Powder metallurgy andadditive manufacturing
Material characterization solutions

2

3

Shaping the future
Powder metallurgy is an umbrella term that covers
a range of processes for manufacturing metallic
components from metal powders usually by first forming
a dimensionally stable compact and then sintering it. The
main processes include;

In-size range frequency (%)

Lasercladding
45 - 75 µm

Additive Manufacturing is a relatively new technique that
permits local fusing of metal powders using a laser, electron
beam, or by post-sintering adhesive bonded powders.

• Press and SinterThere are a number of reasons for using a powder
metallurgy process instead of a traditional process such asmachining. These include one or more of the following:• Metal injection molding• Significant cost savings• Hot/Cold Isostatic pressing• High dimensional accuracy• Additive manufacturing• Minimal post processing

Traditional powder metallurgy processes such aspress and sinter have been used to produce metallic
components since the 1920s while processes such as
Hot Isostatic Pressing (HIP) and Metal Injection Molding(MIM) have been employed since the 1960s and 70s
respectively.

• Good part to part reproducibility

Brazing
53 - 150 µm

Representation of an
as-atomized particle
size distribution

Laser melting
15 - 45 µm
Electron beam
melting
45 - 106 µm
Cold spray
5 - 45 µm
Metal injection
moulding <38 µm• Greater dimensional freedom andcompositional complexity

Press and Sinter>45µm• Reduced waste

Isostatic pressing(Whole distribution)
10

100

1000

Particle diameter (µm)
Powder metallurgy refers to the production andworking of metals as fine powders which can bepressed and sintered to form objects.

Press and sinterPowder characteristics are important for press and sinter,as for other powder metallurgy processes, with particle
packing and apparent density of the powder blend
critical.

Metal powder manufacture
Metal powders are common to all powder metallurgy
processes hence the powder manufacturing process andresultant powder properties are critically important andintrinsically linked.

The choice of powder manufacturing route depends onthe metal / alloy, the powder metallurgy process, and thepowder properties required for that process.

The main routes for manufacturing metal powders are:

• Particle size distribution• Comminution of solid metal• Precipitation of a salt from solution• Thermal decomposition of metal
carbonyl (Carbonyl process)• Solid state reduction of metal oxide• Electrodeposition• Atomization of molten metal

Key powder characteristics are:
• Particle shape• Micro-structure• Surface condition• Elemental composition• Flowability

A lower apparent density gives greater compaction
and cold-welding of particles on pressing, resulting
in a stronger green body. Interparticle friction is also
important and facilitates contact, deformation anddensification of the structure during pressing.

1• Measure and control batch-to-batch
variability in the metallic powder• Ensure alloys have the correct elemental
composition and phase structure• Determine residual stress, strain andtexture of sintered parts2

2. Die compaction - the powder blend ispressed in a die to form a compact‘green body’
3. Sintering – the ‘green body’ is heated
to below its melting point to form thesintered component• Comprehensive determination of sintering behavior• Ensure optimum flowability and packing in the die
to prevent defects in the sintered component

Metal powder hardness also affects pressing
performance and can depend on phase composition
and grain size. Malvern Panalytical’s and NETZSCH’s
characterization solutions for Press and Sinter can beused to:
1. Powder blending - metal powder is mixed
with a suitable lubricant• Predict and control powder packing to give the required
volume reduction and degree of cold-welding

3
Force

Powder loose

Powder partiallypressed

4
Force

Powder fullypressedGreencompact45Additive manufacturing
In powder bed fusion processes a metal powder
layer is applied to a building platform and a laser orelectron beam is used to selectively melt or fuse thepowder. After melting the platform is then lowered
and the process repeated continually until the build iscomplete. The unfused powder is removed and either
reused or recycled depending on its condition.

Malvern Panalytical’s and NETZSCH’s characterization
solutions for Additive Manufacturing can be used to:• Ensure a consistent powder supply andprevent variations in product quality• Identify suitable powders for machines withdifferent spreader or rake designs• Predict and optimize powder packing
density and flow characteristics

Injection molding

Feedstock

DebindingSintering• Determine residual stress, strain andtexture of manufactured components• Optimize melting and crystallization behavior

Powder feedpistonMixing• Ensure powders have the correct elemental
composition and phase structure

The particle size directly influences these properties
and is a key specification for this process, with the
optimum particle size being in the range 15-45 μm
for SLM and 45-106 μm for EBM for example.

Powder feed
supplyBinder• Optimize atomization conditions toachieve desired powder properties

The efficiency of powder bed additive manufacturing
processes and the quality of finished components
is largely dependent on the flow behavior
and packing density of the powders.

Laser

Metal powder

Isostatic pressing

Scanning
mirrorUnfusedpowderRollerBuildchamberBuildpistonFused
powderBuild
objectMetal injection molding
The rheological properties of the feedstock are of major
importance for MIM applications since they influence
the homogeneity of the molten feedstock, how wellit flows through the die into the mold cavity, and themechanical properties of the green part on cooling.
Rheological properties are influenced by anumber of factors including; binder molecularweight and structure; solids loading; particle
size and shape; temperature and flow rate.

Isostatic pressing is a forming process wherepressure is applied uniformly (using gas or liquid) to ahermetically sealed container filled with compacted
metal powder. The benefits of isostatic pressing overpress and sinter are equal compaction in all directions
and more uniform density in the final component.

Phase composition and crystallite size arealso important since these can affect powder
hardness and melt properties which impact
pressing efficiency and sintering behavior.

Isostatic pressing can be performed at elevatedtemperatures (Hot Isostatic Pressing (HIP)) or atambient temperature (Cold Isostatic Pressing (CIP)).
Although HIP is a direct manufacturing route formetal components it can also be used for densifying
parts from other powder metallurgy processes.

• Predict and control packing density andminimize void formation in the sintered part

Spherical powders with a relatively wide but consistentparticle size distribution are preferred for HIP as
they give higher fill densities. For CIP, some particle
irregularity may help increase cold-welding, ideally
without compromising powder flow and packing.

Malvern Panalytical’s and NETZSCH’s characterization
solutions for Isostatic Pressing can be used to:• Specify and control metal powder quality• Optimize powder flow in the mold andmaintain process efficiency• Ensure powders have the appropriate phasestructure and elemental composition

Slight particle irregularity can be beneficial to givemechanical strength to green and brown parts.
Malvern Panalytical’s and NETZSCH’s characterization
solutions for Metal Injection Molding can be used to:• Optimize particle loading to minimize
part shrinkage and void formation• Ensure appropriate feedstock rheology duringmolding, and dimensional stability post-extrusion

Most metals can be used in MIM if they have the correct
powder properties, including particle size and shape.

• Optimize binder properties including
molecular weight and structureHigh packing densities are required, so spherical particles
with the correct size distribution are preferable, as are
smaller particles (< 38μm) that sinter more readily.

• Characterize debindering and sintering
behavior of green/brown parts• Ensure consistent metal powder supplyFill container withmetal powder

Heat under vacuum
to remove volatilecontaminants

Hermetically seal
container

Apply pressureand heatRemove sinteredcomponent

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7Morphologi 4

What do your customers say?

Direct measurement of metal powder size and shape

Wall Colmonoy invest in Morphologi 4 to improve their metal
powder products and manufacturing processes

The Morphologi 4 is an advanced yet easy-to-use, particle
characterization tool for measuring particle size and shapefrom 0.5 microns to several millimeters. The instrument
offers the flexibility required for R&D and troubleshooting
applications, as well as the user-independent results
and validation required for automated QC analysis.
For many powder metallurgy applications, particle shape
can be just as important as particle size. The Morphologi
4 reports shape information using parameters such aselongation, circularity, convexity to quantify particle
irregularity and surface roughness. More efficient than manual
microscopy and electron microscopy, automated imaging
provides statistics on tens of thousands of particles.

Rough

SmoothRegularElongated

Wall Colmonoy is a leading global materials
engineering group of companies engaged
in the manufacturing of Colmonoy® andWallex® surfacing and Nicrobraz® brazing
products, precision castings, coatings, andengineered components across aerospace,automotive, oil & gas, mining, energy andother industrial sectors. Headquartered in
Madison Heights, Michigan, Wall Colmonoy
have been an established name in metallurgy
since 1938, with several sites in the US andEuropean headquarters in Swansea, UK.
Wall Colmonoy manufactures over 500 different
metal powder products at their Pontardawe facility in
Swansea and have a comprehensive suite of analyticalequipment for characterizing their powders: including
laser diffraction, chemical analysis, rheometry, optical
microscopy and electron microscopy. With a recent
move into Additive Layer Manufacturing, where powder
properties such as particle size and shape are often
more critical, there was a need to expand their analyticalcapabilities.
“We know that particle shape directly influences Additive
Layer Manufacturing performance and our customers
expect a high-quality product with the correct size
distribution and a spherical morphology” said Tom
Roblin, Process Engineering Manager. “We have manual

FeaturesBenefits

Particle size range from 0.5 μm to 1000 μm

Make size measurements of powders for all powder metallurgy applications

Measurement of non-spherical particles
in terms of their length and width

Provides a more relevant size measurement of irregular particles

Automated image analysis that reports
a range of shape parameters

Quantify particles in terms of the degree of irregularity or surface roughness

Automation of manual methods
such as microscopy

Perform microscopy measurements faster and lesssubjectively, while freeing up resource

Integrated dry powder dispersion unit

Easy, reproducible sample dispersion which is
critical to achieving meaningful results

Optimized microscope optics and highsignal to noise CMOS camera

Generation of high quality particle images and image analysis data

Automated SOP control from sample
dispersion to results analysis

Simple, intuitive operation and robust, repeatable measurement protocols

microscopy and electron microscopy which allow us toqualitatively check the products we manufacture but wealso needed a technique that could provide quantitative
data on a statistically representative sample.”
The technical team recognized that an automated opticalimaging platform capable of analyzing a large number ofparticles was required. They also needed image analysis
capabilities that could automatically quantify the size andshape distribution of those particles. “We identified threeplatforms that we thought could meet our requirements.
This included two Dynamic Imaging systems and theMorphologi 4 Static Imaging system from Malvern
Panalytical” said Roblin. “While Dynamic Imaging was able
to analyze a larger sample volume, the superior image
clarity provided by the Morphologi 4 was of greater
importance to us and also gave more consistent results”.
The Morphologi 4 has found multiple applications within
the laboratory, not just for Additive Layer Manufacturing
powders, but for many of their other products also.
“Morphologi 4 is used to quantitatively measure theparticle shape of our atomized alloy powders. By
investing in this measurement equipment, we canbenchmark and improve our current processes andproducts.” said Roblin. “It will also aid in the developmentof a new range of Wall Colmonoy powders for Additive
Layer Manufacturing. For us, it is a valuable tool thatprovides clear images, quantitative analysis andconsistent results.”89Mastersizer 3000

OMNISEC

Accurate particle size with minimum effort

The most advanced multi-detector GPC/SEC system

The Mastersizer 3000 is the latest generation of theworld’s most widespread particle sizing instrument,
used by many thousands of companies and research
institutes across a wide range of industries.

OMNISEC is a Gel Permeation Chromatography (GPC)/ Size Exclusion Chromatography (SEC) system for themeasurement of absolute molecular weight, molecularsize, intrinsic viscosity, branching and other parameters.

OMNISEC can accurately measure the mostimportant characterization parameters, including:

The system includes OMNISEC RESOLVE, the integrated
GPC/SEC module, OMNISEC REVEAL, the integrated
multi-detector module and OMNISEC software, for thecharacterization of synthetic and natural polymers.

• Intrinsic viscosity and molecular structure

Malvern Panalytical’s considerable experience andapplications know-how has gone into every stageof the design of the Mastersizer 3000 instrument,from fundamental particle sizing performance rightthrough to user ergonomics and method advice.
The Mastersizer 3000 also has an optional
dynamic imaging module called Hydro Insightallowing simultaneous particle images andparticle shape information to be generated.

Many of the disadvantages of traditional sieve
analysis are addressed by the Mastersizer 3000:• Faster and simpler analysis• Increased measurement range
including very fine particles• Better measurement resolution forimproved product quality• Trouble free maintenance• Absolute molecular weight andmolecular weight distribution• Particle images and shape information• Sieve correlation algorithm

FeaturesBenefits

FeaturesBenefits

Measure particles in the size range 0.01 µm – 3.5 mm

Enable accurate measurement of almost any
metal powder fineness and formulation

Highly sensitive light scattering (LS) detector

Measure molecular weights of polymers, oligomers and waxes down to 200 g/mol

High accuracy, repeatability andreproducibility (< 1% variation)

Verifiable instrument-to-instrument
performance that you can rely on

Integrated differential viscometer

Measure intrinsic viscosity (IV) to investigate molecular structure and branching

Temperature controlled detectors

Achieve better baseline stability for improved accuracy and sensitivity

Easy sample loading and cleaning

Reproducible dispersion with minimal
sample to-sample contamination

Workflow oriented software

Makes GPC/SEC measurements and analysis as easy and intuitive as possible

Rapid measurements (<20 sec)

Increased throughput/productivity andmore efficient process control

Integrated column oven

Improve separation quality and resolution

Refractive Index (RI) detector

Measure the concentration of almost any solute

TCP/IP or Autolab driver remote control via Malvern Link™ II

Feed results directly to the plant process control system

Triple detection (RI, IV and LS)

Modern and intuitive software interface

Streamlined method development and built-in expert advice

Combine data to determine as hydrodynamic radius (Rh),radius of gyration (Rg) and Mark-Houwink parameters

Meets all the recommendations for ISO13320

Guarantees quality and compliance

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11

EpsilonZetiumBenchtop XRF spectrometers for simple elemental analysis

Floor-standing XRF for elemental excellence

X-ray fluorescence (XRF) is routinely used by metal
powder producers and component manufacturers
for determining the elemental composition of
metal alloys and for detecting the presence ofcontaminants. Elemental composition is particularly
important for alloys since small variations in theconcentration of alloying elements can affect its
chemical and physical properties, including strength,
hardness, fatigue life and chemical resistance.

Designed to meet the most demanding process control
and R&D applications, the Zetium spectrometer leads
the market in high-quality design and innovative
features for quantitative analysis of elements ranging
from beryllium (Be) to americum (Am), and is thepreferred choice when light element analysis andanalytical precision is important. The modular design
also allows for various task-oriented enhancements
to meet specific application requirements.

The Epsilon range of Energy Dispersive X-ray fluorescence(EDXRF) analyzers are capable of simple element
identification and quantification from sodium (Na) toamericium (Am). They are easy to operate, compact and
X-ray safe instruments without the need for additional
chemicals. Considerable savings in time and cost are
two of the many benefits EDXRF can bring comparedto alternative analytical techniques such as ICP.

FeaturesBenefits

Analysis with/without reference standards

Can be calibrated with reference materials for most accurate
data or without for samples with unknown composition

Versatile sample presentation

Can analyze sample types including liquids andslurries, pressed powders, loose powders, fusedbeads and irregularly shaped objects

Both systems have compact design with Epsilon 1
having a built-in computer and touchscreen.

Requires less bench space and allows for easy anddirect instrument operation in the lab or at-line

detector
Epsilon 4 has optional SDD
for ultra light element analysis

Analysis of ultra light elements such as carbon,
nitrogen and oxygen down to 1 wt%

Epsilon 4 has a 10-position removablesample changer with spinner

Automatic processing of sample batches and minimalerrors caused by non-homogeneity of sample

Epsilon 1 has optional small spot capability (1 mm spot size)with camera for easy positioning

Quantify inclusions and contaminants to determine their origin

Ultra

Zetium uses SumXcore technology which brings
together the benefits of WDXRF (Wavelength Dispersive)and EDXRF (Energy Dispersive) XRF with uniqueadvantages for the analysis of metals, including:• reduction in analysis time and improved precision• identification of unexpected elements in samples
For inclusion or contaminant detection, small
spot mapping and elemental distribution
analysis can be performed.

FeaturesBenefits

Analysis with/without reference standards

Can be calibrated with reference materials for most accurate
data or without for samples with unknown composition

Versatile sample presentation

Can handle sample types including pressed powders, loose
powders, fused beads and irregularly shaped objects

High-capacity sample changer

High-throughput analysis of up to 240 samples per 8-hour shift

System enhancement packages

Can be easily adapted and upgraded to meet future testing requirement

SuperQ software with Virtual Analyst

Simple and intuitive task-oriented workflow with expert guidance for ease-of-use

Small spot analysis with elemental mapping

Determine spatial distribution of elements andpresence of inclusions or contaminants

SumXcore - Combined WD/ED XRF

Reduced measurement times with improved precision and sensitivity

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13

EmpyreanAeris

The multi-purpose X-ray diffractometer

Phase analysis made simple

Empyrean is a multipurpose X-ray diffractometer for
determining the micro-structural characteristics of metal
powders and their fabricated components, including;Empyrean features a MultiCore Optics system thatenables a large variety of different measurements to be
performed automatically without manual intervention.

• phase composition

Empyrean has the unique ability to measure a variety ofsample types including powders, thin films, nanomaterials
and solid objects, over a wide range of temperatures.

Aeris is a user-friendly compact X-ray
diffractometer that provides fast, reliable andaccurate phase identification and quantificationof your metal powders. Aeris makes X-ray
diffraction simple and accessible to everyone.

• crystallite size
• texture (crystallite orientation)• residual stress/strain
These characteristics can affect properties such as
hardness, strength and fatigue life, and are influenced
by thermal and mechanical processes such as
atomization, laser melting and powder pressing.

It has an unrivaled collection of sample stages andoptical components, including a tensile stage forsample analysis under stress, that can be easilyinterchanged to allow a wide range of diffraction,
scattering and imaging applications, including
computed tomography, to be performed.

FeaturesBenefits

MultiCore optics (iCore and dCore)

Automates measurements including multiple measurement
geometries to maximize instrument utilization and obtaina more complete understanding of your materials

Pre-aligned fast interchangeable X-ray modules (PreFIX)

Enables the diffractometer to be reconfigured in a few minutes
without module re-alignment, saving time and effort

Wide range of sample types

Can measure all sample types - from powders to thin films, fromnanomaterials to solid objects - even during tensile testing

Full suite of configurable modules andmeasurements including a tensile stage

The unique touch screen user interface
lets you proceed effortlessly through themeasurement process and results can also be
analyzed in the HighScore software to provide
a wealth of crystallographic information.

Aeris’ low cost of ownership delivers maximum returnon investment since it has limited infrastructure
requirements. For example, it has a small footprintand does not require compressed air or watercooling. It also has a much lower power consumption
compared to floor standing systems and its
X-ray tube has a virtually unlimited lifetime.
Aeris is also the first compact diffractometerto be fully automatable and can be easily
incorporated into a relevant process.

FeaturesBenefits

Simple touch-screen user interface

Intuitive operation that make measurements quick and easy even for the novice

Minimal infrastructure requirements

Provides access to a wide range of diffraction, scatteringand imaging applications on a single platform

No cooling water, no chiller, no compressed air - the only
thing you need is a single-phase power socket

HighScore/HighScore Plus Software

A range of non-ambient chambers for analysis
at temperatures ranging from -260ºC to 2000ºC
and under different atmospheric conditions

Study the effect of temperature, pressure, gas atmosphereand mechanical stress on phase transformation,
chemical reactions, recrystallization, etc.

Provides comprehensive phase identification, profile fitting,Rietveld, crystallographic and extended cluster analysis

Powerful search-match algorithm for
multiple reference databases

Optimizes search criteria across a wide range of reference databases
making it easier to identify minor phases in the diffractogram

HighScore/HighScore Plus Software

Provides comprehensive phase identification, profile fitting,Rietveld, crystallographic and extended cluster analysis

Automatable bench-top thatcan connect to a belt

Automate a process or perform high-throughput analysis

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15

Sample preparation equipment

Real-time particle sizing

What is fusion and why should I use it in my laboratory?

A watchful eye to optimize your process

Fusion is a sample preparation method developed in the
mid 50s. It involves dissolving a fully oxidized sample(at high temperature) in a suitable solvent (a flux) in aplatinum, zirconium or graphite crucible. The melted
mixture is agitated and poured into a mold to create aglass disk for XRF analysis. It can also be poured into abeaker to create a solution for AA or ICP analysis.

Manufacturing high quality metal powders economicallydemands exemplary process control. Establishedin-line and on-line particle sizing technologies
provide continuous process monitoring and a data
stream that supports complete process automation.
Such technology therefore makes it easier to makehighly consistent products to a tight particle size
specification at the lowest possible variable cost.

This universal technique has numerous benefits when
you compare it with other sample preparation methods
such as pressed pellets or acid digestion. One of the main
advantages of using fusion in the preparation of metals
is that the technique is not affected by mineralogical orparticle size effects, thus enhancing the precision andaccuracy of XRF results.

Why should I use fusion in my lab?

At the same time, continuous particle sizing has a role toplay in managing the re-use of high-value AM powders,a critical issue for economic viability. With a proventrack record and strong reliability, in-line and on-line
particle sizing technology holds considerable value formetal powder manufacturers establishing robust supply
chains for the PM industry, and for AM users looking
to optimize their powder management processes.

Atomization tower

This universal technique has numerous benefits when you compare it with other sample preparation methods such aspressed pellets or acid digestion

FusionPressed pellets

Affected by mineralogy

No

Yes

Affected by particle size

No

Yes

Desirable size of powder (microns)

50 - 100 (Easy)

5 - 30 (Difficult)Accuracy

≤1%

≤10%

Easy clibration with synthetic standards

Yes

No

Application of matrix correction

Yes

No

Product
cycloneCoolerTransfer
Water cooling

LeNeo fusion instrument prepares glass disks for XRF analysis
as well as borate and peroxide solutions for AA and ICP analysis.
This automatic electric instrument has one fusion position andis easy to use. It guarantees safety for the operator as wellas superior analytical performance in the laboratory.
TheOx Advanced fusion instrument has been designed by ourexperts to suit our customers’ ever-changing needs. This instrument
is powered by electricity and has six fusion positions. It is used toprepare glass disks for XRF analysis as well as borate and peroxide
solutions for AA and ICP analysis. Its extra features enhance
analytical performance and safety, benefiting users at all levels.
The Eagon 2 is a fully automatic fusion instrument that prepares glass
disks for XRF analysis. Its innovative patented design ensures performance,
operator safety and ease of use. The Eagon 2 instrument makes fusion
and the consequent benefits for accurate XRF analysis easily achievable.

Sieving unit

Laser diffraction (Insitec)

Real-time measurement system makes it possible toinstantly observe the effect of decreasing the speed ofrotation of the atomizing disk and the time taken for theprocess to re-establish a steady state. (Green Dv10, blue
Dv50, orange Dv90, red is transmission).

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17

Insitec

ParsumRobust, reliable, real-time particle sizing for process control

Real-time size measurements for screening applications

Insitec analyzers are on-line laser diffraction systems
that provide continuous particle size analysis, forefficient, cost-effective monitoring and control ofindustrial process streams. This includes dry powders,slurries, and sprays in the size range 0.1 μm to 2.5 mm.

The Parsum probe measures particle size distributionsand velocities of solid particles in gas streams using apatented spatial filtering velocimetry technique. It hasa size range of 50 μm to 6 mm and is widely used formonitoring and optimization of screening operations.
Real-time particle distribution data enables the user toreduce variability during processing and detect screen
breakages by monitoring for oversized particles.

spray drying, atomization, milling and screening, andreact in real-time to production fluctuations.
Malvern Link™ II software interface, enables full
integration with your plant control system and unlocks
the potential value of timely particle size measurement.
The dedicated analysis software, automation anddata reporting can be customized to meet individual
requirements.

Insitec provides real-time particle size distribution forautomatic ‘closed loop’ process control, enabling theoperator to optimize and control processes such as

The probe contains an array of light sensitive detectors
which are illuminated by a laser. This array can detect

single particles as they pass through the laser beam
within the probe measurement zone. The shadow
produced by each particle can be used to calculate theparticle velocity and its chord length (particle size).
The detector signals are sampled very rapidly (up to
10,000 particles per second) and particle size distribution
data is continuously updated during operation to produce
a real time particle size trend. This provides direct insight
into the performance of the process without the need forsample extraction.

FeaturesBenefits

FeaturesBenefits

Measure particles in the size range 0.1 µm – 2500 µm.

Enable accurate measurement of metal powder from a range of processes

Optical head and sample path certified to
Pressure Shock Resistance of 11bar(a) (PSR11)

Withstands extreme conditions of metal powder production

Real-time measurement of particles in the size
range 50 µm to 6 mm during processing

Continuous and uninterrupted monitoring of processes
such as sieving, pneumatic transport and mixing

Measure up to 20,000 particles in real-time

Ceramic linings protect critical, highvelocity areas of the sample pathway andpurging protects windows from dust

Maintenance requirements are minimal

Fast and statistically representative data for confident
decision making and optimum process control

Wide range of accessories, such as inline
dispersers and cleaning cells

Provides a so-called “process interface” for adapting themeasurement probe to different conditions within the process.

Provides continuous particle size data

Operators can react quickly and confidently
when making control decisions

Range of different probes for various
processes and environments

Make real-time measurements inside mixing vessels, undersieve-decks and during conveying, even in ATEX zones

Meets all the recommendations for ISO13320

Guarantees quality and compliance

IPP measuring software

Measures representative sample volume

Statistical reliability for process control

Flexible and adaptable system of programmes and interfaces thatcan control 4 probes simultaneously and gives real-time updatesof particle size distributions and sieve fractions/throughputs

Control system integration options –OPC, Modbus, Profibus, wired IO

Ease of reporting

Integrated software interface for plant automation

Deliver results in real-time to your control room and allow automation ofroutine tasks such as cleaning, maintenance and background checks

18

19

Rheology

Thermal analysis

Capillary and rotational rheometry forprocess-relevant material testing

Relevant thermal analysis solutions for metals and alloys

Rosand capillary rheometers allow the characterizationof polymer or suspension viscosities at shear rates andtemperatures applicable for extrusion and injection
processes. During MIM, shear rates in the rangeof 100 s-1 to 100,000 s-1 are created, which can becovered with the Rosand capillary rheometers.

The thermal behavior and thermophysical propertiesof metal powders is an important criterion for thequality of products manufactured by 3D printing. Heattransfer characteristics during, e.g., selective laser
melting process, the temperature distribution andmolten pool dimensions build the base of modeling.

Twin bore barrels enable absolute shear viscosity
measurements and simultaneous measurement ofextensional viscosities. Rosand Flowmaster™ software
also provides a comprehensive data acquisition andanalysis package for determining properties suchas thermal stability, wall slip and melt fracture.

Therefore, the thermal behavior (melting, crystallization,etc.) and thermophysical properties such as
thermal diffusivity, thermal conductivity, specificheat capacity, and density should be known.

Kinexus is an advanced rotational rheometerthat can measure complex shear rheology,
including viscoelasticity, on all material
types from liquids through to solids.
Rotational rheometry is ideal for evaluatingchanges in thermal properties due to compositionalor microstructural differences and can help to
optimize product and process performance.
Kinexus is capable of measuring time, temperatureand low shear properties of materials in oscillatory
shear using small sample volumes. It can measuretemperature transitions of binders and the effect ofparticle composition on feedstock viscoelasticity.
Other rheological properties such as yield stress,
creep and stress relaxation can also be measured.
Advanced Axial Capabilities allow Squeeze Flow
tests to be performed as well as thermal expansion
or shrinkage of the feedstock to be determined.

These properties influence the linear energy density,
volume shrinkage, scanning track length, hatch spacing
and time interval between two neighboring tracks on thetemperature distribution and molten pool dimensions.
The results of thermoanalytical measurements
support the improvement of temperature
distribution and molten pool dimensions.
Shorter track, shorter hatch-spacing andless time interval can lower the temperature
gradient and increase the temperature of eachtrack. The thermophysical properties provide
favorable values for the numerical simulation.

MethodRecordable Information

Temperature Range

Thermogravimetric Analysis (TGA)

Mass changes, thermal stability, decomposition

RT to 2400°C

Differential Scanning Calorimetry (DSC)

Phase transformation temperatures andenthalpies, specific heat capacity-180 to 1650°C

Simultaneous Thermal Analysis (STA)

Phase transformation temperatures and enthalpies,
specific heat capacity, mass changes, thermal stability-150 to 2400°C

Gas Analysis (EGA) Coupled
to Thermal Analysis

Characterization of gases emitted bymeans of MS, FT-IR, GC-MS-180 to 2000°C

Dilatometry (DIL) / ThermomechanicalAnalysis (TMA)

Dimensional changes, CTE (Coefficient oflinear thermal expansion), density changes-180 to 2800°C

Laser / Light Flash Analysis (LFA)

Thermal conductivity and thermal diffusivity-125 to 2800°C

Seebeck Coefficient (SBA)

Seebeck coefficient, electrical conductivity-125 to 1100°C

80.000

60.0000.1

20

2140.00020.000Differential scanning calorimetry
Unlike traditional metals manufacturing processes, metals
manufactured by Additive Manufacturing (AM) undergo
localized thermal cycles during fabrication. As a result,the liquid-solid phase transformation requires control. In
addition, thermal cycles create a challenge with respect
to solid-solid phase transformations. These thermal
effects can be investigated by means of Differential
Scanning Calorimetry (DSC). In accordance with ISO
11357-1, a sample and a reference are subjected to acontrolled temperature program (heating, cooling or
isothermal).

Measurement results by DSC

The actual measured properties are the temperatureof the sample and the temperature difference between
the sample and reference. From the raw data signals,
the difference in heat flow between the sample andreference can be determined.

• Liquid crystal transitions

Simultaneous thermal analysis
0

0

100

Temperature/°C

0.0
300

200

Hyphenated techniques for more insight• Specific heat capacity (cp)• Melting temperatures and enthalpies (heat of fusion)• Crystallization temperatures and enthalpies• Post-crystallization• Reaction temperatures and enthalpies• Phase transitions (solid-solid, solidliquid, phase diagrams)• Eutectic purity

Simultaneous Thermal Analysis (STA) generally refers to
the simultaneous application of Thermogravimetry (TGA)
Thermal Conductivity/[W/(m∙K)]
and Differential Scanning Calorimetry(DSC)
to one andSpecific Heat/[J/(g∙K)]
Thermal Diffusivity/(mm2/s)
the
10 same sample in a single instrument. The7 advantages
2.0
areboth the
9 obvious: The test conditions are identical for 1.8
6
TGA
and
DSC
signals(same
atmosphere,
gas
flow
rate,
8
1.6
water vapor pressure, heating rate, thermal 5contact with7
1.4
the sample crucible and sensor, radiation effect, etc.).
6
1.2
Furthermore, sample throughput is improved4 as more
5
1.0
information is gathered from each test run.
3

4

0.8

• Oxidative stability

Coupling
Gas Analyzers to Thermal Analyzers
3
0.6
2• Decomposition onset

0.4
By2 couplinga Thermobalance(TG, TGA), Simultaneous
ThermalDiffusivity
1
Thermal Conductivity
ThermalAnalyzer(STA)
or
Dilatometer
(DIL)
with
a
1
0.2
Specific Heat
Quadrupole
Mass Spectrometer (QMS), it is 0possible
to
0
0.0
0
100
200
300
detect and identify evolved
gases in exact time.
Temperature/°C• Kinetic studies

Measurement results by TGA• Mass changes• Temperature stability• Corrosion studies• Oxidation/reduction behavior• Decomposition• Compositional analysis• Kinetic studies• Rate-controlled mass lossDecomposition onset• Kinetic studies

Measurement results by hyphenation• Decomposition stability• Solid-Gas Reactions• Compositional AnalysisTG/%

Cp /(J/(g*K))

DSC/(mW/mg)↓ exo
1368.5 °C
2

108

1.4

Literature

106

Measured3.60 J/g

1.2

236.71 J/g
1061.1 °C
61.92 J/g

104

• Evaporation

1080.3 °C

587.4 °C
-323.66 J/g

388.2 °C

• Identification

0

-2

1.0

629.7 °C

102-4
595.1 °C

0.8
100

-6

0.6
98

200

400

600

800
1000
Temperature /°C

1200

1400

Highly accurate determination of the specific heat
capacity of a polycrystalline Al sample across a wide
temperature range.

200

1600

400

600
800
Temperature/°C

1000

1200

-8

STA measurement on amorphous Fe alloy; the DSC curve
Specific Heat Capacity/[J/(g∙K)]shows endo- and exothermal effects and the TGA
curve
1.40
0.40
Thermal Diffusivity (LFA)
exhibits the mass loss behavior.

Thermal Diffusivity α/(mm2/s)

Specific Heat Capacity (LFA)

1.35

0.35

1.30

0.30

Features (STA 449 F1/F3/F5 Jupiter®)

1.25

0.25

1.20

0.20

1.15

0.15

1.10
Variety of furnaces and sensors easily

0.10

1.05

0.05

Wide temperature range from -150 to 2400°C

interchangeable by the user

DSC F1/3 Pegasus®

Water-vapor furnace
1.00
0
50
100
150
Vacuum-tight design

FeaturesBenefits

Wide temperature range from -150 to 2000°C

DSC and DTA measurements on a broad range of metals and alloys

Variety of furnaces and sensors easilyinterchangeable by the user

For each application the right furnace and sensor
combination; future-proof for upcoming applications

Vacuum-tight design

Measurements under reduced pressures and pure atmospheres

Oxygen trap system (OTS®)

Avoiding oxidation of oxygen-sensitive materials

Determination of the specific heat capacity (cp)

Determination of a thermophysical property for developing
performance data and optimum material design

STA F1/3 Jupiter® coupled to QMS 403 Aeolos®

200
250
Temperature/°C

300

350

400

450

0.00

Benefits
Combined DSC/DTA-TG measurements, two analyticalmethods applied to one and the same sample
For each application the right furnace and sensor
combination; future-proof for upcoming applications
Tests in humid atmospheres up to 1250°C (e.g., corrosion studies)
Measurements under reduced pressures and pure atmospheres

Thermal Conductivity λ/[W/(m∙K)]
3.00

Oxygen trap system (OTS®)

Avoiding oxidation of oxygen-sensitive materials

2.50

Temperature-modulated DSC

Separation between reversible and non-reversible thermal
effects for an improved resolution and sensitivity

2.00

Determination of the specific heat capacity (cp)1.50

Determination of a thermophysical property for developing
performance data and optimum material design

1.00

Coupling to gas analyzer systems

Deep insight and better understanding of thermal reactions

0.50

Wide temperature range from -150 to 2400°C

0.00

0

50

100

150

200
250
Temperature/°C

Electrical Conductivity σ/(S/cm)
1800
1700
1600

Electrical Conductivity_Run 1
Electrical Conductivity_Run 2
Electrical Conductivity_Run 3
Seebeck Coefficient_Run 1
Seebeck Coefficient_Run 2

300

350

400

Combined DSC/DTA-TG measurements, two analyticalmethods applied to one and the same sample
450

Seebeck Coefficient S/(µV/K)
180
170
160

-5
40000

-10

1906.9 °C

104melting

TGA
102

20000

-15

DTA/(µV/mg)
↓ exo
1.0

TG/%

22

-20
0

100

200

300

400

500 600 700
Temperature/°C

0.5

800

0
1000 1100 1200

900

23

40.64 μVs/mg
100

Dilatometry

0.0

DTA

1886.6 °C

98

-0.5

-39.11 μVs/mg

Seebeck Coefficient/(µV/K)
20

Laser / light flash analysis-1.0

Dilatometry (DIL) is the method of choice to study lengthchange phenomena, thus revealing information regarding
their thermal behavior and about process parameters or
sintering (and curing) kinetics.
Due to the wide dynamic range of the measurement
system of the NETZSCH DIL 402 Expedis series, it
is possible to measure both soft and hard samples
without impairment of the properties in the temperature
range from -180°C to 2000°C (depending on furnace).
Additionally, it enables force modulation and builds a
bridge to thermo-mechanical analysis (TMA).
All NETZSCH dilatometers are based on, e.g., DIN EN 821,
DIN 51045, ASTM E831, ASTM E228.

92°C
Measurement
Results by1878.4
Dilatometery
90
1700
1750
1800
1850
1900
1950
• Linearthermalexpansionand coefficient
Temperature/°Cof thermal expansion (CTE)

-2.0
2000

Thermal Expansion/%•1.0Volumetric expansion and density change•0.9Shrinkage steps

Mo: Sample 1-1
Mo: Sample 1-2•0.8Phase transitions
Mo: Sample 2-1
Mo: Sample 2-2•0.7Sintering temperatures and steps•0.6Influence of additives and raw materials•0.5Debinding•0.3Rate-Controlled Sintering (RCS)•0.2Kinetic analysis (Kinetics Neo)
0.1
0

200

400

600
800
Temperature/°C

1x105

1000

1200

2

2,0x10-5
150

10Researchers and engineers are interested in the best
way to thermally characterize highly conductive materials
at cryogenic and elevated temperatures. Reduced
development times and costs, optimization of the
manufacturing processes and lower masses in spiteof increasingly higher demands on thermally stressedcomponents are important goals in industry. Many
challenges can only be met with precise knowledge of
two fundamental thermal properties: thermal diffusivity
and thermal conductivity.
Laser/Light Flash Analysis (LFA) allows for the meetingof challenges typically arising in heat transfer processes
such as, e.g., determining how quickly an aluminum ingot
solidifies, figuring the temperature gradient in a part
during use, determining the thermophysical properties ofparts, etc.

•0.4Anisotropic behavior

0.0(dL/Lo)/% DSC/mW
m.CTE / K
200

8x104

crystallization-1.5

Each time a material is exposed to temperature changes– it shows a variation in its dimension. Whether it is in
the course of its regular thermal expansion, by passing
a phase transition or while it undergoes sintering, thesubstance will either be shrunk or elongated.

S/cm

DIL (m. CTE)

96
94

Curie
α→γ
Point

0,0
6x104 1

Over the past two decades, NETZSCH has led the way
100-2,0x10in this technology, extending our application
4x10 range from
0-125°C to 2800°C.
0-5

4

DIL (dL/L0)-4,0x10-5 50

2x10
DSC
In carryingout a LFA measurement, the lower
surface ofa plane-parallel sample is first heated by a short energy0-1 -6,0x10-10pulse.
The
change0200 resulting
400
600 temperature
800
1000 1200
1400 on the upper
Temperature/°C
surface of the sample is then measured with an infrared
detector. The thermal diffusivity (a) and finally thethermal conductivity (λ) can be calculated by means of
the following formula:4-5

DSC/(mW/mg)
↓ exo

0.004

λ(T) = a(T) · cρ(T) · ρ(T)

0.002

2nd Heating (Annealed Material)

33.3°
0
λ=
thermal conductivity[W/(m·K)]-0.47
J/g-0.002a = thermal diffusivity [mm²/s]
400.7 °C

1st Heating (After Cold-Forging)cₚ = specific heat capacity [J/(g·K)]

1400-0.004

ρ = bulk density [g/cm3]
300.0

350.0

400.0
450.0
Temperature/°C

Density/(g/cm3)
10.3

Volumetric Expansion/%
3

500.0

550.0

Specific Heat/[J/(g∙K)]
Thermal Conductivity/[W/(m∙K)]
6300

Thermal Diffusivity/(mm2/s)
60
50Volumetric Expansion
Density Change

10.2

5

a(T)

40

2

200

30

4

20

10.1

Solid Phase
10

λ(T)

3

100

Liquid Phase

0

1

2

10.0
cp(T)

0

DIL 402 Expedis® Supreme

0

200

400

600
800
Temperature/°C

1000

1200

1400

0

1

9.9

Specific Heat/[J/(g∙K)]

Densitydetermination based on volumetric expansion
0.4

0

LFA 467 HyperFlash®

100

200

300

400

500 600 700
Temperature/°C

dV/Vo/%

800

0

900

Density/(g/cm3) c-DTA®/K↓ exo 2.70

Density:
Thermaldiffusivity by means of LFA (red), specific heat10
12
2.66 g/cm
capacity by means of DSC (corrected by subtracting
2.65 the8
621.8°C
10
latentheat of melting, black) and the calculated
thermal6
2.60
conductivity(blue)
8
3

0.35

Mo: Sample 1-1
Mo: Sample 1-2
Mo: Sample 2-1
Mo: Sample 2-2

4

2.55

0.30
6
559.0°C

2.50

4

0.25

2.45
2

FeaturesFeaturesBenefits 0.20

Benefits0

Friction-free construction

Small contact forces for green bodies and soft samples

Temperature range RT … 2800°C

High measuring range

0.15
Measurementof large length changes (expansion, shrinkage)-200 -100 0 100 200 300 400 500 600 700 800 900 1000 1100 1200 1300

Adjustable flash pulse andmaximum measurement time

Measurements on high-conducting and/or thin specimens
up to thicker specimens becomes possible

Specimen holders

100.10 and large specimens up to 25,4 mm
Measurements on small
possible, different shapes and geometries are allowed

Variety of software models for theevaluation of the signals

Each model can be 100.06
combined with different baseline corrections and withor without pulse correction,
radial and facial heat loss, model wizard
100.04Highest temperature range from -180°C to 2800°C

Measurements on high-melting materials

Controlled contact force

Constant sample
80 load during the entire measurement

Measurements in different atmospheres

Oxidizing reducing and inert atmospheres and under vacuum

Thermal Diffusivity/(mm2/s)

70

60

50

100

200

300

600

2.40

-6

700

TG/%

100.08

Mo: Sample 1-1
Mo: Sample 1-2
Mo: Sample 1-3
Mo: Sample 2-1
Mo: Sample 2-2
Mo: Sample 2-3

100.02Mass Change: 0.150 %Mass Change: 0.082 %100.00
1st heating

Mass Change: 0.066 %99.98
3rd heating
99.96

40

0
-2
-4

2.40 g/cm3

400
500
Temperature/°C
Various instruments for a broad application range

Temperature/°C2

5th heating
200

400

600
Temperature/°C

800

1000

1200

NETZSCH Analyzing
and Testing

We draw on the power of our analytical instruments
and services to make the invisible visible and theimpossible possible.

The NETZSCH Group is an owner-managed,
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Through the chemical, physical and structural analysis
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With over 2300 employees, we serve the world, andwe are part of Spectris plc, the world-leading precision
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Our performance standards are high. We
promise our customers Proven Excellence –exceptional performance in everything wedo, proven time and again since 1873.
When it comes to Thermal Analysis, Accelerating
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Thermophysical Properties, Rheology andFire Testing, NETZSCH has it covered.
Our 50 years of applications experience, broadstate-of-the-art product line and comprehensive
service offerings ensure that our solutions
will not only meet your every requirement
but also exceed your every expectation.

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