IBA from an old U-120 Cyclotron to a new 3 MV TANDETRON- a Real

Challenge

Dorin Dudu, Ofelia Muresan, Herman Schubert, Ion Vata

DFNA-Cyclotron NIPNE

(New Experiments and ideas for the 3 MV TANDETRON )

Long-term Goal New, modern R&D vision in Surface Sciences and

Technology by:- New basic and applied researches in Astrophysics, Life,

Environment ,Earth, Archaeology Sciences and last but not least Industry/Technology

- New approach in using Ion Beams in characterization of nanostructured materials

- On line and off line measurements of the modifications produced by irradiation

Increase the national/international attractiveness and visibility of our Institute, offering the 3 MV Tandetron as a interesting R&D infrastructure

Development certified analytical services using nuclear methods:

Cheaper analysis More customers and users Increase beam time (the degree of occupation) Improve the economical efficiency

Customers and Users

There are two kind of customers and users: Local customers and users and external

customers and users Local customers and users: - are familiarized with the IBA experiments - have not possibilities to prepare “interesting”

samples The external customers and users are not very

well familiarized with IBA methods but THEY are preparing samples and being interested in characterization of the results of applied technologies

The “parts” must be interested in collaboration

Customer needs/requirements

We cooperated with scientists involved in nanotechnologies and new material discovery/ production and we observed that they are interesting for:

Chemical stoichiometry samples Element identification Layered samples structures (depth profile):

- order and thickness, in μm-nm range;- chemical composition;- interfaces resulted as effect of the diffusion, migration or implantation of some ions)

To not deteriorates the samples To have comparative studies on the same sample To identify the effect of technological procedures ( thermal

annealing, etc)

Exemples of Fulfilling Customer Needs at U-120 Cyclotron

We implemented a dedicated infrastructure for RBS at U-120 Cyclotron and methods aiming to enlarge the analytical possibilities:

STOICHIOMETRY (composition) determination - Materials with form memory - Optical fiber Thickness of layers measurements -Hard nano-structured coatings (superlattices) - Structured thin deposition possible to be used in

fusion experiments - Thin magnetic material ( spin valves) - Thin and thick PZT or BZT amorphous composites Depth profiling of composition - Implanted samples - Interfaces at the borders of different layers

Implementation of a dedicated infrastructure for IBA at U-120 Cyclotron

Accelerated beams at U-120 Cyclotron for IBA

Beam line and reaction chamber (End station) with spectroscopic chains and acquisition data system

Dedicated software for experimental data processing and simulations and etalons and references used for checks and calibration

Accelerated beams at U-120 Cyclotron for IBA

Particle/Energy[MeV]

Intensity on target [μA] Transversal section Application

/2,7-5 0.01-1 1-30mm2 RBS, PIXE, analysis and controlled changes and defects induced by particles irradiation

d/1,3-2,5 0.01-1 1-30mm2 RBS , NRA analysis

14N+ (2+)/4-10 0.01-0,1 1-30mm2 RBS , ERDA analysis

Beam line and reaction chamber -Old Ortec and new NEC RC41 End station

for IBA

Five axes goniometer Micron deplacement Minutes rotation

Many samples holder system and canal lock PC based application for movement, acquisition and data analysis

Dedicated software for experimental data processing/simulations and etalons/reference samples

2000 2025 2050 2075 2100 2125 2150 2175 2200 2225 2250 2275 23000

1000

2000

3000

4000

5000

6000

7000

8000

9000

Y A

xis

Title

X Axis Title

238Pu241Am

5105,5keV

5156,6keV

5442,8keV

5485,6keV

Thin radioactive source of 238Pu241Am for calibration of SSB detector and spectroscopic chain

SIMNRA software for analyzing samples

AuCrSi_repetat0grd.txtSimulated

Channel1,1001,0501,000950900850800750700650600550500450400350300250200150100500

Cou

nts

3,200

3,000

2,800

2,600

2,400

2,200

2,000

1,800

1,600

1,400

1,200

1,000

800

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200

0

200 400 600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800

Energy [keV]

Au Cr Si

100nm 16nm > 300μm

Dedicated software for experimental data processing/simulations and etalons/reference samples

Certified etalon of 5+4 alternative layers of 56 nm Cr and Ni, having the same thickness of layers with 2% precision, deposited on Si

[Red: experimental data, Blue: simulated data for deduced parameters.]

Concern for infrastructure and methods developments aiming to enlarge the analytical possibilities

In order to extend the field of IBA’s, we have been looking for possibilities to achieve micro beams with our cyclotron introducing a conical glass capillary (up left) into the beam line, we could achieve micro beams with reasonable intensities and acceptable quality (Energy spread, divergence etc.).

Analyzing the RBS spectra of a 50nm gold foil on Al with and without glass capillary substrate results than:-initial energy and energy dispersion is conserved;-app. 15% of the output beam has an energy loss or energy degradation from the initial energy going at energies of less than 100keV

STOICHIOMETRY (composition) determinationused as technological support - materials with form memory -

P1 netratata.datSimulatedC TiNiNb

Channel1,1001,000900800700600500400300200

Cou

nts

4,800

4,600

4,400

4,200

4,000

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0

600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600

Energy [keV]

Nb

Ni TiC

P1 netratata.datSimulatedC TiNiNb

Channel1,1001,000900800700600500400300200

Coun

ts

4,800

4,600

4,400

4,200

4,000

3,800

3,600

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Energy [keV]

NETRATAT SimulatedC O

Channel1,7001,6001,5001,4001,3001,2001,1001,000900800700600500400

Cou

nts

1,350

1,300

1,250

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950

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0

1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 3000 3200 3400 3600 3800 4000

Energy [keV]

O O C

Nr. strat

Grosime Compoziţie

1 90nm C -65%O -35%

2 ∞* Ti -47%Ni -43%Nb -10%

TRATAT cu DeuteroniSimulatedC O TiNiNb

Channel1,2501,2001,1501,1001,0501,000950900850800750700650600550500450400350300250200150100500

Coun

ts

580

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Energy [keV]

P2 (P1 după tratament)

NRA analysis of the sample before and after a thermal annealing shows a strong (app. 300nm) migration of C (contaminant) below the surface.

STOICHIOMETRY (composition) determination-optical fiber with microbeam-

Stoichiometry measurementMicrobeam

GlassSimulatedO SiClCaMnCuAgYb

C hannel370360350340330320310300290280270260250240

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nts

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Energy [keV]

Si0.6638O 0.33C a0.00486C r0.0006C u 0.0005Y b 0.000045

Thickness of layers measurements

0 50 100 150 200 250 3000

10000

20000

30000

40000

Semnale pentru Si

Semnale pentru Ti de aderenta Semnale pentru Zr

Nr.

even

imen

te

Energie [10keV/can.]

exp. sim.

?

RBS cu He+ la 2,7MeV pentru proba P3

P6_30grd_Azot2_23_05_06.txtSimulated

Channel800750700650600550500450400350300250200150100500

Coun

ts

1,4001,3501,3001,2501,2001,1501,1001,0501,000

950900850800750700650600550500450400350300250200150100500

400 600 800 1000 1200 1400 1600 1800 2000

Energy [keV]

30o

RBS cu N la 3MeV pentru proba P3

65o

45o

5x2straturi Zr(C)N/Ti(C)N

ZrN ZrCN

TiN TiCN

ZrN ZrCN

TiN TiCN

d1 d2 ~400nm ~300μm

Ti Si (substrat)

Strat de aderenţă

Measurement of the layers thickness for nano-layered samples : d1, d2 =15-20nmusing ions of He and N

Thickness of layers measurements-spin valves-

Using the simulating program SIMNRA vs. 6.05, the following structure for (a) was obtained: Mo0,9O0,1/Fe0,25Co0,35O0,4 /Cu1,0/ Fe0,30 Co0,65O0,05

/Fe0,25Mn0,75/ Mo0.9 O0.1/Si0,33 O0,67 on Si substrate with the corresponding layer thicknesses: 4[nm]/5,5[nm]/12,2[nm] /6[nm]/18[nm]/10[nm]/32[nm]/∞

By the same procedure, the elemental composition for (b) was established as: Mo0,9O0,1/Fe0,5Co0,5/Cu1,0/Fe0,4 Co0,6/Fe0,7Mn0,3/ Cu0,9O0,1 on Si substrate with the thicknesses of the layers being: 3[nm]/4[nm]/6[nm]/14[nm]/15[nm]/7[nm]/ ∞

p4 herez 60grd.datSimulatedO SiMnFeCoCuMo

C ha nne l700650600550500450400350300250200150100

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E ne rg y [k e V]

p3he_70grd bis.datSimulatedO SiMnFeCoMoIrAu

Channel700680660640620600580560540520500480

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Energy [keV]

ZrN_TiN_1run.datSimulatedN O SiTiZrAgIn

Channel1,000900800700600500400300

Cou

nts

1

10

100

1,000

800 1000 1200 1400 1600 1800 2000 2200 2400 2600

Energy [keV]

Element identification-sample containing N, O, Si,Ti,Zr,Ag,Ir-

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Channel

P4 experimental P4 simulated C O Si

C on surface

Buried O

0 50 100 150 200 2500

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nts

Channel

experimenta simulated C O SiC on surface

Buried O

O on surface)(FFmO

11

1

)Si(Si

)SiO(Si

HH

F

Depth profiling of element concentration-Oxygen implanted in Si-

0 50 100 150 200 250 300 350 400 450 500 550 600 650 700 750 8000.0

0.1

0.2

0.3

0.4

0.5

Con

cent

ratia

de

O in

Si

Adancimea fata de suprafata probei [nm]

Conc.OinP5 Conc.OinP4

323nm

323nm

51nm

Depth profiling of implanted O in Si before and after thermal annealing shows a 50nm migration of O layer toward inside of bulk Si

Depth profiling of element concentration-interfaces structures-

Substrat netratat.txtSimulatedSiTiPt

Channel1,000900800700600500400300

Coun

ts

19,000

18,000

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Energy [keV]

Substrat tratat.txtSimulatedO SiTiPt

Channel1,000900800700600500400300

Cou

nts

10,000

9,500

9,000

8,500

8,000

7,500

7,000

6,500

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Energy [keV]

Buffer layer Pt100nm /Ti20nm /SiA) Sample as depositedB) PtTiSi interface after annealing at 800oC

BA

Depth profiling of element concentration-interfaces structures-

Ti on Si deposition by magnetron sputtering (buffer layer) analysis:

- RBS spectrum shows an non uniform concentration of deposited Ti layer. For a good fit with simulated spectrum, was necessary to involve 4 sublayers of TiNO of app. 68nm thickness with different stoichiometry.

- This result suggest the influence of residual gases inside deposition chamber which are combining with Ti ions from produced plasma.

RBS405025.datSimulated

Channel400380360340320300280260240220200180160140120100806040200

Cou

nts

40,000

38,000

36,000

34,000

32,000

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26,000

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22,000

20,000

18,000

16,000

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0

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Energy [keV]

1 2 3 40

102030405060708090

100C

once

ntra

tii [%

]

Strat

Ti N O

New Fields and new possible experiments/applications at the 3 MeV tandetron

New possible experiments/applications at the 3 MV tandetron

Channeling of ions into crystalline structures is a powerful tool to inspect the disorder in crystals as well as to find and locate the position of impurities in crystals. Also, in crystalline heavy matrices, channeling technique allow the measurement of light elements (C, O, N) impurities Complex simultaneously/successive IBA methods aiming a better characterization of a large class of samples (RBS, PIXE, PIGE, NRA, HIRBS).Microbeam scanning of surface micro-structured samples:

New possible experiments/applications at the 3.5MeV tandetronStudies of beams scattering at large grazing angles on amorphous and crystalline samples (studies of phenomenon which occur in focusing effect of tapered glass capillaries and so called “surface channeling of ions”). In this way it is possible to obtain in a simple way “nano-beams” for analytical applications. The existing beam line dedicated for implantation of ions in solid open exciting ways for collaborative R&D applications: - nanocavities layers induced by different ions ions implanted in semiconductors acting as getter for metallic impurities and silicon nanocrystals embedded in silicon dioxide which exhibit a strong room temperature luminiscence

XTEM images showing the microstructure and disorder around bubbles and nanocavities in Si following 100 keV H implantation to a dose of 3x1016 cm-2 and annealing to a) 500oC and b) 750oC.

a) RBS Au profiles both as-implanted and after 850oC annealing for an 8x1014 Au cm-2 implant into Si that has a cavity band at a depth of 1μm. b) An XTEM micrograph of the cavity band region after annealing.

Ion irradiation for cell surgery with glass capillaryY. Iwai et al., Appl. Phys. Lett. 92 023509 (2008).

Strengths and Advantages

Very good parameters of the accelerated beams (energy stability and resolution, micro beam facility), easy handling (computer controlled of the accelerator and beam transport)

Possible use of simultaneous methods (RBS, PIXE, NRA, PIGE)

Large number of ion species being accelerated

Dedicated beam line for complex Ion Beam Analysis

Dedicated beam line for ion implantation

Existing experience in IBA applications at IFIN-HH

Important national/international teams involved in material sciences can have benefits of this R&D infrastructure for IBA as a powerful tool for more complete characterization of sample as composition and structure

Thank You for Your attention