The effectof reaction productlayerson copper corrosionin ...kyt2018.vtt.fi/copper_corrosion_2/Aromaa...

The effect of reactionproduct layers on copper corrosion in repositoryconditions

Jari Aromaa, Alexander Chernyaev, Vesa Lindroos, Atte TenitzAalto UniversityHydrometallurgy and Corrosion Research Group

Contents

• Introduction

• Environments and corrosion rates

• Copper corrosion mechanisms

• Oxide films and corrosion

• Corrosion tests

• Copper corrosion products

• Characterization tests

• Summary

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Introduction

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• The interior of the final disposal

canister is made of cast iron to

resist the mechanical stresses.

• The outer part of the canister is

made of nominally 49 mm thick

copper.

• The purpose of copper is to protect

the cast iron insert and the fuel

assemblies from the groundwater.

http://www.posiva.fi/en/final_disposal/basics_of_the_final_disposal/the_final_disposal_c

anister

Introduction

• Canister ensures containment of the spent nuclear fuel,

safety depends on mechanical strength of the cast iron

insert and corrosion resistance of copper.

• Buffer contributes to mechanical, geochemical and

hydrogeological conditions that are predictable and

favourable to the canister, and protect canisters from

external processes that could compromise the safety of

complete containment.

• Deposition tunnel backfill contributes to favourable and

predictable mechanical, geochemical and hydrogeological

conditions for the buffer and canisters.

Source: Posiva Report 2014-03

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Introduction

• Canister material is phosphorus-alloyed oxygen-free copper

with 30-100 ppm P.

• Nominal thickness of cylinder is 49 mm, bottom and lid

50 mm.

• Outer surface defects accepted if 35 mm copper thickness

remains.

• 5.6 - 8.0 tons of copper for each canister.

• Outer surface area 13.67 – 19.18 m2.

• Casting, hot forming and machining of tube, bottom and lid.

• Electron beam welding (EBW) or friction stir welding (FSW).

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Introduction

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• The alternative manufacturing methods are pierce and

draw, and extrusion.

• Starting from up to 16 ton billet.

• The pierce and draw process makes an integral base and

only the lid requires welding.

• Both the lid and base must be welded if the copper tube

is manufactured by extrusion.

Introduction

• From the perspective of corrosion behaviour, the important

characteristics of the initial state of the canister include:

• Nature and thickness of the surface film (oxide) on the copper overpack

• Nature and concentration of the surface contaminants

• Canister dimensions (corrosion allowance) and mechanical properties

• Maximum weld defect size

• Mechanical damage and cold work

• Level of residual stress

• Residual water and gas content.

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Introduction

• Hot processing causes oxidation of copper surface, these

films are removed by pickling before non-destructive tests

for quality control.

• The canisters components will be cleaned before assembly,

mainly to remove cutting fluid residues, but also other

impurities.

• The canister components are typically at room temperature

during the spent fuel encapsulation, but canister surface

temperature has been estimated to be 50-60 ºC, maximum

100 ºC.

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Source: Posiva Reports 2012-13 & 2012-16

Introduction

• The canister surface will have an oxide layer when

it is put into the disposal hole.

• The aims of the REPCOR project are:

• Produce oxide films on the surface of clean copper

• Characterize the oxide film composition and thickness

• Measure the effect of oxide film on corrosion rate in differentcorrosive environments.

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Environments and corrosion rates

• The corrosion loads for the canister are:

• atmospheric corrosion during manufacturing and storage

• aerobic corrosion in the deposition hole

• inner corrosion due to radiolysis of residual water

• outer corrosion due to radiolysis of external water

• localised corrosion (mainly due to Cl- )

• general corrosion due to sulphide ions from groundwater, buffer and backfill (including microbially-induced corrosion).

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• Corrosive environments during the encapsulation and

deposition process:

1. Canister manufacturing and assembly, atmospheric corrosionat ambient temperature.

2. Encapsulation, atmospheric corrosion in indoors, urban orunderground environment, elevated surface temperature.

3. Canister in unsaturated bentonite, up to 100 years, atmospheric and/or immersion, high redox, hightemperature.

4. Canister in saturated bentonite, porewater replaced byground water, up to 10000 years, immersion, redox and temperature decreasing.

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• The atmospheric corrosion of the copper shell during the

storage time before emplacement is estimated to be a

couple of months at most

• It is considered negligible in spite of the elevated

temperature of about 60-70 ºC in the storage facility.

• A layer of copper oxide with a thickness of a few tens to a

few hundreds of nanometres will form on the canister

surface.

• Even if the storage time would extend up to 2 years, the

total corrosion attack would be less that 1 mm.

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• Posiva Report 2011-01 gives (max.) pollutant levels as SO2

100 mg/m3, NO2 75 mg/m3, NH3 <20 mg/m3 and H2S <3 mg/m3.

• Time scale few weeks.

• Corrosion rates are based on literature: In urban

atmosphere 6-27 nm/a at 20 oC and 60-270 nm/a at 50 oC.

• The total corrosion attack even after two years storage will

be less than 1 mm.

• The most likely corrosion product will be copper oxide, not

stated whether Cu2O, CuO or both.

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• The corrosivity of the atmosphere depends on impurities

and time of wetness. Corrosion rate decreases with time.

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Category, ISO

9223, ISO 9224

1st year, mm/a 10 years, mm/a 30 years, mm/a

C1 <0.1 <0.05 <0.03

C2 0.1-0.6 0.05-0.3 0.03-0.2

C3 0.6-1.3 0.3-0.6 0.2-0.4

C4 1.3-2.8 0.6-1.3 0.4-0.9

C5 2.8-5.6 1.3-2.6 2.6-4.6

CX 5.6-10 0.9-1.8 1.8-3.2


• The emplaced canister will be covered by an air-formed

oxide with a thickness of a few tens to a few hundreds of

nanometres.

• The canister wall is expected to reach up to 100 ºC.

• RH is 50-80%, enough to cause condensation.

• The corrosion depth ranges from 90 nm in case of oxidation

of the surface to 90 mm in case of corrosion under a

condensation film.

• Maximum possible loss of thickness is estimated to be less

than 1 mm based on available oxygen.

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• Corrosion during bentonite saturation can lead to localized

corrosion due to uneven water saturation and bentonite

swelling.

• Areas with lower oxygen supply will become anodic.

• Saturation phase will take several years.

• Immersion in groundwater/pore water

• Evaporation and condensation of water causing

atmospheric corrosion.

• Dry deposits becoming moist and dissolving again can lead

to very concentrated solutions.

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• Corrosion analysis after water saturation phase assumes

mass transport of species to and from the canister surface

by diffusion through water-filled pores and unlimited water

on the surface.

• General change from warm and oxic to cool and anoxic

conditions.

• First increase in Cl- concentration from groundwater

infiltration to bentonite, later Cl- decreases.

• Corrosion is controlled first by oxygen and later by sulfide

compounds.

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Constituent Baseline

At closure,

infiltration into

unsaturated

bentonite

After closure

and saturation,

up to 100 years

After closure

up to 10000

years

pH 7.6-8.1 6.8-8 6.8-8 6.9-7.8

Redox, mV -300…-200 -250 to oxic -250…-150 -220…-170

Cl-, mg/L 6000-16000 2500-16000 2000-9000 300-3500

SO42-, mg/L <40 0-400 0-400 80-400

DIC, mmol/L <0.3 0.1-3 0.1-3.5 1-5

Na+, mg/L 2400-4800 1000-4800 1000-3300 250-1500

Ca2+, mg/L 800-4800 250-4800 100-2300 60-600

Mg2+, mg/L 25-70 40-150 70-150 20-200

K+, mg/L 10-20 5-20 5-20 5-20

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Posiva Report 2011-1, Potential hydrogeochemical conditions at Olkiluoto site


Constituent

Infiltrating

groundwater at

closure

After closure and

saturation, up to

100 years

After closure up

to 10000 years

pH 6-8 7-9 7-9

Redox, mV -250 to oxic -250…-150 -220…-170

Cl-, mg/L 1060-16000 1770-16000 280-350

SO42-, mg/L 0-400 3800 3800

DIC, mmol/L 0.1-3.5 0.3-3 0.3-3

Na+, mg/L 920-4600 6900-11500 6900-9200

Ca2+, mg/L 1200-4800 1600-16000 1600-16000

HS-, mmol/L 0-1 0-1.3 0-1.1

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Posiva Report 2011-1, Estimated bentonite porewater evolution at Olkiluoto site


• After emplacement of the capsule in the disposal hole

atmosphere can no longer be controlled.

• Posiva Report 2011-01 states that if oxygen supply is unlimited, corrosion rate is 100-300 mm/a.

• Dominant corrosion product most likely Cu2O.

• Assuming all oxygen in a disposal hole is used in coppercorrosion, the maximum even thinning would be 300 mm.

• Based on models, corrosion rate for oxic conditions is 7 mm/a.

• Aspö HRL results <100 nm/a at 75 oC, corrosion productCu2(OH)3Cl, possibly also Cu2O. (Taxén, Mat. Res. Soc. Symp. Proc. Vol. 807, 2004 )

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• Corrosion rates during bentonite saturation have

been reported using different bentonite-solution

setups and methods.

• Posiva Report 2011-01 references give 3 mm/a, 7 mm/afor oxic conditions, from 10-25 mm/a down to 1 mm/a with increasing chloride, and 30-50 mm/a.

• SKB Report R-13-13 0.2-1.3 mm/a, typically 0.4-0.8 mm/a.

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• Corrosion rates after bentonite saturation and

compaction.

• Posiva Report 2011-01 references give 0.06 mm after6000 years, from less than 6 mm to about 30 mm in 50000 years, and 38-86 mm after 105 years.

• SKB Report TR-13-17 gives 0.12-0.38 mm/a at 30-60 oCand 1.72 mm/a at 130 oC.

• Kinetic models by King et al. presented in Posiva Report 2011-01 show that corrosion depth is less than 0.1 mm and corrosion virtually stops after 100-200 years.

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Copper corrosion mechanisms

• Atmospheric corrosion is electrochemical with dissolved

oxygen as oxidant.

• 4 Cu + 2 H2O + O2 = 4 Cu+ + 4 OH-

• 4 Cu + O2 = 2 Cu2O

• In atmospheric corrosion the corrosion rate is controlled by

mass transfer of oxidant to the surface.

• The first product will be Cu2O that can react to other

compounds depending on the environment.

• In typical atmospheres this will be seen as copper surface

turning to brown or black due to Cu2O and then formation of

the colorful patina layer.

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Source: Krätschmer et al. Corrosion Science 44(2002), 3.


• Electrochemical corrosion follows mixed potential

theory.

• An oxidant in the system reacts cathodically and

this in turn starts the anodic dissolution of copper.

• The surface films on copper can affect the rates of

electrochemical reactions.

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• The electrochemical

corrosion of copper

follows mixed

potential theory.

• Increase in [Cl-] will

increase the driving

force.

• Increase in [O2] will

increase cathodic

reaction rate.

• Both will increase

corrosion rate.



• A steady-state model

of general corrosion

with varying [Cl-] and

[O2] shows icorr from

10-2 mA/cm2 in oxic to

10-5 mA/cm2 in low-

oxygen system.

• Roughly 0.1 mm/y in

oxic and 0.1 nm/y in

low-oxygen.

• Source: Posiva Report

2011-1

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Copper Corrosion

Model in oxygen

containing

compacted buffer

material by King et

al.

Source: Posiva Report

2011-1


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Copper

Sulphide Model

by King et al.

Source: Posiva

Report 2011-1


• Copper corrosion by formation of Cu-Cl complexes

• 2 Cu + 4 Cl- + 2 H2O = 2 CuCl2- + 2 OH- + H2

• 2 Cu + 6 Cl- + 2 H2O = 2 CuCl32- + 2 OH- + H2

• Copper corrosion under oxygen-free systems by

auto-ionisation of water:

• 2 Cu + H2O ⇒ Cu2O + H2

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Low equilibrium

constant k values, not

probable reactions.

Calculated with HSC 8.1

Reaction Equations

module.

See also King & Lilja,

CEST 46(2011) 2, p. 153.

Oxide films and corrosion

• Two corrosion test series and two oxide film

characterization series.

• First corrosion test series by Mr. Vesa Lindroos 2015.

• Second corrosion test series by Mr. Atte Tenitz 2016.

• First oxide film series by Atte Tenitz 2016.

• Second oxide film series by Mr. Alexander Chernyaev on-going 2017.

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Immersion tests to measure corrosion rates.

Glass reactor with glycol heater jacket

• Porvoon Lasilaite

QCM sensor and potentials

• SRS QCM 200 for mass change and Cu potential measurements, Pt counter electrode, SCE reference

• Hanna Instruments pH, DO and EC probes, WTW [Cu²⁺] probe

Acrylic reactor lid

• CNC-machined to fit all of the probes and gas inlet

• Sealable with original reactor clamp

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• Short time immersion tests, up to 16 hours.

• OL-SR synthetic groundwater acidified to pH = 4

with nitrogen bubbling.

• DO levels typically 2.5 ppm (room temp.) and 0.5

ppm (50 ºC) before test.

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• Fresh copper, OL-SR, pH = 4, 25 ºC, 191±103 mm/a.

• Fresh copper, OL-SR, pH = 4, 50 ºC, 985±60 mm/a.

• Oxidized 16 h 25 ºC, OL-SR 25 ºC, pH = 4, 920±170 mm/a.






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• The base solution was OL-SR synthetic ground water.

• OL-SR water total dissolved solids is 14500 ppm, moreconcentrated solutions were 34500 ppm and 54500 ppm.

• pH-levels 4, 6 and 8.

• Temperatures 40, 60 and80 oC.

• Air or nitrogen purging during the 24 hour test.

• Electrodeposited copper on QCM crystals

• First series for copper, second for copper oxidized at

90 ºC for 7 days.

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y=-0.0026xR²=0.99656

-250

-200

-150

-100

-50

0

0 7200 14400 21600 28800 36000 43200 50400 57600 64800 72000 79200 86400

Mass

loss

,m

icro

g/c

m2

Time,s

Copper,S=14500ppm,T=45C,pH=4,air.


S = salinity ppm, T = temperature ºC, gas: air = 1, N2 = 0

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Copper mm/a = -431.4 + 0.004509´[Cl ]+ 4.933´°C+

+611.5´ gas- 0.005518´[Cl ]´ gas-8.197´°C´ gas

Oxidized mm/a = 381.4 + 26.39´°C+357.8´gas-22,80´°C´gas


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MLR model measured vs. predicted thinning mm/year.


• Corrosion rates in room temperature OL-SR water under

nitrogen purging were 1-2 mm/a for copper and oxidized

copper, several hundred mm/a in hot, oxic solution.

• Corrosion rates were high and variation was large

• Copper 1-670 μm/a

• Oxidized copper 5-2100 μm/a

• Copper in nitrogen purged 1,4-91 μm/a

• Oxidized copper in nitrogen purges 2,6-141 μm/a

• Large variation in aerated conditions.

• Increase in aeration increases corrosion rate.

• Increasing pH decreases corrosion rate.

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Copper corrosion products

• Copper exposed to air containing moisture and

pollutants will form various corrosion products on

surface.

• Cuprous oxide (Cu2O) forms at an early stage of the

corrosion process.

• Further oxidation produces new layer of cupric oxide

(CuO) that grows preferentially over the Cu2O layer.

• Eventually, corrosion products on copper change to a

stable patina, whose composition depends on the

anions in the environment.

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• The outer patina layer is usually precipitated basic

Cu(II) compounds such as:

• Atacamite or Paratacamite Cu2(OH)3Cl (chloridecompound)

• Brochantite Cu4(OH)6SO4 (sulfate compound)

• Posnjakite Cu4(OH)6SO4·H2O (sulfate compound)

• Malachite Cu2(OH)2CO3 (carbonate compound)

• Copper sulfides, mainly Cu2S, can form on copper

surfaces in atmosphere containing H2S or in a

solution containing S2- ions.

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• Copper oxides can be

reduced in very alkaline

solution.

• The oxides can be

separated as long as

they are not too thick.

• The examples are for

approximately 1 mm films

and 1 cm2 samples.

• Scan rate 1 mV/s.

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S. Nakayama et al. J.Elchem. Soc., 2001.


• Electrochemical reduction of copper compounds:

• Cu2O + H2O + 2 e- 2 Cu + 2 OH-

• CuO + H2O + 2 e- Cu + 2 OH-

• Using the charge from reduction tests the

thickness of oxide film can be calculated using

Faradays law and oxide density.

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• Cu-OF copper samples embedded in epoxy.

• Polishing with 1200 grit sandpaper, immersion in 10% citric acid for 2 minutes three times with rinsingbetween dips, followed by rinsing with distilled waterand ethanol, and dried with hot air.

• Electrochemically deposited copper on QCM

crystals.

• Rinsing and drying after deposition.

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A1 = Cu2O

A2 = CuO

C1 = CuO

C2 = Cu2O

C4 = unknown,

appeared in some

very oxidized

samples

-1.5 -1.0 -0.5 0.0 0.5

-0.05

0.00

0.05

0.10

0.15

0.20

C2C1

A2

I (A

)

E (V vs. Ag/AgCl)

s1

s4

A1

C4


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Background current density ∼0.5 mA/cm2, no reduction peaks.


• Cu-OF molded in epoxy and QCM crystals

• Fresh or oxidized at 100-110 ºC for 1, 3 or 7 days.

• Immersion in air or nitrogen purged OL-SR

groundwater at 40, 60 or 80 ºC.

• Samples in air for 1-3 days 29-160 nm Cu2O.

• Samples oxidized in oven 100 nm Cu2O.

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Oxidation (days) Thickness (nm)

Sample Oven Immersion T = 40 C T = 60 C T = 80 C Oxide

Crystal 1 1 360 510 1200 Cu2O

3 1 670 1100 900 Cu2O

7 1 490 1300 1200 Cu2O

Copper 1 1 480 1500 2100 CuO/Cu2O

3 1 600 1000 1600 CuO/Cu2O

7 1 500 900 1700 Cu2O


• Cu2O was the dominant oxide in almost all tests.

• Small amounts (10 nm) of CuO reduced in the tests

with water temperature 40 ºC and the samples were

oxidized in oven for one and three days.

• No CuO was reduced on samples which were

oxidized in oven for seven days before immersion

test.

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Oxidation products

on copper after 24 h

immersion in aerated

OL-SR groundwater

at 40 ºC.

-1.6 -1.4 -1.2 -1.0 -0.8 -0.6-0.10

-0.09

-0.08

-0.07

-0.06

-0.05

-0.04

-0.03

-0.02

-0.01

0.00

I (A

)

E (V vs. Ag/AgCl)

s2-T2

s2-T1

s3-T3


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Oxidation products



OL-SR groundwater

at 60 ºC.

-1.6 -1.4 -1.2 -1.0 -0.8-0.12

-0.10

-0.08

-0.06

-0.04

-0.02

0.00

I (A

)

E (V vs. Ag/AgCl)

s1-T1

s3-T2

s5-T3

s4-T3

s3-T2


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Oxidation products



OL-SR groundwater

vapour at 60 ºC.

-1.6 -1.4 -1.2 -1.0 -0.8

-0.14

-0.12

-0.10

-0.08

-0.06

-0.04

-0.02

0.00

I (A

)

E (V vs. Ag/AgCl)

s4-T1

s5-T1

s4-T2

s5-T2

s6-T2

s1-T3C2

C3


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Oxidation products

on copper first

oxidized at 90 ºC for

7 days and then 24 h


OL-SR groundwater

at 60 ºC.

-1.6 -1.4 -1.2 -1.0 -0.8-0.07

-0.06

-0.05

-0.04

-0.03

-0.02

-0.01

0.00

I (A

)

E (V vs. Ag/AgCl)

s4-T1

s5-T1

s6-T1

s1-T2

s5-T3

s6-T3


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Oxidation products

on copper first

oxidized at 160 ºC

for 24 hours and

then 24 h immersion

in aerated OL-SR

groundwater at 60

ºC.

-1.6 -1.4 -1.2 -1.0 -0.8 -0.6 -0.4-0.3

-0.2

-0.1

0.0

0.1

0.2

I (A

)

E (V vs. Ag/AgCl)

s5-T1

s6-T1

s1-T2

s2-T2

s4-T3

C1

C2

A1


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0

20

40

60

80

100

120 120°C 24 h oven

120°C 48 h oven

160°C 24 h oven

40°C 24 h SGW

60°C 24 h SGW

90°C 7 d oven + 60°C 24 h SGW

160°C 24 h oven + 60°C 24 h SGW

60°C 24 h in SGW vapor

Film

thic

kness (

µm

)

Summary

• In the corrosion rate analyses the estimated

corrosion hasdecreased during last 20 years.

• The estimated general corrosion rates are in the

range 1-3 mm/a, often less than 1 mm/a.

• Deep pitting is not considered probable.

• The combined effect of different stages on loss of

thickness is usually maximum few millimeters for

105 or 106 years.

• Some situations can result in high corrosion rates,

but these are expected to be short.

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Summary

• Short time tests to estimate the effect of

environment and oxide layer by using QCM tend to

produce corrosion rates that are often much too

high compared to long-term studies.

• Especially the hot, acid and aerated systems tend

to result in high and varying corrosion rates.

• The oxidized samples lose weight faster than clean

copper surfaces.

• The thickness of the copper oxide layer shows very

strong variation from less than 1 mm to tens of mm.

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References• POSIVA 2011-01, An Update of the State-of-the-art Report on the Corrosion of

Copper Under Expected Conditions in a Deep Geologic Repository. Fraser King,

Christina Lilja, Karsten Pedersen, Petteri Pitkänen & Marjut Vähänen, July 2012,

246 p.

• POSIVA 2012-13, Canister Design 2012. Heikki Raiko, April 2013, 156 p.

• POSIVA 2012-16, Canister Production Line 2012. Design, Production and Initial

State of the Canister. Heikki Raiko, Barbara Pastina, Tiina Jalonen, Leena Nolvi,

Jorma Pitkänen & Timo Salonen, December 2012, 174 p.

• POSIVA 2014-03, Safety Case for the Disposal of Spent Nuclear Fuel at Olkiluoto

FEP Screening and Processing. Posiva Oy, January 2014, 148 p.

• SKB TR-13-17, LOT A2 test parcel. Compilation of copper data in the LOT A2 test

parcel. Paul Wersin, December 2013, 28 p.

• Atmospheric Corrosion of Copper 450 Metres Underground. Results From Three

Years Exposure in the Äspö HRL. Claes Taxén, MRS Proceedings, 807, 2003.

doi:10.1557/PROC-807-423.

• Scientific basis for corrosion of copper in water and implications for canister

lifetimes. Fraser King & Christina Lilja. CEST 46(2011) 2, pp. 153-158.

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