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FAILURE

ANALYSIS
REPOR
T

Case Study
Group 1
StudBolt Failure
dueto
Hydrogen
Embrittlement

TechnicalRepor
t

MetallurgyandMaterialDepartmentmakesnorepresentationsorwarranties,eithe
r expressedorimplied,

andspecificallyprovidestheresultsofthisreportasisbasedon
theinformationprovidedbyclient

Executive Summary
PT.SulzerTurboServicesIndonesiareportedthatitsstudbolthad

failedinservice.

AsreportedbyPT.SulzerTurboServicesIndonesia,thefailure

occurredonthe

threadpartofthestud bolt.Thethreadwaslocatedonbothendsofthestudboltbut thefailed


partonly occurredonone endofthestudbolt.Ourstudy showedthatthe studbolt failed
due

to

hydrogenembrittlementthatresultedfromitslongexposureto

atmosphere

duringoperation.

oflocalizedprecipitatesinthe

Thepresenceofthe

failedstudboltacceleratedthe

hydrogengas

areawitha

number

failurebecausethis

localizedprecipitates wasthemostfavorablesitefor hydrogenmoleculesthatcame from


the inner container to re-combined

and then

produced the pressurized

hydrogengas in themetal. Once this pressurized hydrogengas existed,it weakened


the

bondingbetween

metalatoms.As

aresult,thestudbolt

materialfracturedin

brittlemode.Inmostcases,oncethehydrogengasis
formedinthemetalandandweakensthemetal atombonding,thecrack propagationwould
occurautomatically withoutthe external stress becausethis produced hydrogen has
enough pressureto create andpropagate thecracks.

Background Information
PT.

SulzerTurboServicesIndonesiareportedthatitsstud

service.AsreportedbyPT.SulzerTurboServicesIndonesia,the

bolthad

failedin

failureoccurredon

thethread part ofthestud bolt. Thethreadwaslocatedon both ends ofthestudbolt


butthe

failedpartonly

occurredononeendofthestudbolt.Principally,theboltis

usedtojointwo parts likeflange or others. Thebolt hastwo(2)similar nuts on each


endwhichistightenedduring

application.Figure1illustratesthe

principalworkof

studboltinjoiningmethod.ThefailedsamplewasthensubmittedtoCMPFAfor
failure analysis(Fig. 2).

Objectives
The assessmentwas carried out in Metallurgyand Material Department,
University

ofIndonesia,inordertofindouttherootcausefailureofstudboltandto

make

recommendations.
Thescope ofwork wasasfollows:

1. .
2.
3.
4.

InvestigationResults
Visualexamination
The failedstud bolt was visually
condition(Fig.1).Forabetter

examined

and photographed in

as-received

examination,thefracturesurfaceofthefailedstudbolt

wasobservedbyopticalmicroscopeatmagnificationof7X(Fig.2).Asobserved
fromthemacrophotography,thecrackseemstobeinitiatedfromaspotatthe
threadandtopropagateinacircumferentialmode.Thecracksurfacehadawide
smooth area(crackpropagationroute) androugharea(final rupture).

Chemical
Test
Inorder

Composition

toobtaininformation

aboutthechemical

subjectedtothechemicalcompositiontest

composition,thesamplewasthen

usingOptical

EmissionSpectroscopy

(OES).Table1showsthechemicalcompositionoffailedsamplein

comparisonwith

ASTMA564Grade 630.Theresults revealthatthere isaslight differencebetween


thenickel(Ni)contentsinthetestedsample

andtheoneinthestandard.

Thetested

samplecontains 5.13%Ni,whichis 0.13% higher thanthe maximum nickelcontent


allowedforASTMA564Grade30
withthestandard

material(3.0-5.0%Ni).Theother

materialrequirement,

as

elementscomply

canbeseeninthetable.Thisslight

differenceinnickelcontentmay notsignificantly impairthemechanicalproperties of


thestud bolt.Nickel isintentionally addedtointroduce the toughness intothis type of
material.

Tensile Test
The tensiletest was

conducted to

obtain the information about

mechanical

properties ofthe bolt, i.e.tensilestrength, yieldstrengthand elongation. Table2


showsthetensile

propertiesofsampleincomparisonwithASTM

A564Grade630.

Thetensilestrengthofthe failedtestedsampleis1245MPa,whichisabout65MPa below


thestandard

material.Itsyieldstrengthis1225MPa,whichis55MPahigher

overthestandard

materialanditselongationis

than

10.86%(0.86%higherthanthe

standardmaterial.

Hardness test
Toobtainanother

mechanical

propertiesinformation,hardnesstestwasperformed

onthefailedsample.Table3showsthehardnessvalueofsampleincomparison
withASTMA564Grade630.Theresultshowsthatthehardness
theminimumvaluerequiredby

valueisslightly

thestandard.Thefailedsamplehasa

below

hardness

valueof38HRCwhile thestandard is 40HRC(minimum).

Metallographicanalysis
Themetallographictestwascarried out onthecross sectionofthefailed thread.The
testwasinaccordancewithASTME3

forthemetallographicpreparationtoobserve

thegrainofthetestedmaterial.Thesamplewas etchedusingAquaRegiasolution.

Informationobtainedfromthe

microstructure

photosisthat

studboltcontainsmartensitephases.Thecrackpropagating

the

basematerialofthe

along

thegrain

boundarywas observed onthefailedsample.

Fractographyanalysis by SEM and EDS


The

fracturesurface

wasobservedusingScanningElectronMicroscopy

(SEM)to

gathermoreinformationabouttheinitialcracksandotherrelatedfactorsaffecting the mode


offailure.

TheEDSanalysiswasalsoperformedonthe

fracturesurface

analyzeanypossiblecontributionofenvironmentormicrophaseofthematerialto

to
the

failure.Thecrackpropagatingfromthethreadwasobservedonboththefracture
surfacesofthefailedsample.Figure 8 and9 showthe propagatingcrack.
The

fracturesurface

sincenoevidence
indicatethat

observed

fromSEMimagesindicatesthatitisbrittle

ofdimpleslocatedinthe

the

fracturemodeisductile.

transgranular.Intergranularbrittle
thegrainboundaries.

fracturearea.

fracture

Thepresencesofdimples

Brittlefracturecanbe

intergranularor

fracturecanbetheresultofembrittlement

along

Precipitateswerefoundwithinthematrixofbase
hardenedstainlesssteel;itmainly

composed

metalsinceitisaprecipitateofFe-Cr.Butan

thattheprecipitateswithinthefailedsamplewereconcentratedat

anomalywasfound
onepoint.Some

precipitateswereaccumulated at some spot onthe thread edge.Table 4showsthe


EDSresultsofthetestedspot.Theseinhomogeneouslydispersedprecipitateswere
observedusingBackscatteredSecondaryElectron(BSD).Somecrackswerefound
tobeinitiatedfrom these precipitates.

Based

ontheEDSresultsshowed

onTable

4and5,thecompositionofFe

andCr

thedark spotandthe basemetal is quitethesame.Itcanbeconcludedthatthedark


spotsare precipitatethatcomposedofFe andCr.Precipitates, incaseforthis stainless
steel,

areintroducedtogivestrengthtothematerial.

Some

disadvantages

arethenfoundiftheyarenotwelldispersed(inhomogeneous).
The accumulated precipitates could generate weak areasincestress concentration
willbelocatedonthatspot.Thiswillbetheinitialspotforfatiguecrackpropagation.
Afatiguecrackwilltypicallyinitiateatadiscontinuityinthematerialwherethecyclic
stressismaximum.Sincethestudboldexperiencedthetensilestressandalso
vibrationduringapplication,thecombinationoftensilestressandvibrationcould
facilitate thefatiguefailure tooccur..

Discussion
Thestudboltiscommonly usedasa fastener tojointwoparts altogether;thepart suchas
flangeisjoinedusingthiskindofbolt(seeFig.1).Based
compositiontest(see

Table1)

thestud

onthechemical

andmetallographicexamination(seeFig.

5,6&

7),

boltwasmadeofprecipitated-hardenedstainlesssteel

withmartensitephasematrix.TheEDSimage

analysis

results

showed

thattheprecipitates(seeFig.
11) mainly composed ofFe-Crthatcame fromthealloying elementsofthestainless
steel.Inpractice,whenthenutisfastened,astress(tensile)isthenintroducedto
thestudbold.

Sincetheboltwasapplied

onaturbine

part,thevibration

during

operationcouldbealsotransferredtotheboltgeneratingacyclicload.

its
The

combinationbetweenatensilestressandavibrationcouldpossiblytriggerthe
fatiguefailure.
Theboltswereappliedontheturbinesystemconsumingfuelmainlycomposed
nitrogen(N2)andhydrogen(H2)withsmall

of

fractionofargon(Ar),methane(CH4),

carbondioxide(CO2)andcarbonmonoxide(CO).Thecorrosivegasinthissystem

isCO2.However,stainlesssteelisrelatively

resistanttoCO2corrosion.Noevidence

ofcontamination fromchloride(Cl) and hydrogen sulfide (H2S)werefound on the


failedsample.

Themechanicalproperties(seeTable2&3)test

showedthatthe

tensilestrengthandhardnessofthefailedsampledidnotconformtotheASTM

A564Grade

630materialwhiletheyieldstrengthandelongation did.Pleaseremind that thetensile test


was performed on the failed part of stud bolt. The lowmechanicalproperties may
indicatethatanexcessivecrackhaspropagatedinthe
decreaseinthemechanicalproperties

material,leadingtoa

whenitwastested.A

new

materialwhichcanbetakenfromthestudboltwiththesame heatnumberand has notbeen


used is basically required to evaluate the issue of the use of downgradematerial.
Inadditiontothevisualexamination,thefractographyoffailedsamplewasalso
examinedusingSEM

andEDSto

obtaininformationaboutthecracksurface.Based

ontheSEMimages(seeFig.8&9),the cracksinitiated fromthethreadedge propagating


circumferentially.

Thecrackspropagatedintergranularlyalong

boundarygeneratingthebrittle
(Backscattered)

image,

fracturemode(seeFig.5&

thegrain

6).BasedontheBSD

precipitateswerefoundinhomogeneouslydispersedwithin

thethread(seeFig.

14);someprecipitateswereaccumulated

generating

stress

concentrationspotonthethread(seeFig.12&13).Thehard precipitated particles could


beafactor

forcrackinitiationsinceamaximumstresswillbemainly

focusedonthoseparticleswhenthestressis
effectwillbecatastrophic

ifthe

workinginthe

precipitatesare

bolt.BasedontheSEM

accumulatedat

material;

accumulated

or

moreover,this

atcertainspotonthe

observation,anumberofprecipitates

werefoundatthethread(seeFig. 13);that makethis locationastheweakestspot andcould


fail

duetocyclic

load(fatigue).Nevertheless,it

mightbe

notindicatingthat

fatiguewastherootcauseofthefailure.Itwaspossiblytriggeredby

otherinitiation

sinceverylittle evidencefounduponthefacture surface.


Theindicationofembrittlement

duetohydrogenwas

SEMimages,thecrackspropagated
dimplewere

also

observed.Based

alongthegrainboundary.

onthe

Noevidences

observedonthsductilematerialthusindicating

of

thatthecracks

propagatedduetoembrittlement(seeFig.15).Theatmospherecontainshydrogengas(H2)
thatpossiblybethesourceofhydrogenatomsdiffusingintothemetal
matrixcreatingembrittlement.

Ascan beseeninTable 6, hydrogengasmakesup almost 74% ofthetotal gas


compositioninthesystem.Inthiscase,the
impurities.

othergases

may

beconsideredasthe

Severalliteratureshavereportedtheeffectsofhydrogenembrittlement

gaseousimpurities.Gasimpuritiescaninhibit,accelerate,
hydrogenembrittlement.Asdocumentedelsewhere,CH4

of

orhavenoeffectupon
andN2

gaseshaveno

effectonhydrogenembrittlement,H2SandCO2gases act as accelerators of hydrogen


embrittlement[6].
Along

exposureofthemetallikethestud

bolttothehydrogengasinthecontainer

could

promotethehydrogenatomsto
migrateintothemetalmatrix.Someofthehydrogenatomsre-combinedwithcarbon atoms
toformmethane

gas(CH4)inside

methanegascreatedpressurewithinthe
thatcouldreducetheductility
withintheminuscule

ofa

minusculevoids(see

Fig.17)

metalcreatingembrittlement.Not

voidswherehydrogenwaspresentbut

boundariessincetherewerealsocavitiesdue
direction.

minusculevoids.The

tothedisorder

also

only

withinthegrain

arrangementofatomic

Thefailedstudboltwasexposedtotherelatively

hightemperature

Accordingtotheliterature,underambient

(around160C).

temperature,hydrogenatomscanbe

absorbedtothe metallatticeanddiffusethroughthegrainboundaries.Thecrack inducedby


stress

underthisconditionwillpropagatetransgranularly.Otherwise,

hightemperature,theabsorbed

under

hydrogenatomstendtogatherinthegrain

boundariesandthecrackswill

propagateintergranularly[4].Someresearchers

describethetheappearanceas beingsimilartobrokenrockcandy [9].Thistypeof broken


rock candy-like fracture can be seen in Figs. 20 and 21.In addition,the
hydrogeninthecontainer also diffusesinto the metal,gravitating towardsthe area
withthegreateststress

[8].Inthecaseofthis

failedstudbolt,the

areawiththe

greateststress isthe areacontaininga localized precipitation(seeFig. 11).


ASMEBoilerandPressureVesselCommittee[10]establishedthe
container

projectteamin2004statesthatthe

hydrogenstorage

maximumworking

pressure

systemis103Mpa,whichismuchhigherthantheactualworkingpressurein
system,i.e.

around6Mpa(around60Bar).

Thus,thereis

forthis
Sulzers

noissueof

overpressurecontributingto thefailure.

Conclusion
Thestudboltfailed duetohydrogenembrittlementthatresulted fromitslong exposureto
hydrogengas

atmosphereduring

operation.Thepresence

withanumberoflocalizedprecipitatesinthefailedstudbolt
becausethislocalizedprecipitates
moleculesthat

acceleratedthefailure

wasthemostfavorablesitefor

camefromtheinnercontainertore-combined

ofthearea
hydrogen

andthenproducedthe

pressurizedhydrogengasinthe metal.Once this pressurizedhydrogengas existed,


itweakenedthebonding
fracturedina

betweenmetal

atoms.Asaresult,thestudboltmaterial

brittlemode.Inmostcases,oncethehydrogengasisformedinthe

andandweakensthe

metal

metal

atombonding,thecrackpropagationwouldoccur

automaticallywithoutthe externalstress becausethisproducedhydrogenhas enough


pressuretocreateand propagate thecracks.

Recommendations
1. Usethematerial withtheunwantedprecipitates as lowas possible.
2. Athouroughmaterial selectionstudyalongwith thelaboratorytestare
commonlyrequiredforthematerials thatwould becontinuouslyexposedto
hydrogengas.

Reference
1. FatigueFailure ResultingfromVariableLoading(http://highered.mcgrawhill.com/sites/dl/free/0073121932/365766/chapter06.pdf )
2. Fractography,ASM Handbook Vol 12,ASM International,OH.
3. http://www.corrosionist.com/hydrogen_embrittlement_stainless_steels.htm
4. http://events.nace.org/library/corrosion/Forms/embrittlement.asp
5. http://www.contech.com/Failure_Analysis.htm
6. Barthelemy,H.EffectsofPurityandPressureonTheHidrogenEmbrittlement ofSteel
andOther Metallic Materials. AirLiquide.
7. http://events.nace.org/library/corrosion/Forms/embrittlement.asp
8.http://www.ehow.com/info_8402999_effects-hydrogen-embrittlementsteel.html
9. Greenslade,Joe.2005.HereisWhataHidrogenEmbrittlementFailureReally
LooksLike.Distributors LinkMagazine,Spring
10.Jinyang, Zhenget al. 2012. Development ofHigh Pressure Gaseous
HydrogenStorageTechnologies.ScienceDirect.