No es on heological measu emen s
P ojec Ti le: Polyme In o ma ics Tools o Sus ainable 3D P in ing (PITS3D)
Fellow: D . Pe a Bačo á
Hos Ins i u ion: Uni e sidad de Cádiz, Spain
Hos Ins i u ion o Secondmen : Polyme and Colloid Science G oup,
IESL-FORTH, C e e, G eece, P o . Dimi is Vlassopoulos
Du a ion o he secondmen : 3 mon hs
1 Execu i e Summa y
This documen summa ises my no es on linea heological measu emen s unde aken du ing my sec-
ondmen a IESL-FORTH, C e e, G eece. This secondmen was a pa o my PITS3D p ojec and
i aimed o p o ide me wi h aining in expe imen al heological echniques. This expe ience was
used o he de ailed heological cha ac e iza ion o comme cially a ailable poly(lac ic acid) (PLA)
and unen angled PLA samples syn hesized in he hos ins i u ion. The ul ima e goal o PITS3D was
o co ela e hese expe imen al indings wi h compu a ional and heo e ical app oaches, he eby ad-
ancing polyme cha ac e iza ion wi hin he hos g oup and acili a ing knowledge ans e in he ield.
Conside his documen a eely a ailable se o ins uc ions, c ea ed wi h he hope o aiding any-
one who uses i .
2 B ie summa y o he used ma e ials
Comme cially a ailable PLA3D850 was used as he aining ma e ial. PLA3D850 was in a o m o
pelle s and he e o e, he samples o heology we e p epa ed by a ho p ess. Some no es a e also
ela ed o he unen angled PLA samples, which we e in a o m o powde and he e o e, he samples
we e cold p essed in a mold and hen ca e ully ans e ed o he pla e.
3 Me hods
3.1 P epa a ion o he samples by a cold/ho p ess
• he pieces, which he ho p ess consis s o , a e shown in Fig. 1
•se up he acuum
•p ess: enough o apply up o 1 on
•sample weigh a ound 55 mg o a disc o diame e 8 mm and hickness o 1 mm
•sample weigh a ound 250 mg o a pla e o 25 mm and hickness o 0.6 mm
•in he case o he comme cial sample, he pelle s we e i s ly squeezed in he mold by a cold p ess
and hen he p ess was hea ed o 190◦C. This empe a u e was kep o 5 minu es and hen he
sample was slowly cooled o he oom emepe a u e.
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Figu e 1: Top: Pieces used o he p ess: bo om pa o he ou e chambe , bo om pa o he
inne chambe , inne chambe , cylinde wi h he hole o diame e 8mm, s ick wi h he diame e 8 mm,
ubbe bands, uppe load, uppe lid o he ou e chambe . Bo om Le : Assembled pa s. Bo om
Righ : Ho p ess. The le e on he igh is used o apply p essu e.
3.2 Desc ip ion o he heome e
•ARES, ai a mosphe e
•O ches a o p og am o se up he pa ame e s
•uppe pa senso ( ansduce )
•lowe pa oscilla ing (mo o )
•senso showing he no mal and o que o ces
• he mocouple o con ol he empe a u e
•pla e 8 mm o he comme cial samples, o he unen angled samples 25 mm pla e because o he
low o que
3.3 S a ing he expe imen
•swi ch on he ansduce 2 o a ach he pla es: U ili ies→Se ice→T ansduce
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•place he he mocouple: i he empe a u e does no change om -220 o he oom empe a u e,
we go o U ili ies→Se ice→Ins umen Con igu a ion and change he Tempe a u e Loop Con ol
o Sample
•align he pla es: he bo om pa should be a 0 angle
•se he no mal o ce o 0 (NORM CLR) when he pla es a e no ouching each o he
•se he gap o 0: ini ia e he con ac be ween he pla es and when he no mal o ce posi i e,
p ess GAP CLR
Se ing he empe a u e:
•se he empe a u e o he e e ence one: icon wi h he he mome e , en i onmen al con olle
ON, mo o ON
• he chambe is closed, he pla es a e no ouching, wai 15-30 minu es o he pla es o each he
desi ed empe a u e
•se he no mal o ce o 0
•se he gap o 0, because i has changed due o he he mal expansion: i he coe icien o he
he mal expansion is unknown, w i e down he gap be o e se ing i 0 and calcula e he coe icien
(gap(T1)-gap(T0))/(T1−T0), ha ing in mind ha gap(T0)=0 and T0is he oom empe a u e
Loading he sample:
•cool down he pla es o he oom empe a u e
•cen e he sample on he pla e and lowe he pla es o ouch he sample. I he sample is
unen angled and in a o m o a p essed powde , i migh be con enien o i s mel he sample
(i.e., o inc ease he empe a u e abo e he mel ing empe a u e) and hen lowe he op pla e
o ouch i .
•wa m up he sample: as he sample is going o expand, inc ease he gap con inuously un il he
shape o he edges is conca e (see Fig. 2)
•wai 15 minu es o mel
•check he shape and change i o donu shape (i.e., ounded edges, see Fig. 2)
3.4 Remo ing possible bubbles in he sample
•P ess Con ol-Edi /S a Ins umen Tes
•se Geome y-Pa allel Pla e Geome y, Edi geome y: pu he dimensions o you sample (di-
ame e 8 mm and he cu en gap)
•S ep a e es -Edi (pu se ings below)
!! i he measu emen doesn’ s a immedia ely, check Op ions in S a Ins umen Tes , he e may
be a delay se on om he p e ious measu emen
P eshea : S ep Ra e Tes
•Tes ype: S ain-con olled
•Measu emen Type: T ansien
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Figu e 2: Le : Conca e shape. Righ : Donu shape
•Mo o ON
•sampling mode log
•poin s pe zone 350
•shea a e 0.5 s−1(o 0.1 −1is he sample is sensi i e, hen longe ime)
• ime 60 s o un il necessa y
•clockwise
Se ing mo o a e p eshea
• he mo o is misplaced: in o de o pu i in 0 posi ion, he mo o in empe a u e mus be
swi ched o , hen he mo o is mo ed manually o he posi ion 0
• hen he Con ol→Mo o →Mode Dynamic
•Go o Tempe a u e and se Mo o on
Dynamic Time Sweep Tes
• ixed equency: 100 ad/s
• ixed s ain 0.5 %
• un o a leas 30 minu es
•inc ease s ain i he bubbles do no mo e
• he shape o he sample can be conca e
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3.5 Linea Rheology Measu emen s
Gene ic p ocedu e
•Dynamic S ain Sweep
•Dynamic F equency Sweep
•Tempe a u e Ramp Tes (i desi ed)
Dynamic S ain Sweep
•swi ch o ansduce 1 (U ili ies-Se ice-T ansduce )
• es o ind he maximum s ain a which he esponse o he ma e ial is linea a he gi en
empe a u e: i needs o be epea ed e e y ime when we change he empe a u e
•Measu emen ype: Dynamic
• equency: 100 ad/s
•se ings: γmin=0.5, γmax=100
•s op when he moduli s a o decay ab up ly
•w i e down he alue o he s ain be o e he decay
Dynamic F equency Sweep
Checking he slip: i is necessa y o ind he gap a which he esul s a e ep oducible: educe he
alue o he gap and pe o m he linea heology measu emen s (see se ings below) un il he da a a e
consis en and o e lap, i.e., he da a emain consis en wi h espec o he las measu emen :
•s a dynamic equency sweep, wi h he se ings below, he a iable will be he gap in Geome y
Se ings
•se he gap ha is shown on he sc een
•measu e he spec a
•dec ease he gap, so ha he second decimal numbe changes, ca e ul o no squeeze he sample
oo much: keep he se ings o he DFS he same, change he Geome y Se ings
•measu e he spec a again and o e lay hem o see i hey o e lap: double click on he spec a,
O e lay-selec he da a se
• epea un il he da a o e lap, i.e., hey a e consis en
When he da a a e consis en keep his gap ixed in Geome y Se ings du ing he whole measu emen ,
so e en i he empe a u e is changing. Dec ease he gap only manually, using he alue calcula ed
om he he mal expansion coe icien . Fo example, i he he mal expansion is 2.5 µm/◦C and he
change in he empe a u e be ween wo measu emen s is 10◦C, educe he gap 25 µm.
Measu emen se ings o di e en empe a u es:
•se Pa allel Pla e in Geome y Se ings
•se Dynamic mode
•se he maximum s ain ob ained om DSS, measu e om equency 100 o 0.1 ad/sec.
• epea he measu emen o di e en empe a u es:
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–change he empe a u e in Tempe a u e se ings and wai o 10 min
–change he gap manually when he new empe a u e is se in heome e o compensa e o
he he mal expansion o he pla es
–do no change he Geome y Se ings
–once he sample is equilib a ed, epea DSS and DFS wi h he new empe a u e se ings
Tempe a u e Ramp Tes
•measu e i s DSS and DFS a he e e ence empe a u e and check i he da a a e consis en
wi h he p e ious measu emen s. No e: some samples may deg ade and he e o e hei G’ and
G” may be below he e e ence da a.
•se he empe a u e a he beginning o he measu emen and lea e he sample o equilib a e
•se ings: equency (1-10 ad/s), ini ial and e minal empe a u e, amp a e (1-10◦C/min),
s ain (0.5%)
•impo an o change he gap manually du ing he whole measu emen , usually a e 10◦C, as i
changes due o he he mal expansion and i may cause a sample de achmen a low empe a u es
•in he c ys alliza ion egion, i may be necessa y o swi ch o he T ansduce 2 o a oid o e load
• o semic ys alline samples, he delay in se ing he hea ing measu emen igh a e he cooling
measu emen may cause a misma ch in he i s alues o G’ and G” o hea ing and he las
alues o cooling, as he sample con inued o c ys allise du ing he ime ha he measu emen
was se
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