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PLA filament is not equal to PLA filament: Experimental studies of the influence of the type of pigment on the mechanical and thermal properties of poly(lactic acid) products

Jacek Iwko
Jacek Iwko
, 
Tomasz Jaruga
Tomasz Jaruga
, 
Oliwia Trzaska
Oliwia Trzaska
 y 
Tomasz Stachowiak
Tomasz Stachowiak
   | 25 ago 2023
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Publicado en línea: 25 ago 2023
Páginas: 177 - 190
Recibido: 22 mar 2023
Aceptado: 25 jun 2023
DOI: https://doi.org/10.2478/msp-2023-0015
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© 2023 Jacek Iwko et al., published by Sciendo
This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International License.

Fig. 1.

PLA test samples printed in different colours
PLA test samples printed in different colours

Fig. 2.

Bending curves for natural samples
Bending curves for natural samples

Fig. 3.

Flexural strength of the tested materials
Flexural strength of the tested materials

Fig. 4.

Flexural modulus of the tested materials
Flexural modulus of the tested materials

Fig. 5.

Compression curves for natural samples
Compression curves for natural samples

Fig. 6.

Compressive strength of the tested materials
Compressive strength of the tested materials

Fig. 7.

Compression modulus of the tested materials
Compression modulus of the tested materials

Fig. 8.

Impact strength of the tested materials
Impact strength of the tested materials

Fig. 9.

Vicat softening point of the tested materials
Vicat softening point of the tested materials

Fig. 10.

The course of the DSC curves for the tested materials for the first heating (respectively from the bottom: natural, white, yellow, orange, red, magenta, green leaf, sky blue, dark blue, silver, iron gray, black)
The course of the DSC curves for the tested materials for the first heating (respectively from the bottom: natural, white, yellow, orange, red, magenta, green leaf, sky blue, dark blue, silver, iron gray, black)

Fig. 11.

DSC curve of the first heating at a constant rate of 10 K/min for the natural sample – two temperature peaks can be observed appearing in the melting area
DSC curve of the first heating at a constant rate of 10 K/min for the natural sample – two temperature peaks can be observed appearing in the melting area

Fig. 12.

DSC curve of cooling at a constant rate of 10 K/min for black and natural samples; in the case of black, one can observe an exothermic peak characteristic of the crystallisation process
DSC curve of cooling at a constant rate of 10 K/min for black and natural samples; in the case of black, one can observe an exothermic peak characteristic of the crystallisation process

Summary of the data produced from DSC testing of first heating scan for the PLA filaments considered including heat capacity (Cp) at temperature of glass transition, glass transition temperature (Tg), cold crystallisation temperature (Tc), enthalpy of cold crystallisation (ΔHc), melting temperature (Tm), enthalpy of melting (ΔHm) and degree of crystallinity (X)

I heating
J/(g*K) ΔCp °C Tg °C Tc J/g ΔHc °C Tm1 °C Tm2 J/g ΔHm % X
natural 1,463 63,4 106,4 29,24 162,5 153,9 43,34 13,2
white 0,884 61,8 98,2 24,55 160,6 149,6 40,98 15,4
silver 0,930 65,2 103,1 25,91 152,8 35,95 9,5
iron gray 0,555 64,0 101,8 24,33 153,0 38,10 13,0
black 0,752 64,6 101,4 18,31 155,0 148,0 36,20 16,8
green leaf 1,622 64,6 106,0 28,63 152,5 35,25 6,2
yellow 1,461 65,5 103,4 19,98 151,8 39,67 18,5
orange 1,425 65,7 100,2 21,74 153,7 34,39 11,9
red 1,327 64,8 101,3 27,88 155,2 148,3 32,67 4,5
magenta 1,149 66,2 95,0 21,60 161,9 38,88 16,2
sky blue 0,933 66,1 96,0 28,05 162,8 38,99 10,3
dark blue 0,995 64,3 97,1 30,12 162,8 40,17 9,4

Table of R2 coefficients between the parameters determined in the DSC test and the mechanical properties of the tested materials

bending modulus [MPa] flexural strength [MPa] compress. modulus [MPa] compress. strength [MPa] impact strength [kJ/m2] Vicat softening temp. [C]
X [%] 0,20 0,01 0,01 0,02 0,02 0,07
Tg 0,15 0,04 0,16 0,38 0,00 0,27
Tc (I) 0,08 0,01 0,00 0,00 0,00 0,04
Tc (II) 0,03 0,00 0,30 0,04 0,03 0,02
Tm1 (I) 0,01 0,08 0,07 0,06 0,02 0,00
Tm1 (II) 0,09 0,04 0,17 0,04 0,03 0,02
Cp 0,00 0,17 0,11 0,01 0,01 0,02
Hc (I) 0,10 0,03 0,08 0,00 0,01 0,11
Hm (I) 0,07 0,14 0,06 0,07 0,11 0,00
Hc (II) 0,00 0,00 0,01 0,03 0,01 0,11
Hm (II) 0,11 0,01 0,03 0,02 0,00 0,20

Parameters for printing test samples set on the HBOT 3D F300 printer

parameter size
Working table temperature [°C] 60
Nozzle temperature [°C] 235
Nozzle diameter [mm] 0,60
Layer height [mm] 0,30
Sample filling degree [%] 100
Filling type rectangular
Printing direction horizontal
Print speed [mm/s] 50

Table of R2 coefficients between the parameters determined in the DSC study

X [%] Tg Tc (I) Tc (II) Tm1 (I) Tm1 (II) Cp Hc (I) Hm (I) Hc (II) Hm (II)
X [%] 1,00
Tg 0,00 1,00
Tc (I) 0,03 0,06 1,00
Tc (II) 0,36 0,16 0,11 1,00
Tm1 (I) 0,01 0,03 0,33 0,00 1,00
Tm1 (II) 0,00 0,02 0,14 0,19 0,71 1,00
Cp 0,06 0,04 0,19 0,06 0,02 0,00 1,00
Hc (I) 0,57 0,06 0,01 0,45 0,16 0,21 0,03 1,00
Hm (I) 0,28 0,17 0,01 0,00 0,41 0,25 0,01 0,02 1,00
Hc (II) 0,00 0,02 0,41 0,04 0,14 0,00 0,15 0,03 0,04 1,00
Hm (II) 0,08 0,01 0,19 0,41 0,01 0,16 0,20 0,05 0,02 0,66 1,00

Determined wma and wra parameters for the tested materials

Δcp X wma wra
[J/gK] - - -
natural 1,463 0,13 0,73 0,14
white 0,884 0,16 0,44 0,40
silver 0,930 0,09 0,47 0,44
iron gray 0,555 0,13 0,28 0,59
black 0,752 0,16 0,38 0,46
green leaf 1,622 0,06 0,81 0,13
yellow 1,461 0,19 0,73 0,08
orange 1,425 0,12 0,71 0,17
red 1,327 0,05 0,66 0,29
magenta 1,149 0,17 0,57 0,26
sky blue 0,933 0,10 0,47 0,43
dark blue 0,995 0,09 0,50 0,41

Summary of the data produced from DSC testing of second heating scan for the PLA filaments considered including cold crystallisation temperature (Tc), enthalpy of cold crystallisation (ΔHc), melting temperature (Tm) and enthalpy of melting (ΔHm)

II heating
°C Tc J/g ΔHc °C Tm1* °C Tm2** J/g ΔHm
natural 131,4 3,575 158,6 3,564
white 124,3 44,900 155,7 159,2 42,360
silver 126,3 15,340 152,9 16,430
iron gray 124,3 25,780 152,2 25,130
black 102,7 17,240 150,4 153,9 42,500
green leaf 126,6 14,210 152,6 13,570
yellow 105,9 20,850 149,2 38,360
orange 122,2 33,090 152,1 28,490
red 127,7 13,560 153,8 13,140
magenta 116,5 12,110 159,4 7,293
sky blue 113,1 47,870 155,2 161,3 46,310
dark blue 118,4 52,560 155,5 160,9 45,020
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Materials Sciences, other, Nanomaterials, Functional and Smart Materials, Materials Characterization and Properties
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