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Helium Retention Studies in Tungsten S. Gilliam a , S. Gidcumb a , N. Parikh a , J. Hunn b , L. Snead b , R. Downing c a University of North Carolina at Chapel Hill, Chapel Hill, NC 27599-3255, USA b Oak Ridge National Laboratory, P.O. Box 2008, Oak Ridge, TN 37831-6138, USA

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slide1
Helium Retention Studies in Tungsten

S. Gilliam a, S. Gidcumb a, N. Parikh a, J. Hunn b, L. Snead b, R. Downing c

a University of North Carolina at Chapel Hill, Chapel Hill, NC 27599-3255, USA

b Oak Ridge National Laboratory, P.O. Box 2008, Oak Ridge, TN 37831-6138, USA

c National Institute of Standards and Technology, Gaithersburg, MD 20899-3460, USA

HAPL Meeting, ORNL, March 22, 2006

Ion Beam Materials Analysis and Modifications Group

University of North Carolina at Chapel Hill

slide2
IFE Reaction Chamber

Tungsten

He

DT pellet

Helium threat spectrum most damaging of all ionic debris

First wall temperature ~850°C with periodic spikes to ~2500°C

slide3
Energy spectrum of slow debris ions in the IFE reactor

# of ions vs. energy (keV)

UCSD ARIES program on fusion energy technology

J. Perkins, http://aries.ucsd.edu/aries/wdocs/aries-ife/spectra/

slide4
Energy spectrum of fast ions in the IFE reactor

# of ions vs. ion energy (keV)

UCSD ARIES program on fusion energy technology

J. Perkins, http://aries.ucsd.edu/aries/wdocs/aries-ife/spectra/

slide6
Previous studies with monoenergetic helium

SEM of blistered tungsten

Implanted helium is trapped and accumulates to form stable bubblesBubbles grow until the pressure blisters the surface

1.3 MeV 3He implanted at 850°C to a dose of 2 x 1021 He/m2 followed by a flash anneal at 2000°C

slide7
NDP

Neutron Depth Profiling

Si detectors

Technique: Neutron Depth Profiling (NDP) measures elemental concentration profiles up to a few micrometers in depth for elements that emit a charged particle following neutron capture. (R.G. Downing, et al., NIST J. Res. 98 (1993)109.)

Elements Analyzed: boron, lithium, helium, nitrogen and several additional light elements with less sensitivity.

Sample Environment: In an evacuated chamber, samples are irradiated with a beam of low energy neutrons. A small percentage of the emitted reaction particles are analyzed by surface barrier detectors to determine their number and individual energies.

Principles: The emission intensity is compared to a known standard to quantitatively determine the elemental concentration. The emitted particles lose energy at a predicable rate as they pass through the film; the total energy loss correlates to the depth of the reacting nucleus.

Advantage: NDP is non-destructive. NDP analysis allows repeatedly determinations of the sample volume following different treatments.

Neutron beam flux at sample: ~7.5x108 n/cm2-s

Beam area: from a few mm2 to ~110 mm2

Neutron monitor

Neutron

q

Sample

beam

NDP Experimental Arrangement

1e22

1e20

1e18

1e16

1e14

1e12

NDP of boron in silicon

Depth range: 15 nm – 3.8 µm

XRF

FTIR

RBS

NDP

Detection limit (at/cm3)

TOF-SIMS

TXRF

Dynamic SIMS

1000 Å 1µm 10 µm 100 µm 1 mm 1 cm

Sample Dimension

slide8
Neutron Depth Profiling

Neutron Reactions of Merit

slide9
3He(d, p)4He nuclear reaction analysis

Tungsten Target

780 keV deuterons

3He profile

depth = 1.7 m

~13 MeV protons, ~2 MeV alphas, backscattered deuterons

12.6 m Mylar foil

Preamplifier

Amplifier

MCA

1500 m depletion depth

detector at 155 with respect

to the incident beam direction

  • Used proton yield from the reaction to compare helium retention
slide10
Less retention with cyclic implantation and annealing

Implanted 10193He/m2 at 850°C followed by a flash anneal at 2000°C

Same total dose was implanted in 1, 10, 100, and 1000 cycles of implantation and annealing

Relative 3He retention for single crystal and polycrystalline tungsten with a total dose of 1019 He/m2. Percentage of retained 3He compared to implanting and annealing in a single cycle.

slide11
Current project objective
  • More accurately mimic the IFE reactor conditions to study effects of helium irradiation on the first wall.
  • Produce the IFE helium threat spectrum and implant tungsten samples
how do we produce a helium threat spectrum
How do we produce a helium threat spectrum?

Degrade the monoenergetic beam by transmission through a thin Al foil

Tilting a single foil provides a range of degraded energies by varying the path length d through the foil material where  = 0° is normal incidence

Foil

Tungsten

E0 He beam

E = E0 – Efoil

t

Transmitted energy is approximated as a Gaussian centered at Ei = (E0 – Efoil)and broadened by the energy straggling through the foil 

slide13
Approximating the threat spectrum

Helium threat spectrum is approximated as a function f(E)

Approximate f(E) as a linear combination of the Gaussian degraded energieswhere f(Ej) is a point on the profile, wij is a weighting coefficient, Gi is the ith Gaussian contribution to the jth point on the profile f(E)

computing the solution
Computing the solution

Many of the matrix elements will be zero because Gaussians far away from Ei won’t contribute to the point f(Ei)

Weighting coefficient matrix elements correlate the Gaussians to each other

Diagonalize W to find the weight for each individual Gaussian function so that the linear combination approximates the desired energy spectrum f(E)

Weighting coefficients determine the dose to implant and each Gaussian has an associated tilt angle

Assuming a constant beam current, then dose  timeTherefore, we have tilt angle  vs. time

Apply a polynomial fit to this  vs. t plot and use the time derivatives (i.e. angular velocity and acceleration) to program the tilt position motor

slide15
2.5 MV Van de Graaff

Scattering Chamber / Electronics

Control Panel / Bending Magnet

Energy degrader foil and sample holder

energy degraded 3 he implantation
1.8 MeV He beam transmitted through Al foils ranging 1.5 to 5.5 microns thickDegraded energies: 1400 – 100 keVAl stopping power: ~300 keV/micron

Compare theoretical and experimental values of Efoil and  through foils

Implanted tungsten samples with 1.8 MeV 3He degraded by various foil thicknesses listed below. Dose was 1 x 1020 He/m2 for each sample.

Energy degraded 3He implantation
e foil and from neutron depth profiling
Efoil and  from Neutron Depth Profiling
  • NDP uses 3He(n, p)T reaction to measure the helium depth profileNumber of protons is proportional to helium concentrationDetected proton energy converted to depth scale by energy loss
  • Projected range Rp and the longitudinal straggle Rp related to Efoil and 

Tungsten

neutrons

Rp

protons

Helium

Rp

Helium depth profile for tungsten implanted with 1.3 MeV 3He to a dose of 1020 He/m2

slide20
Efoil and  from Rutherford backscattering

Backscattering used to measure energy straggling through foils for comparison to theoretical predictions such as the Bohr model

The key is a heavy energy marker such as Au on each side of the target foil

System resolution is E1 = (EDet2 + EBeam2)1/2 = 25 keV

Measured straggle of the transmitted beam is E42 = E2 + EDet2 + EBeam2 = 46 keV

Energy straggling due to the degrader foil alone E = (E42 – E12)1/2 = 39 keV

D+ beam

1.5 m Al

Al E1

E4

E1 E4

Au

1.7 MeV deuterium backscattering spectrum for 1.5 m Al foil target with Au energy markers

current varied energy implantation
Current varied energy implantation
  • Polycrystalline W implanted at 850°C with 3He to a dose of 5 x 1019 He/m2
  • 1.7 MeV 3He beam transmitted through 1.5 and 3.0 m Al foilseach tilted 0 – 60° to create a broad continuous range of energies
  • A second sample is to be generated under similar conditions except with periodic heating to 2000°C during implantation.
  • NDP analysis will allow measurement and comparison of resulting helium depth profiles in each case.
where we are now
Where we are now
  • Programming required for all calculations and foil tilt motion is near completion
  • After we successfully produce the IFE helium threat spectrum

1) Implant tungsten samples with the helium threat spectrum to study surface blistering and retention characteristics

2) Introduce implantation at 850°C and flash annealing at 2000°C as we did with monoenergetic helium implantation

thermal desorption spectroscopy
Thermal Desorption Spectroscopy
  • Wish to study thermal desorption of helium from tungsten and how it depends on implantation and flash heating parameters
  • Study single crystal and polycrystalline W to determine differences in desorption characteristics
  • Doses ranging from 1016 to 5 x 1020 He/m2 implanted at RT or 850°C
  • Residual gas analyzer (mass spectrometer) monitors He partial pressure while temperature is ramped from RT to ~2000°C
  • Temp. ramping rate typically ~2°C/s
slide26
Unimplanted polycrystalline tungsten sample ramped from RT to 2200°C

Background partial pressure level of 3He remained constant (~5x10-12 Torr)

Mass 2 is always present in mass spectrometery scans

We have conducted TDS on 3He and 4He implanted W samples to determine if the tail of the mass 2 peak affects the mass 3 peak value

So far we conclude that the mass 2 peak tail is not a great concern.

TDS Data: unimplanted polycrystalline tungsten

slide27
TDS Data: Poly W implanted with 3x10204He/m2 at RT
  • Ramped sample temperature from RT to 2200°C
  • Small pulses of desorbed He around 600°C
  • Observed significant He desorption above 2000°C which correlates to simultaneous blistering of the sample surface
  • Surface was blistered after completing the TDS experiment

Time (s)

Temp. (°C)

RT 600 2000 2200

slide28
TDS Data: Poly W implanted with 5x10203He/m2 at RT
  • Ramped sample temperature from RT to 2200°C
  • Small pulses of desorbed He around 600 and 2000°C
  • Significant He desorption above 2000°C correlates to surface blistering
  • Higher partial pressure of 3He detected due to higher dose of 3He

Time (s)

Temp. (°C)

RT 600 2000 2200

future work
Future work
  • Study helium irradiation surface damage (blistering) and retention characteristics of SiC and high porosity sprayed tungsten.
  • Automate heating and data collection of TDS
  • Carry out 3He desorption studies of single crystal, polycrystalline, and sprayed W, and also SiC to evaluate helium trapping characteristics
slide30
AcknowledgementThis research is supported under the US Department of Energy High Average Power Laser Program managed by the Naval Reactor Laboratory through subcontract with the Oak Ridge National Laboratory.

Publications

S. Gilliam, S. Gidcumb, D. Forsythe, N. Parikh, J. Hunn, L. Snead, G. Lamaze, Helium retention and surface blistering characteristics of tungsten with regard to first wall conditions in an inertial fusion energy reactor, Nuclear Instruments and Methods B, 241 (2005) 491-495.S. Gilliam, N. Parikh, S. Gidcumb, B. Patnaik, J. Hunn, L. Snead, G. Lamaze, Retention and surface blistering of helium irradiated tungsten as a first wall material, Journal of Nuclear Materials, 347 (2005) 289-297.

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