x 4 mm2

3 4 1 2 131nm 128nm 130nm 127nm Thicknesses (ellipsometry)

  • N. Vaissière, PhD

Heteroepitaxial area

Workshop Diamant et détecteurs, LPSC, June 9, 2015

2013 7 x 7 mm2 2015

  • K. H. Lee, PhD
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Heteroepitaxial diamond

Workshop Diamant et détecteurs, LPSC, June 9, 2015

HRTEM

Diamond film grown on Ir / SrTiO3 / Si (001)

Presented at Spring MRS 2015

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Cross-section studied by Raman and CL

Material quality comparable to the state of art

  • H. Bensalah et al., ICDCM conference 2014

Workshop Diamant et détecteurs, LPSC, June 9, 2015

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Charge Collection properties

Workshop Diamant et détecteurs, LPSC, June 9, 2015

  • E. Berdermann,

ADAMAS collaboration, Dec 2013

Heteroepitaxial diamond (M. Shreck et al.)

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Workshop Diamant et détecteurs, LPSC, June 9, 2015

Conclusions and perspectives

CVD Diamond

Single Crystal: excellent performances for detection limited size (< 7 x7 mm2), substrate dependent Polycrystalline: size up to 4 inches deteriorated performances vs single crystal Heteroepitaxial: not commercially available size 7 x 7 mm2(towards 10 x10 mm2) performances for detection under testing

HIRIS

2013-2015

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Acknowledgements

  • K. H. Lee, N. Vaissière, A. Chavanne, F. Marsolat
  • N. Tranchant, D. Tromson, H. A. Girard, M. Pomorski,
  • P. Bergonzo, S. Saada
  • H. Bensala, I.Stenger, J. Barjon
  • R. Bachelet, B. Vilquin
  • A. Tallaire, O. Brinza, J. Achard

Workshop Diamant et détecteurs, LPSC, June 9, 2015

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Thank you for your attention!

Diamond Sensors Laboratory

Workshop Diamant et détecteurs, LPSC, June 9, 2015