Working Report 2012-03

Creep Properties of EB Welded

Copper Overpack at 125175 C

Stefan Holmstrm

Jorma Salonen

Tuomo Kinnunen

January 2012

POSIVA OY
FI-27160 OLKILUOTO, FINLAND
Tel +358-2-8372 31
Fax +358-2-8372 3709
 Working Report 2012-03

Creep Properties of EB Welded

Copper Overpack at 125175 C
Stefan Holmstrm

Jorma Salonen

Tuomo Kinnunen

VTT

January 2012

Working Reports contain information on work in progress

or pending completion.

The conclusions and viewpoints presented in the report

are those of author(s) and do not necessarily
coincide with those of Posiva.
ABSTRACT

Electron Beam welds (EBW) chosen as primary sealing method by Posiva welding the
over-pack canister lids of oxygen-free phosphorus micro-alloyed copper (OFP) have
been tested for material properties relevant to long term creep life prediction. Creep
rupture results are presented for the ruptured 175 C tests and for the ongoing long term
tests at 150 C and 125 C. The current status (test time, creep strain and strain rate) of
the ongoing tests are reported. The initial (175 C) results indicate that the EB welds are
weaker than the parent material and that both round bar and spark eroded square test
specimens produce weld strengths of about 0.75 at tests durations of 5000 h. The
downward trend is however expected to continue for the longer test durations. The creep
ductility shows decrease for the longer tests.

Life estimates for the EB weld have been calculated at 100 C for both 50 and 80 MPa
with the so far lowest measured EB weld strength factor (WSF=0.77). The state-of-the-
art model on the available data give estimated lives of 21000 and 3000 years
correspondingly. However, simulated to the expected temperature profile of the
repository service the life fraction reached after 10000 years of service is 1 % and 7 %
for the same stress levels. It is though important to remembered that the 80 MPa
assumption is very conservative in nature and that the predictions do not take into
account relaxation of stresses, further decline of the WSF or anisotropy of the weld and
are therefore still to be considered indicative only. It is also to be remembered that there
is only limited data in the long term regime for the weldments and that the estimates are
based on the few EB data available in the public domain added with the Posiva data of
this project. Improvement of the models and predictions are expected from the ongoing
125 C and 150 C long term tests.

Keywords: EB-welds, creep, OFP-copper.

ELEKTRONISUIHKUHITSATTUJEN NYTTEIDEN VIRUMISOMINAISUUDET
LMPTILOISSA 125175C

TIIVISTELM

Elektronisuihkuhitsattujen nytteiden (hapeton, fosforilla mikroseostettu kupari OFP)

virumiskestvyytt testataan pitkaikaisilla kokeilla eri lmptiloissa hitsien pitk-
aikaisarviointia varten. Tss raportissa esitelln koesarjan ensimmiset tulokset
175 C:ssa virutetulle murtuneelle nytteelle sek vlitulokset 150 C ja 125 C:ssa
meneilln oleville kokeille (aika, virumisjnnitys ja muodonmuutosnopeus). Alustavat
tulokset 175 C :ssa osoittavat, ett elektronisuihkuhitsatut nytteet ovat heikompia kuin
perusmateriaalista tehdyt nytteet ja ett pyreiden sauvojen sek kipintystettyjen
neliskanttisten nytteiden hitsauslujuustekij (WSF = Weld strenght factor) on 0.75
5000 tuntia kestneess kokeissa. Tulosten laskevan trendin voidaan olettaa laskevan
viel pidemmill koeajoilla. Mys virumissitkeys nytt laskevan ajan funktiona.

Elektronisuihkuhitsien elinikarviot on laskettu 100 C:ssa, 50 ja 80 MPa:n jnnityk-

sess virutetuille nytteille (hitsauslujuustekij WSF = 0.77). Kytetty malli ennustaa
elinikarvioiksi 50 MPa:n nytteelle 21 000 vuotta ja 80 MPa:n nytteelle 3 000 vuotta.
On kuitenkin syyt ottaa huomioon, ett 80 MPa:n oletus on erittin konservatiivinen
arvio ja se ei ota huomioon jnnitysten laukeamista, mik laskee hitsauslujuustekij tai
hitsin anisotropiaa ja siten tulokset ovat vain suuntaa-antavia. Kytettviss olevan
pitkaikaisen datan mr on kuitenkin tss vaiheessa hyvin rajallinen ja arviot
perustuvat julkisesti saatavaan dataan sek tss tutkimuksessa Posivan nytteist
saatuihin tuloksiin. Malleihin ja arvioihin tullaan saamaan parannusta ja varmennusta
meneilln olevien pitkaikaisten kokeiden (125 C ja 150 C) edetess.

Avainsanat: Elektronisuihkuhitsit, viruminen, OFP-kupari.

 1

TABLE OF CONTENTS

ABSTRACT
TIIVISTELM

1 INTRODUCTION .................................................................................................... 3
2 MATERIALS AND METHODS ................................................................................ 5
3 RESULTS ............................................................................................................... 9
3.1 Tensile testing ............................................................................................... 9
3.2 Creep testing results ................................................................................... 11
3.3 Creep strain and strain rate results for the long term 125-150C tests ....... 17
3.4 Microstructural investigation........................................................................ 18
3.4.1 Parent material ................................................................................ 18
3.4.2 Microstructural investigation on EB-welds ...................................... 20
4 LOCAL MATERIAL PROPERTIES IN THE WELD ZONE .................................... 29
4.1 Hardness profile over the EB-weld.............................................................. 29
4.2 Local strains ................................................................................................ 31
5 INITIAL LIFE PREDICTION OF CASE STUDY .................................................... 37
6 FUTURE WORK ................................................................................................... 43
REFERENCES ............................................................................................................. 45
APPENDICES 1 - 3 ...................................................................................................... 47
2
 3

1 INTRODUCTION

The Finnish (and also the Swedish) concept of managing spent fuel from nuclear power
plants involves encapsulation of the fuel bundles in metal canisters over-packed with
oxygen-free phosphorus micro-alloyed copper [1]. These canisters are to be placed deep
into a bedrock repository. Posiva and SKB are jointly carrying out development on
manufacturing and sealing and inspection of the copper-iron canisters for spent fuel.
Posiva has chosen electron beam welding (EBW) for as primary sealing method. Posiva
is also following the friction stir welding (FSW) development chosen by SKB as an
alternative sealing method to be implemented if EBW encounters major difficulties. The
EBW will be further developed during 2010-2012, especially concentrating on the issue
of high residual stresses from a long-term safety point of view (potential early canister
failure) [1].

The temperature of the canister is foreseen to reach a maximum of 80-90 qC during the
first 100 years, with gradual cooling to the level of the bedrock environment. One of the
potential damage mechanisms expected in the repository conditions is creep [2,3].
However the estimation to the required service life is a significant challenge due to the
extensive extrapolations needed. The extrapolations are one to four orders in magnitude
longer than for ordinary engineering structures designed against creep.

The objective of this work is to provide a comprehensive understanding of the long term
creep properties of the EB-weld. The main tool to achieve this is by mechanical testing
of the EB welds at raised temperatures to attain sufficient data for life assessments. Also
the local material properties in the weld are sought by optical measurements (at room
temperature) and by local displacement measurements during test interruptions (long
term creep). The material properties of the different regions within the weld will provide
the basis for an advanced finite element analysis at a later stage.
4
 5

2 MATERIALS AND METHODS

The EB cross weld test material was received as two batches of test samples sectioned
from the Posiva test slabs X259 and X258, the expected average chemical composition
from EB welded test slabs is presented in Appendix 1. Each EB weldment batch
consisted of 15 samples each with the cross section dimensions of 20 mm x 20 mm and
135 mm in length. The samples were punch marked A2-O2 on the parent material end
section. For example the X259A2 marking on the specimen defines the weld as follows;
X259A signifies it being the first specimen in order (A) taken from the X259 test
slab, 2 signifies that the sample is a taken from the mid section of the weld in the
weld penetration direction (see Table 1 and Table 2). The positioning of the EB-
sampling is shown in Figure 1. Note that the surface (1) and root (3) weld locations are
not tested in this investigation.

Figure 1. The weld slab and the location of tensile and creep specimens (marked in
grey).
A total of 28 parent material samples have also been received (20 x 20 x 175 mm), all
marked as X259. To date three tensile tests have been performed and two creep tests are
running. The tensile tests were done on round cross section test specimens whereas the
creep specimens are spark eroded rectangular cross section specimens (see Table 3).
The EB-samples have been machined and utilised as described in Table 1 for the X258
batch and in Table 2 for the X259. Some samples were rejected due to NDT surface or
internal flaw indications.

Two types of creep specimens are used in this work. The initial testing (tensile and most
175 C creep test) have been performed with round bar creep specimens (see Appendix
2) with a nominal diameter of 10 mm. For the 150 and 125 C creep test only the spark
eroded specimen type (8.9x8.9 mm, see Appendix 3) has been used. Both specimen
types are proportional test pieces with the same initial gauge length of 50 mm. The
 6

decision to change test specimen type was made on the request of Posiva due to
indicative cold working of the rotary-machined test specimen.

6.00 cm

Figure 2. Schematic presentation of the actual canister EB weld, the lid is presented as
white and the cylinder part as striped.
Table 1. Batch X258 EB test pieces, specimen type, their usage and test results. The
samples are coded as 8=X258, followed by the letter A to O. all specimens are from mid
section of the EB-weld.

Test piece Specimen type Comment / Test Result

8A spark eroded spec. 150 C / 100 MPa running + 22000 h
8B no specimen pores, 1 mm flaw rejected
8C round bar spec. 225 C / 95 MPa 210 h
8D spark eroded spec. 150 C / 90 MPa running + 22000 h
for creep test
8E spark eroded spec. Spare, Aramis
area: 8.55 x 8.9 mm
8F Hot tensile 0.5 mm / min 125 C
8G Hot tensile 0.5 mm / min 150 C
8H spark eroded spec. 150 C / 70 MPa running + 22000 h
8I spark eroded spec. 175 C / 100 MPa 4656 h
8J round bar spec. 175 C / 130 MPa 194 h
8K no specimen flaw detected rejected
8L no specimen flaw detected hardness profile
8M Hot tensile 0.5 mm / min 175 C
8N round bar spec. 175 C / 100 MPa 4405 h
indentation and
hardness and local
8O spark eroded spec. straining, 175 C, 100
strain measurement
MPa
 7

Table 2. Batch X259 EB test pieces, specimen type, their usage and test results. The
samples are coded as in Table 1.

Test piece usage comment Test

local strain meas. Aramis test piece, local strain, RT
9A
20x20 mm sample flaw 2 mm load increments
NDT small pores
9B no specimen spare
detected
9C round bar spec. damaged rejected
NDT pores
9D no specimen spare
detected
9E spark eroded spec. for creep test spare
9F Hot tensile 0.5 mm / min 125 C
9G Hot tensile 0.5 mm / min 150 C
9H spark eroded spec. 125 C / 70 MPa running + 17000
9I spark eroded spec. 125 C / 115 MPa running + 17000
9J round bar spec. 175 C / 120 MPa 471 h
9K spark eroded spec. 125 C / 100 MPa running + 17000
9L no specimen 1 mm flaw detected rejected
9M Hot tensile 0.5 mm / min 175 C
9N round bar spec. 175 C / 115 MPa 844 h
9O spark eroded spec. for creep test spare

Table 3. Parent material (PM) specimens from batch X259.

Test piece usage comment Test

9P1 round bar spec Hot tensile 125 C Rm= 173
9P2 round bar spec Hot tensile 150 C Rm= 167
9P3 round bar spec Hot tensile 175 C Rm= 160

9pv1 spark eroded spec. 150 C / 100 MPa running + 22000 h

9pv2 spark eroded spec. 125 C / 100 MPa running + 17000 h
9pv3 spark eroded spec. 175 C / 100 MPa spare
8
 9

3 RESULTS

The test results presented in this report is the updated status on tensile, creep and
microstructural investigation conducted up to 3.9.2010.

3.1 Tensile testing

The results of the conducted hot tensile tests (round bar test specimens) for parent
material (PM) and EB-welds (EBW) are presented in Table 4, Figure 3 and Figure 4.
The ruptured parent material tensile specimen 9P3 (175 C) is shown in Figure 5 and
the EB-weld tensile specimen 9G in Figure 6.

The reduction of area (Z) for EB-welds (both tensile and creep) is calculated assuming
an elliptical surface area by measuring minor (welding direction) and major axes
(penetration direction) as shown in Figure 8 for the creep specimen 8N. The rupture
strain (A5) is the engineering strain and the yield (Rp0.2) and rupture strengths (Rm) are
calculated from tensile test data (see Appendix 4). Note that the yield strength results
for the EB-welds can be considered indicative only due to localisation of the strain. The
indicative yield strength results however raised the question on cold work in the
standard round cross section test specimens (see Figure 11 in creep results section)
resulting in changing the specimen type.

Table 4. Tensile testing at raised temperature for parent material (PM) and EB-welds
(EBW). Note that the yield strength results for the EB-welds can be considered
indicative only.

Specimen Type Temp C Rp0.2 Rm A5 % Z%

8F EBW 125 (84) 159 26 82
9F EBW 125 (64) 158 27 82
9P1 PM 125 56 173 53.5 84
8G EBW 150 (61) 153 28 84
9G EBW 150 (57) 152 29 85
9P2 PM 150 55 167 55 84
8M EBW 175 (59) 147 30 80
9M EBW 175 (57) 147 30 82
9P3 PM 175 47 160 53 83
 10

175

170
Ultimate strength (Rm), MPa

165

160

155

150 Rm-X259-PM
Rm-X258-EBW
Rm-X259-EBW
145
120 130 140 150 160 170 180
Temperature, C

Figure 3. Ultimate tensile strength (Rm) as a function of temperature for parent

material (PM) and EB-welds (EBW).

90

85

80
Yield strength (Rp0.2), MPa

75

70

65

60

55

50
Rp0.2-X259-PM
Rp0.2-X258-EBW
45
Rp0.2-X259-EBW
40
120 130 140 150 160 170 180
Temperature, C

Figure 4. Yield strength for parent material (PM) and indicative results for EB-welds
(EBW). Note that the local yield can be something entirely different from the value
assuming homogenous straining over the full gauge length.
 11

Figure 5. Hot tensile test specimen 9P3 (parent material) tested at 175 C.

Figure 6. Hot tensile specimen 9G (EB-weld) tested at 150 C.

3.2 Creep testing results

Creep testing results of the EB-welds are shown in Table 5. The test 8I at 175 C / 100
MPa (Figure 9) is a repetition of the test 8N at the same stress and temperature
(Figure 8) with the spark eroded test specimen. The ruptured specimens 9J (175 C /
120 MPa) is shown in Figure 7.

Note also that the measured reductions of area in all creep samples are smaller than for
the tensile tests. The trend is as expected in creep testing decreasing for longer test
durations as shown in Figure 10.
 12

Table 5. Creep testing status (20.10.2010) of EB-welds and parent material.

Stress V/Rm Time init. strain Z Hf

Spec. Type Temp % status
MPa (PM) h strain (UB) % %
8J EBW 175 125 0.85 194 11.0 - 67 23 rupt
9J EBW 175 120 0.82 471 8.3 - 59 25 rupt
9N EBW 175 115 0.78 844 7.4 - 55 20 rupt
8N EBW 175 100 0.68 4405 3.3 - 52 15 rupt
8I EBW 1) 175 100 0.68 4656 5.6 - 44 16 rupt
8C EBW 225 95 0.75 210 (0.4) - 34 10 rupt
8A EBW 1) 150 100 0.66 22000+ 3.82) 9.1+ - - runnig
8D EBW 1) 150 90 0.59 22000+ 3.02) 6.5+ - - runnig
8H EBW 1) 150 70 0.46 22000+ 0.32) 3.3+ - - runnig
9H EBW 1) 125 70 0.44 17000+ (1.2)3) 3.1+ - - runnig
9I EBW 1) 125 115 0.73 17000+ (6.8)3) 11.7+ - - runnig
9K EBW 1) 125 100 0.63 17000+ (4.4 )3) 8.3+ - - runnig
9pv1 PM 1) 150 100 0.60 22000+ (3.5)2) 9.4+ - - runnig
9pv2 PM 1) 125 100 0.58 17000+ (4.4 )3) 8.4+ - - runnig
1) Spark eroded creep specimen
2) based on measured creep strain on first interruption (3160 h)
3) based on measured creep strain on first interruption (4200 h)

The initial strain at 175 C tests is clearly lower for the round bar specimen than for the
spark eroded specimen. The step-wise loading at the start-up of the creep test is shown
for specimen 8I and 8N as in Figure 11. The Posiva concern of the round bar specimens
being cold worked at manufacture seems to have been justified. The short term creep
properties of the cold worked specimens are likely to be somewhat over conservative
[4] but the long term creep properties should not be affected. No significant difference
in creep rates and time to rupture was however found for the 175 C tests as seen in
Figure 12. The conclusion was made that the performed creep tests with round bar
specimens are valid and can be used for life predictions of the EB weld.
 13

Figure 7. Creep test specimen 9J (EB-weld) tested at 175 C / 120 MPa with a rupture
time of 471 h.

Figure 8. Creep test specimen 8N (EB-weld) tested at 175 C / 100 MPa with a rupture
time of 4405 h. The rupture cross section is shown below together with simplified
description used for calculation of reduction of area (assumed elliptical).
 14

Figure 9. Creep test specimen 8I (EB weld) tested at 175 C / 100 MPa with a rupture
time of 4656 h.

level for tensile tests

80 %
Reduction of area (Z)

70 %

60 %

50 %

40 %
100 1000 10000
Time to rupture (h)

Figure 10. Reduction of area as a function of rupture time at 175 C. The creep
ductility drops towards longer rupture times. The corresponding values for tensile tests
are around 80 %. The longest test shows a lower reduction of area value for the spark
eroded test specimen (square) than for the round bar specimen (circles).
 15

120

Nominal stress (MPa) 100

80

60

40

20
8N round
8I square
0
0% 1% 2% 3% 4% 5% 6%
Strain (%)

Figure 11. Initial strain response at step wise loading in the start of creep tests
(nominal over gauge length) for specimens 8N and 8I (175 C / 100 MPa). The spark
eroded specimen (8I) shows yielding at lower stress values.
1.E-04
Nominal strain rate (1/h)

1.E-05

N8 - round bar
I8 spark eroded

1.E-06
100 1000 10000
Time (h)
Figure 12. Calculated strain rate (nominal over gauge length) for specimens 8N and 8I
at 175 C / 100 MPa. The strain rate for the spark eroded test specimen does not differ
from the test conducted at the same stress level with the round bar test specimen; also
the rupture time is almost identical.
 16

The creep rupture test results for the EB-weld is plotted against public domain data for
EB-welds and parent material in Figure 13.

160

150

140
Stress (MPa)

130

120

W SF<0.75 125 MPa, 194 h (8J)

110 FSW (SKB, TR-05-08)
PM (SKB, TR-99-39)
PM (IM-3327) 120 MPa, 471 h (9J)
EB (SKB, TR-05-08)
100 FSW (SKB, TR-05-08) 115 MPa, 844 h (9N)
POSIVA (VTT)
PM (IM-3327)
100 MPa, 4405 (8N)
90
10 100 1000 10000 100000 1000000
Time (h)

Figure 13. Creep test results (POSIVA-VTT) at 175 C plotted against public domain
parent material (PM [4, 6], friction stir weld (FSW [5]) and electron beam weld
(EB[5]) data.
As seen the strength versus rupture time is for the EB-welds steeper in comparison to
parent and friction stir welds (FSW). The weld strength factor (WSF) defined according
to ECCC recommendations (Eq. 1, [7]) is for the EB-welds around 0.75 for the longest
test of 4656 hours. A continuing decline is expected for longer test durations. However
it is to be remembered that the parent material creep strength level has not yet been
thorougly established and the WSF is calculated on the mean parent material strength
(Ru/t/T) in Eq. 1.

The WSF is defined as;

Ru (W ) / t / T
WSF Eq. (1)
Ru / t / T

where Ru (W ) / t / T is the predicted strength of the weld at specified time and temperature
and Ru / t / T is the corresponding strength of the parent material.

The WSF can also be determined through a new method utilizing the Wilshire equation
presented later in this report.
 17

3.3 Creep strain and strain rate results for the long term 125-150C tests

The measured strain rates of the running tests at 150 C is presented in Figure 14 and
the tests at 125 C are shown in Figure 15. The parent material (PM) results are
compared in Figure 16. The 150 C tests have been interrupted for manual displacement
measurement at 3163 h and the 125 C tests at 4200 h of testing time. The EB weld area
was found to deform (plastic and creep) unequally in the welding and depth direction.
This phenomenon will be described closer later in this report.

1.0E-04

manual strain measurement (3163 h)

Nominal strain rate (1/h)

1.0E-05

1.0E-06
PM-100 EB-100

EB-90 EB-70

1.0E-07
10 100 1000 10000 100000
Time (h)

Figure 14. Measured strain rates (nominal over gauge length) for specimens 8A (100
MPa), 8D (90 MPa) and 8H (70 MPa) tested at 150 C. The parent material test
9pv1(100 MPa) is showing very similar strain rates as the EB-welded specimen.

1.0E-04

manual strain measurement (4200 h)

1.0E-05
Nominal strain rate (1/h)

1.0E-06

1.0E-07 G-PM100 H-EB100

F-EB115 E-EB70

1.0E-08
10 100 1000 10000 100000
Time (h)

Figure 15. Measured strain rates (nominal over gauge length) for specimens 9H (70
MPa), 9I (115 MPa) and 9K (100 MPa) tested at 125 C. The parent material test 9pv2
(100 MPa) is showing very similar strain rates as the EB-welded specimen.
 18

1.0E-04

Nominal strain rate (1/h)

1.0E-05

1.0E-06

PM-100-150C
PM-100-125C

1.0E-07
10 100 1000 10000 100000
Time (h)

Figure 16. Measured strain rates (nominal over gauge length) for parent material test
9pv1 and 9pv2 (100 MPa) at 150C and 125C respectively.

3.4 Microstructural investigation

The microstructural investigations are based on parent material and EB-welds tested for
tensile and creep properties in the temperature range 125-175 C.

3.4.1 Parent material

Microstructural investigation has to date been conducted for the parent material on
tensile specimen (9P3, 175 C, Figure 17). The microstructure of the tested parent
material shows a grain size of around 100 m. Towards the necking area the grains
become more and more deformed. Extensive elongated grains are to be found close to
the rupture location. The tensile specimen unexpectedly also shows grain boundary
cavitation at least to a distance of 25 mm from the fracture (Figure 18). This cavitation
has similar appearance as the cavitation usually connected with long term creep
damage.
 19

Figure 17. Tensile specimen 9P3 (parent material), test at 175 C (see macro in
Figure 5).

Figure 18. Grain boundary cavitation found in the tensile specimen 9P3 (175 C).
 20

3.4.2 Microstructural investigation on EB-welds

Microstructural investigation has been performed on the tensile specimen 9G and the
creep test specimens 9J and 8N. The macro-structure of the EB weld is presented in
Figure 19. For the EB-welds the grain size is considerably larger than in the parent
material and it is dependent on the direction. The anisotropic material properties
becomes evident from the shape of the ruptured round bar specimens, the fracture
surface becomes elliptical.

B
Figure 19. EB-weld seen as A) in penetration direction and B) perpendicularly in the
welding direction (welding proceeding downwards).

EB tensile test specimen

The tensile test specimen 9G, tested at 150 C was sectioned (Figure 6) and the
microstructure investigated. The fracture was situated in the weld metal centre line (see
Figure 20). The columnar grains and their extensive elongation in the weld metal are
indicating heavy localisation of strain and damage in the weld metal. The grain
formation at the fusion line seems to be epitaxial (see Figure 21 and Figure 22) i.e. the
 21

grain structure in the melted material is copied from the un-melted forming a
continuous transition with larger grain size towards the weld centre. The EB welding
produces segregation lines in parallel with the propagating solidification front
(Figure 21). The impact of these segregation lines for long term creep properties is not
known.

Figure 20. Rupture location of tensile specimen 9G, tested at 150 C (see macro in
Figure 6). Note elongated grains and large reduction of area (>80 %).
 22

Figure 21. Weld fusion line section of necked tensile specimen 9G (150 C, macro in
Figure 6). Note epitaxial grain formation at the fusion line and segregation lines (dark
curved lines in weld metal) at the propagating solidification front.

Figure 22. Weld fusion line close-up of tensile specimen 9G. Note the grain size
increase towards weld metal (right).
 23

Creep specimens:

The corresponding microstructural study on creep specimens have been conducted on

specimens 9J and 8N. The reduction of area in all creep samples is smaller than for the
tensile tests as earlier discussed (Figure 10).

Specimen 9J (see Figure 23, ruptured at 471 h) shows damage typical to short term tests
(large cavitation and local strain, Figure 24) and also cavitation typical to long term
creep damage localised in the grain boundary (see Figure 25 and Figure 28).

Figure 23. Creep specimen 9J, tested at 175 C / 120 MPa with a rupture time of 471 h.
Detail of the greyed areas A and B are presented in Figure 24 and Figure 25
respectively (see macro in Figure 7)

Figure 24. Creep specimen 9J, detail magnification of the greyed area A in Figure 23.
Note large voids typical of short term (tensile) testing.
 24

Figure 25. Creep specimen 9J, detail magnification of the greyed area B in Figure 23.
Note grain boundary cavitation typical of long term creep testing.

The longest round bar creep test (specimen 8N, 4405 h) has been sectioned in the
penetration direction as shown in Figure 26. The specimen was further sectioned
perpendicularly (halved) for investigation of the welding direction as shown in
Figure 27. The rupture surface is heavily elliptical as has been the case with all ruptured
EB-welds. The largest reduction in radius is in the direction of weld penetration.
Extensive cracking can be seen in the weld vicinity of the weld centre line. The damage
is concentrated at grain boundaries perpendicular to the load direction (cross weld). The
solidification structure is thereby evidently directly linked to the damage localisation
and expected creep life.
 25

Figure 26. Fracture seen in the weld penetration plane (spec. 8N, orientation as in
Figure 19A). Note that the cracks in Figure 27 look like voids in cross section.

Figure 27. Fracture seen in the welding direction plane (spec. 8N, orientation as in
Figure 19B). Note cracks propagating towards centre line of the weld.
 26

Figure 28. Grain boundary cavitation in creep specimen 8N.

Locally the grain boundaries both in the parent and weld metal were observed to contain
a thin layer of unknown origin (see Figure 29, 30). Layers with similar grain boundary
changes and appearance have been observed in long term multiaxial specimens of OFP
copper [2].

Figure 29. Grain boundary change in welding direction close to fracture location in
weld metal of specimen 8N. Also note grain boundary micro crack.
 27

The grain boundary change seems metallic in nature and has a maximum thickness of
around 5 Pm. This change is evidently forming during creep and is time, temperature
and perhaps also stress and strain dependent.

Figure 30. Grain boundary change in welding direction close to fusion line in parent
material of creep specimen 8N.

.
28
 29

4 LOCAL MATERIAL PROPERTIES IN THE WELD ZONE

As became evident from the tensile and creep testing results the local material
properties of the EB weld region itself will have a significant role in the prediction of
long term life. The investigation of the local material parameters has been conducted
with hardness testing over the weld and through manual strain measurements between
hardness indentations after loading. As an entirely new measurement type the ARAMIS
3D deformation analysis system has been used for measurements of local strains. The
high accuracy, three-dimensional deformation and strain measurement system has been
used at room temperature to determine the local axial strains of an un-machined EB
sample (9A). The interesting feature of the test run is that the ARAMIS analysis system
found the 2mm surface flaw that had been reported found in the X-ray (non destructive)
testing conducted by Posiva (see Table 2).

Posiva has additional test data from ARAMIS testing at room temperature for numerous
locations within the EB weld. This data will be utilized in later work on the EB weld
material property determination.

4.1 Hardness profile over the EB-weld

The hardness profile (HV 1) was taken across the EB weld of one un-machined sample
(8L) and one spark eroded test specimen (8O). The target spark eroded specimen 8O is
shown in Figure 31. The hardness profiles of the as-received sample 8L is shown in
Figure 32 and for the spark eroded specimen 8O in Figure 33. The hardness values
acquired can be compared to parent material values [6] for parent material OFP copper.
The corresponding hardness (100 g micro-Vickers hardness) for parent material with
varying grain sizes (100-2000 m) and phosphorus contents (1-106 ppm) range between
53 (30 ppm P, 450 m grain size) and 64 (60 ppm P, 2000 m grain size).
 30

Figure 31. Hardness measurement and local strain measurement markings of specimen
8O. To be compared with the situation after loading situation in Figure 34.

83
82
81
80
79
83
Hardness

78
77 82
76 81
75 80
74 79
Hardness

73 78
72 77
3 76
2 75
Re l

1
0 74
ativ

-1 73
-2
Y

-3 72
-4
10
5
0
-5
-1 0
-1 5

Relativ X

Figure 32. Hardness measurement distribution (HV 1) taken across the EB-weld (as-
rec.) of test piece 8L. Note that the fitted function is indicative only to show the
hardness dip in the EB-weld and does not represent the material behaviour outside the
measured area.
 31

64
63
62
61 64
Hardness (HV1)

60 63
59 62
58 61

Hardness (HV1)
57 60
56 59
55 58
54 57
3
2 56
1 55
Re

0
l

-1
at

54
iv

-2
Y

10
-3

5
0
-4
-5
-1
-1

0
5

Re lativ X

Figure 33. Hardness measurement distribution (HV 1) taken across the EB-weld of the
spark eroded specimen 8O; Note that the fitted function is indicative only to show the
hardness dip in the EB-weld and does not represent the material behaviour outside the
measured area.
The surface of the as-received test specimen is about 20 (HV1) higher than for the spark
eroded test specimen showing surface cold working related to the plate manufacturing
process.

4.2 Local strains

To determine the local strains of the EB-weld the specimen (8O) was loaded stepwise to
100 MPa identically as was done for specimen 9N (at 175 C). The loading sequence of
the interrupted creep test led to local strains in the weld as shown in Figure 34. The
local distances between hardness indentations were measured from the image. The
localisation of the strain becomes evident from measuring the dimensional changes over
and across the centre of the weld. The centre has a compressive strain of 8 % calculated
over the centreline of the weld and strains calculated from longitudinal (cross weld)
changes in indentation distances vary between 4-9 %.

From this test it seems that local strain measurements are difficult to acquire from
indentation point movement in a plane. Only a rough estimate can be acquired due to
straining also in the depth dimension. From these findings it was concluded that the
long term creep deformation could be roughly followed by six thickness measurements
over and adjacent to the EB weld (both welding direction and perpendicular to it in mid
weld metal and on both sides of the weld on the parent material side).
 32

Figure 34. Interrupted creep test; loading to 100 MPa / 175C (specimen 8O), the
measured nominal strain over the gauge length is 6 % whereas the dimensional change
(width) in the weld indicates a local strain of 8 % at the centre of the weld in the
penetration direction. The weld experiences an additional 3 % stress increase in the
weld due to necking effect (reduction in weld cross section in relation to
corresponding reduction of parent material cross section). Compare with results in
Figure 11.
Aramis local strain measurements (3D) were initiated at room temperature. The
localisation of strain into the weld zone is described in Figure 35 to Figure 38. Below
yield no difference is detected but immediately above yield the localisation is evident.

Figure 35. ARAMIS axial strain distribution across the EB-weld 9A at 65 MPa, The
strain measurement was reset below 40 MPa (less than yield).
 33

Figure 36. ARAMIS axial strain distribution across EB-weld 9A at 70 MPa. Note red
dot (surface flaw) appearing on the left hand side (arrow).

Figure 37. ARAMIS axial strain distribution across EB-weld 9A at 75 MPa.

 34

Figure 38. ARAMIS axial strain distribution across EB-weld 9A at 77.5 MPa.
The Aramis system will hopefully be utilised for further studies of strain localisation
both in tensile and creep (short term) at a later stage of the EB weldment
characterisation work.

The local deformation was also found in the weld material zone of the creep specimens.
The local constriction seen in Figure 39 was measured by taking replicas and measured
with surface displacement measurements. The results show that the measurement was
sensitive to the replica bending, but gave results in the expected range of about few
tenths of a millimetre (see Figure 39 and Figure 40).

Figure 39. Local deformation in EB weld at interruption (3163 h) for strain correction
and replica sampling (150 C creep tests).
 35

Figure 40. Measured necking in EB weld measured from replica sample taken from
8A (150 C, Local deformation in EB weld at interruption (3163 h) for strain correction
(150 C creep tests).
36
 37

5 INITIAL LIFE PREDICTION OF CASE STUDY

As presented in many sources (for example in [9]) a rough assumption of 50 MPa at

100C has been set as the target condition for life extrapolation of the copper overpack,
however resent papers on simulated cases the local stresses in the weld region relevant
for the EB weld can potentially reach to stress levels exceeding 40 MPa [13] . Here
these stress levels have been predicted with the below presented Wilshire model [8] and
with the classical Larson-Miller parameter extrapolation for 50 and 80 MPa, the latter
being exceptionally high, mainly intended for later reference to FSW welds. The
Wilshire model has earlier been optimised for OFP cupper in [11].

The Wilshire model is based on normalised stress (nominal divided by tensile strength).
The normalised stress value will therefore not exceed unity at the short-term end. The
Wilshire equation for time to rupture tr (note in seconds) at stress V (MPa) and
temperature T (K) can be expressed as;
ln(V / V TS )  k[t r exp(Qc* / RT )]u (2)
where k and u are constants obtained by fitting to the test data, Qc* is the apparent
activation energy and VTS is tensile strength at the same temperature. Application of this
model obviously requires data from both creep rupture testing and hot tensile testing.
The parent material constants are presented in Table 6. It is to be noted that the
predictions are sensitive to the optimized apparent activation energy and that the value
applied in this work is the one giving the optimal fit for the data base available
following Wilshire methodology. A somewhat larger Q*c has been calculated with also
excellent fit in [11] where the linear relationship of the k and u parameters of the
original Wilshire methodology was bypassed. The predicted rupture times with this
methodology are somewhat longer.

Table 6. Wilshire equation parameters for time to rupture of parent material OFP
copper.

Parameter Value
Apparent activation energy, Q*c-ref 89 200 J/mole
kref 1.6288
uref 0.297
VTS-ref[T(C)] 216-0.339T(C) MPa

The results of the life predictions are shown in Figure 41-43 and the results are listed in
Table 7.

It is to be stressed that so far the life assessment of the EB welds is based on only a
limited data set with a maximum rupture time of less than 5000 h, and strain data up to
22000 h.

Further life assessments have to be conducted on a larger data set when available.
 38

160
EB (TR-05-08)
EB (IM 3327)
140 EB (Posiva-VTT)

120
Stress (MPa)

100

80

60
assumed trend Linear
50
4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0
Larson-Miller (C=11)
Figure 41. Larson-Miller life prediction (extrapolation) for EB welds.

175C
1.2

0.8
s/RUT

0.6

0.4

0.2
1 10 1 10 1 10 1 10 1 10
3 4 5 6 7
1 10 100

Time (h)

Figure 42. Wilshire life prediction (175 C) for parent material (red line) with EB-
prediction (blue line, IM data, triangles) and the Posiva data (diamonds) at 175 C.
 39

ww
w
w ww
w
ww
w w
w

w
V/VTS

Wilshire BM model
batch 400 (PM)
batch 500 (PM)
SKB (PM)
IM (PM)
w EB welds

0.000001 0.00001 0.0001 0.001 0.01 0.1 1

tf*exp(Q/RT)
Figure 43. Wilshire model fit to parent material (PM, circles) and EB-welds (w) from
both public domain and Posiva tests.
 40

Table 7. Rupture predictions (in years) for running creep tests and the case studies at
50 and 80 MPa / 100 C.

rate
Stress Time strain (Hc) tr pred
Spec. Type Temp V/Rm(T) at Hc
MPa h % (a)
(1/h)
8A EBW 1) 150 100 0.66 22000+ 4.6+ 1.4e-6 3
8D EBW 1) 150 90 0.59 22000+ 2.4+ 8.0e-7 9
8H EBW 1) 150 70 0.46 22000+ 2.4+ 5.0e-7 48
9H EBW 1) 125 70 0.44 17000+ 2.1+ 1.1e-6 398
1)
9I EBW 125 115 0.73 17000+ 4.8+ 3.7e-6 8
1)
9K EBW 125 100 0.63 17000+ 2.3+ 2.5e-6 35
1)
9pv1 PM 150 100 0.60 22000+ 5.2+ 1.5e-6 172
1)
9pv2 PM 125 100 0.58 17000+ 3.6+ 2.7e-6 1 400
Wilshire 100 50 0.30 - - - 45000
Parent material 100 80 0.48 - - - 10000
Wilshire 100 50 0.30 - - - 21000
EB-weld
WSF=0.77 100 80 0.48 - - - 3000

Larson-Miller 100 50 - - - - > 230000

Linear, EB-weld,
C=11 100 80 - - - - > 30000
(see Figure 42)

The WSF values used in the predicted life assessment of the EB welds are done by
replacing tr in the parent material Wilshire equation with the rupture time of the EB
weld test [12]. This gives an expected V/VTS for weldment in relation to that of
reference (PM) material. Then the weld strength factor WSF, or cross weld strength
divided by reference (PM) material strength at the same time and temperature is as
shown in (Eq 3), or

V EB
WSF (3)
exp(k ref [t r  EB exp(Qc*ref / RT )]u ref ) V TS ref

where VEB is the test stress, T temperature and trEB the time to rupture for the weld. The
tensile strength VTS-ref and the constants uref, kref and Q*c-ref are those specified for the
reference (parent) material. The calculated WSFs for the 175 C are given in Table 8
and plotted as a function of stress and temperature in Figure 44.
 41

Table 8. Weld strength calculation for the ruptured EB weld specimens.

Stress tr
Spec. Type Temp WSF
MPa h
8J EBW 175 125 194 0.86
9J EBW 175 120 471 0.84
9N EBW 175 115 844 0.83
8N EBW 175 100 4405 0.77
8I EBW 175 100 4656 0.77
8C EBW 225 95 210 0.78

0.9

0.9
0.85

0.85 0.8

WSF
0.8 0.75
WSF

0.75 0.7

0.7 0.65
45 0
46
0.65 47 0
48 0 0
0.8 5 49 )
0.7 0.7 5 50 0 0 p (K
m
0.6 0.6 5
51
52 0 0 Te
s /U T 0.5 0.5
S 5 53 0
0.4
Figure 44. Wilshire based WSF presentation as a function of stress ratio and
temperature for the available EB tests data.

Using the Raiko [14] expected temperature profile for the life estimates of the EB
welds the calculated consumed life factor (time in service divided by predicted time to
rupture) at 80 and 50 MPa was, when assuming the lowest measured EB weld strength
factor (WSF=0.77) to be constant, after 10000 years of service 7 % and 1 %
correspondingly.
42
 43

6 FUTURE WORK

The test programme will be continued for both 125 C and 150 C until rupture or
specified strain or strain rate. Some additional testing (outside the planned test matrix)
might have to be conducted to improve the data base for EB welds. Further work on the
impact of localised strain should be done and the low temperature models for life
estimation should be improved. The Posiva Aramis tensile data will be a good starting
point for this work. Also, further development in measurement tools suitable for long
term creep tests, i.e measurement at interruptions should be found and applied. Further
work is also required in the identification of grain boundary changes developing under
creep conditions. For further insight in the creep ductility and creep cracking issues a
testing programme including compact tension specimens (CT testing) should be
initiated. The CT- tests would also serve as a good base for creep damage modelling
including multiaxial constraint.
44
 45

REFERENCES

[1] TKS-2009, Nuclear Waste Management at Olkiluoto and Loviisa Power Plants
Review of Current Status and Future Plans for 20102012, February 2010.

[2] Auerkari, P., Holmstrm, S., Salonen, J. & Nenonen, P. Creep performance of
OFP copper for the overpack of repository canisters. 29th International Symp. on
the Scientific Basis for Nuclear Waste Management (MRS 2005), September 12-
16, 2005, Ghent, Belgium. 8 s.

[3] Holmstrm, S., Salonen, J., Auerkari, P. & Saukkonen, T. Long-term integrity of
copper overpack. SKI Report 2007:38, ISSN 1104-1374.

[4] Seitisleam, F., Henderson, P. & Lindblom, J. Creep of copper for nuclear waste
containment results of creep and tensile tests on Cu-OF, Cu-OFP, Cathode
copper and welded joints. Swedish Institute for Metals Research, IM-3327, Feb.
1996.

[5] Andersson, H., Seitisleam, F. & Sandstrm, R. Creep testing of thick-walled

copper electron beam and friction stir welds at 75, 125 and 175 C. SKB
Technical Report TR-05-08, Jan 2005.

[6] Andersson, H., Seitisleam, F. & Sandstrm, R. Influence of phosphorus and

sulphur as well as grain size on creep in pure copper. SKB Technical Report
TR-99-39, Dec. 1999

[7] ECCC Recommendations, Creep data validation and assessment procedures,

S. R Holdsworth et al. (Eds.). ERA Technology Publ., 2001 (a) Vol. 1: Overview,
(b) Vol. 2. Terms and terminology, (c) Vol. 3. Data acceptability criteria, Data
generation, (d) Vol. 4. Data exchange and collation, (e) Vol. 5. Data assessment.

[8] Wilshire, B., Scharning, P.J. & Hurst, R. A new methodology for long term creep
data generation for power plant components. International Conference on Life
Management and Maintenance for Power Plants. Helsinki-Stockholm-Helsinki,
12-14 June 2007. Vol. 1. Pp. 196-207.

[9] Petterson, K. Development of a constitutive model for the plastic deformation and
creep of copper and its use in the estimate of creep life of the copper canister.
SKI Report 2007:12, ISSN 1104-1374, Dec. 2006.

[10] Lindblom, J., Henderson, P. & Seitisleam, F. Creep testing of oxygen-free

phosphorus copper and extrapolation of results. Swedish Institute for Metals
Research, IM-3197, ISSN 0284-2378, 1995.

[11] Holmstrm, S. & Auerkari, P. Predicting creep rupture from early strain data.
Materials Science and Engineering A., Vol. 510 511, 2009, pp. 25-28.
 46

[12] Holmstrm, S. & Auerkari, P. Improved approach for predicting weld creep
strength factors of ferritic steels. Energy Materials, Materials Science &
Engineering for Energy Systems, Vol. 4, No. 1, 2009, pp. 23-27.

[13] Raiko, R., Sandstrm, R., Rydn, H. & Johansson, M. Design analysis report for
the canister. SKB Technical Report TR-10-28, 2010.

[14] Raiko, R. Disposal canister for spent nuclear fuel Design report. Posiva Report
2005-02. 61 p.
APPENDIX 1 CHEMICAL COMPOSITION (in ppm exept for Cu in %).

Spec. EN 1976 Cu- Spec. EN 1976 Cu- Average Parent Average Weld
Accuracy STD parent material SDT weld material
OF and OFP OF1 and OFP material material

Cu_cal 99.99% rem. 99.9922 99.9922 0.0009 0.00015 0.00014

Ag 25 25 14.5 14.6 3.1 0.196 0.112
Al < 0.30 0.30 0.3 0 0
As 5 5 1.07 1.09 0.3 0.050 0.033
Bi 1 0.14 0.13 0.08 0.005 0.004
Cd < 1 0.00 0.00 0.004 0 0
Co < 0.03 0.03 0.03 0 0
Cr < 0.10 0.10 0.1 2.28127E-09 2.28127E-09
Fe < 10 10 0.80 0.80 0.8 1.82501E-08 1.82501E-08
Mn < 0.5 0.50 0.50 0.5 0 0
47

Ni 10 1.00 1.11 0.4 0.05 0.03

P 30-70 30-70 52.86 53.62 7.3 1.03 0.61
Pb 5 5 0.27 0.28 0.13 0.003 0.044
S 8 8 5.22 5.34 3 0.23 0.21
Sb 4 4 0.06 0.07 0.05 0.005 0.003
Se 3 2 0.20 0.20 0.2 4.56253E-09 4.56253E-09
Si < 2.67 2.32 2.1 1.09 0.44
Sn 2 0.05 0.08 0.04 0.004 0.004
Te 2 2 0.09 0.08 0.04 0.005 0.005
Zn < 1 0.30 0.30 0.3 0 0
Zr < 0.30 0.30 0.3 0 0

Spec. EN 1976 Cu- Average Parent Average Weld

OF1 and OFP material material
As+Cd+Cr+Mn+Sb 15 1.74 1.76
Co+Fe+Ni+Si+Sn+Zn 20 4.84 4.64
Bi+Se+Te 3 0.42 0.41
Se+Te 3 0.29 0.28
48
APPENDIX 2 STANDARD (ROUND BAR) CREEP AND TENSILE TEST SPECIMEN

130
23,5 12,5 3
50 40
B 45 45 A
5,7
0,8

Kartio
1:5

M16
I12
1 1

I10,1
I12,5
49

I10 0,02
Yleistoleranssi 0,1

0,05 A-B

3,2 0,8

Osa Nimitys Piir. n:o Aines Kpl Huom!

Kok.piir. Pinta Projisointi Suhde Pvm. Nimi
Toleranssit 1:1 Piir. 28.4.1994 TH
Paino Tark.

VIRUSAUVA M16 TIK941D

50
APPENDIX 3 - SPARK ERODED (SQUARE CROSS SECTION) CREEP AND TENSILE TEST SPECIMEN.
51
52
 53

APPENDIX 3 Cont.

Tensile testing results for EBW and parent material OFP copper

Figure 1. Initial shape of hot tensile tests of EB-welds

Figure 2. Initial shape of hot-tensile tests of parent material X259

54