March 29, 2017

Martin Doornheim

1

Evaluation of ERT nPLA compounds

Background

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• ERT developed Earthmatter compounds, which are based on PLLA, PDLA and sc-PLA microfiber. See tables below for the formulations.

• Three types of Earthmatter compounds were received, injection molded at the WUR and results compared with PLLA L130 and PLLA L130 + 5% PDLA D120 benchmark.

• Injection molding was performed using a mold temperature of 30°C and 103°C to identify properties differences of amorphous versus semi-crystalline specimen.

Experimental

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Raw materials: • PLLA L130 (lot 20151004) • PLLA L130 + PDLA D120, compounded at Total-Corbion • Earthmatter formulation #1 (lot f1-161121-001-A) • Earthmatter formulation #6a (lot f6a-161121-003-A) • Earthmatter formulation #18 (lot f18-161208-001-A)

Drying: Minimal 4 hours @ 80°C in a descicant hot air dryer.

Injection molding: Temperature profile: 25-160-195-195-195°C Mold temperature: 30°C & 103°C Holding time: 15s Cooling time: 35s Specimen: tensile samples according ISO 527-2, Impact and HDT samples according ISO 294 Conditioning: 1 week conditioning at 20°C/50% RH

Characterisation: DMTA, tensile properties (ISO 527-1), HDT/B (ISO 075) and impact properties (ISO 179/1eA and 1eU).

Sample Specimen T Mold (°C)

Processing Injection pressure (bar)

L130 Tensile 30 Automatic 1300-1800

L130 + 5% D120 Tensile 30 Automatic 1350

Earthmatter F1 Tensile 30 Automatic 1200-1300

Earthmatter 6A Tensile 30 Automatic 950

Earthmatter F18 Tensile 30 Automatic 700-800

L130 Tensile 103 Semi-automatic 1150-1300

L130 + 5% D120 Tensile 103 Automatic 1100-1300

Earthmatter F1 Tensile 103 Automatic 1050

Earthmatter 6A Tensile 103 Automatic 950-1200

Earthmatter F18 Tensile 103 Automatic 700-750

Results – Injection molding process

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Results – Injection molding process

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Sample Specimen T Mold (°C)

Processing Injection pressure (bar)

L130 Impact/HDT 30 Automatic 1000-1500

L130 + 5% D120 Impact/HDT 30 Automatic 1000

Earthmatter F1 Impact/HDT 30 Automatic 1250

Earthmatter 6A Impact/HDT 30 Automatic 850-1050

Earthmatter F18 Impact/HDT 30 Automatic 500-650

L130 Impact/HDT 103 Semi-automatic 900-1000

L130 + 5% D120 Impact/HDT 103 Semi-automatic 850-1000

Earthmatter F1 Impact/HDT 103 Automatic 800

Earthmatter 6A Impact/HDT 103 Automatic 700

Earthmatter F18 Impact/HDT 103 Automatic 500

Results – DMTA

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Results – DMTA

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Results – DMTA

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• All materials injection molded using a mold temperature of 30°C remains amorphous. • PLLA L130 injection molded using a mold temperature of 103°C was not fully crystallized. • PLLA L130 nucleated with PDLA D120 and all Earthmatter compounds were fully

crystallized. • The storage modulus above glass transition temperature is at a higher level if PDLA is

added.

Results – Tensile properties

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sample

Mold temperature (°C)

L130 + 5% D120L130ERT F18ERT F1ERT 6A

1033010330103301033010330

5000

4000

3000

2000

1000

0

E-m

od

ulu

s (M

Pa)

E-modulusDependence on mold temperature

• Talc in the ERT F1 formulation increases the modulus.

• PDLA increases the modulus of semi-crystalline specimen vs. amorphous specimen.

Results – Tensile properties

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• The maximum stress levels of Earthmatter compounds are somewhat lower than neat PLA specimen.

Results – Tensile properties

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• The elongation at break levels of the Earthmatter compounds are significant higher than neat PLA resins.

• The effectiveness of the Earthmatter compounds on elongation at break levels are the highest for amorphous specimen.

sample

Mold temperature (°C)

L130 + 5% D120L130ERT F18ERT F1ERT 6A

1033010330103301033010330

250

200

150

100

50

0

Elo

ng

ati

on

@ B

reak (

%)

Elongation @ breakDependence on mold temperature

Results – Notched impact resistance

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• The notched impact resistance of semi-crystalline Earthmatter compounds are significant higher than neat PLA resins.

• The notched impact resistance of amorphous Earthmatter compounds only slightly higher than neat PLA resins.

sample

Mold temperature (°C)

L130 + 5% D120L130ERT F18ERT F1ERT 6A

1033010330103301033010330

25

20

15

10

5

0

No

tch

ed

im

pact

(kJ/

m2

)

Notched impact resistanceDependence on mold temperature

Results – HDT/B

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• The HDT/B levels are the highest for semi crystalline PLA specimen.

• The HDT/B levels of semicrystalline Earthmatter compounds are slighty lower than neat PLA.

• The HDT/B levels for all amorphous specimen are around the glass transition temperature of PLA.

• The HDT/B values are in accordance with the DMTA results.

sample

Mold temperature (°C)

L130 + 5% D120L130ERT F18ERT F1ERT 6A

1033010330103301033010330

140

120

100

80

60

40

20

0

HD

T/B

(°C

)

HDT/BDependence on mold temperature

Conclusions/Discussion

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• Earthmatter compounds were successfully injection molded using standard conditions for nucleated PLA compounds.

• Interesting improvements versus neat PLA achieved for: Impact resistance for semi crystalline specimen. Elongation at break for semi-crystalline specimen. Elongation at break for amorphous specimen.

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Raw data

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