Der CAMSIZER XT

Creative Optimization with Additive Manufacturing Webinar - Additive Manufacturing with Particle Size and Shape Analysis

Many Additive Manufacturing (also called 3D printing) techniques such as selective laser sintering (SLS), selective laser melting (SLM) and electro-beam melting (EBM) use metal particle powders as a raw material (Aluminum, Titanium, Steel, Nickel, Tungsten and many Alloys). The particle size, size distribution and shape have a strong effect on the manufacturing result. Therefore it is important for manufacturers and suppliers to control the particle size and shape of their powders used in this process. In order to control particle size and shape these parameters must be measured. We discuss how to use the CAMSIZER technology to improve additive manufacturing results by monitoring the incoming particles. Value of Dynamic Image Analysis in 3D additive manufacturing How does Dynamic Image Analysis work? Why two cameras can control and monitor dust and oversize? Check the manufacturing and production of Additive Manufacturing powders Check the incoming raw material and the recycled powder for reuse

1 CAMSIZER XT & CAMSIZER X2

Additive Manufacturing December 5th of 2017

Julie Chen HORIBA Scientific

Gert Beckmann Retsch Technology GmbH Processes Classification Technology Description Materials

Binder Jetting 3D Printing Creates objects by depositing a Metal, Polymer, Ink-Jetting binding agent to join powdered Ceramic S-Print material. M-Print Direct Energy Direct Metal Deposition Builds parts by using focused Metal powder, Deposition Laser Deposition thermal energy to fuse materials as Metal wire Laser Consolidation they are deposited on a substrate. Electron Beam Direct Melting

Material Fused Deposition Modelling Creates objects by dispensing Polymer Extrusion material through a nozzle to build layers. Material Jetting Polyjet Builds parts by depositing small Photo-polymer, Ink-Jetting droplets of build material, which Wax Thermojet are then cured by exposure to light. Powder Bed Direct Metal Laser Sintering Creates objects by using thermal Metal, Polymer, Fusion Selective Laser Melting energy to fuse regions of a powder Ceramic Electron Beam Melting bed. Selective Laser Sintering

Sheet Ultrasonic Consolidation Builds parts by trimming sheets of Hybrids, Lamination Laminated Object Manufacture material and binding them together Metallic, in layers. Ceramic VAT Photopoly- Stereolithography Builds parts by using light to Photo-polymer, merisation Digital Light Processing selectively cure layers of material in Ceramic a vat of photopolymer.

3 Processes Classification Technology Description Materials

Material Fused Deposition Modelling Creates objects by dispensing Polymer Extrusion material through a nozzle to build Filament layers. Material Jetting Polyjet Builds parts by depositing small Photo-polymer, Ink-Jetting droplets of build material, which Wax Thermojet are then cured by exposure to light. Powder Bed Direct Metal Laser Sintering Creates objects by using thermal Metal, Selective Laser Melting energy to fuse regions of a powder Fusion Electron Beam Melting bed. Polymer, Selective Laser Sintering Ceramic

4 Processes

Type Technologies Materials Fused deposition modeling Thermoplastics, Eutectic metals, Edible materials, Extrusion (FDM) or Fused Filament Rubbers, Modeling clay, Plasticine, Metal clay Fabrication (FFF) (including Precious Metal Clay) Robocasting or Direct Ink Writing Ceramic materials, Metal alloy, Cermet, Metal matrix (DIW) composite, Ceramic matrix composite Light polymerized Stereolithography (SLA) Photopolymer Digital Light Processing (DLP) Photopolymer Powder bed and inkjet head 3D Powder Bed Almost any metal alloy, Powdered polymers, Plaster Printing (3DP) Electron-Beam Melting (EBM) Almost any metal alloy including Titanium alloys Titanium alloys, Cobalt Chrome alloys, Selective Laser Melting (SLM) Stainless Steel, Aluminium Selective Heat Sintering (SHS) Thermoplastic powder Selective Laser Sintering (SLS) Thermoplastics, Metal powders, Ceramic powders Direct metal laser sintering Almost any metal alloy (DMLS) Laminated Object Manufacturing Laminated Paper, Metal foil, Plastic film (LOM) Powder Fed Directed Energy Deposition Almost any metal alloy Electron Beam Freeform Wire Almost any metal alloy Fabrication (EBF3)

5 Processes

6 Manufacturing of Metal Powders

Direct iron ore reduction (into iron powder) (+) Fast (-) but irregular particle shape

Atomization (iron and other metals) Gas atomization (+) Smoother rounder shape and narrow size distribution (-) but slower and cost intensive

Liquid atomization (+) Fast (-) but irregular particle shape and wider size distribution

Separating Particle Sizes and Shapes (for manufacturing and/or testing)

Size Classification: - Sieving or Air Classification

Shape Classification: - Sieving with special shaped meshes - Sieving (fast and slow)

- Air Classification

Separating Particle sizes by Sieving or Air Classification

After Atomization (Sieving or Air Classification )

For Recycling (Sieving off defects, dust, twins, agglomerates)

10 Example for 3D printing

Automotive, Airospace Industry, Fast Prototyping => small numbers => individual modifications Paper => Plastics => Metal Laser Melting (3D Metal Printing) Vacuum or Nylon Casting

3D printing with metal: The final frontier of additive manufacturing

Digital Image Analysis

STATIC DYNAMIC (ISO 13322-1) (ISO 13322-2)

• Particles do not move during measurement • Particles in motion relative to camera • High resolution > 0,5 μm • Few 100 particles are analyzed • Resolution > 1 μm (low statistic) • Few million particles are analyzed • Limited measurement range (representative measurement) • Time consuming • Wide measurement range • Particles detected in stable orientation • Fast (2 Dimensions) • Particles measured in random orientations (3 Dimensions)

Instrument

1. Measurement principle

2. Results

Applications

3. Markets and applications

4. Alternative analysis methods

Accurate measurement of big particles is not possible, even if they fit into the field of view: Upper measurement Big particles are limit defined by the touching the edge too field of view often  reliable quantification not possible.

Particle size ~ 1/3 of field of view

Large amount Small particles in of big particles high resolution

Basic Camera Zoom Camera

ISO 13322-2: Smallest detectable CCD Basic CCD Zoom particle: 1 pixel One pixel is element of a projection when at least half of the pixel is covered.

Advanced, patented optics design

Sample flow

Basic Camera

Light source 2

Zoom Camera

Light source 1

Advanced, patented optical design

Why is perpendicular orientation* better? Focal plane is always in the measurement plane

* Light † Measurement Plane

What is the size of this particle?

x x area x cmin “diameter over Femax “width” projection surface” “length”

A xc min

xFe max

CAMSIZER results are compatible

A‘ = A area

with x sieve analysis

Better Size Analysis due to Understanding of Particle Shape: Length, Width, Average Diameter

• Width/length = 1 (aspect ratio) xc min < 1 xFe max

• Roundness P (sphericity) A

• Symmetry r2

r1 S

• Convexity A convex

A real

Q3 (round) =32.8 %

xc min

xFe max

67.2 %

CAMSIZER P4 and CAMSIZER X2

Krumbeins Roundness and Sphericity For proppants, sands, and other non-round, angular particles Compatible with ISO 13503-2 and API

Krumbein Roundness RDNS_C measures the „angularity“, or „corner curvature radius“

Average diameter of all corners divided by diameter of maximum inscribed circle

Krumbein Sphericity SPHT_K measures the elongation of the particles (like w/l = b/l).

Analysis for size and shape

New Image database New Tool for improved understanding and documentation

Typically ~100.000 single particle pictures per measurement

3D-Display of data points

Powerful tool for distinguishing particles with different size and / or different shapes

Sorting metals by Roundness (“Willingness” to roll)

Particle Size Range from 1µm to 3mm

Three modes in 2 modules (dry and wet):

X-Fall: for dry and free flowing particles X-Jet: air pressure dispersion for fine and agglomerated powders X-Flow: wet module for emulsions and suspensions, with ultrasonic probe, optional for organic solvents

Size range: 1.6 µm to 3 mm Extended size range: 0.8 µm to 8 mm New optics: New optics: Resolution: 1.6 µm per pixel Higher resolution: 0.8 µm per pixel (with integration => 2.5µm) Larger field of view (□Basic) Smaller field of view ( Basic) ▫ New cameras: New cameras: Higher resolution 2 * 4.2 Mpixel Camera resolution 1.3 Mpixel 310 frames per second/much 270 frames per second higher data rate (factor 3.6)

Flexible configuration for a wide application range

simple • safe • fast

Dry Dispersion Inserts (2 Plug-In Options)

X- Fall X-Jet (Gravity dispersion) (Air pressure dispersion)

Dry Dispersion with X-Fall

Measurement range from 10 µm to 8 mm

For free flowing materials

similar to standard CAMSIZER

Sample recovery after analysis • Complete sample recovery • No contamination

Wet Dispersion with X-Flow

Measurement range from 1 µm to 600 µm for emulsions and suspensions

stronger dispersion with ultrasonic module

Optional for organic solvents

Highlights of the optics setup design: • More than 275 images per second • Full frame cameras with > 1.3 Megapixel resolution • Separate light sources for optimised brightness, homogenity, and contrast • 2 Cameras: High resolution combined with excellent statistic for a wide dynamic range • Image processing in real-time: Each particle in each image is analysed • Hundreds of particles in each image: Excellent statistics in short time

CAMSIZER XT can measure in a wider dynamic range with better statistics and reproducibility than any other image processing system

fast repeatable and precise reproducible

maintenance free and robust

Dry Dispersion with X-Jet

Measurement range from 1 µm to 3 mm

For fine powders and agglomerating materials

Dry Dispersion by pressurized air

For agglomerating powders

- Metal powder - Coal dust - Wheat flour

Particle size

Q3 [%] q3 [%/µm]

90 9 Powder-#8-X-Jet-30kPa_vvv_xc_min_Mv.rdf Powder-#8-X-Jet-30kPa_TP1_vvv_xc_min_001.rdf 80 Powder-#8-X-Jet-30kPa_TP2_vvv_xc_min_002.rdf8 Powder-#13-X-Jet-30kPa_TP1_vvv_xc_min_001.rdf 70 Powder-#13-X-Jet-30kPa_TP2_vvv_xc_min_002.rdf7 Powder-#13-X-Jet-30kPa_vvv_xc_min_Mv.rdf 60 Powder-#27-X-Jet-30kPa_TP1_vvv_xc_min_001.rdf6 Powder-#27-X-Jet-30kPa_TP2_vvv_xc_min_002.rdf Powder-#27-X-Jet-30kPa_vvv_xc_min_Mv.rdf 50 5

40 4

30 3

20 2

10 1

0 0 10 15 20 25 30 35 40 45 50 xc_min [µm]

Customer had sent 30 different samples to Retsch Technology but some of these samples were the same (red, blue and green). We found out the groups and showed to the customer the good reproducibility of CAMSIZER XT (and proofed his sample splitting as well) © Retsch Technology GmbH 58 CAMSIZER XT for Metal Powders

Reproducibility and Instrument-to-Instrument agreement Δ = 0.1µm – 0.3µm

Metal Powder

Calibration Reticule

Static Calibration

- Traceble to an International Standard - Covering the Whole Measurement Range - Instrument to Instrument Agreement

Calibration Reticule

Static Calibration

Whitehouse Glass Bead Standard XX030 for X-Dry and X-Fall

Dynamic Calibration

q3 [%/µm]

50 Duke10um12um_gl0_xc_min_009.rdf Duke10um12um_gl0_xc_min_010.rdf Duke10um12um_gl0_xc_min_011.rdf 45 Duke10um_xc_min_002.rdf Duke10um_xc_min_003.rdf 40 Duke10um_xc_min_004.rdf

0 4 6 8 10 12 xc_min [µm] Particle size

Particle size

Particle size distribution: 2.5 µm and 5 µm

High resolution for small particles.

Instrument

1. Measurement principle

2. Results

Applications

3. Markets and applications

4. Alternative analysis methods

• Digital image processing with patented 2-camera system (ISO 13322-2)

• Wide dynamic range from 1µm to > 3mm

• Newly developed optical system with ultra bright LEDs for sharp contrasts and large depth of focus

• Short analysis time 1 – 3 minutes for few million particles

• Safe detection of oversized and undersized

• Modules for dry and wet dispersion

• Analysis results compatible to sieve analysis

Instrument

1. Measurement principle

2. Results

Applications

3. Markets and applications

4. Alternative analysis methods

• Industrial labs • Research institutes • Production control • Quality control for final products • Quality control of incoming raw materials • Immediate control and optimisation of production processes

Typical sample materials

• Pharmaceutical powders, granules or small pellets • Pulverized and granulated food, spices • Detergents, enzymes, fillers for washing powders • Metal or ore powders • Abrasives (medium and small grit) • Sand and cement, building materials, limestone • Fibres

Instrument

1. Measurement principle

2. Results

Applications

3. Markets and applications

4. Alternative analysis methods

0.8µm - CAMSIZER X2 - 8mm

Sieving CAMSIZER XT Size range 10µm - 63mm 1µm – 3mm Shape analysis no yes Detection of oversized few big particles each particle particles from < 0.1% Vol. Resolution poor high resolution Multi-modal distributions poor size resolution better resolution Repeatability and „difficult“ superior lab-to-lab comparison Comparison with sieving identical results possible simple, Handling easy and fast but time consuming

Identical results to sieve analysis

Q3 [%]

30 Ca-hydrogenphosphate_100kPa-T38567-vvv_xc_min_005.rdf Ca-hydrogenphosphate_100kPa-T38567-vvv_xc_min_003.rdf 20 Ca-hydrogenphosphate_100kPa-T38567-vvv_xc_min_004.rdf T38567-Sieve-Analysis-Customer-Site.ref

0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 xc_min [mm]

Spheroidal Particles

Passing [%]

90 Sample-1__xc_min_002.rdf 80 Sample-1__xc_min_001.rdf Sieving-Nominal-S1.ref

70 ∅ = d = Xc min xc min = 60 particle-width

0 200 400 600 800 1000 1200 x [µm]

Influence of Mesh Width

Mesh sizes weft Mesh sizes warp

1400µm 1400µm 1429.5µm

Theory: Reality:

Nominal Sieve Mesh = 1400µm Real Sieve Mesh >1400 = 1455

only beads < 1400µm Upper mesh size range ~1455µm sieve No. 03033531 will pass the sieve mesh (nominal 1400µm) beads > 1400µm will not pass the sieve mesh

Real Mesh Width

Passing [%] 90 Sample-1__xc_min_002.rdf 80 Sieving-upper-range-S1.ref

0 200 400 600 800 1000 1200 x [µm]

Q3 [%] Solder_Sample_G_xc_min_001.rdf 90 Solder_Sample_G_xc_min_002.rdf Solder_Sample_G_xc_min_003.rdf Tin-Solder_Sample_G__xc_min_001.rdf 80 Tin-Solder_Sample_G__xc_min_002.rdf Tin-Solder_Sample_G__xc_min_003.rdf 70 RT1763 Sieve-Analysis G customer-site-nominal.ref RT1763 Sieve-Analysis_G_AS200tap_real-sizes.ref 60

0 10 20 30 40 50 xc_min [µm] Sample Reproducibility of CAMSIZER XT measurements

of xc min (red, and blue) with Basic + Zoom or Zoom only, Retsch sieve result (real mesh sizes from optical inspection) AS 200 TAB (*black), Customer nominal sieve results (*blue)

Identical results to the

sieve analysis

Q3 [%]

0 0.04 0.1 0.2 0.4 1 2 xc_min [mm]

Automatic reports, many languages available

Worn out sieves

• high amount of time and work • low resolution, small number Disadvantages of investigatable classes • limited sample amount (overloading is critical) • Difference between nominal and real sizes Sieving Problems (here Blinding and Overloading)

1. Move

2. Sliding friction

3. Static friction

Q3 [%] q3 [%/mm] 5454_PT100_xc_min_008.rdf 90 5454_random_xc_min_009.rdf 450 5454_Huntsman-sieve.ref

80 400

70 Round 350

60 particles with 300 low density 50 250 are captured 40 without 200 30 rerelease 150

20 100

10 50

0 0 0.5 0.6 0.7 0.8 0.9 1.0 xc_min [mm]

If sieve analysis is used for quality control within the context of DIN EN ISO 9000:2000 then both the sieve shaker and the test sieves must be subjected to test agent monitoring. d

Technical requirements & testing Ø according to ISO 3310

Tolerance for mean value (Y): w The mean value of the mesh width must not differ from the nominal value w by more than the tolerance ± Y.

w Ø d

w = mesh width d = wire diameter CAMSIZER XT finding Fibers in Beads

Finding the Fibers

Laser sizer CAMSIZER XT Size range down to 20nm > 1µm Shape analysis no yes Detection of oversized few big particles percent range particles < 0.1% Vol. better resolution for Resolution good for fines large particles better volume model, Multi-modal distributions more difficult better size resolution Comparison with sieving not possible identical results black box + Information content pictures mathematics

Microscope CAMSIZER XT Size range 0.5 – 500 µm 1 µm -3 mm yes Shape analysis yes superior image quality Detection of oversized few big particles no particles < 0.1% Vol. Resolution better good Low, Statistics million particles/minute few 1,000 particles Comparison with not possible identical results possible sieving Handling time consuming fast Representative Sample difficult, only narrow yes, small and large Amounts distributions amounts

Digital Image Analysis

STATIC DYNAMIC (ISO 13322-1) (ISO 13322-2)

Q3 [%]

PPO-646_xc_min_001.rdf 40 RT1766_ppo646_sieve.ref

0 200 400 600 800 1000 xc_min [µm]

CAMSIZER CAMSIZER XT Size range 30 µm – 30mm 1 µm -3 mm Shape analysis yes yes Detection of oversized yes yes particles Images / second 60 277 Resolution CCD-Cameras 790,000 1,300,000 identical results identical results Comparison with sieving possible possible Handling fast fast Representative Sample yes, small and large yes, small and large Amounts amounts amounts

Q3 [%]

70 [email protected] 60

XT-with-X-Jet-#30-Einzel-250kPa_xc_min_005.rdf 40 XT-with-X-Jet-#30-Einzel-250kPa_xc_min_006.rdf XT-with-X-Jet-#30-Einzel-250kPa_xc_min_007.rdf 30 XT-with-X-Jet-#30-Einzel-250kPa_xc_min_008.rdf #30-classic-CAMSIZER-Repeatability-xc_min_013.rdf 20 #30-classic-CAMSIZER-Repeatability-xc_min_014.rdf #30-classic-CAMSIZER-Repeatability-xc_min_015.rdf #30-classic-CAMSIZER-Repeatability-xc_min_Mv.rdf 10

0 15 20 25 30 35 40 45 50 xc_min [µm]

Results of CAMSIZER (black) and CAMSIZER-XT (red) of sample #30

CAMSIZER distribution is wider, the results are not that accurate and repeatable as results from CAMSIZER XT.

 Wide dynamic measurement range (factor of >1500)

 High resolution, length and diameter!  Shape analysis

 Very Sensitive for over- and Q3 (round) = 32.8 % undersized particles, 0.001% xc min

 Results compatible to sieve xFe max analysis 67.2 %  Different dispersion options  Measurement ranges  CAMSIZER P4 20µm – 30mm  CAMSIZER X2 0.8µm – 8mm