Qualifying and quantifying powder flowability for powder bed fusion technology

Powder production routes[1], actual AM process and recycling methods all influence particles characteristics. In powder bed fusion, these properties affect the homogeneity and density of the powder layers spread across the build platform and, in turn, the process repeatability and the parts quality.  Quantifying a combination of factors defining a ‘good’, process-able powder is still required for AM. Yet little has been studied to link traditional powder measurements to its flowability and to its AM process-specific spreading abilities. In this post, let’s discuss suitable parameters and values to qualify flowability of metal powders for selective laser melting (SLM).

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Much time and efforts focus on developing processing maps for commercial metal powders. In addition to laser parameters as well as physical and chemical properties of the raw material, powder layer properties directly affect the processing window: by changing laser absorption properties[2] (with density);  by affecting the melt pool dynamics and influencing pores formation[3]; etc
In that respect, it is intuitive to assume that “good” natural powder flowability is required to facilitate layer recoating. To describe flowability for SLM, it is necessary to define meaningful parameters and to establish their acceptable range of values.
Various different techniques are used for general powder flow measurement [4-7]. Few of them are meaningful in the context of AM: the Hausner ratio HR, defined as the ratio between tapped and bulk density [8] is widely used and described in ASTM D7481-09 [9]. The angle of repose defined in ISO-4490 [10] /ASTM B213 [11] is described as the slope angle of the cone formed by powder particles after they’ve flown freely through a funnel onto a plate. It is generally considered as a measure for powder flowability and recommended by ASTM as the characterisation method for metal powders for AM [12].

In the context of AM technology, two main methods are typically used to assess powder flowability [13]:
1. A qualitative optical evaluation, mostly based on experience;
2. A quantitative evaluation based on the avalanche angle and the surface fractal of the powders. measured using a revolution powder analyzer.

Qualitative method: optical assessments

Let’s assume a few batches of powders with particles varying in size between 4-75um. Their  usability in SLM machines equipped with recoating blades and powder reservoirs is limited to 2.5 to ensure homogeneous layers. This limit may vary with different recoating configurations.
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experience-based optical assessment of powders for AM [13]
Quantitative method: avalanche angle with powder revolution analyser

Measuring the avalanche angle only requires a simple set up. A rotating, transparent drum is filled with a known amount of powder. A camera records backlit binary images of the powder free surface and the cross-sectional area of powder inside the drum.
Picture analysis extrapolates different avalanche angles that vary with powder flowability.
This technique can be used to quantify powders based on the avalanche flow index (AFI) and cohesive interaction index (CoI)[14]. It has been used successfully to characterise different Ti6Al4V powders for SLM [15] and plastic powders for SLS [16].

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powder revolution analyser [13]
Before testing the flowability, a fluidisation cycle is commonly used to normalise the powder condition in the drum: this gets rid of gravity (the powder ‘settles’) and handling effects.

The avalanche test also allows a statistical analysis of many different parameters such avalanche angle, surface fractal, volume expansion rate, etc:
• Avalanche angle: angle between the horizontal reference line and the linear fit of the free powder surface just before an avalanche starts;
• Avalanche surface fractal: measure of the fractal dimension (=’jaggedness’) of the surface profile [17]. This parameter fits the perception of a powder level of cohesiveness and is an indirect measure of inter-particle forces.
• Volume expansion ratio [16]: ratio between the volume measured inside the drum and the volume occupied by the powder in the preparation container.

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Optical assessment vs Hausner ratio [13]
The aim is to derive a quantitative assessment of the flowability in order to evaluate the usability of powders in powder bed fusion AM. This is done by evaluating the results of optical assessment, Hausner ratios HR, volume expansion ratio, avalanche angle and surface fractal.

Differences between experience-based evaluation and Hausner ratio HR indicate that HR is not sufficiently representative of flowability in the case of fine metal powders.
 
Practically, measuring avalanche angle and fractal surface seem more meaningful phenomenological parameters. They naturally encompass inter-particles forces, morphology impact, size distribution, etc…


That may be why the direct comparison of the optical evaluation with the measured avalanche angle and surface fractal values shows a clear correlation.

For powders exhibiting natural ‘good’ flowability, avalanche angle and surface fractal have low values and narrow standard deviations. It is assumed the presence of particles clusters would trigger more irregular occurrence of avalanches and a more jagged powder surface.
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optical assessment vs avalanche angle and surface fractal values [13]
To sum up

Using a revolution powder analyser shows it is possible to quantify powders flowability for AM. The results correlate with optical qualitative, experience-based evaluations.

Yet, this doesn’t take into consideration machine-specificities such as spreading mechanism, or required flowability limits… Besides, additional layer properties, including density and physical and optical layer properties, need to be defined and quantified. Measuring correlation between flowability, powder density, particle size distribution and particle shape would present great interest to assess their impact on SLMed part quality.

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References
[1] Jason Dawes, Robert Bowerman and Ross Trepleton Introduction to the Additive Manufacturing Powder Metallurgy Supply Chain, JOHNSON MATTHEY technology review Volume 59, Issue 3, July 2015
[2]. Boley CD, Khairallah SA, Rubenchik AM (2015) Calculation of laser absorption by metal powders in additive manufacturing. Appl Optics (in press):11
[3]. Gu¨rtler FJ, Karg M, Dobler M, Kohl S, Tzivilsky I, Schmidt M (2014) Influence of powder distribution on process stability in laser beam melting: analysis of melt pool dynamics by numerical simulations. In: Bourell D (ed) Solid freeform fabrication symposium. SFF, Austin, pp 1099–1117
[4]. Krantz M, Zhang H, Zhu J (2009) Characterization of powder flow: static and dynamic testing. Powder Technol 194:239–245. doi:10.1016
[5]. Castellanos A (2005) The relationship between attractive interparticle forces and bulk behaviour in dry and uncharged fine powders. Adv Phys 54(4):263–276
[6]. Schulze D (1996) Measuring powder flowability: A comparison of test methods. Part I. powder and bulk engineering. CSC Publishing Inc., St Paul
[7]. Schulze D (1996) Measuring powder flowability: a comparison of test methods. Part II. powder and bulk engineering. CSC Publishing Inc., St Paul
[8]. Hausner HH (1981) Powder characteristics and their effect on powder processing. Powder Technol 30(1):3–8. doi:10.1016/0032-5910(81)85021-8
[9]. ASTM_International (2009) ASTM D7481-09, standard test methods for determining loose and tapped bulk densities of powders using a graduated cylinder.  ASTM_International, West Conshohocken, PA
[10]. International Standardisation Organisation (2014) ISO 4490:2014—Metallic powders—Determination of flow rate by means of a calibrated funnel (Hall flowmeter). ISO
[11]. ASTM_International (2013) ASTM B213-13: standard test methods for flow rate of metal powders using the hall flowmeter funnel. ATM_International, West Conshohocken, PA
[12]. ASTM_International (2014) ASTM F3049-14: Standard guide for characterizing properties of metal powders used for additive manufacturing processes.  ASTM_International, West Conshohocken, PA
[13] A. B. Spierings, M. Voegtlin, T. Bauer,  K. Wegener, Powder flowability characterisation methodology for powder-bed based metal additive manufacturing, Prog Addit Manuf , july 2015, DOI 10.1007/s40964-015-0001-4
[14] Soh JLP, Liew CV, Heng PWS (2006) New indices to characterize powder flow based on their avalanching behavior. Pharm Dev Technol 11(1):93–102. doi:10.1080/10837450500464123
[15]. Gu H, Gong H, Dilip JJS, Pal D, Hicks A, Doak H (2014) Stucker BE effects of powder variation on the microstructure and tensile strength of Ti6Al4 V parts fabricated by selective laser melting. In: Bourell D (ed) Solid freeform fabrication symposium. SFF, Austin, pp 470–483
[16]. Amado F, Schmid M, Levy G, Wegener K (2011) Advances in SLS powder characterization. In: paper presented at the proceedings of the annual international solid freeform fabrication symposium, Austin, Texas, August 3–5
[17]. Allen M, Brown GJ, Miles NJ (1995) Measurement of boundary fractal dimensions: review of current techniques. Powder Technol 84(1):1–14. doi:10.1016/0032-5910(94)02967-S

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