El CNA como centro de ensayos de irradiación dentro de una ICTS interdisciplinar.

El CNA como centro de ensayos
de irradiación dentro de una
ICTS interdisciplinar
Presented by Yolanda Morilla
Conferencia de Posgrado FdI-UCM, 18 de Mayo de 2021
1

Parque Científico
Tecnológico Cartuja
Avda. Tomás Alba Edison nº 7
E-41092 – Sevilla. Spain
http://www.cna.us.es
Director: Dr. Rafael Garcia-Tenorio
(gtenorio@us.es)
2

CNA – MAIN EQUIPMENTS
Spanish ICTS (singular scientific and technological infraestructure) Interdisciplinary research
3 MV Tandem accelerator 18/9 Cyclotron accelerator Co-60 Gamma-irradiator
1 MV Tandem AMS
MICADAS
PET / CT SCANNERS
Radiopharmacy
3

A little bit of history...
• 1997, agreement between Universidad de Sevilla, Junta de Andalucía and CSIC
• 1998, the 3MV tandem accelerator settled in Sevilla
• 1999, the laboratory is opened to the scientific community (public or private enterprise),
mainly to perform ion beam analysis (IBA)
• 2003, the cyclotron accelerator is installed
• Agreement CNA-Schering España. Radiopharmacy and PET research.
• 2005, the compact system for accelerators mass spectrometry (AMS) is put into operation
• 2005/06, the movable line for ion implantation and irradiation is designed and installed to be
shared with tandem and cyclotron accelerators
• 2006, routine service in IBA techniques accessible
Agreement CNA-IBA Molecular-SAS. Radiopharmacy service for all the Andalusian
hospitals.
• 2008/09, Total dose and Microdosimetry irradiation tests (static and dynamic mode)
• 2012/13, 60Co irradiation tester and 0.5 MV AMS MICADAS have been installed
• 2013 up today, improvements of facilities and expansion of activities (projects,
agreements…)
4

Main working scopes
– Material Science
Thin films, ceramics, metallic alloys
– Medicine and Biology
Organic fluids, tissues, radiopharmacy
– Art and Archaeometry
Metals, ceramics, paintings
– Environmental research
Water, aerosols, sediments, soils
- Basic Nuclear Physics
Astrophysics, detectors, nuclear electronic
- Mass Spectrometry with accelerators
Carbon dating, environmental applications
- Accelerated irradiation testing
Astrophysics, detectors, nuclear electronic
- Scholar and scientific outreach activities
Academic training, high and secundary school visits
www.cna.us.es
5

TANDEM
Laboratory
IBA Techniques
Materials Modification
Irradiation Damage
Física nuclear
6

Ion-Solid Interaction
Técnicas IBA / Modificación de materiales / Reactions
dx
dE
E
S
E
S
N e
n 

 )]
(
)
(
[
Transmited ions
Channelled ions
Neutrons
Scattered ions
Reaction products
Ions
γ rays
electrons
X rays
Sputtered atoms
Backscattered
ions
Incident Ion
Beam
Electrons
Atoms
Nuclear collisions
Lattice
Ion
Teoría LSS
(Linhard-Scharf-Schiøtt)
Energy Loss
Nuclear & Electronic stopping
Ion Range
Different events
Cross section
 

E
e
n E
S
E
S
dE
N
R
0
)
(
)
(
1
7

- Particle detectors (RBS, NRA, ERDA)
- X-ray detectors (SiLi, LeGe) for PIXE
- γ-ray detector (HPGe) for PIGE
- Sample holder 150x112 mm2
- X-Y movement
- Minimum spot size (Ø~0.5 mm)
- Electron gun
8

- Sample holder (Ø~5 cm)
- Four axis (X-Y, θ-Φ) goniometer
- Minimum spot size (Ø~0.5 mm)
Specially to study crystalline samples
- Particle detectors (RBS, NRA, ERDA)
- X-ray detectors (SiLi, LeGe) for PIXE
9

BS/C with 3.5 MeV alpha particles
Damage distribution and simultaneous analysis of C & Si sublattices
MUESTRA
DOSIS
(Al2+/cm2)
DENSIDAD
CORRIENTE
(nA/cm2)
DESORDEN MÁXIMO
RELATIVO-Si
DESORDEN
MÁXIMO
RELATIVO-C
A 2 X 1014 21 34 % 50 %
B 2 X 1014 83 36 % 52 %
C 2 X 1014 105 40 % 58 %
D 4 X 1014 86 90 % 100 %
E 7 X 1014 86 100 % 100 %
400 600 800 1000 1200 1400 1600 1800 2000
0
200
400
600
800
1000
1200
1400
Rendimiento
de
retrodispersión
Energía(keV)
Virgen
A
C
D
E
Random
100 150 200 250 300 350 400
0
100
200
300
400
500
600
700
800
900
1000
1100
Rendimiento
de
retrodispersión
Canal
AExperimental
ASimulado
RandomSimulación
VirgenSimulación
Random
Virgen
6H-SiC Implantation
2 MeV Al2+ , tilt = 61º , room T
100 200 300 400 500
0
200
400
600
800
4300 keV
4321 keV
4341 keV
4360 keV
4380 keV
4280 keV
4241 keV
4261 keV
4226 keV
Channels
Y
ie
ld
4He2+ ~4.26 MeV Backscattering in channeling geometry {resonance 12C(α,α)12C}
Y. Morilla, J.
García-López, G.
Battistig et al.
10

- Particle detectors (RBS, STIM)
- Secundary electrons detector (SEM)
- X-ray detector (SiLi) for PIXE
- γ-ray detector (HPGe, NaI) for PIGE
- Minimum Ion beam size ~ 3μm
- Scanning system, elemental maps
- Small sample holder
- Electrons gun
11

Heavy Metals in neurons
Parkinson’s disease
Decrease [dopamine]
Increase of [Fe.]
Increase [dead cells]
A. Carmona (CNA), R. Ortega (CENBG) et al.
Organometallic compound
Dopamine -Fe
Nuclear microprobe analysis of
arabidopsis thaliana leaves
M.D. Ynsa and F.J. Ager (CNA), J.R. Domínguez, C. Gotor
and L.C. Romero (IBVFSE-CSIC)
20um
Ca Ka1: PIXE3( 113- 123)
Contaminated soils
Phytorecovery
Heavy metals acumulation sites
Fe, Cd, Zn…
12

- Ion beam size ~ 50-100μm
- Versatile sample holder
-Two X-ray detectors (SiLi, LeGe) for PIXE
13

Tartesic Gold Jewellery:
Ébora treasure
Two kind of solders:
brazing, forging
Necklace, 700 - 500 B.C.
Archaeological Museum of Seville
0 5 10 15 20 25
0
2
4
6
8
10
Ag K
Ag K
Cu K
Au L
Au L
Energía
Au L
Cu K
Patrón de Oro
Detector Si(Li)
Haz Externo CNA
KeV
Study of paintings and ceramics
from Teotihuacán
Different colors characterization
Differencial-PIXE; Non destructive stratigrafy
Painting thickness
M.A. Ontalba, I. Ortega, Respaldiza et al.
14

- Exotic nuclei studies
- Cross section determination for astrophysical applications
- Development of nuclear electronics and detectors
15

The last installed in the 3MV Tandem accelerator before the 90º magnet
Based on deuteron nuclear reactions p(7Li,n), d(D,n), p(9Be,n) & d(9Be,n), from
thermal neutrons up to 9 MeV beams.
HISPANoS: pulsed / continuous neutron source at CNA
16

Cyclotron Laboratory
(18 MeV H+ / 9 MeV D+)
Nuclear Medicine
Irradiation Damage
High Energy PIXE
Cyclotron vault
Experimental vault
2 m thick concrete wall
Cyclotron CNA model
17

Radiopharmacy
(PET isotopes)
Biomolecules marked with 18F and 11C
13NH3 and H2
15O
Research - Dispensation 18
Human & Micro-PET / TC scanning
systems for medical imaging research
using short life isotopes
PET (Positron
Emission
Tomography)

AMS Laboratory
(14C, 10Be, 26Al, 129I, 239Pu, 240Pu, 236U )
IAEA – CNA agreement
surface seawater off Namibian coast
19
Carbon dating in Spain

Co-60 gamma Laboratory
GAMMABEAM ® X200 (Best Theratronics)
Induction of Mutagenesis in Rice seeds
20
Gammagraphy / TC for arts

National Accelerators Centre,
a facility for irradiation testing
21

Severe natural environment above Earth’s atmosphere
‐ Electrons (~keV‐7 MeV)
‐ Protons (~keV‐800 MeV)
‐ Heavy ions
‐ X ‐ Radiation (100 eV – 100 keV)
‐ γ ‐ Radiation
‐ Neutrons (atmospheric level)
Image Source: ESA
22

Radiation effects on components
From Federico Faccio ‐ CERN
From the point of view of the effects, the degradation will differ according to
the energy of the particles, to their nature and to the mission orbit.
It is necessary to understand the instrument technology and geometry to
determine the vulnerability to the environment. Radiation effects important to
consider for instrument and spacecraft design fall roughly into three categories:
degradation from Total Ionizing Dose (TID), Displacement Damage Dose
(DDD), and Single Event Effects (SEE).
24

TID is due to ionizing radiation, by primary protons and
electrons and secondary particles
It causes threshold shifts, leakage current and timing skews
It is possible to reduce this with shielding
The effect first appears as a parametric degradation of the
device and ultimately results in functional failure
Displacement damage is long-term structural damage on
semiconductors caused by protons, electrons, and neutrons
Produce defects mainly in optoelectronics components
SEEs result from ionization by a single charged particle as it
passes through a sensitive junction of an electronic device,
mostly caused by heavier ions but also protons
The severity of the effect can range from noisy data to loss of
the mission, depending on the type of effect and the criticality
of the system in which it occurs
Shielding is not an effective mitigation technique because they
are induced by very penetrating high-energy particles.
Generation and transport of charges by the effect of a SEE in the drain region of a NMOS transistor.
Image Source: [S. Sordo, Thesis IMSE-US https://idus.us.es/handle/11441/52295]. 25

Radiation Hardness Assurance - RHA
Activities undertaken to ensure that the electronic piece parts placed in the space
system continue to perform according to their design specifications after exposure
to the space environment
From Christian Poivey ‐ ESA
To produce a system tolerant to the radiation environment
26

• Field analysis
– Based on reports of reparations and replacing of components
– When there is enough statistic data the products are obsolete
– It is necessary to spend several years
• Real time tests
– Based on the study of numerous chips running under natural environment
– It is necessary to spend a lot of time and this is very expensive
• Accelerated tests (static or dynamic)
– Based on the simulation of the natural radiation environment (100 years in
a few minutes)
– Adequate method but expensive (NORMATIVAS / ESCC – DLA…)
• It is required to use radiation sources and equipments associated
(particle accelerators, nuclear reactors, radioactive sources as Co60 or
Cs137)
• Laser tests
– Based on photoelectric prompt, try to emulate the particle track
– It is a lower cost experiment
 Development of fault injection emulators
 Faults prevention in the design phase of the devices
Materials and devices testing
They require to be checked by the accelerated tests 27

• The nature of the radiation, energy, flux and fluence of the beam determine
the type of test, which in turn will depend on the structure, design and use
of the device
• The parameters used in the tests will be determined by the flight conditions and
service of the spacecraft or equipment (usually 10-30 years exposure real-time)
Accelerated tests / Irradiation tests
Space and other hostile environments
Irradiation capabilities at the CNA
PHOTONS Low E-IONS & NEUTRONS
28

Cyclotron
• Protons18 MeV
Deuterons 9 MeV
• Lower Energies by
degraders
Possibility to work on air or vacuum
3MV Tandem
• Ions from H to Au
• Proton Energies
550 KeV - 6 MeV
• Differents spot sizes
PHOTONS
60Co Irradiator system
(Gammabeam ® X200, Best
Theratronics)
• Photons energies 1,17 and
1,33 MeV
• Kerma rate up to 160 Gy/h
(September 2019)
Low E-IONS & NEUTRONS
Irradiation capabilities at the CNA
29

• RENASER / RENASER+ / RENASER3 / RENASER4: Análisis integral de circuitos y sistemas
digitales para aplicaciones aeroespaciales (Spanish calls R&D 2007‐2010 ; 2011‐2013; 2016‐2019)
(Total analysis of digital circuits and systems for aerospace applications)
• RADLAB: Laboratorio para Ensayos de Irradiación (Spanish calls R&D‐ INNPACTO 2011/2014)
(Laboratory for irradiation tests)
• PRECEDER: Predicción del Comportamiento Eléctrico de Dispositivos Electrónicos bajo Radiación
(Andalussian calls Proyecto CEI 2020/00000158)
(Prediction of the behavior for electronic devices under radiation applying “machine learning”)
• RADNEXT: RADiation facility Network for the EXploration of effects for indusTry and research
H2020 INFRAIA‐02‐2020: Integrating Activities for Starting Communities EU Project 101008126
The CNA is the Spanish Centre for combined irradiation tests,
implemented as a consequence of the projects:
30

60Co Irradiator system (Gammabeam ® X200, Best Theratronics)
• Photons energies 1,17 and 1,33 MeV
(1,25 MeV average)
• Activity 144 TBq (September 2020)
RadLab Gamma irradiation tests with Co-60
ALTER TECHNOLOGY TÜV Nord S.A.U. / CNA Project RADLAB (IPT-2011-1603-370000), Spanish MICIIN, Subprograma INNPACTO
Square flat radiation fields.
Areas from about 110 cm x 110 cm meet standards homogeneity requirement,
although dose rate nonuniformity ≤ 1% is also available for a wide range of field
size.
Attenuation System allows to obtain different dose rates, over several irradiation field areas, to carry out independent tests,
under different dose rate conditions, simultaneously.
rad(Si)/h
krad(Si)/h
u ≤ 4%
30 rad(Si)/h
420 rad(Si)/h
220 rad(Si)/h
Remote access & staff support
Dynamic study can be checked by user
Step measurements in collaboration
31

Calibration and certification by SSDL PTW-Freiburg.
compliance with TRS-398 and TRS-469 IAEA protocols.
Dosimetry Intercomparison exercises
- Based on ionization chamber; ESA/ESTEC, CNA-ALTER/RadLab and UCL/CRC (2013)
- Based on the study of the filterbox with european, american and russian institutions (2018-2021)
- Based on allanine dosimetry with ESA/ESTEC; SL & TRAD (2020-2021)
Alter Technology agreement
ESCC 22900 and MIL-STD-883/750 test methods 1019
(ISO17025; DLA Lab suitability)
Novelty incoming
Current activity In the frame of PRECEDER Project
Prediction of the behavior for electronic devices
under radiation applying “machine learning”
Objective: to be included in VIRTUAL-LAB
https://www.altertechnology-
group.com/en/news/news-details/article/virtual-lab/
32

Materials & static tests
Optical & Electronic devices
New technologies or applications
Gamma Radiation Effects on HfO2-based RRAM Devices
Shared laboratory
Attenuation System
Different dose rates
simultaneous tests
Thorough dosimetry
study
Exclusive use of laboratory
No attenuation System
RadLab Versatile laboratory
220 rad(Si)/h
SOLARMEMS
IMSE
335 Gy(Si)/h
UCAM
33
Before and after a total
cumulative dose of 22.1 Mrad(Si)
HUVM
0.08-2.5 Gy(Si)/h

Hostile environment Application
Total Ionising Dose (TID) gamma radiation testing of
the lift’s electronics for Tokamak building (ITER project)
The lifts will be exposed up to 25 µGy/h over a lifetime of 25 years.
(Gy) Accumulated Dose (Gy) Total Test Dose

Possibility to carry out temperature cycles while samples are being irradiated.
FACILITY UPDATE IN PROGRESS
Elevated temperature / cryogenic temperature testing
First TID testing with temperatura cycles
(UV AlGaN/GaN Power HEMT / UC3M PUF / ETSI-US QFG MOS)
Dosimetry systems are currently under study
Design and comissioning
(Project CECI – RENASER3)
Compatible system with particles and Ƴ
radiation labs;
in air, in vacuum or another atmosphere.
Current T range from -70ºC to 150ºC (±1ºC)
in the DUT
35
P. Martin-Holgado PhD Thesis
Normalized forward gate current of
GaN HEMTs as a function of total dose
0
500
1000
1500
2000
2500
3000
3500
5000
6000
0
2
4
6
8
10
12
14
16
18
Dose (krad(SiO2))
I
G
/I
G
@0krad
MISHEMT control p-GaN control
MISHEMT @ 400VDS MISHEMT @ 400VDS Average
MISHEMT @ 400VDS/-5VGS MISHEMT @ 400VDS/-5VGS Average
MISHEMT Shorted MISHEMT Shorted Average
p-GaN (All bias) p-GaN (All bias) Average
Ann24h25ºC
Ann168h100ºC

Compact 18/9 Cyclotron (IBA):
 Available quasi-monoenergetic (FWHM 1 – 3 %) 1H+ 18 MeV and 2H+ 9 MeV
 Lower energies are available by using foils degraders (usually 1H+ 16-10 MeV)
 H [LET(Si) ~0.02 - 0.04 MeV-cm2/mg / Range ~700-2000 microns]
 External beam line. (Possibility to couple vacuum chamber)
 Maximum achievable >90% uniform irradiated area at 10 MeV (Ø 3.5 cm)
3 MV Tandem Pelletron (NEC):
• Available quasi-monoenergetic (FWHM 0.2 - 0.03 %) ion beams
• 1H+ [LET(Si) ~0.2 - 0.05 MeV-cm2/mg / Range ~7-300 microns]
• Heavier ions (Range in Si, máximum in the order of tens of microns)
• Neutrons up to 9 MeV by nuclear reaction using >5MeV deuteron as primary beam
 Energy range from ~600 keV to several MeV
(E=(1+q)V; p.e. 600 keV to 6 MeV for H+)
 Different ion beam sizes
Irradiation beam line (usually 1cm2)
Microprobe (beam resolution ~ µm)
 Maximum irradiated área (scanning systems):
Irradiation beam line, 16x20 cm2 (for mE/q2=18)
Vacuum Microprobe line, 2.5x2.5 mm2 (for mE/q2=3)
 Vacuum system (P ~ 10-6 mbar)
 Several opto-electrical feedthroughs
Irradiation tests with LEP, HI and n
Irradiated area uniformity better than 10% Fluence u ~ 10-20%
36

- Scanning system
Double magnetic coils
High stability power supplies
Variable scanning frequency
1cm2 spot scanned up to 20x20 cm2
- Sample holders
- Maximum 20x16 cm2
- X-Y movement
- Complete turnabout
- Heating / Cooling possibility
- Others
- Lighting possibility
- Temperature control
- Opto-electrical feedthroughs
DOSIMETRY
Current integration on sample holder and/or on the
isolated sample holder and/or slits.
This is biased up to 300 volts in order to collect the
secondary electrons
Integration limits the working flux, specially on real
time monitoring
Brookhaven integrator
Flux range: ~ 6 x 1012 to ~ 1 x 108 p/cm2s
Possibilities of different particle detectors
Flux range: < 1 x 107 p/cm2s
First designed for ion implantation (fixed energy, high fluxes and fluences)
Adaptation to irradiation testing (variable energy steps, low fluxes and fluences)
Decrease flux increasing the scanning beam area / defocusing the beam (worse quality beam)
37

Although there is not possibility of scanning, it allows for a diverse range of irradiation
areas by playing with the material of the exit window and the target distance.
EXIT FLANGE
Various sizes available
Internally covered with a 5 mm carbon film to
avoid the activation.
Different graphite collimators with several hole
diameters
Several windows
SAMPLE HOLDER
Remote control (step 0.06 mm)
X 200 mm; Y 200 mm; Z 100 mm
Manual movable structure
DOSIMETRY on device under test (DUT)
Aligned masks and collimators
Control beam spot with scintillator foils and
radiochromic films
Flux monitoring on isolated graphite collimator
Previous calibration
Correlation factors depending on the set-up
ARTE ALTER
INTA
UC3M
38

LEP Space Applications
Proton Energy
Proton Energy
p+cm-2 Fluence
Proton Energy
p+cm-2 Fluence
p+cm-2 Fluence
Proton Irradiation Test on Solar Cells
cables and shielding materials
Usual requirement T<40ºC on the samples; easy reached with prompt flux <1E13 p/cm2
SPASOLAB
p+cm-2 Fluence
39

Irradiation campaign CNA-UCM on COTS SRAM – 65 nm at low bias voltage
TID in RadLab (Cobalt-60)
DR = 750 rad (Si) / h ; TID = 18 krad (Si)
SEE campaign 15 MeV
protons in the 18/9 Cyclotron
Flux 1 x108 p/cm2s
Fluence 1x1010 p/cm2
Estimated TID ~5 krad (Si)
M. Rezaei PhD Thesis
40

Irradiation campaign CNA-UCM on COTS SRAM & FRAM
G.Korkian PhD Thesis
41

LEP Applications; Space, Radiation monitors
Low energy proton direct ionization testing on FPGAs
Single Event Effects (SEE) cross sections
90 & 65 nm
COTS and RADSAGA SRAMs (ESR15)
SRAM <65 nm
MFlux 2E7 – 2E9 p/cm2s
PFlux 8E8 – 3E10 p/cm2s
Tilts (15º/30º/45º/60º)
Fluence 4E8 – 8E11 p/cm2
MFlux 3E4 – 4E8 p/cm2s
PFlux 5E7 – 1.3E11 p/cm2s
Complementary Si diode system (by ChipIR)
MFlux 1.5E2 – 5E5 p/cm2s
Fluence 1.1E6 – 1.2E11 p/cm2
42

SINGULAR EXPERIMENT AT CNA
Proton & neutron irradiation campaigns on the same device
First time in our facility performing both, proton and neutron fault injection campaigns, to evaluate and compare
the different robustness achieved in a microprocessor via different models of hardening software.
Beam Flux
(#/scm2)
Time
(s)
Total
events
Detected
events
Non detected
events
Protons 4.3·108 3718 311 85.2% 14.8%
Neutrons 1.1·106 27360 135 82.2% 17.8%
15.0 MeV protons - CYCLOTRON
Exit window: Mylar® 125 µm; WDD Air 59 cm
Flux uniformity >90% in 15 mm diameter area
Benchmark based on Matrix multiplication (MMULT) with an additional circuit
PDTC to observe and detect microprocessor errors during execution.
DUT on Zybo boards, Zynq-7000 Xilinx FPGA
28 nm technology.
ARM A9 microprocessor core, 650 MHz clock
6.1 to 8.6 MeV neutrons TANDEM 3MV
2H(d,n)3He Reaction
5.48 MeV deuteron primary beam
10 mm diameter focusing
TD1D Air 11 mm; DUT 17mm x 17mm
UC3M/UA/CNA
43

ID & DDD experiments with low energy beams
CMOS Image Sensors
Adaptation to perform microdosimetry
irradiadiation test (static & dynamic mode)
First CNA-SEU experiments with 11 to18 MeV O and C microbeams
CNES
0.5 to 6 MeV H+; 0.5 MeV D
8/11 MeV O; 11 MeV Al; 6/10 MeV C
Another particles applications
ETSI-US
44

APPLICATIONS FOR USE
Previous contact (Yolanda Morilla; ymorilla@us.es) is recommended to know in advance
the test feasibility and to obtain custom budget
The use of CNA facilities requires the approval of the Scientific Committee.
– FILL IN THE CORRESPONDING “BEAM TIME REQUEST”.
The template are available in www.cna.us.es
http://institucionales.us.es/solicitudescna/index.php/en/information-and-documents-for-use-of-accelerators
Facilitates the tedious procedure through your contact
– SEND THE APPLICATION TO solicitudescna@us.es.
Your contact will keep you informed of the procedure progress.
– When the application is accepted, the experiment date is planned according to the user
and depending on the staff and facility availability.
– Usually, the full process is completed in less than two months.
– The current tariffs charged will be a day of using the accelerator/irradiator system
http://institucionales.us.es/solicitudescna/index.php/en/rates
300-600 €/day [24 h (gamma lab); less staff involvement on real time; specific use]
400-1000 €/day [8 h (particle labs); Staff limitations; multidisciplinary use; time limitation]
45

Acknowledgements
Projects PRECEDER-2020/00000158
ESP2015-68245-C4-4-P & IPT-2011-1603-370000
To the users and collaborators from public institutions and private companies
Your requirements are our improvements !!!
46

El CNA como centro de ensayos de irradiación dentro de una ICTS interdisciplinar.

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