Production of Pb-Li eutectic - The National Fusion Laboratory - Ciemat
Production of Pb-Li eutectic - The National Fusion Laboratory - Ciemat
Production of Pb-Li eutectic - The National Fusion Laboratory - Ciemat
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<strong>Production</strong> <strong>of</strong> <strong>Pb</strong>-<strong>Li</strong> <strong>eutectic</strong>:<br />
cover gases or molten salts<br />
during melting ?<br />
Mª. I. Barrena, J. Mª. Gómez de Salazar, A. Soria,<br />
L. Matesanz<br />
Dpto. Ciencia Materiales e Ing. Metalúrgica. F. CC. Químicas. Universidad<br />
Complutense de Madrid. UCM, Spain<br />
M. Fernández and J. Quiñones<br />
CIEMAT. Avda. Complutense, 22. 28040-Madrid, Spain
Outline<br />
•Rationale <strong>of</strong> the activity<br />
•Review <strong>of</strong> current production<br />
techniques<br />
•Design proposals<br />
•Conclusions and future
Rationale -1<br />
• Since early 70´s, <strong>Pb</strong>-<strong>Li</strong> <strong>eutectic</strong> (LLE, <strong>Pb</strong>15.7<strong>Li</strong>) represents today the most<br />
consolidate liquid breeder material.<br />
• 6 <strong>Li</strong> enriched LLE should be manufactured for diverse ITER TBM (EU-<br />
HCLL, US-DCLL, IN-LLCB) according to nuclear material standards.<br />
• Several tones <strong>of</strong> <strong>Pb</strong>15.7(2) 6 <strong>Li</strong> should prospectively to be procure by ITER<br />
parties<br />
• LLE characteristics should be established according to nuclear material QA<br />
requirements<br />
– ISO3131/- 1, /-5, <strong>Li</strong>ght Metals and light alloying metal: methods for processing and<br />
treatment<br />
• <strong>Li</strong> chemical activity determine LLE activity: title has large impact on NFT.<br />
• 3 H solubility in LLE would largely depends on <strong>Li</strong>-disproportioning by bad<br />
mixing or local aggregation.<br />
– Other properties less modified<br />
• 2 at% <strong>Li</strong> deviations are unacceptable from QA <strong>of</strong> LLE as Nuclear Material
Uncertainty in the <strong>eutectic</strong> composition ( T-soly)<br />
- overestimation depending on the<br />
experimental protocole for production<br />
and for its determination<br />
- W-T data for a total <strong>of</strong> 52 points {0 < x <strong>Li</strong><br />
(at%)
Rationale -2<br />
Key QA aspects:<br />
1. Material certified application database according with the<br />
material design functionalities [see., E. Mas de les Valls et al.,<br />
JNM ]<br />
2. Certified characterization techniques supporting database<br />
3. QA demands to (LLE) characteristics: constitutive and<br />
compositional<br />
- QA constitutive specifications: & <strong>Li</strong> aggregation<br />
- Compositional specifications apply for <strong>Li</strong> title<br />
certification & impurity levels<br />
<strong>Production</strong> and material testing routes should be fixed<br />
according to QA standards<br />
In the EU, TBM Consortium <strong>of</strong> Associates (CIEMAT) is<br />
generating a procurement plan for 6 LLE according to<br />
nuclear standards
Roadmap for <strong>Pb</strong> - <strong>Li</strong> <strong>eutectic</strong> QA procurement<br />
• Revision <strong>of</strong> set <strong>of</strong> ISO norms<br />
– ISO3131/- 1, /-5, <strong>Li</strong>ght Metals and light alloying metal: methods for<br />
processing and treatment, in force for Nuclear Materials and IAEA<br />
Regulations.<br />
• Fixing Material specification in terms <strong>of</strong>:<br />
– maximum allowable impurity contents<br />
– <strong>Li</strong> contents global deviations (ex. < ± 0.2 <strong>Li</strong> at%)<br />
– Homogeneity criteria (ex. maximum size and distribution <strong>of</strong> <strong>Li</strong> and other<br />
<strong>Li</strong>-<strong>Pb</strong> phases aggregates<br />
• Establishment <strong>of</strong> a production route (with specification <strong>of</strong> endorsing<br />
ISOs) according to previous material QA criteria.<br />
• Establishment <strong>of</strong> set <strong>of</strong> certification tests for Material QA (fine<br />
calorimetry at <strong>eutectic</strong>, x-ray phase study, Atomic Absorptions<br />
Technique, …)<br />
Lack <strong>of</strong> database reproducibility for key FT properties can<br />
not even more potentially be justified in terms <strong>of</strong> material<br />
uncertainties
Programme goals<br />
• In parallel to EU ITER/DA F4E activities<br />
(GRT-030) Spanish TECNO_FUS<br />
2009/2012 Programme (CIEMAT, UCM) is<br />
facing production <strong>of</strong> 6 LLE according to<br />
ITER QA standards<br />
6 LLE FUNCTIONAL (REPRODUCIBLE)<br />
DATABASE<br />
CERTIFIED CHARACTERISATION<br />
6 LLE PRODUCTION ROUTES
Certified characterization<br />
Present EU <strong>Pb</strong> –<strong>Li</strong> alloy specs.<br />
INGOTS A 15.8-16.1±0.2%at <strong>Li</strong><br />
Institute <strong>of</strong> Physics <strong>of</strong> the<br />
University <strong>of</strong> Latvia (IPUL)<br />
INGOTS B 18.8±4.1–19.4±3.5%at <strong>Li</strong><br />
"Jost-Hinrich Stachov Metahandel",<br />
Germany<br />
MICROSTRUCTURE NEARLY EUTECTIC<br />
MICROSTRUCTURE HYPEREUTECTIC
<strong>Pb</strong>-<strong>Li</strong> binary diagram<br />
Y Ref. at.% <strong>Li</strong> Alloy origin T-control Analysis Uncertainties<br />
88 [5] 16.98 CEA, <strong>Li</strong>(99.5) and<br />
<strong>Pb</strong>(99.994)<br />
-- -- --<br />
Figure 1: Phase diagram <strong>of</strong> <strong>Pb</strong>-<strong>Li</strong> system<br />
[Tegze and Hafner, 1989]<br />
91 [6] 16.55 Alloyed at home Poor detail N.S.<br />
91 [3] 16.98 laboratory, <strong>Li</strong>(99.4) from<br />
Metallgesellschaft with<br />
0.5 Na, 0.01 K, 0.03 Ca,<br />
Experimental Procedure<br />
• Material<br />
– Ingot A<br />
– Ingot B
Previos work – Temperature distribution<br />
• Ingot A<br />
– Homogeneous distribution<br />
• Wall solidification<br />
• Ingot B<br />
– T f >> del ingot A<br />
• High temperature areas<br />
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Ingot B
conc. <strong>Li</strong> / % at<br />
conc. <strong>Li</strong> / % at<br />
Previous work – Chemical analysis<br />
Ingot A<br />
Ingot B<br />
50<br />
50<br />
<strong>Li</strong>ngote A<br />
<strong>The</strong>rmoX ELAN<br />
<strong>Li</strong>ngote B<br />
<strong>The</strong>rmoX ELAN<br />
6<br />
<strong>Li</strong><br />
6<br />
<strong>Li</strong><br />
40<br />
7<br />
<strong>Li</strong><br />
[<strong>Li</strong>] A<br />
= 18.31 ± 0.50 % at<br />
40<br />
7<br />
<strong>Li</strong><br />
[<strong>Li</strong>] A<br />
= 24.04 ± 1.38 % at<br />
Composición nominal fabricante<br />
Composición eutéctico <strong>Pb</strong> - <strong>Li</strong><br />
Composición nominal fabricante<br />
Composición eutéctico <strong>Pb</strong> - <strong>Li</strong><br />
30<br />
30<br />
20<br />
20<br />
10<br />
10<br />
0 2 4 6 8 10<br />
muestra<br />
0 2 4 6 8 10<br />
muestra
Y<br />
Y<br />
Y<br />
Y<br />
Previos work –<strong>Li</strong> elemental analysis<br />
• %at <strong>Li</strong><br />
(distribution)<br />
– A < B<br />
– >> first solidification<br />
areas<br />
– >> <strong>eutectic</strong><br />
– >> nominal<br />
composition<br />
– Dependence with<br />
position<br />
– Similar behaviour<br />
than T<br />
2.0<br />
1.5<br />
1.0<br />
0.5<br />
0.0<br />
0 1 2 3 4<br />
2.0<br />
1.5<br />
1.0<br />
0.5<br />
Ingot A1<br />
X<br />
Ingot A3<br />
30<br />
29<br />
28<br />
27<br />
26<br />
25<br />
24<br />
23<br />
22<br />
21<br />
20<br />
19<br />
18<br />
17<br />
16<br />
15<br />
14<br />
30<br />
29<br />
28<br />
27<br />
26<br />
25<br />
24<br />
23<br />
22<br />
21<br />
20<br />
19<br />
18<br />
17<br />
16<br />
15<br />
14<br />
2.0<br />
1.5<br />
1.0<br />
0.5<br />
2.0<br />
1.5<br />
1.0<br />
0.5<br />
Ingot B E<br />
0.0<br />
0 1 2 3 4<br />
X<br />
Ingot B int<br />
0.0<br />
0 1 2 3 4<br />
X<br />
0.0<br />
0 1 2 3 4<br />
X
Temperatura / 0 C<br />
Temperatura / 0 C<br />
Previous Work<br />
320 ASM (up dated 1993)<br />
Hubberstey et al.;<br />
300<br />
280<br />
Este trabajo<br />
<strong>Li</strong>ngote A<br />
Czochralski & Rassow;<br />
; <strong>Li</strong>ngote B<br />
Grube & Klaiber<br />
Pogodin & Schtilineshkii<br />
320<br />
ASM (up dated 1993)<br />
Hubberstey et al.; Grube & Klaiber<br />
Czochralski & Rassow; Pogodin & Schtilineshkii<br />
Este trabajo<br />
<strong>Li</strong>ngote A: Tf c<br />
= ; Tf e<br />
= ; <strong>Li</strong>ngote B: Tf c<br />
= ; Tf e<br />
300<br />
280<br />
260<br />
260<br />
240<br />
240<br />
220<br />
0 5 10 15 20 25 30<br />
<strong>Li</strong> / % at<br />
0 5 10 15 20 25 30<br />
Measurement T eut(M) ≈237 °C y T eut(S) ≈231 ° C<br />
– Ingot A shows the highest homogeneity<br />
220
Basic scheme <strong>of</strong> our melting system<br />
A: Induction Furnace (8 kW)<br />
B: Reactor (Cr-Ni Alloy)<br />
C: Gases battery
Equipment designed<br />
Vacuum<br />
<strong>The</strong>rmocouple<br />
Gas Innlet<br />
Windows<br />
SiC crucible & <strong>Pb</strong>-<strong>Li</strong> ingots
Experimental description<br />
• Material<br />
– <strong>Pb</strong>(s) ultrapure<br />
– <strong>Li</strong>(s) ultrapure<br />
• Experimental condition<br />
– Atmosphere<br />
• N 2 , Ar, molten salt,...<br />
– Temperature<br />
• 350 – 800 °C<br />
– Time?<br />
– Crucible<br />
• C, CSi, SiO 2
Crucible material selection - Reactivity <strong>of</strong> the LLE
Experimental setup<br />
Group Ingot Temp (°C) time (min) Gas Crucible<br />
I<br />
<strong>Pb</strong><strong>Li</strong> 0 450<br />
<strong>Pb</strong><strong>Li</strong> 1 550 15 N 2 (T)<br />
C<br />
<strong>Pb</strong><strong>Li</strong> 2 650 SiC<br />
<strong>Pb</strong><strong>Li</strong> 4 600 15<br />
SiC<br />
II<br />
Ar<br />
<strong>Pb</strong><strong>Li</strong> 3 650 30 SiO 2<br />
III <strong>Pb</strong><strong>Li</strong> 5 700 - 800 5-15 Ar (BIP) SiC<br />
IV<br />
<strong>Pb</strong><strong>Li</strong> 10 350 8<br />
<strong>Pb</strong><strong>Li</strong> 8 400 15<br />
<strong>Pb</strong><strong>Li</strong> 7 450 15<br />
<strong>Pb</strong><strong>Li</strong> 6 700 5<br />
V <strong>Pb</strong><strong>Li</strong> 9 400 3<br />
VI <strong>Pb</strong><strong>Li</strong> 11 350 8<br />
Ar (BIP)<br />
+ <strong>eutectic</strong> <strong>Li</strong>Cl/KCl<br />
Air + <strong>eutectic</strong><br />
<strong>Li</strong>Cl/KCl<br />
Ar (BIP) + <strong>eutectic</strong><br />
<strong>Li</strong>Cl/KCl<br />
C<br />
SiC<br />
SiC<br />
SiC
Results - Chemical characterization by ICP-MS<br />
Group Ingot %at <strong>Li</strong><br />
<strong>Pb</strong><strong>Li</strong> 0 16.6<br />
I<br />
<strong>Pb</strong><strong>Li</strong> 1 17.5<br />
<strong>Pb</strong><strong>Li</strong> 2 16.4<br />
II<br />
<strong>Pb</strong><strong>Li</strong> 4 17<br />
<strong>Pb</strong><strong>Li</strong> 3 15.8<br />
III <strong>Pb</strong><strong>Li</strong> 5 17.3<br />
<strong>Pb</strong><strong>Li</strong> 10 15.5<br />
IV<br />
<strong>Pb</strong><strong>Li</strong> 8 16.6<br />
<strong>Pb</strong><strong>Li</strong> 7 13.5<br />
<strong>Pb</strong><strong>Li</strong> 6 13.7<br />
V <strong>Pb</strong><strong>Li</strong> 9 15.2<br />
VI <strong>Pb</strong><strong>Li</strong> 11 31.55
Q (mW/mg)<br />
Results - Microstructure & DSC characterization<br />
0,5<br />
0,4<br />
0,3<br />
0,2<br />
Eutectic<br />
Eutectic <strong>Pb</strong>-<strong>Li</strong> ingots<br />
0,1<br />
0,0<br />
-0,1<br />
-0,2<br />
-0,3<br />
-0,4<br />
-0,5<br />
-0,6<br />
-0,7<br />
-0,8<br />
-0,9<br />
Eutectic<br />
0 100 200 300 400 500<br />
T (ºC)
Q (mW/mg)<br />
Results - Microstructure & DSC characterization<br />
0,4<br />
0,3<br />
0,2<br />
0,1<br />
Eutectic<br />
Solidification<br />
Hipo<strong>eutectic</strong> <strong>Pb</strong>-<strong>Li</strong> ingots<br />
0,0<br />
-0,1<br />
-0,2<br />
Melt<br />
-0,3<br />
-0,4<br />
-0,5<br />
-0,6<br />
-0,7<br />
Eutectic<br />
0 100 200 300 400 500<br />
T (ºC)
Q (mW/mg)<br />
Results - Microstructure & DSC characterization<br />
0,3<br />
0,2<br />
Eutectic<br />
Solidification<br />
Hiper<strong>eutectic</strong> <strong>Pb</strong>-<strong>Li</strong> ingots<br />
0,1<br />
0,0<br />
-0,1<br />
-0,2<br />
-0,3<br />
oxidation<br />
Melt<br />
-0,4<br />
-0,5<br />
Eutectic<br />
0 100 200 300 400 500<br />
T (ºC)<br />
Intermetallic <strong>Pb</strong>-<strong>Li</strong>
XRD pattern <strong>of</strong> the oxidized phases<br />
<strong>Li</strong>3N and <strong>Pb</strong>O
Results – Melting points
Ongoing efforts<br />
• Impurity control<br />
• Optimization <strong>of</strong> the melting process<br />
– Impurity control<br />
– Design <strong>of</strong> the thermal treatment<br />
– Reduce <strong>of</strong> oxidation process<br />
• <strong>Li</strong>