Webinar - Adding to Additive Manufacturing with Particle Size and Shape Analysis

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Webinar - Adding to Additive Manufacturing with Particle Size and Shape Analysis Many Additive Manufacturing (3D printing) techniques such as selective laser sintering (SLS) and selective laser melting (SLM) use particle powders as a raw material. The particle size 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 production of 3D printing powders Check the incoming raw material and the recycled powder for reuse 1

CAMSIZER XT 3D Printing Additive Manufacturing June 23 of 2016 Jeff Bodycomb HORIBA Scientific Gert Beckmann Retsch Technology GmbH

Classification Technology Description Materials Developers (Country) Binder Jetting Direct Energy Deposition Material Extrusion Material Jetting Powder Bed Fusion Sheet Lamination VAT Photopolymerisation 3D Printing Ink-Jetting S-Print M-Print Direct Metal Deposition Laser Deposition Laser Consolidation Electron Beam Direct Melting Fused Deposition Modelling Polyjet Ink-Jetting Thermojet Direct Metal Laser Sintering Selective Laser Melting Electron Beam Melting Selective Laser Sintering Ultrasonic Consolidation Laminated Object Manufacture Stereolithography Digital Light Processing Processes Creates objects by depositing a binding agent to join powdered material. Builds parts by using focused thermal energy to fuse materials as they are deposited on a substrate. Creates objects by dispensing material through a nozzle to build layers. Builds parts by depositing small droplets of build material, which are then cured by exposure to light. Creates objects by using thermal energy to fuse regions of a powder bed. Builds parts by trimming sheets of material and binding them together in layers. Builds parts by using light to selectively cure layers of material in a vat of photopolymer. Metal, Polymer, Ceramic Metal powder, Metal wire Polymer Photo-polymer, Wax Metal, Polymer, Ceramic Hybrids, Metallic, Ceramic Photo-polymer, Ceramic ExOne (USA) VoxelJet (Germany) 3D Systems (USA) DV3D (USA) NRC-IMI (Canada) Irepa Laser (France) Trumpf (Germany) Sciaky (USA) Stratasys (USA) Delta Micro Factory (China) 3D Systems (USA) Stratasys (USA) LUXeXcel (Netherlands) 3D Systems (USA) EOS (Germany), Renishaw (UK) Phenix Systems (France) Matsuna Machinery (Japan) ARCAM (Sweden) 3D Systems (USA) Fabrisonic (USA) CAM-LEM (USA) 3D Systems (USA) EnvisionTEC (Germany) DWS Srl (Italy) Lithoz (Austria) 4

Processes Type Technologies Materials Fused deposition modeling Thermoplastics, Eutectic metals, Edible materials, Extrusion (FDM) or Fused Filament Fabrication (FFF) Rubbers, Modeling clay, Plasticine, Metal clay (including Precious Metal Clay) Robocasting or Direct Ink Writing (DIW) Ceramic materials, Metal alloy, Cermet, Metal matrix composite, Ceramic matrix composite Light polymerized Stereolithography (SLA) Photopolymer Digital Light Processing (DLP) Photopolymer Powder Bed Powder bed and inkjet head 3D Printing (3DP) Almost any metal alloy, Powdered polymers, Plaster Electron-Beam Melting (EBM) Almost any metal alloy including Titanium alloys Selective Laser Melting (SLM) Titanium alloys, Cobalt Chrome alloys, Stainless Steel, Aluminium Selective Heat Sintering (SHS) Thermoplastic powder Selective Laser Sintering (SLS) Thermoplastics, Metal powders, Ceramic powders Direct metal laser sintering (DMLS) Almost any metal alloy Laminated Laminated Object Manufacturing (LOM) Paper, Metal foil, Plastic film Powder Fed Directed Energy Deposition Almost any metal alloy Wire Electron Beam Freeform Fabrication (EBF 3 ) Almost any metal alloy 5

Example of 3D Printing 6

Example for 3D printing 7

3D Printing (Plastic and Metal Powder) Applications Plastic, Ceramic & Metal Powder Automotive, Airospace Industry, Fast Prototyping => small numbers => individual modifications Paper => Plastics => Metal Laser Melting (3D Metal Printing) Vacuum or Nylon Casting 8

Product Examples (3D Printing Powders) The world s first 3D printed dress The world s first 3D printed metal gun is a beautiful.45 caliber M1911 pistol 9

3D Printing of Metal Construstions 3D printing with metal: The final frontier of additive manufacturing 10

CAMSIZER XT 3D Printing & Rapid Prototyping 11

CAMSIZER XT 3D Printing & Rapid Prototyping Now 12

CAMSIZER XT 3D Printing & Rapid Prototyping Future? Present! 13

Content Instrument 1. Measurement principle 2. Results Applications 3. Markets and applications 4. Alternative analysis methods 14

Measurement principle Resolution Detection of particles One pixel is element of a projection when at least half of the pixel is covered. CCD - Basic CCD - Zoom

Measurement principle (CAMSIZER XT) Advanced, patented optics design Sample flow Basic Camera Light source 2 Zoom Camera Light source 1 16

Measurement principle (CAMSIZER XT) Advanced, patented optics design Sample flow Basic Camera Light source 2 Zoom Camera Light source 1 17

Measurement principle (CAMSIZER XT) Advanced, patented optics design Sample flow Basic Camera Light source 2 Zoom Camera Light source 1 18

Measurement principle (CAMSIZER XT) Advanced, patented optics design Sample flow Basic Camera Light source 2 Zoom Camera Light source 1 19

Measurement Results What is the size of this particle? 20

Particle Size x c min width x area diameter over projection surface x Fe max length x c min A x Fe max CAMSIZER results are compatible with sieve analysis A = A x area 21

Results X-Jet Better Size Analysis due to Understanding of Particle Shape: Length, Width, Average Diameter 22

Particle Shape (CAMSIZER and CAMSIZER XT) Breadth-/ Length-Ratio x c min x Fe max Roundness A P Symmetry r 1 C r 2 Convexity A convex A real 23

Roundness with Krumbein s Chart 24

Manual Roundness Measurement 25

Correlation RDNS_C - Roundness Roundness (RDNS_C CAMSIZER) 1.0 0.9 2 0.8 R² = 0.9694 0.7 3 0.6 0.5 4 0.4 0.3 0.2 5 0.1 Roundness (visual ISO procedure) 0.0 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 1 1 2 3 4 5

Powdered Metal Sorting metals by Roundness ( Willingness to roll) 27

Reports and Warnings 28

Optical Process Control Analysis for Size and Shape 29

Dispersion Modules (CAMSIZER XT) Particle Size Range from 1 µm to 3 mm 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 30

Modular "X-Change" Concept Flexible configuration for a wide application range simple safe fast 31

Dispersion Modules (CAMSIZER XT) Dry Dispersion Inserts (2 Plug-In Options) X- Fall (Gravity dispersion) X-Jet (Air pressure dispersion) 32

Advantages fast repeatable and reproducible precise maintenance free and robust 33

Dispersion Modules (CAMSIZER XT) Dry Dispersion with X-Jet Measurement range from 1 µm to 3 mm For fine powders and agglomerating materials Dry Dispersion by pressurized air 34

Measurement principle X-Jet 35

Results For agglomerating powders - Metal powder - Coal dust - Wheat flour Particle size 36

Lower Measurement Range 37

Reproducibility of Metal Powder Results Q3 [%] 90 80 70 60 50 40 30 20 10 q3 [%/µm] 9 Powder-#8-X-Jet-30kPa_vvv_xc_min_Mv.rdf Powder-#8-X-Jet-30kPa_TP1_vvv_xc_min_001.rdf Powder-#8-X-Jet-30kPa_TP2_vvv_xc_min_002.rdf 8 Powder-#13-X-Jet-30kPa_TP1_vvv_xc_min_001.rdf Powder-#13-X-Jet-30kPa_TP2_vvv_xc_min_002.rdf 7 Powder-#13-X-Jet-30kPa_vvv_xc_min_Mv.rdf Powder-#27-X-Jet-30kPa_TP1_vvv_xc_min_001.rdf 6 Powder-#27-X-Jet-30kPa_TP2_vvv_xc_min_002.rdf Powder-#27-X-Jet-30kPa_vvv_xc_min_Mv.rdf 5 4 3 2 1 0 10 15 20 25 30 35 40 45 50 xc_min [µm] 0 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) 38

CAMSIZER XT for Metal Powders 39

CAMSIZER XT for Metal Powders Reproducibility and Instrument-to-Instrument agreement Δ = 0.1µm 0.3µm Metal Powder 40

Features of the CAMSIZER Calibration Reticule Static Calibration - Traceble to an International Standard - Covering the Whole Measurement Range - Instrument to Instrument Agreement 41

Features of the CAMSIZER XT Calibration Reticule Static Calibration 42

Features of the CAMSIZER XT Calibration Reticule Static Calibration 43

Physical Dynamic Partical Standards Whitehouse Glass Bead Standard XX030 for X-Dry and X-Fall Dynamic Calibration 44

Size Range and Sieve Correlation 45

System Comparison 46

Results X-Flow Particle Size Distribution 2.5 µm + 5 µm, Wet Dispersion Particle size 47

Results X-Flow (Calibration) Particle Size Distribution 10 µm + 12 µm, Wet Dispersion q3 [%/µm] 50 45 40 35 Duke10um12um_gl0_xc_min_009.rdf Duke10um12um_gl0_xc_min_010.rdf Duke10um12um_gl0_xc_min_011.rdf Duke10um_xc_min_002.rdf Duke10um_xc_min_003.rdf Duke10um_xc_min_004.rdf 30 25 20 15 10 5 0 4 6 8 10 12 Particle size xc_min [µm] 48

Content Instrument 1. Measurement principle 2. Results Applications 3. Markets and applications 4. Alternative analysis methods 49

Advantages Digital image processing with patented 2-camera system (ISO 13322-2) Wide dynamic range from 1 µm to > 3 mm 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 50

Content Instrument 1. Measurement principle 2. Results Applications 3. Markets and applications 4. Alternative analysis methods 51

Application areas Industrial labs Research institutes Production control Quality control for final products Quality control of incoming raw materials Immediate control and optimisation of production processes 52

Application areas 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 53

Content Instrument 1. Measurement principle 2. Results Applications 3. Markets and applications 4. Alternative analysis methods 54

Alternative Methods 55

Sieving CAMSIZER XT Sieving CAMSIZER XT Size range 10 µm - 63 mm 1 µm 3 mm Shape analysis no yes Detection of oversized particles each particle few big particles from < 0.1% Vol. Resolution poor high resolution Multi-modal distributions poor size resolution better resolution Repeatability and lab-to-lab comparison Comparison with sieving Handling difficult superior identical results possible simple, but time consuming easy and fast 56

Results X-Jet Identical results to sieve analysis Q3 [%] 90 80 70 60 50 40 30 20 Ca-hydrogenphosphate_100kPa-T38567-vvv_xc_min_005.rdf Ca-hydrogenphosphate_100kPa-T38567-vvv_xc_min_003.rdf Ca-hydrogenphosphate_100kPa-T38567-vvv_xc_min_004.rdf T38567-Sieve-Analysis-Customer-Site.ref 10 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 xc_min [mm] 57

Sieving CAMSIZER XT Spheroidal Particles Passing [%] 90 80 Sample-1 xc_min_002.rdf Sample-1 xc_min_001.rdf Sieving-Nominal-S1.ref 70 60 50 = d = Xc min x c min = particle-width 40 30 20 10 0 200 400 600 800 1000 1200 x [µm] 58

Sieving CAMSIZER XT Influence of Mesh Width Mesh sizes warp Mesh sizes weft 1400µm 1400µm 1429.5µm Theory: Reality: Nominal Sieve Mesh = 1400µm Real Sieve Mesh >1400 = 1455 only beads < 1400µm will pass the sieve mesh beads > 1400µm will not pass the sieve mesh Upper mesh size range ~1455µm sieve No. 03033531 (nominal 1400µm) 59

Sieving CAMSIZER XT Real Mesh Width Passing [%] 90 80 Sample-1 xc_min_002.rdf Sieving-upper-range-S1.ref 70 60 50 40 30 20 10 0 200 400 600 800 1000 1200 x [µm] 60

Results of Metal Powder Q3 [%] 90 80 70 60 Solder_Sample_G_xc_min_001.rdf Solder_Sample_G_xc_min_002.rdf Solder_Sample_G_xc_min_003.rdf Tin-Solder_Sample_G xc_min_001.rdf Tin-Solder_Sample_G xc_min_002.rdf Tin-Solder_Sample_G xc_min_003.rdf RT1763 Sieve-Analysis G customer-site-nominal.ref RT1763 Sieve-Analysis_G_AS200tap_real-sizes.ref 50 40 30 20 10 0 10 20 30 40 50 xc_min [µm] Sample Reproducibility of CAMSIZER XT measurements of x c 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) 61

Applications: Metal powders Material: Cu Identical results to the sieve analysis Q3 [%] 90 80 70 60 50 40 30 20 10 0 0.04 0.1 0.2 0.4 1 2 xc_min [mm] Automatic reports, many languages available 62

Competing Measuring Methods Comparison of Methods: Sieving Advantages robust and industrial-suited easy handling references available from user Worn out sieves Disadvantages high amount of time and work low resolution, small number 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 F 1 3. Static friction F 2 Q3 [%] 90 5454_PT100_xc_min_008.rdf 5454_random_xc_min_009.rdf 5454_Huntsman-sieve.ref q3 [%/m m] 450 80 70 60 50 40 30 Round particles with low density are captured without rerelease 400 350 300 250 200 150 20 100 10 50 0 0.5 0.6 0.7 0.8 0.9 1.0 xc_min [mm] 0 64

Test Sieves that comply with standards 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. Technical requirements & testing according to ISO 3310 Ø d Tolerance for mean value (Y): The mean value of the mesh width must not differ from the nominal value w by more than the tolerance ± Y. w w Ø d w = mesh width d = wire diameter

CAMSIZER XT finding Fibers in Beads Finding the Fibers 66

CAMSIZER XT finding Fibers in Beads Finding the Fibers 67

CAMSIZER XT Laser sizer Laser sizer CAMSIZER XT Size range down to 20 nm > 1 µm Shape analysis no yes Detection of oversized particles Resolution Multi-modal distributions percent range good for fines more difficult few big particles < 0.1% Vol. better resolution for large particles better volume model, better size resolution Comparison with sieving not possible identical results Information content black box + mathematics pictures 68

CAMSIZER XT Optical Microscope Microscope CAMSIZER XT Size range 0.5 500 µm 1 µm -3 mm Shape analysis Detection of oversized particles yes superior image quality no yes few big particles < 0.1% Vol. Resolution better good Statistics Comparison with sieving Low, few 1,000 particles not possible million particles/minute identical results possible Handling time consuming fast Representative Sample Amounts difficult, only narrow distributions yes, small and large amounts 69

CAMSIZER XT Optical Microscope 70

CAMSIZER XT Optical Microscope Q3 [%] 90 80 70 60 50 40 PPO-646_xc_min_001.rdf RT1766_ppo646_sieve.ref 30 20 10 0 200 400 600 800 1000 xc_min [µm] 71

CAMSIZER XT CAMSIZER CAMSIZER CAMSIZER XT Size range 30 µm 30mm 1 µm -3 mm Shape analysis yes yes Detection of oversized particles Images / second 60 277 Resolution CCD-Cameras 790,000 1,300,000 Comparison with sieving yes identical results possible yes identical results possible Handling fast fast Representative Sample Amounts yes, small and large amounts yes, small and large amounts 72

Comparison of CAMSIZER and CAMSIZER XT Results of Metal Powder Q3 [%] 90 80 70 60 50 40 30 20 10 XT-with-X-Jet-#30-Einzel-250kPa_xc_min_005.rdf XT-with-X-Jet-#30-Einzel-250kPa_xc_min_006.rdf XT-with-X-Jet-#30-Einzel-250kPa_xc_min_007.rdf XT-with-X-Jet-#30-Einzel-250kPa_xc_min_008.rdf #30-classic-CAMSIZER-Repeatability-xc_min_013.rdf #30-classic-CAMSIZER-Repeatability-xc_min_014.rdf #30-classic-CAMSIZER-Repeatability-xc_min_015.rdf #30-classic-CAMSIZER-Repeatability-xc_min_Mv.rdf 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. 73

CAMSIZER XT for 3D Printing Powders Applications Plastic, Ceramic & Metal Powder Unique, almost 100% agreement with sieve results (particle width = xc min) Reliable detection of oversized and undersized particles down to 0.01% Fast: typically 1-3 minutes per measurement Flexible dispersion options (air pressure, liquid, free fall) Shape analysis (roundness, aspect ratio, circularity, etc.) Surface area calculation Independent measurement of particle length and width provides more details CAMSIZER s equivalent circle area (xarea) to compare with laser particle sizers Very repeatable and reproducible results, with excellent instrument-to-instrument agreement Very high resolution (excellent capability to detect multimodal distributions!) Easy to operate, results independent from operators 74

Thank you for your attention!