Experience of MeV Electron Beam Application for In Situ Studies of - - PowerPoint PPT Presentation

Experience of MeV Electron Beam Application for In Situ Studies of Solids

Yuri Petrusenko

petrusenko@kipt.kharkov.ua

NATIONAL SCIENCE CENTER Kharkov Institute of Physics & Technology

“CYCLOTRON” Science & Research Establishment Kharkov, Ukraine

Ivan Neklyudov Alexander Bakai Oleksandr Astakhov Valeriy Borysenko Dmitro Barankov Vladimir Gann Igor Michailovskij

Forschungszentrum Juelich, Germany

Rainer Hoelzle Reinhard Carius Fridhelm Finger

Hahn Meitner Institut Berlin, Germany

Mikhael-Peter Macht,, Crystian Abromeit Nelly Wanderka

Co-operation:

NATIONAL SCIENCE CENTER Kharkov Institute of Physics & Technology

National Science Center “Kharkov Institute of Physics & Technology”

Kharkov, Ukraine www.kip.kharkov.ua

National Science Center Kharkov Institute of Physics & Technology

Found – in 1928 Staff – 2500

Institutes:

• Institute of Solid State Physics Materials

Science & Technologies

• Institute of Nuclear Physics
• Institute of Plasma Physics
• Institute of Plasma Electronics & New Methods
• f Accelerating
• Institute of Theoretical Physics

Accelerators – more then 15

“CYCLOTON” Science & Research Establishment

Status: Center of Joint Use of Accelerator Facilities

Permanent staff: 17 (now) / up to 31 Basic facilities:

• ELIAS electrostatic accelerator

(High Voltage Corporation, USA)

• Compact Cyclotron CV-28

(The Cyclotron Corporation of Berkeley, USA)

Parameters of “ELIAS” accelerator

20 кW Power consumption

1x10-7 mbar

Vacuum in the electron beam line 0.1 cm Diameter of electron beam (with focusing), for 90% capacity 1.0 сm Diameter of electron beam (without focusing) 10-4 radian Electron beam disperse up to 500 µА Maximum beam current (with scanning) 0.5-150 µА Beam current (without scanning) 0.5- 3.0 MeV Energy of accelerated electrons

Values Parameters

Irradiation with MeV electrons

• Coulomb scattering of electrons by nuclei takes place,

and recoil atoms appear: Tmax(E) = E * (E +E0) * 2 / ( A * mp c2)

(E0 = me c2, me – electron mass, mp – proton mass)

• Damage cross-section:
• Damage production (dpa):

D = σD*Ф

(Ф –electron fluence)

∫

ν σ = σ

) (

max

) ( ) , ( ) (

E T E D

d

dT T dT T E d E

“ELIAS” electrostatic accelerator

as precise generator of point defects in solids

(E = 0.5 -3.0 MeV)

“ELIAS” Accelerator

Critical current and vortex pinning in high-Tc single crystals irradiated with MeV eltctrons

• Whether point defect are effective pinning centers ?
• A.V. Bondarenko, A.A. Prodan, Yu.T. Petrusenko et al. Phys. Rev. B (2001) 64, 092513.
• Yu. T. Petrusenko and A. V. Bondarenko, Pinning and dynamics of vortices in YBaCuO

crystal in magnetic field applied in vicinity of the ab-plane, to be published.

• Yu. T. Petrusenko and A. V. Bondarenko, Interplay of point and planar defects in the

formation of phase state and dynamics of vorties in YBa2Cu3O7-δ crystals, to be published

• Experimental
• Samples: High-quality YBaCuO single crystals, Tc ≈ 93 K.
• Irradiation: 2.5 MeV electrons a liquid helium cryostat at

temperatures T ≤10 K at doses up to 3x1018 el/cm2.

• temperature range for operation from 10 to 400 K.
• magnetic field up to 6T.
• accuracy of temperature control and regulation 0.005 K.
• a goniometric sample holder to rotate the crystals with

respect to the vector of the magnetic field.

• Technique: Current-voltage characteristics measured by

dc-resistivity method.

10 20 30 40 50 60 70 80

0.5

0.4 0.3 0.2 0.1

2.0 3.1 1.2 Fluence x10

18 el/cm 2

YBa2Cu3O7-X single crystal T=77 K , anglH,ab=14

• , H=1.5 T

Current density , kA/cm

2

E , mV/cm

1x10

18

2x10

18

3x10

18

5 10 15 20 25 30 35

86 K 83 K 79 K 77 K

Fluence , el / cm2 Jcirr / Jco , arb. un.

• Conclusion

It has been first demonstrated that point defects generated by the ~MeV electron beam are the effective pinning centers of magnetic vortices in high-Tc crystals, and this determines a substantial rise in the critical current density in irradiated superconductors.

“ELIAS” Accelerator

• Point Defects and Recovery Kinetics

in Irradiated Bulk Metallic Glasses

• Yu. Petrusenko, A.Bakai, I. Neklyudov,et al.,VANT, No 2, (2008).
• Yu. Petrusenko, A. Bakai et. al., Mater. Res. Soc. Symp. Proc. Vol. 1048 (2008).
• Yu. Petrusenko, A. Bakai, et. al., Proc. 6th Int. Conf.on Bulk Metallic Glasses (2008).
• Yu. Petrusenko, Proc. 5th Int. Conf. on Advanced Materials and Processing (2008)

The problem of structural properties and structural defects of amorphous solids is still of vital importance. To make clear whether stable point defects exist in metallic glasses (MGs), we have studied the accumulation and recovery kinetics of radiation defects in ZrTiCuNiBe and ZrTiCuNiAl bulk MGs irradiated with 2.5 MeV electrons at T ~ 80 K.

• Experimental
• The method: - low-temperature electron irradiation
• isochronal annealing
• electrical resistance measurements
• Samples:

amorphous alloys, Zr41Ti14Cu12,5Ni10Be22,5

• Zr52.5Ti5Cu17.9Ni14.6Al10,
• 0.05 mm in thickness, prepared by the spinning method
• Irradiation:

2.5 MeV electrons at ELIAS electrostatic accelerator

• Maximal exposed dose 7.5x1019 e-/cm2

Temperature of irradiation Tirr ~80 K.

• Isochronal annealing: temperature range 85-300 K, 10 K step
• Electrical resistance measurements: at T= 80.5 K by precise

fore-probe method, accuracy - 5 ppm

• Dependence of total and partial displacement damage cross-

sections on electron energy for Zr52.5Ti5 Cu17.9 Ni14.6 Al10

0,0 0,5 1,0 1,5 2,0 2,5 3,0 5 10 15 20 25 30 35 40

s

(Al)

s

(Ni)

s

(Ti)

s

(Zr)

s

(Cu)

e > Zr52.5Ti5 Cu17.9 Ni14.6 Al10

σD, s

(i), barn

E, MeV

• Dependence of total and partial displacement damage cross-

sections on electron energy for Zr46.8Ti8.2Cu7.5Ni10Be27.5

0,0 0,5 1,0 1,5 2,0 2,5 3,0 5 10 15 20 25 30

s

(Be)

s

(Ti)

s

(Ni)

s

(Cu)

s

(Zr)

e --> Zr46.8Ti8.2 Cu7.5 Ni10 Be27.5 σD , s

(i), barn

E, MeV

Dose dependences of relative electrical resistance for ZrTiCuNiBe and ZrTiCuNiAl irradiated with 2.5 MeV electrons at 85 K.

20 40 60 80

0,9992 0,9994 0,9996 0,9998 1,0000 1,0002 1,0004 1,0006 1,0008 1,0010 1,0012 1,0014 1,0016

ZrTiCuNiAl ZrTiCuNiBe D, x10

18 e

• /cm

2

Rirr/R0

Recovery of irradiation-induced resistance of ZrTiCuNiBe irradiated with 2.5 MeV electrons at 85 K to dose 7.5x1019 e-/cm2.

50 100 150 200 250 300 20 40 60 80 100

100-(Rirr-Rann)/(Rirr-Ro) , % Tann , K

Recovery of irradiation-induced resistance of ZrTiCuNiAl irradiated with 2.5 MeV electrons at 85K to dose 7.5x1019 e-/cm2

50 100 150 200 250 300

• 180
• 170
• 160
• 150
• 140
• 130
• 120
• 110
• 100
• 100-(Rirr-Rann)/(Rirr-Ro)

Tann , K

Recovery spectrum of irradiation-induced resistance for ZrTiCuNiBe irradiated with 2.5 MeV electrons at 85 K to dose 7.5x1019 e-/cm2.

50 100 150 200 250 300

• 1,0x10
• 6

0,0 1,0x10

• 6

2,0x10

• 6

3,0x10

• 6

4,0x10

• 6

5,0x10

• 6

dR / dT Tann , K

Recovery spectra of irradiation-induced resistance of ZrTiCuNiAl irradiated with 2.5 MeV electrons at 85K to dose 7.5x1019 e-/cm2

50 100 150 200 250 300

• 1,0x10
• 6
• 5,0x10
• 7

0,0 5,0x10

• 7

1,0x10

• 6

1,5x10

• 6

2,0x10

• 6

2,5x10

• 6

dR /dT Tann , K

Effective activation energies of recovery stages for ZrTiCuNiAl and ZrTiCuNiBe bulk metallic glasses irradiated with 2.5 MeV electrons (Estimated data)

• ZrTiCuNiBe:

E150K = 0.46 eV

• E225K = 0.69 eV
• ZrTiCuNiAl:

E135K = 0.40 eV

• E225K = 0.69 eV

A fragment of the 2-D polycluster Intercluster and inner boundaries are shown. • -regular sites, circles with dot are coincident sites, semicircles with dot are noncoincident sites

Field ion microscopy image of the intercluster boundaries of the bulk metallic glass Zr41Ti14Cu12,5Ni10Be22,5

A.S. Bakai et al. JETP Letters, 76 (2002) 218

(a)

Subclusters

(b) FIM images of bulk ZrTiCuNiBe alloy, obtained in result of field evaporation (а) and stimulating field etching in hidrogen (b)

The autoelectronic evaporation image of the Zr41Ti14Cu12,5Ni10Be22,5 bulk metallic glass

The evaporation field energy along the shown cross-section

• It is seen that the width of the intercluster boundary is

nearly 1nm, while the binding energy of atoms within the boundaries is on 0.13-0.43 eV less than in the cluster bulk

5 10 15 20 25 0,0 0,2 0,4 0,6 0,8 1,0 1,2 1,4

∆Q/Q x10

2

L,í ì

Sinks of point defects

• Intercluster boundaries are the most probable

sinks of the point defects.

• The cluster sizes are varying from 5 to 10 nm.
• The density of the point defects sinks is rather

high, up to 10-2 per atom.

• CONCLUSIONS:
• Point defects are stable in metallic glasses and

the defect mobility is a thermally activated process.

• Activation energies of recovery processes in

metallic glasses are lower than migration energy of vacancies in crystals.

• Structural model of densely random-packed

spheres or free volume model is irrelevant to bulk metallic glasses investigated;

• The results are in accord with the polycluster

structure of bulk metallic glasses.

Effect of Electron Irradiation on the Newest BMGs

(under study)

• NATIONAL SCIENCE CENTER

Kharkov Institute of Physics & Technology

• UNIVERSITY OF TENNESSEE

Department of Materials Science & Engineering BMGs:

• Ti 41.5 Zr 2.5 Hf 5 Cu 42.5 Ni 7.5 Si 1
• (Z 55 Al 10 Ni 5 Cu 30) 0.99 Y1
• (Cu 55 Zr 40 Al 5) 0.98 Er 2
• Fe 75 Mo 5 P 10 C 7.5 B 2.5

??? (very brittle)

Testing conditions for materials studies:

• Atmosphere or vacuum conditions
• Compression or tension deformation
• Deformation rates 0.01 – 4.5 mm/min
• Temperature range 77 -1300 K

Possibilities for materials studies:

• Static load (tension - compression deformation) +

ultrasonic pulse impact

• Effect of acoustic softening (ultrasonic amplitude)
• Ultrasonic fatigue properties
• Ultrasonic pretreatment at different temperatures and

time

“ELIAS” Accelerator

The Role of Defects in the Electronic Transport in Thin Film Silicon

• O. Astakhov, Y. Petrusenko, et al. J. Non-Cryst. Solids 352 (2006) 1020.
• O. Astakhov, R. Carius, Yu. Petrusenko et al., Mater. Res. Soc. Symp. Proc. 989 (2007)
• O. Astakhov, R. Carius, Yu. Petrusenko, et al, Physica Status Solidi-RRL 1 (2007) R77.
• O. Astakhov, F. Finger, R. Carius, et al, Thin Solid Films 515 (2007) p. 7513.
• O. Astakhov, R. Carius, A. Lambertz, et al, J. Non-Cryst. Solids 354 (2008) 2329

Material for cheap production:

• Large area electronics
• Photovoltaics
• Photosensors
• Thin Film Transistors (TFT displays)
• Defects strongly affect the quality of devices
• In order to improve devices quality the nature of

defects and their role is investigated

• Electron bombardment – a tool for the defect

density manipulation

a-Si:H and µc-Si:H

NSC KIPT FZJ-IPV

Sample preparation Investigation

ESR (40-300К) Dark and photoconductivity Spectral absorption, etc.

Irradiation Transportation at 77 K Transportation E=2 МэВ е- J=5мкА*сm-2 Tirr ~80 K Dmax=1019е*сm-2

Reloading

at 77К Test measurements µс-Si:H – materials for solar cell, photosensors and large scale electronic device production

Deposited Irradiated 50

• C

80

• C

120

• C

160

• C

10

15

10

16

10

17

10

18

10

19

µc-Si:H

NS (cm

• 3)

e-

Deposited Irradiated 50

• C

80

• C

120

• C

160

• C

a-Si:H

e-

Treatment

2.02 2.01 2.00 1.99

Annealed Deposited

ESR intensity g-value

Irradiated

Spin density NS in as-deposited material (black circles) and NS after irradiation (black stars) as a function of silane concentration (SC=SiH4/SiH4+H2). The ratio NS Irr/NS Dep is shown with triangles.

Conclusions:

• Effective use of low-temperature electron irradiation as a

method of increasing the defect density in thin-film silicon without changing its microstructure.

• Extraction of the effects solely related to the defects in the film
• Reversible increase of the defect density three orders of

magnitude.

• observation of the bright effects
• extraction of the hidden features and properties of defects
• Elucidation of the role of defects in electron transport in Si-films
• The results are of importance for improving the silicon-

based thin-film device production technology.

Primary defect production and recovery process in binary Zr- based alloys

(Zr-Sc, Zr-Y, Zr-Gd, Zr-Dy, Zr-La)

“ELIAS” Accelerator

Recovery of irradiation-induced resistance for Zr-based alloys irradiated with 2 MeV electrons at ~80K to fluence 1.4x1019 e-/cm2

100 150 200 250 300 350 10 20 30 40 50 60 70 80 90 100

∆ρ(T)/∆ρo, %

T, K Zr Zr-Sc Zr-Dy Zr-Y Zr-Gd Zr-La

Recovery spectrum of irradiation-induced resistance for Zr-based alloys irradiated with 2 MeV electrons at ~80K to dose 1.4x1019 e-/cm2

100 150 200 250 300 350 0,0 0,5 1,0 1,5 2,0

• d[(∆ρ(T)/∆ρo]/dT, % K
• 1

T, K Zr Zr-Sc Zr-Dy Zr-Y Zr-Gd Zr-La

Conclusions:

• Alloying atoms of rare earths have been

found to interact effectively with point defects in the zirconium matrix.

• The observed processes effects on

annihilation and redistribution of radiation defects and, therefore, must be taken into account in the development of radiation- resistant zirconium-base alloys.

Compact Cyclotron CV-28

(The Cyclotron Corporation of Berkeley, USA)

Compact Cyclotron CV-28

100 мкA 50 мкA 10 мкA 8 – 28 MeV

4He++

150 мкA 70 мкA 15 мкA 5– 36 MeV

3He++

500 мкA 100 мкA 100 мкA 3 – 14 MeV D+ 500 мкA 70 мкA 70 мкA 2 – 24 MeV H+ Internal Current External Current at Maximum Energy External Current at Minimum Energy Beam Energy Range Particles

Switching magnet

Damage parameters for Cyclotron’s ions

~ 50 dpa ~10-3 dpa/sec 50мкA 28 MeV

4He++

~10 dpa ~2x10-4 dpa/sec 50мкA 36 MeV

3He++

~5.0 dpa ~10-4 dpa/sec 50 мкA 14 MeV D+ ~0.25 dpa ~5x10-6 dpa/sec 50 мкA 24 MeV H+ Max Dose Max Dose Rate Average Current Max Beam Energy Particles

“Neutron source ”

based on Compact Cyclotron CV-28

(Thick target Be source)

9Be(d,n)10B

D+ beam Be target ~MeV neutrons

Max Flux Density ~1012 n/cm2sec Max Neutron Dose ~ 1017 n/cm2

(for D+ Beam Energy -14 MeV, Beam Current -100 mkA)

Compact Cyclotron CV-28

Future studies:

• The processes of radiation damage in constructive

materials for nuclear power plants.

• Investigation and production of isotopes for

medical and industrial applications.

• Development and testing of neutron detectors.
• Element analysis.
• Neutron effects on biological materials.
• etc.

WELCOME

for realization of joint Projects