May 14th - 15th, 2013

Flowing Performance of SLS

Powders at Elevated
Temperature

Felipe Amado, M. Schmid & K. Wegener

Inspire AG - Institute for Rapid Product Development (irpd)
St. Gallen 9014, Switzerland
www.inspire.ethz.ch

May 14th – 15th, 2013 Erfurt, Germany

© inspire irpd – a joint project with the University of Applied Sciences St. Gallen

May 14th - 15th, 2013

Agenda

► Introduction of inspire Irpd

Organization & Core Competences

► SLS Polymer Powder Characterization

State of the Art & Characterization Methods

► Experimental Device & Methodology

Operational Principle & Experimental Set up

► Results & Analysis

Flowability - Fluidization at high Tº & SLS correlation

► Summary
Principal Achievements & Future work

© inspire irpd – a joint project with the University of Applied Sciences St. Gallen

1
 May 14th - 15th, 2013

Introduction

© inspire irpd – a joint project with the University of Applied Sciences St. Gallen

May 14th - 15th, 2013

Introduction

Rapid Prototyping (RP) Additive Manufacturing (AM)

Technologies

Medical
Manufacturing Selective Laser Sintering (SLS), 3D-Printing (3DP)
LaserCUSING® (SLM) Reverse Engineering

Process and Material Development

© inspire irpd – a joint project with the University of Applied Sciences St. Gallen

2
 May 14th - 15th, 2013

SLS Polymer Powder Development

Absorption
(10.6 µm)

According to Dr. M. Schmid

(inspire AG, Switzerland)

© inspire irpd – a joint project with the University of Applied Sciences St. Gallen

May 14th - 15th, 2013

SLS Polymer Powder Characterization

Intrinsic characterization test Non-intrinsic characterization test Author/

Production
Research
Technology MFI/ Particle Tap/Bulk
DSC TG *Others PSD **Others Group
Rheo. Shape Density

Powder mixing
 
    [7][10][12]

(polymer, fiber,   
    [13][14][15][16]
beads)



    [17]
Melt mixing &



   [18]
cryogenic
grinding/spray


    [19]
drying




   [11][20]




   [21]
Dissolution-
precipitation




   [22]





   [23]
Mechano-   



[6][8]
chemical
alloying/




 [9]
Solid state
 

   [24]
Other characterization methods: *FTIR, EDX, XRD, etc.; **Angle Of Repose, Carr Index, etc.

In general, extrinsic properties are barely reported or just not considered

Trial & error tests dominate over any preliminary characterization

Several authors achieve adequate intrinsic properties for processing, but fail during the
spreading step
Source: Amado et al. 2011

© inspire irpd – a joint project with the University of Applied Sciences St. Gallen

3
 May 14th - 15th, 2013

SLS Polymer Powder Characterization

Test Method Measurement Characterization Measurement Measurement

Name Concept Parameters Temperature Procedure
Dynamic powder Powder bed expansion
Standard
Fluidimeter expansion under vertical height versus Not specified
conditions (25ºC)
fluid flow drag effect upstream fluid flow
Vertical powder deposition
Heap or pile angle of Standard
Angle of Repose through a funnel / orifice DIN ISO 4324
repose conditions (25ºC)
under the gravity effect
Quasi-static powder
Failure locus of shear
stability on an annular Standard
Ring Shear Cell force versus normal ASTM D6773
container under conditions (25ºC)
pressure
compression and shear
Powder density ratio
between a compacted and Tap and bulk apparent Standard
Bulk/Tap Density ASTM D7481
loose state under powder density conditions (25ºC)
mechanical tapping
Powder
Stress
Which system suites the best powder State
characterization towards SLS? Compacted

Not a general theory for powder behaviour is available

SLS

Results provided by each method are strongly dependent upon the spreading
powder stress condition and packing (HR=Bulk/Tap widely used)

In principle all systems present complementary information
Loose

More accurate results for systems that emulate the final handling
condition

Temperature effect/variations are not taken into account with standard Measurement
methods Static Dynamic Condition

© inspire irpd – a joint project with the University of Applied Sciences St. Gallen

May 14th - 15th, 2013

Experimental Device & Operational Principle

(φ 50 mm)

Similar dynamic handling

Near stress state condition

Allows adjustments at different processing speeds

Temperature variation range: 30ºC-110ºC
Schematic diagram of rotating and image acquisition system
Powder
Stress
State
Compacted

SLS
spreading

Loose

SLS powder spreading systems: Roller (3DSystems) & Blade

(EOS) (adapted from Alscher 2000) Measurement
Static Dynamic Condition

© inspire irpd – a joint project with the University of Applied Sciences St. Gallen

4
 May 14th - 15th, 2013

Experimental Device & Indexes

Test Index Definition

Flowability Fluidization Avalanche
Angle obtained from a linear regression of the free surface at the
maximum potential energy prior to the start of the powder avalanche
Angle
occurrence
Flowability
Fractal dimension D obtained from the free surface of the powder. D
Surface
corresponds to a dimensionless parameter based on the self-similarity
Fractal
concept and constitutes a powder rearrangement indicator
Total Volume Ratio between the total volume measured inside the drum (expanded
Expansion volume) and the volume occupied by the powder in the preparation
Fluidization Ratio sample container (tap density volume: 25 cc)
Fluidized Fraction of the total volume that develops a fluidized state defined by
Volume quasi-horizontal powder surface inside the drum
- Drum speed +
L : length estimate
Surface Fractal D : ε : measurement scale

© inspire irpd – a joint project with the University of Applied Sciences St. Gallen

May 14th - 15th, 2013

Previous Results: Flowability (Room Temperature)

Cumulative Avalanche Angle Distribution

Materials with a near spherical shape
present the lowest avalanche angle and a
narrow distribution (span).

Powders with a broader particle
morphological distribution increase their
Increase of
pile stability average value

A second phase (mixture) has a mayor
influence when different particle aspect
ratios are present (HST v/s Alumide)

Highly geometrical distorted particles
depict a higher d50 and span

But what happens

at higher
temperetaure?

Source: Amado et al. 2011

© inspire irpd – a joint project with the University of Applied Sciences St. Gallen

5
 May 14th - 15th, 2013

Experimental Set Up: RPA & SLS Tests Previous

work Actual
research

RPA Heated Set Up:

2 semi-crystalline materials: icoPP (Inspire) & PA2200 (EOS)

Flowability and Fluidization analyses considered

3 different temperatures for each material were selected:
- icoPP: 30ºC, 45ºC & 60ºC (powder sticks on surface)
- PA2200: 30ºC, 70ºC & 110ºC (equipment limitation)

Drum speed:
- Flowability: 10 rpm
- Fluidization: 50 rpm - 90 rpm

SLS Set Up: Solid

cube Upper Layer:
Laser Power

DTM Sinterstation 2000 machine variation
Hollow

Solid cubes and hollow boxes (powder/sintered dens.) box

Roller Speed Feed Part Bed

Material Lower Layer:
[mm/s] Temperature [ºC] Temperature [ºC] Scan Spacing
variation
icoPP 90, 180 45, 60 116 Dimensions in mm

PA2200 90, 180 70, 110 171

LP variation
High SS variation
Constant layer thickness (0.1 mm) & scan speed (5 m/s) Speed
Low Feed
Temperature LP variation
Low SS variation
Target: To correlate RPA results with SLS Powder Speed
Packing Density

© inspire irpd – a joint project with the University of Applied Sciences St. Gallen

May 14th - 15th, 2013

Results & Analysis: Flowability (Heated Drum)

Avalanche Angle Distribution
500 65
At 30ºC (or close to room
Avalanche Angle icoPP [deg]

temperature) the avalanche angle

Cum. Avalanche Count [N°]

D50 60
400 distribution of icoPP presents a
55
lower median and narrower
300 50
distribution in comparison to
icoPP 45
200 PA2000
40
30°C
100 45°C 35
In case of icoPP the avalanche
60°C angle distribution remains almost
0 30ºC 45ºC 60ºC
20 30 40 50 60 70 80 Temperature [°C] constant with an increase of the
Avalanche Angle icoPP [deg] drum temperature (no statistically
difference between medians at a
500
significance level of 5%)
Avalanche Angle PA2200 [deg]

70
Cum. Avalanche Count [°N]

400 D50
In case of PA2200 at the highest

60
temperature the avalanche angle
300 distribution presents a slight
PA2200 50
increase above its median.
200
However the differences are not
30°C 40
100
statistically significant
70°C
110°C
0 30ºC 70ºC 110ºC
20 30 40 50 60 70 80 Temperature [°C]
Avalanche Angle PA2200 [deg]

© inspire irpd – a joint project with the University of Applied Sciences St. Gallen

6
 May 14th - 15th, 2013

Results & Analysis: Flowability (Heated Drum)

Surface Fractal Distribution
500
At 30ºC (or close to room
temperature) the surface fractal

Surface Fractal icoPP [/]

Rate: 1.3e-2 [1/ºC]
Cum. Avalanche Count [N°]

5
400 distribution of icoPP presents a
4 considerable lower median and
300
narrower dispersion in comparison
icoPP 3
200 to PA2000
30°C 2
100 45°C
In case of icoPP the surface fractal
60°C distribution continuously increases
0 30ºC 45ºC 60ºC
1 2 3 4 5 6 Temperature [°C] with an increment of the drum
Surface Fractal icoPP [/] ∆ Surface Fractal temperature (statistically
Rate =
∆ Temperature differences between medians at a
500
Surface Fractal PA2200 [/]
6
significance level of 5%)
Cum. Avalanche Count [°N]

Rate: 7.8e-3 [1/ºC]

400 5
In case of PA2200 at the lowest
4
temperature the surface fractal
300 distribution presents a high median
PA2200 3 and broad dispersion of values.
200
30°C 2
100
At 70ºC a significant reduction is
70°C
110°C
1 observed, even below icoPP
0 30ºC 70ºC 110ºC results. The authors relate this
1 2 3 4 5 6 Temperature [°C]
Surface Fractal PA2200 [/]
effect with the transition above the
glass point (~50ºC)

© inspire irpd – a joint project with the University of Applied Sciences St. Gallen

May 14th - 15th, 2013

Results & Analysis: Fluidization (Heated Drum)

Total Vol. Expansion Fluidized Volume
1.4 50
As the rotational speed increases
icoPP 30°C icoPP both materials experience a higher
Total Vol Expansion Ratio [/]

45°C 40
total volume expansion ratio and
Fluid Vol Fraction [%]

1.35
60°C High Fluidization Rate
30
fluidized volume
1.3
20
In case of icoPP the total volume
30°C
expansion curve presents a non-
1.25
∆T=15ºC 10 45°C linear expansion rate in contrast to
60°C the linear behavior of PA2200
1.2 0
50 60 70 80 90 50 60 70 80 90

As the temperature increases
icoPP presents a vertical shift of
1.4 50
the volume expansion curves. In
PA2200 30°C
case of PA2200 the total volume
PA2200
Total Vol Expansion Ratio [/]

40 70°C expansion experiments a first

Fluid Vol Fraction [%]

1.35
110°C reduction from 30ºC to 70ºC. This
30 reduction corresponds to a better
1.3 Low Fluidization Rate
rearrangement of the particles in
∆T=40ºC 20
concordance with the surface
Improved
1.25
powder
fractal behavior
10
rearrangement

1.2 0
The fluidization rate is higher for

50 60 70 80 90 50 60 70 80 90 icoPP in comparison to PA2200
Rotational Speed [RPM] Rotational Speed [RPM]

© inspire irpd – a joint project with the University of Applied Sciences St. Gallen

7
 May 14th - 15th, 2013

Hollow
Results & Analysis: SLS Packing Density box

Lower Volume
Packing density values were

Expansion normalized by 0.90 g/cm3 (icoPP)
and 1.05 g/cm3 (PA2200)
(datasheet values)
Higher Volume
Expansion
icoPP achieves a higher
normalized packing density in
comparison to PA2200 for all
parameter combinations

As the powder deposition speed

increases there is a slightly
increase of the packing density

For icoPP as the feed temperature

increases, the packing density
reduces its value

Higher packing density is achieved

for a:
- Lower Volume Expansion
- Higher Fluidization Rate
- Lower Surface Fractal-Tº Rate
Higher Lower Higher Surface Lower Surface
Fluidization Rate Fluidization Rate Fractal-Tº Rate Fractal-Tº Rate

© inspire irpd – a joint project with the University of Applied Sciences St. Gallen

May 14th - 15th, 2013

Solid
Results & Analysis: SLS Sintered Density cube

Low Feed Temperature High Feed Temperature

1 1
The normalized density achieved
1 3 for icoPP is higher in comparison to
icoPP
PA2200 and correlates with the
Norm. Si ntered Density [/]

0.9 0.9
comparative higher initial packing
Low Speed

deposition
0.8 0.8
PA2200
PA2200 LP

icoPP curves present less sintered
PA2200 SS
0.7 0.7 density variations in comparison to
icoPP LP
icoPP SS PA2200 due to the higher part bed
0.6 0.6 temperature (closer to the onset
0.05 0.1 0.15 0.2 0.25 0.05 0.1 0.15 0.2 0.25 point than PA2200)

Scan space variation curves

1 1 present equal or lower values than
2 4 laser power variation curves
Nor m. Sintered Density [/]

0.9 0.9 (particularly at lower energy density

High Speed

values)
0.8 0.8 Scan Spacing
variation (red)
1 2 4
0.7 0.7 3
Laser Power
variation (blue)
0.6 0.6
0.05 0.1 0.15 0.2 0.25 0.05 0.1 0.15 0.2 0.25
Energy Density [J/mm3] Energy Density [J/mm3]

© inspire irpd – a joint project with the University of Applied Sciences St. Gallen

8
 May 14th - 15th, 2013

Summary

A new powder characterization system has been introduced that emulates a near SLS
spreading stress state when the powder is mechanically agitated inside a turning drum at
elevated temperatures.

The commercial powders PA2200 (EOS) and icoPP (Inspire) were studied in detail and
the correlation with the SLS powder packing density was presented.

New aspects regarding the dynamic powder behavior characterization were analyzed
and correlated to SLS process conditions: Avalanche Angle constitutes a first rough
invariant estimator about powder flowability, but Surface Fractal, Volume Expansion
Ratio and Fluidized Volume parameters enhance the detailed analysis.

This research was limited to semi-crystalline materials. Analyses of other thermoplastic

materials are going to be addressed in the future.

These results can be used to complement the existing methods to achieve a more
accurate and detailed understanding about SLS powder suitability and thus reduce the
powder development cycle time.

© inspire irpd – a joint project with the University of Applied Sciences St. Gallen

May 14th - 15th, 2013

Thanks for your attention!

Questions?

© inspire irpd – a joint project with the University of Applied Sciences St. Gallen