16

of 175C and 162-173 C respectively. POM is

semi crystalline polymer with 75-85 %degree of
crystallinity.
Asengineeringplastics, PolyOxyMethylene
(POM) has two types, homopolymer and
copolymerwhichdiffer slightlyinitsmeltingpoint
INTRODUCTION
Kala Kunci: Analisisretak, Polioksimetilen,Derajatkristalinitas,Termal
ANALISISRETAK POLIOKSIMETILEN MENGGUNAKANSCANNING ELECTRON
MICROSCOPE, ANALISIS TERMAL DAN PROSES. Analisis retak dilakukan menggunakan
Scanning Electron Microscope (SEM) danDifferential Scanning Calorimetry (DSC). Perbandingan
karakteristikbahan antara sampel NG dan standar dilakukan. Analisis SEM menunjukkan bahwa
permukaanretakanpadasampelNGcenderunglebihmudahpatahdibandingkanretakanpadasampel
standar. Retakan didugaberasal dari vicinity gate location. Derajatkristalinitas patahan NGadalah
59,6%lebihrendah dibandingkandengan sampel standard65,8%. Tidakadaperbedaan yangjauh
antarasuhuleleh (164C) dengansuhukristalisasi (1460C).Perubahandanjalur patahan disekitar
gate location berpotensi menyebabkanretakan selamaproses. Berdasarkan hasil SEM dan DSC,
retakandidugaberasal dari setting proses yang tidak tepat yangmenghasilkan derajat kristalinitas
yang rendah danJrozen-in stress. Beban luar yang diterimajuga merupakan salah satu penyebab
terjadinyaretakan.
ABSTRAK
Keywords: Failure, Polyoxymethylene,Crystallinitydegree, Thermal
FAILURE ANALYSISONPOLYOXYMETHYLENE PRODUCT USINGSCANNING
ELECTRON MICROSCOPE, THERMAL ANDPROCESSING ANALYSIS.Failureanalysisof
PolyOxyMethylene(POM) product werecarried out usingScanningElectronMicroscope (SEM),
Differential ScanningCalorymetry(DSC) andparameter processrelatedfactors. Comparationof the
failuremodeandmaterial propertiesbetweentheNGandProvensamplesweretaken. SEM analysis
showedthat failure surfacetent to have more brittle fracture compared with the proven sample
failure.Theoriginof crackwaspredictedfromthevicinityof gatelocation. Degreeof crystallinityof
failurepart was 59.6%, which was lower than the proven products (65.8%). Melting (Tm) and
CrystallizationTemperature(Tc)showednosignificantdifferences, 164Cand146Cformeltingand
crystallizationtemperaturerespectively. Whiteningandmoldedstreamflowwereshownaroundthe
gatelocationwhichpotentiallycausedmoldedinstressandcrackpropagationduringapplicationin
chemical environment. External loadalsofoundinthevicinityof crack. BasedontheSEM, DSC and
process related factor analysis, the failure of product was supposed due to the combination of
impropersettingprocesswhichresultedinlower degreeof crystallinityandfrozen-instress around
thegateandexternal loadreceivedhavetriggered thecrack onproduct.
ABSTRACT
Accepted: 13December 2013 Revised: 13November 2013 Received: 19July 2013
R.Wijaya, A. Rifathin and B. Afrinaldi
Centerfor Polymer Technology(STP) - BPPT
Kawasan Puspiptek; Serpong 15314, TangerangSelatan
FAILURE ANALYSISON POLYOXYMETHYLENE
PRODUCT USING SCANNING ELECTRON MICROSCOPE,
THERMAL AND PROCESSING ANALYSIS
Vol.17, No.1, 2014, hal: 16-19
ISSN: 1410-7864
Majalak Polimer Indonesia
17
approximately10mg,placedintoaluminacrucible.
ThealuminacruciblewasthenplacedinThermal
GravimetryAnalysis(TGA) instrumentation. The
test isconducted under temperature program as
follow: Firstly the sample was heated up from
temperature of 50to 600D C under nitrogen gas.
Thetemperature washeldat600D C for5minutes
nitrogen gasenvirontment. Thetemperature was
then continuing heated up until 900 D C under
oxygen gas. The rate of heating was 10D C per
minute, andthenitrogen/oxygengasflowratewas
50 mL per minute. After measurement was
completely finishedtheTGA-thermograms were
analyzed.
DSC821-Mettler Toledo was used to
measurethethermal propertiesof thesamplessuch
as melting point, glass transition temperature,
thermal history, degree and the growth' of
crystallinity. Thetestwasconducted accordingto
ASTM D 3418-2003. Sample was cut and
weighed approximately 20 mg, placed into Al
crucible. TheAl-cruble was then placed inDSC
sample chamber. The test is conducted under
nitrogen gas environment with temperature
programof "heating-cooling-heating" asfollow:
thetemperature program was started from30to
200 "C, then cooled down to-100Candfinally
heated up to 200 C. The rate of heating was
10-cper minute, andthenitrogen gasflowrate
was 50 mL per minute. After the test was
completely finishedtheDSC-thermograms were
analyzed.
Figure 2. FTIR test results of NG and proven
samples
i I
~' -,-
._
Thefailure POM product was received as
failured-part appliedinmotor cycle.
To identify the main material, possible
degradation andsemi quantitatively analysis the
material composition, we used FT-IR-Bruker
Tensor 27, ATR method. Placed the sample on
ATRcrystal. Touchedthesamplesurfaceperfectly
onthecrystall bysetting downthestainless steel
tip. Samples analysis werecarried out byOPUS
software(Figure2).
To measure the material composition.
Thetest was carried out inaccordance toASTM
1131-1998. Sample was cut and weighed
EXPERIMENTAL METHOD
Figure 1. Frozen-inorientation(top) andpoten-
tial shrinkagenear tothegate(bottom)
t Edge p.le
\\~I
\ I '>:
~I/ :/'_____
POM aregenerally processed ininjection
molding with special runner system. Hot runner
types are commonly applied in POM. Wrong
selection of runner type could result in loss of
pressureduringprocess. Toovercomethepressure
reduction, operators usually increase the
temperature. Unfortunately this could severethe
material todegradation.
The melt entering the cavity will form
orientationduringfillingphase.Andmelt adjacent
tothemoldwill freeze:firstandleadtohighinterfacial
shear stress between themelt andthesolid layer.
Thisfrozen-inorientationwill continuetodevelop
duringholdingpressureinordertocompensatefor
volumeshrinkage, particularlynearthegateregion
of thepart (Figure 1). However, fast cycle time
during production is required. Those process
parametersinfluentthemicrostructureof partwhich
alsoaffect theproperties andperformances.
In this paper, we analyzed the effect of
settingprocesstothermal propertiesascontribution
of potential causesof failurebyobservingthecrack
pattern onthefailedsurface.
Failure Analysis on PolyOxyMethylene Product Using Scanning Electron Microscope, Thermal and Processing
Analysis (R. Wijaya)
Figure 4. DSCtestresultsofNG (a) andproven
(b) samplesoncoolingphaseafter first heating
'---';"::;';';;"j
,
_ _ _ _ _ _ _ _ . ' . _ H ._ _ , ' _ " ' _ _ . . . , _ . _ _ _ . _ _ _ , _. ._ ' . .
~: I" to ~, (;~.
!.... ~
.., .
.~-- ..... --....... ~-----"":;-;.;~=. ~~--=,~--""""u=~=,:=,
;~~.:;;::~:.;\.~- ~-::::;i:'!~;~~_,.:. ..
_-6l"l.'Ii
\ ,)'U~'.ll':<;;:.~
\
\.
:.;.~
/ \
!\
:1 (a)
--_ .._----,._-------,
:
___ ._" .1
Figure 3. DSCtestresultsofNG (a) andproven
(b) samplesonheatingphase
--_.._---------
.. '" , ., ""
..._.", , ';j
:
~'"':' ...:...:"._-;=-~-- .. _--- ... ~--.-.-~.-.-.-------."-.'--.-----.-- .. -.
~ ._..._( -._..- ,
:. !:-<" " , ~, -,
18
Degree of crystalinity of the NG sample
showalittlebitlower(Figure3),whilecrystalization
rateishigher andthecrystal distribution (which
indicates thesizeof crystaline) islower thanthe
provenone. (Figure4)
Figure 5shows crack that occurednear to
thegate. Smoothlbrittle patternof crack foundon
thecracksurfaceofNG sample. Ontheotherhand,
thefracturepatternof provensampleshowedmore
ductile(seeFigure6).
Crack supposed initially occuredfromthe
outer totheinner surfaces andwascausedbythe
extemalload.Thiswasshownwithwhiteningcircle-
likedefect onouter surface (seeFigure4).
Lowerdegreeof crystallinitywhichisfound
ontheNG sample isusually related tohigh the
Test M ethods Proven sample NG sample
FTIR, polymer type Polyoxymethylene Polyoxymethylene
TGA , % polymer 100 99.99
DSC
Heatingphase
M eltingpoint (OC) 164.51 164.06
DeltaH (Jig ) 156.1098 149.6349
Crystallinity (%) 65.8 59.6
Coolingphase
TempofCrytalline 145.80 146.45
C C C )
Crystallinerate 0.31 0.29
(min)
Crystallinedistr 0.38 0.32
(min)
Table 1. Comparativetest results of NG and proven
samples.
.Nosignificance differences onspectra of
NG and proven samples. Both show the POM
material accordingtoOPUS softwareanalysis.No
degradation is indicated both samples. Table 1
shows theresults of FT-IR, TGA and DSC.
RESULTS A ND DISCUSSION
ScanningElectronM icroscopy J EOL J SM -
6510LA was applied to observe the fracture
surface inorder to see the crack initiation and
propagation.
Inordertoanalyzetherootcausesof failure,
thecomparativemethod between thefailureand
thenewprovenproduct arecarriedoutonthetest
results.
VoL17, No.1, 2014, hal: 16-19
ISSN: 1410-7864 Majalah Polimer Indonesia
19
REFERENCES
[1]. DuPont, 2008, Problems withHot Runners.
[2]. DuPont, DuPont Delrin acetal resin
MoldingGuide:Technical Information.
[3]. ARCHODOULAKI VM, LUFTL S,
KOCH T, SEIDLER S, Property changes
inpolyoxymethylene (POM) resultingfrom
processing, ageingandrecycling, Pol Degrad
Stab, 92 (2007) 2181-2189
[4]. MALLOY RA., Plastic Part Design for
InjectionMolding: AnIntroduction, Hanser
Gardner Publications Inc. (1994)
Theauthors aregrateful toTheCenter for
Polymer Technologyfor supporting thisproject.
ACKNOWLEDGMENTS
Extemalload onthesurfaceofhighly frozen-
instresspart duetoimproper settingprocess tend
toformbrittle onthesurface and layer between
thesurface. Theinner corepart resulted incrack
beginning from the outer surface part and
propagate toward theentirepart of thickness
CONCLUSION
Figure 7.Delaminationformonthefracturesur-
face, supposed due to layer formation between
theskinandthecore.
Figure 6. Different patternsurfacefracture
Provensample.
NGsample.
Figure 5. Crack around the gate (bottom) and
(top) ofNG sample.
cooling rate. The setting process also tend to
increase the frozen-in stress orientation on the
surface near to the gate (see Figure 2). This
supposedcausetwolayersformation, surfacepart
withhighly frozen-in stress orientation (smooth!
brittlesurface-patterncrack);delaminationformed
andductile fracture mode intheinner corepart.
This isinaccordance totheinformation received
aboutthecyclingtimereductionduringproduction
(Figure7).
Frozen-in stress inmicrostructure andthe
external load applied from outer surface has
resulted ininitial crack andpropagate to entire
thickness product.
Failure Analysis on PolyOxyMethylene Product Using Scanning Electron Microscope, Thermal and Processing
Analysis (R. Wijaya)