Cermet coating deposition by
DC reactive co-sputtering process
controlled by voltage
aintech@ain.es
Cermet coating deposition by DC
reactive
co-sputtering
process
controlled by voltage
Beatriz Navarcorena, Julián Rodrigo, Gonzalo G. Fuentes,
José A. García, Ramón Escobar, Carlos Prieto, José Angel
Sánchez, Eva Céspedes, J. M. Albella

IVC-19 2013 – September 9-13, Paris, FRANCE
Index

1

Objective

2

Introduction

3

Selective coating design

4

Deposition and characterization

5

Conclusions
Index

1

Objective

2

Introduction

3

Selective coating design

4

Deposition and characterization

5

Conclusions
Objective

To

develop

coating

a

solar

selective

for the parabolic trough solar
collectors that allows the operating temperature
of the transfer fluid to reach 600ºC, and to
develop an application method for them (PVD).
Index

1

Objective

2

Introduction

3

Selective coating design

4

Deposition and characterization

5

Conclusions
Introduction
Parabolic trough solar collector

Parabolic mirror

Absorber tube
Introduction
Key component: Absorber tube
AR-coated glass tube
(high solar transmittance)

Glass-to-metal seal

Selective absorber coating
(high solar absorptance and low
thermal emittance)

Vacuum Insulation
(minimized heat convection
losses)
Introduction
↑ Solar absorptance

1,44 µm

↓ Thermal emissivity
Index

1

Objective

2

Introduction

3

Selective coating design

4

Deposition and characterization

5

Conclusions
Selective coating design
Literature review

Anti-reflection coating
LMVF cermet absorbing layer
HMVF cermet absorbing layer
IR-reflective metal
Substrate
Selective coating design
Our stack

SiO2
SiO2:Mo (LMVF)
SiO2:Mo (HMVF)
IR-reflective metal (Ag)
Stainless steel
Selective coating design
Software simulations
To optimize the optical parameters
Dependence with the metal volume fraction
Dependence with the cermet thickness
SiO2 64 nm
LMVF-20% 70 nm
HMVF-40% 113 nm
Ag
Index

1

Objective

2

Introduction

3

Selective coating design

4

Deposition and characterization

5

Conclusions
Selective coating deposition
DC-Reactive Magnetron Sputtering
Elemental targets: Al, Ti, Si, etc.
Reactive gases: O2, N2, etc.
Inert gases: Ar, etc.

SiO2, Al2O3, Si3N2…

HYSTERESIS
EFFECT
Selective coating deposition
The hysteresis effect
Constant power
Metallic mode

Voltage

Reactive mode

Reactive gas flow rate
Selective coating deposition
The hysteresis effect
Control Methods
Increasing the pumping speed
Increasing the target-to–substrate distance
Obstructing reactive gas flow to the cathode
Pulsed reactive gas flow
Plasma emission monitoring
Voltage control
I.Safi “Recent aspects concerning DC reactive magnetron sputtering of thin films: a review” Surface and
Coatings Technology 127 (2000) 203-219
Selective coating deposition
The hysteresis effect

Stoichiometry

K.Koski et al. “Voltage controlled reactive sputerring process for aluminium oxide thin films” Thin Solid
Films 326 (1998) 189-193
Selective coating deposition
position
The hysteresis effect
Deposition rate

K.Koski et al. “Voltage controlled reactive sputerring process for aluminium oxide thin films” Thin Solid
Films 326 (1998) 189-193
Selective coating deposition
The hysteresis effect
Control method used

speedflo™ Mini is a multichannel closed-loop control
system
for
high
speed
adjustment of a reactive gas for
magnetron sputter processes.
Selective coating deposition
The hysteresis effect
SiO2

Power Si constant = 2000 W

loop point of maximal
deposition rate
Selective coating deposition
Characterization by FTIR: SiO2
Selective coating deposition
The hysteresis effect
SiO2:Mo

In co-Sputtering, the hysteresis loop of Si target
changes when the Mo target is on
Selective coating deposition

Silicon power
(W)

23

3000

60

4000

97

1000
2000

Deposition rate
(nm/min)

1000
1000

Molybdenum power
(W)

45

2000

62

3000

83

4000

111
Selective coating deposition
Characterization by ellipsometry
Si(1000W):Mo(4000W)
Selective coating deposition
Optical simulations with real optical values
Selective coating deposition

Silicon power
(W)

23

3000

60

4000

97

HMVF

1000
2000

Deposition rate
(nm/min)

1000
1000

Molybdenum power
(W)

45

LMVF

2000

62

3000

83

4000

111
Selective coating deposition

Layer

Material

MVF

Thickness (nm)

IR mirror

Ag

-

250

HMVF cermet

Mo/ SiO2

0.28

100

LMVF cermet

Mo/ SiO2

0.1

90

AR layer

SiO2

-

50
Optical characterization of the stack
FTIR dual MIR/NIR Spectrometer
Rango: NIR: 11000-3000 cm-1 (0.9 - 3.3 µm)
MIR: 4000-400 cm-1 (2.5 – 25 µm)

UV-Vis-NIR Spectrophotometer
Range: 200 nm – 3.3 mm
Optical characterization of the stack

Sample

Up-scaled

Temperature

λ2

∫λ

1

A(λ )

ε thn

0,804

0,047

0,804

0,076

0,804

0,111

650 °C

α sol

0,025

600 °C

∫
(θ , T ) = λ

0,804

500 °C

1

0,001

400 °C

∫λ [1 − R(λ ,θ )]A(λ )
=

0,804

300 °C

λ2

ε2

RT

λ2

α2

0,804

0,130

E (T , λ )[1 − RS (λ ,θ )]dλ

1

λ2

∫λ

1

E (T , λ )dλ
Index

1

Objective

2

Introduction

3

Selective coating design

4

Deposition and characterization

5

Conclusions
Conclusions

DC-reactive sputtering technique has important advantages for
depositing multipurpose oxide films controlled by voltage.

DC-reactive Magnetron process requires fast control methods in order
to obtain high deposition rates with the desired stoichiometry, and
with a low reactive gas flow rate.

High value CSP technology stack architecture can be achieved by cosputtering with a previous optical simulation.
Acknowledgments
The research leading to these results has
received funding from the European Community's
Seventh Framework Programme.

Thanks for your attention!

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