Institute of Mineral Engineering

Department of Ceramics and Refractory Materials

Univ.-Prof. Dr. rer. nat. R. Telle

Testing of Refractories and Refractoring

Testing of Refractories
For more than 45 years the Aachen Institute of Mineral Engineering has been successful in
testing and developing refractory materials. During that time requirements for these materials
increased due to both higher processing temperatures and tightening up production efficiency
demands. This guided into optimized conventional refractory products which can only be
achieved by applying high grade, oxide as well as non-oxide, synthetic raw materials and
innovating production technologies. Major impulses in developing high performance materials
have been initiated by process innovations out of steel industries, waste incinerators dispose
and coal gasification.
In order to meet with this specific requirements new test methods have been developed to
assess the suitability and reliability of these materials under extreme operating conditions.
The Aachen Institute of Mineral Engineering intensively participated in development and
approvement of new testing procedures being involved in various expert organisations
and boards. So, tests after DIN, EN-DIN, ASTM, AFNOR and BS -standards, as well as
non-standard tests which simulate special operating conditions are available.

Range of application of refractory materials

Iron making industry Coke ovens Cement and alkaline earths industry
• blast furnaces • rotary kilns for cement, dolomite and magnesite
• hot blast stoves Metallurgical treatment and casting •shaft kilns
• blast tyeres of nonferrous metals
• hot blast main systems • anode-baking furnaces
• melting-holding furnaces for Al
Glass industry
• blast furnace runners • glass melting tanks
• refractory parts in continuous casting systems
• regenerators for glass melting tanks
Steel making industry for Al
• electric furnaces
• pig iron transport vessels • reverberatory furnaces for Cu
• pig iron collector vessels • Pierce-Smith-converters
• anode-drum furnaces for Cu Refractory heat-insulation materials
• oxygen steel converter
• electric arc furnaces • slag-cleaning furnaces for Cu
• Cu-melting furnaces Chemical industry
• steel casting laddles
• combustion chambers
• treatment laddle for secondary metallurgical
Boilers and power plants, fireboxes • hot gas generators
processes
• municipal incinerators • rotary kilns
• steel degassing vessels
• special refuse incinerators • liquid waste incinerators
• refractory parts in continuous casting systems
• melting chamber boilers • sulfur incinerators
• refractories for heating and heat treatment
furnaces: soaking pits, pusher type furnaces, • combustion chambers, burner rigs • crackers
rotary hearth furnaces, walking beam furnaces, • reformers
walking hearth furnaces, roller-hearth furnaces Coal gasification plants • carbon black generators
• petrol chemistry plants
• refractories for hot gas purifyers
Iron- and steel-casting foundry
• cold and hot blast cupolas Ceramic and enamelling industry
• crucible and channel induction furnaces • tunnel kilns
• transport and casting laddles • bugie hearth furnaces
• nozzles • enamelling kilns
• roller furnaces

Refractory and heat resistant materials

SiO2-rich products --------------------
fireclay products ----------------------
high alumina products ---------------
products on base of sesquioxides --
- graphite containing bricks
products on base of zirconium -----
- silicate and zirconia
forsterite bricks -----------------------
-
basic bricks -----------------------------
Shaped refractory products
silica bricks, fused silica products spinel refractories ----------------------- MgAl2O4-, picrochromite-refractories
commercial (groups A 25 - A 40); chromium oxide based refractor ----- Cr2O3
silica-rich, acid-resistant, graphite-containing, SiC-
pitch-/tar-impregnated products ----- based on periclase, dolomite corundum
and cordierite-containing, kaoline-products;
resin- and pitch-bonded products ---- with and without the addition of
groups I and II
graphite resp. antioxidants; magnesia-
alumina-rich fireclay, sillimanite, andalusite, cyanite,
graphite and dolomite-graphite bricks
mullite (sintered and fused), corundum (calcined
alumina, sintered and fused alumina), bauxite fusion cast products based on mullite, corundum, periclase,
products spinel, baddeleyite/corundum, sesqui-
oxides (Al2O3, Cr2O3, Fe2O3)
alumina, chromium oxide
ZrO2, ZrSiO4
nonoxide refractory products --------- based on SiC: silicate, oxidic, Si3N4- or
forsterite, olivine BN-bonded. Si3N4-products
magnesia, magnesia-chrome-, chrome-magnesia,
magnesia-spinel, chromite, dolomite-magnesia
products

Unshaped refractory materials Refractory insulating materials

For monolithic linings, repairs, prefabricated refractory parts, as laying and jointing • insulating materials up to 1100°C ----- based on perlite, vermiculite, expanded
materials, plastic mixes, ramming, gunning, slinging and fritting mixes; refractory castables. clay, calcium silicate
Unshaped refractory and semi-refractory materials for laying, jointing and sealing shaped and
• refractory lightweight bricks up to ---- based on silica, fireclay, sillimanite,
unshaped products: mortars, mastics, adhesives
1900°C bubble alumina
bonding: hydraulic, ceramic, chemical, organic
• ceramic fibre products up to 1800°C -- alumosilicate fibres, Al2O3 and ZrO2-
grogs: oxidic: SiO2, Al2O3, Cr2O3, MgO, CaO; non-oxidic: SiC, Si3N4;C based fibres, with or without organic
refractory castables : regular castables (RC), liquefied (DCC), medium cement (MCC), low and inorganic additives
cement (LCC), ultra low cement (ULCC), no-cement (NCC)
Microstructural Characterisation of Mechanical and Thermo- Corrosion Behaviour
Raw Materials and Refractory Products mechanical Properties (Reaction with gases, volatile dusts, ashes, slag, metallic
melts, vapor and acids)

Chemical analysis Strength at ambient temperatures Carbon desintegration

• x-ray fluorescent analysis • crushing strength (reaction in CO-atmosphere at 500°C / 200 h)
• atomic absorption spectrometry (AAS) • MOR: transverse strength (3- and 4-point bending)
• ion chromatography • Weibull statistics Carbon desintegration
• infrared spectrometry • tensile cleavage strength (reaction in CH4-atmosphere at 900°C / 200 h)
• wet chemistry • static E-modulus
SiC-materials
• coulometry • Young´s modulus
(reaction in steam-saturated atmosphere, up to 1250°C /
- Grindo Sonic number
500 h)
X-ray diffraction analysis - determination of first grade longitudinal resonance
(qualitative and quantitative) frequency (according to Kottas) SiC-materials
• powder diffraction • mechanical fracture behaviour (reaction in CO- and CO / hydrogenous atmosphere, up
• low-angle diffraction - KIC-factor (fracture toughness) to 1500°C)
• high-temperature diffractometry up to 2000°C - determination of work of fracture
• determination of hardness of surfaces
Reaction of alkalies in vapor with
Light microscopy • abrasion resistance
• polarization microscopy in reflected light - Böhme grinding machine refractories up to 1100°C
• fluorescence microscopy in reflected light - sand blasting method (by impact of quartz-, corundum-
• polarization microscopy in transmitted light or SiC- grains) Corrosion by melt or slag
• wetting microscopy up to 1700°C • cup test • modified cup test
High Temperature Strength • stirring method ("tumbling method")
Scanning electron microscopy • hot crushing strength • rod test • rotary kiln test
• including x-ray microanalysis: • hot transverse strength HMOR (3- and 4-point bending) • induction furnace test
- energy-dispersive (EDX, semi quantitative) • tensile cleavage strength
- wavelength-dispersive (WDX) • hot abrasion resistance Resistance to acids
- by grinding
- by sand blasting impact Wetting behaviour
Transmission electron microscopy (TEM, 300 kV)
• high resolution, EDX, STEM Stress/deformation behaviour at high temperatures refractory and ceramic materials:
• sample heater up to 1200°C metallic melts and oxide slags:
sessile drop method
• thermal expansion (dilatometry)
Analysis of macrostructure constant heating rate, without stress, dilatation as a function Thermal shock resistance
of mono- and polyphase polycrystalline structures of temperature
• - air quenching method
• refractoriness under load
Determination of density and porosity - water quenching method
constant heating rate, constant stress, dilatation as a
• true density (pycnometer) • thermal shock between two high temperatures
function of temperature
(array of practical conditions):
• bulk density, shaped or granular materials (fluid displacement and
measure method) • creep in compression at constant temperature maximum quenching temperature: 1550°C
heated at a constant rate and given stress up to required minimum quenching temperature: 450°C
• open porosity (permeable and impermeable)
test temperature, dilatation as a function of both • Peeling test
• true porosity (calculated from density and bulk density)
temperature and time • determination of crack formation depending on
• closed pores (difference between true and open porosity)
heating rate by measuring thermal expansion
• permeability to gases (open permeable pores), gas diffusion • creep under transverse/flexural stress
• pore size distribution constant temperature and stress, compliance as a function of
- mercury displacement method temperature and time Thermal Analysis
- water-air displacement method
• permanent change in dimensions (shrinkage and expansion) for
- systems for the analysis of microstructures
after thermal impact, with and without load • thermal decomposion reactions, vapourisation
• solid reactions
Specific surface Refractoriness • sintering
• single point of adsorption processing (areameter) - determination of thermal softening behaviour by • melting and softening behaviour
• gas adsorption, BET-method pyrometric cone equivalent
• forming of new phases and alternating modifications
• air penetration - melting behaviour determined by hot stage microscope up to
• thermal effects
(1700°C)
- differential thermo-analysis (DTA)
Grain size analysis - differential calorimetry (DSC)
• laser granulometry Thermal properties
thermal conductivity: hot wire method up to 1300°C - thermo gravimetry (TG, DTG)
• sedimentation analysis
• air separator - parallel- and cross-wire method
• screen analysis, particle size analysis - 2 devices

Tests on Specific Refractory Product Types and Raw Materials

Unshaped Products Chemical Bonded Basic Bricks Ceramic Fibre Materials
chemical analysis density, bulk density, permeability to gases diameter of ceramic fibres
- light microscopic methods
distribution of grain size cold crushing strength after preliminary firing - SEM
workability, consistency determination of interzonar strength shot content
sample preparation bulk density, thickness
determination of volatile contents and residual carbon
- refractory castables vibrating, tamping, casting with and contents permanent change in dimensions on heating
without vibration
- light refractory castables vibrating, poking Raw Materials classification temperature
- ramming mixes ramming, pneumatic tamping
- plastic mixes ramming, pneumatic tamping determination of suitability of quartz sands and resilience and compressibility
- gunning mixes pneumatic or mechanical gunning gravels for refractory production according to §3, 4 tensile strength
Tests on prefabricated refractory parts "Bundesberggesetz" (Bberg G, "german federal
mining law") Emission measurements of natural and
Properties at ambient temperature • pyrometric cone equivalent man made fibres
• bulk density Measurements of synthetic fibre dusts
• transverse strength • determination of quartz and quartzite contents by x-ray
• crushing strength diffraction and picking methods emission in production plants
Properties during or after firing determination of suitability of clay and feldspar for • Measurements of inorganic fibrous
• bulk density, porosity proceramic production, not to be considered as tile particles in ambient and industrial air
• permanent linear change products according to §3, 4 of Bberg G according to VDI 3492, 1 guideline by
• cold transverse strength scanning electron microscopy
• pyrometric cone equivalent
• hot transverse strength
• resistance to acids • Investigations characterizing respireable
• softening under load
• creep in compression fibre dusts - application of light microscopy
• sticking ability (refractory mortars) in accordance to ZH1/120.31

Institute of Mineral Engineering

Department of Ceramics and Refractory Materials Please contact:
Mauerstrasse 5, D-52064 Aachen Dr.-Ing. Th. Tonnesen
phone: +49-(0)241-8094968 phone: +49-(0)241-8094988
fax: +49-(0)241-8092226 fax: +49-(0)241-8092226
www.ghi.rwth-aachen.de e-mail: tonnesen@ghi.rwth-aachen.de