Analytical Solutions for Modern Production Processes

Elemental Analysis & Metrologyfor Powder Metallurgy

Innovation with Integrity

Additive manufacturing, hot isostatic pressing and metal injection molding all have one common component: metal powders.

Powder metallurgy enables today’s most demandingproduction processes, and Bruker offers the most comprehensive range of elemental and compositionalanalysis of these advanced materials. Our instrumentsmonitor light elements and argon content, quantifycrystalline phases and determine the morphometry of powder particles.

The content of light elements like O, N, H and C, S canchange. They need to be measured at every processstep. Argon and diffusible hydrogen are especially sensitive because even traces can cause fatal damageto the final workpiece. To ensure product quality internaland external surfaces should be compared to their underlying CAD models. Element mapping, residualstress and texture analysis, and final part inspection are also all required. Only Bruker offers all these analytical solutions.

Powder Metallurgy

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Metal Powders

AdditiveManu-facturing (AM)

Hot Isostatic Pressing (HIP)

Elemental CompositionAccurate analysis of majors, minors andimpurities for incoming material inspec-tion as well as quality control of finalmetal powders. Needs to be fast andcomprehensive – as many different elements as possible in 5 min.

Light Elements: O, N, HUnlike the metal content, the light element content will change during theproduction process of metal powders. O, N, and H strongly influence the material properties and qualities. That’swhy O, N, H must be analyzed before and after the atomization process.

Light Elements: C, SCarbon is the most alloying element insteel but also common in other metals,influencing many mechanical propertiesand determing grades. It is also presentas surface contaminations. Sulfur is agenerally undesirable element.

ArgonThe usage of argon during the atomiza-tion process can lead to unwanted argoninclusions in the metal powders. Thismay cause, even in traces (< 60 ng/g),serious damage to the final parts. It is essential to control the argon content after atomization.

Crystalline PhasesIn addition to the elemental content, therespective crystalline phase compositionand structure is of upmost importance to product quality and process control. Applications range from validation ofprecursor feedstock of metal powdersand binders to quantification of injectionmolding mixtures.

MorphometryThe quantitative analysis of the form of the metal powders needs to includeparameters like sphere size distribution,sphericity, packing, porosity, surface tovolume ratio, surface roughness, convexity, and form factor.

ArgonThe argon content needs to be analyzed two times:For the first time for the incoming inspection of the metal powders, forthe second time after the printingprocess, to obtain information aboutthe residual porosity before the expensive HIP process.

Light Elements: O, N, HAs O, N, H content can change, theselight elements must be analyzed afterevery production step. Besides the incoming inspection of the metal powders and the analysis of the sup-port structures after printing, it is im-portant to monitor the oxidation (O) and the humidity (H) of the metal powder used in the printer, especiallyafter refilling and homogenizing for the next printing job.

Light Elements: C, SThe content of carbon and sulfur needs to be analyzed before the metalpowders are used in additive manufacturing.

Diffusible HydrogenEspecially for ferrous metal powders, the content of diffusible hydrogen (dH)is crucial and even traces may cause serious problems by hydrogen embrittlement. It is of utmost impor-tance to keep the content of diffusibleor trapped hydrogen at an absolute minimum.

CAD ComparisonFor the quantitative comparison between the manufactured part andthe CAD model, deviations need to be measured at each point in 3D, at internal and external surfaces.

ArgonThree reasons why argon is the element to analyze when it comes to HIP:

For a capsuled HIP process it is important that no argon is present in the metal powder. Due to the factthat it is impossible to remove thisargon from the final workpiece, youhave to analyze the argon contentbefore the HIP process.

After the process, an argon measurement shows that the capsuleremained tight during the entire HIPprocess (e.g. due to shrinking and induced micro cracks in the capsulewelds).

Finally, it is important to check the quality and purity of the argonprocess gas before and during theHIP process. Conclusions about thequality and the progression of theHIP process can be drawn by analyzingother gases emitted (e.g. from thecapsule) like CO, CO2, H2O or CxHx.These can be recorded in form of an impurity analysis.

For the post HIP analysis the supportstructures are used, so none of the valuable parts have to be destroyed.

CAD ComparisonFor the quantitative comparison between the manufactured part andthe CAD model, deviations need tobe measured at each point in 3D, at internal and external surfaces.

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Metal Injection Molding (MIM)

Failure Analysis

Diffusible HydrogenEspecially for ferrous metal powders, the content of diffusible hydrogen (dH) is crucial and eventraces may cause serious problems byhydrogen embrittlement. It is of utmostimportance to keep the content of diffusible or trapped hydrogen at an absolute minimum. That’s the reasonwhy the dH level must be analyzed before and after the molding and after the debinding process.

Light Elements: O, N, HFor incoming inspection and after everyprocess step, molding, cleaning and debinding, the content of O, N and Hmust be checked. Because unlike theamount of metals, the content of light elements will change during the production process.

Light Elements: C, SThe content of carbon and sulfur needs to be analyzed before the metalpowders are used. The carbon level inthe intermediate and final products areimportant to monitor the debindingprocess after the MIM process.

CAD ComparisonFor the quantitative comparison between the manufactured part andthe CAD model, deviations need to be measured at each point in 3D, at internal and external surfaces.

Element MappingAnalysis of inhomogeneity, inclusionsand foreign particles in manufacturedparts with 300 µm resolution by high performance XRF2.

Residual Stress AnalysisUnderstanding the stress state that re-mains in a component after processing isessential to maximizing lifetime of manu-factured components. Components withcompressive surface stress traditionallyexhibit prolonged lifespan, while a tensilesurface stress can lead to premature failure.

Texture AnalysisAs materials are pushed to their limits it is important to ensure that every crystallite is in proper alignment. Texture analysis is used to quantify the magnitude and direction of crystallite orientation in a component.

Crystalline PhasesIssues with dimensional stability are not only the consequence of macroscopicissues, but may be also due to an im-proper phase composition and structure.Austenitic phase transformations are aclassic example of this in ferrous alloys.

ArgonTo discover the reasons of argon inducedcracks and voids you have to measure its amount.

Light Elements: O, N, HOxygen is measured to find the reasonsfor corrosion and defects, total hydrogento detect the cause of pores in aluminum.

Diffusible HydrogenHydrogen embrittlement – the name says it all.

Parts InspectionFailed products must be inspected and analyzed for cracks and voids. The contact area at the interface between different materials should be analyzed for defects.

X-Ray Fluoresence (XRF)

Elemental Composition: Ti, Cr, Mn, Fe …

Element Mapping

Inert Gas Fusion Analysis (IGF)

Light Elements: O, N, H

Diffusible Hydrogen: dH

Nobel Gas: Ar

Combustion Gas Analysis (CGA)

Light Elements: C, S

X-ray Microtomography (µCT)

Morphometry: Sphericity, Size, Porosity …

CAD Comparison

Parts Inspection

X-Ray Diffraction (XRD)

Residual Stress Analysis

Texture Analysis

Crystalline Phase Identification

and Quantification

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The combustion analyzerG4 ICARUS is the idealinstrument for rapid andprecise C and S analysisin solids, especially withmetallic materials andother inorganic materials.

Light Elements,solid: C, S

Especially suited for -the detection of surface contaminations, occuredfrom dust or hydrocar-bons, in powder metallurgy.

Ideal for analyzing the-bulk content of C and S.

Monitor the debinding-process after the MIM process.

Monitor the C level -before and after carburization during case hardening.

The S8 TIGER is the mostversatile tool availablefor advanced elementalanalysis in both industryproduction and research.This high-performancewavelength dispersive X-ray fluorescence spec-trometer is analyzing almost the entire periodic table.

ElementComposition

Turn-key solution-METAL-QUANT to covermore than 23 elementsin less than 5 minutes.Elements of interest: -Ti, Cr, Mn, Fe, Co, Ni, Cu, Nb, Mo, W …Traces, down to ppm: -Si, P, S, Cl, Ta, Pb …

Element Mapping

XRF2 small spot mapping-provides detailed mapsof the elemental distri-bution in materials. 300 µm spot and 100 µm-step size based on HighSense™ beam pathfor optimal precision and detection power.

X-ray Fluorescence

S8 TIGERInert Gas Fusion Analysis

G8 GALILEO MSCombustion Analysis

G4 ICARUSX-ray Microtomography

SKYSCAN 1173SKYSCAN 1272

X-ray Diffraction

D8 DISCOVERD8 ADVANCED2 PHASER

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The G8 GALILEO MS is a high-end instrumentdesigned for fast deter-mination of O, N, H, andAr. This analyzer is basedon the inert gas fusionprinciple, coupled to amass spectrometer (MS).

Argon

Detection of Ar in raw-materials and final products down to a few ng/g (ppb).Discovers reliably Ar -inclusions, which maylead to complete partfailures.

Light Elements,gaseous: O, N, H

Reliable detection from-traces up to high concen-trations.

Diffusible Hydrogen: dH

Detection of diffusible-and trapped H. Thermal desorption -mass spectroscopy for analyzing the kineticbonds of H in the material.

Desktop µCT is used for fast, non-destructivecharacterization of sam-ples from the µm to cmscale with a resolutiondown to a few micronswithin minutes.

Morphometry

Quantitative determina--tion of porosity & inclu-sions, volume fractions,orientation, dimensions,surface, and angles.

CAD Comparison

Automatic, quantitative-comparison of externaland internal surfaces. Pass/fail monitoring with-defined tolerances atpre-defined inspectionpoints.

Parts inspection

3D µCT scan, reconstruc--tion and quantitativeanalysis of defects.Reaction of parts to -mechanical stress andtemperature changesusing in-situ stages.

X-ray diffraction is the only method to deter-mine the phase composi-tion, the texture and theresidual stress in a non-destructive way.

Crystalline Phases

Comprehensive phase-identification, quantifica-tion and microstructuralcharacterization of metal powders with a LYNXEYE XE-T 1D detectorand TOPAS software.

Small spot measure--ments of manufacturedcomponents with a mi-crofocus source, largesample stage and a 2Ddetector (XRD2 setup).

Residual Stress

Fast and reliable results-with XRD2 setup andLEPTOS S for analysis.

Texture Analysis

XRD2 setup and -DIFFRAC.TEXTURE soft-ware, the best choice for texture analysis.

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