refractory manufcturing,properties
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Refractory manufacturing Refractory testing
andRefractory properties
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What is refractory ?
Is it a material which should withstand high temperature only ?
The right definition is that it should withstand high temperature,resistance to thermal and thermo chemical load, posses high volume stability, resistant to erosion and abrasion, be tough , and resistant to chemical corrosionetc. Or otherwise it should have high RUL, high PCE, low conductivity , high hot MOR, high creep resistance and optimum CCS etc
Overall it is a compromise with all the above properties.Choice of refractories depend on the operating and mechanicalconditions of the kiln.
There is no refractory material which posses all the above properties 100 %
In general any material which in service > 600 deg C is called refractory
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Refractories
Shaped refractories Unshaped refractories ormonolithics
Acid refractories Basic refractories Neutral refractories
Silica basedrefractories, fire clay
bricks
Magnesia, MagnesiaChromium , Magnesia
Alumina , Dolomite
Alumino silicatesAlumina bricks,Zirconia
based refractories, like zirconal, zircon, etc
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Fire Clay bricks
refractory clays Kaolins extended with chamotte or non plastic argillacious matter unwetted by water Al2O3 content = 30 to 45 %
High alumina bricks
1)Cyanite,andalusite,and siliminite 2) natural hydrated alumina(hydrargillite,bohemite,and disapore contained in bauxite) 3)Artificial calcined hydrated alumina, and natural and electro fused alumina ( Alpha -alumina or
Class A =45 - 60 % Al2O3 Class B = 60 - 70 % Al2O3
Class C = > 75 % Al2O3Silica bricks Dinas
Magnesia bricks
Magnesit ( MgCO3), Dolomite ( MgCO3.CaCO3), Mg(OH)2,Mgo Obtained from
dolomite,saline water and sea water
Spinel bricks
MgO and Al2O3 together sintered or fused MgO from sea water and alumina from alumina industries ,alpha alumina etc)
Raw materials used for manufacturing of bricks
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Acidic Basic
neutral
Raw material user
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ZrO2 Cr2O3
CaOSiO2
ZrSZircon silicate
1775 O C
A3S2mullite 1840 O C
Important mineral phases in refractories
M2SForstrite1890 O C
MCrPicro chromite
C2SBredigit 2130 O C
CA6Hibonite
1850 O CMA-spinel
2135 O C
MgOAl2O3
2180 O C
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Melting point of pure refractory oxide
1200
1400
1600
2000
2200
2400
3000
2800
2600
SiO2 Al2O3 Cr2O3 CaO ZrO2 MgO
1702
2050
2275
26002700 2800
Deg c
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Classification of refractories regarding melting point and alkalinity
1234567891011121314
3000
2750
2500
2250
2000
1750
1500
melting point Deg c
pH value
Cao
MgO
Al2O3
ZrO2
Cr2O3
SiO2
basic neutral acidic
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Process flow chart for manufacturing
Comminution
preparation
classification
mixing
shaping
drying
firing
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SIC crystals ( Silicon carbide)
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ZrSiO4
Zircon crystals ,ZrSiO4
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Refractory manufacturing process
Tunnel kiln Tunnel dryer
Tunnel carsFinished product storage
Brick press machines
Coarsecrusher
Fines crusher
Ball mill
storage
elevatorVibrating screen
Storage silosclassifier
Clay crusher
Clay mill
Drying tower / classifier Binder & liquids
Liquid dosage
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Refractory manufacturing processSchematic diagram of refractory manufacturing
Roughcrushing
Rawmaterial
middlecrushing distribution
finecrushing
Storage byGrain size
Measuringquantity
mixing mouldingdrying
firing
inspection packing shipping
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Refractory clay mine
Opencast mining
Under ground mining
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Cone crusher
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Hydraulic press
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Iso static press machine
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Tunnel dryer
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Tunnel kiln
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Important refractories used in cement industry
Magnesia containing bricks _ mag chrome, mag spinel,dolomite,hercynite, galaxite based, zirconia based
High alumina bricks - 60 - 70 % Al2O3
Fire clay bricks - 30 % Al2O3
Light weight insulating bricks
Unshaped refractories or castables - conventional,low cement castable, ultra low cement castables,insulation castables
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Raw materials for Magnesia bricks are
• Natural magnesite , MgCO3 , Coarse crystalline ,fine crystalline
• Synthetic magnesia,sea water magnesia , salt brine • The principal constituent determining the characteristic
properties of magnesia refractories is periclase
Properties of periclase
0 Melting point = 2800 deg . C0 Thermal conductivity = 3 - 4 w / mk0 Thermal expansion = 1.4 %
Refractory products for the cement kiln
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• Magnesia bricks, MgO, > 80 %
• Magnesia spinel bricks, MgO , 80 - 90 %
• Magnesia hercynite bricks, MgO, 80 - 96 %
• Magnesia Zirconia bricks MgO, 85 - 96 %
• Magnesia chromite MgO, 55 - 80 %
• Chromite bricks Cr2 O3=25%MgO = 25 %
• Forsterite MgO and SiO2
• Dolomite MgO = 60 % and CaO=40 %• Magnesia, galaxite bricks Mgo=91% ,and MnO=2.6%
Basic bricks used in the cement industry
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Mineral Formula Abbreviation Fusiontemp ,Deg CPericlase MgO M 2800 deg CForsterite 2 MgO.SiO2 M2S 1890
Monticellite CaO.MgO.SiO2 CMS 1495Merwinite 3 CaO.MgO.2SiO2 C3MS2 1575
Dicalcium silicate 2CaO.SiO2 C2S 2130Magnesium ferrite MgO.Fe2O3 MF 1750Dicalcium ferrite 2 CaO.Fe2O3 C2F 1435
Tri calcium silicate 3CaO.SiO2 C3S 1900Brown mellarite 4CaO.Al2O3.Fe2O3 C4AF 1395
Dolomite CaO.MgO CM 2450Andalusite Al2O3.SiO2 AS
Mullite 3Al2O3.2SiO2 1840Siliminite Al2O3.SiO2 AS 1545
Important refractory minerals used in refractories
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Andalusite Al2O3.SiO2 ASMullite 3Al2O3.2SiO2 1840
Siliminite Al2O3.SiO2 AS 1545Corundum 2050Hercynite FeO.Al2O3 FA 1760Galaxite Mno.Al2O3 mA
Magnesia aluminaSpinel MgO.Al2O3 MA 2135Gehelinite 2CaO.Al2O3.SiO2 C2AS 1590
Calcium aluminate CaO,Al2O3 CA 1600Anorthite CaO.Al2O3.2SiO2 CAS2 1550
Dicalcium ferrite 2CaO.Fe2O3 C2F 1450Myenite 12CaO.7Al2O3 C12A7 1455
Gehelinite 2CaO.Al2O3.SiO2 C2AS 1590Calcium aluminate CaO,Al2O3 CA 1600
Anorthite CaO.Al2O3.2SiO2 CAS2 1550Dicalcium ferrite 2CaO.Fe2O3 C2F 1450
Myenite 12CaO.7Al2O3 C12A7 1455
Important refractory materials used in refractories
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Major refractory bricks used in cement industries
70 % Alumina bricks Cooling zone ,burning zone,transition zone
60 % Alumina bricks transition zone,calcining zone, t.a.duct,calciner, cooler area
40-50 %Alumina bricks calcining zone, t.a.duct,calciner, cooler area
30 % Alumina bricks t.a.duct, ,calciner, cooler area,pre-heater cyclones
Magnesia chrome bricksDolomite bricks Burning zone
Magesia spinel bricks cooling zone,burning zone ,transition zone
Hercynite ,nochromeGalaxite no chrome transition zone
Location where it is usedType of brick
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Refractory propertiesPhysical properties
1)Bulk density g / cm3
2)Apparent porosity %3)Cold crushing strength N/ mm2
Thermal properties1)Refractoriness under load (RUL)
OCtate
2) PCE ( pyrometric cone equivalent)SK (Arton cone in ASTM standard)
3)Thermal expansion ,lin % (PLC) at 4000c
8000c12000c
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4)Thermal shock resistance (TSR)at 9500 c in airor
Water quenching cycles
5) Thermal conductivity at3000c7000c
10000c Chemical analysisMgOAl2O3Cr2O3Fe2O3CaOSiO2ZrO2 MnO2 etc
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1. Bulk density
Density of all refractories is an indirect measure of their capacity to store heat .2. Apparent porosity
The porosity of a refractory is a measure of % pores to the( summation of open and closed pores)total weight of a brick. This property is significant to decideupon its resistance to penetration by slags and fluxes ,itspermeability to gases and its thermal conductivity
Porosity is controlled by the following1) by controlling the texture of the bricks2) by controlling the size of the particles3) by method of making4) by controlling the firing temperature
Physical properties
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Porosity affects
• the strength of thebrick
• porous bricks are mechanically weak
• lower porosity givesbetter resistance to slag attack
• thermal conductivitypc
po
po
po
po
po
Po –open poresPc –closed pores
po
pc
Pc
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3. Cold crushing strength ( CCS )
Cold crushing strength of a refractory material represents itsstrength .In other words it tells us how much load it can bearin cold condition
The mechanical strength (CCS) of refractory brick is governed largely by the amount and the character of the matrix material between the larger grains. Good tool to provide for evaluatingthe degree of bond formation during production. It indicates theability of the brick to withstand abrasion and impact in lowtemperature application.
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CCS testing machine
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Cold crushing equipment and CCS valuesBrick grade CCS ( N / mm2)Silica 15 -20Fire clay 12 - 70Corundum 35 - 80Magnesia 50 - 110Magnesia chromite 30 - 70Magnesia spinel > 40 Insulating Brick 3 - 20
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Density Coefficient of thermalconductivity
Thermal shock
resistance
Cold crushingstrength
Porosity
Correlation between the physical properties
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Thermal properties1.Refractoriness( fusion temperature or softening temp)
Transition of a solid material into the liquid form underthe influence of heat. A true melting point is temperatureat which the solid and liquid phase of the compositionco-exist in equilibrium.
It is the ability of a refractory to remain rigid at a giventemperature. It is an indirect indication of the amountand the viscosity of any liquid which it may contain.
The reference samples are called seger cones in DIN standards and Norton cones in ASTM standards.
Or PCE (pyrometric cone equivalent)
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Test sampleStandard samples
12 3
45
PCE test(pyro-metric cone equivalent)
Plaque25 mm82 O
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Seger cones before and after firing
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Seger cone and reference temperature
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Determination of the softening behaviour under temperature and load
The three methods evolved are
• Determination of the refractoriness under load
• Determination of the refractoriness load ( diifferential)
• Determination of the thermal expansion under load ( creep)
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Determination of refractoriness under load (RUL)
Characteristic temperatures are Brick grade t a / O c
t a : 0.3 mm compression from the Fire clay 1300 -1550temperature the temperature of Corundum 1600 - 1750highest expansion Silica > 1660( 0.6 % compression of test sample) Magnesia chromite > 1550
t e : 10 mm compression from the Magnesia-hercynite 1600temperature of highest expansion Dolomite 1700(20 % compression of test sample) Magnesia spinel > 1700
t b : temperature of breaking sample: Carbon brick non-softening
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Curve example of refractoriness under load
Determination of the refractoriness under load (differential)
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Determination of the thermal expansion underload ( creep)
Curve example of Creep under load
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Creep test equipments
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Refractoriness under loadThis is a measure of the resistance of a refractory bodyto the combined effects of heats of load.This test helpsto study the behavior of a refractory product when
subjected to a constant load under conditions of progressively rising temperature.The ground mass / matrix helps to bond the entire mass of a refractory brick strongly together. The amount and the strength of the glass is fixed by the alumina - silica ratio, fluxing oxide content and the temperature of firing.
It is an important parameter to decide upon the safer limit of service temperature in a given situation.Contributing factors to the increased resistance to the pressure are
a) More thorough distribution of liquid throughout the brickb) The growth of crystals through the influence of heatc) Crystallization of a portion of the liquid during cooling.
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High temperature creepIn a brick held at constant temperature and pressure,
gradual solution of solid material up to the limits of itssolubility in the liquid may cause some increase in theviscosity of the liquid. This increase is dependent onthe nature of ground mass, glass content. Higher glass content will result higher deformation in thissituation. This property of refractoriness is called hightemperature creep. Lower deformation will ensurerigidity under the service condition.
The creep is the measurement of deformation of arefractory product as a function of time when it issubjected to a constant load and heated at a specifiedtemperature.
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RUL measuring equipment
Carbon or mullite rod
insulating brick lining
Corundum, magnesiteor mullite tube
Steel casing
Metal electrode
Coarse amorphouscarbon
Test specimen
View point
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RUL testing machine and creep test machine
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Creep curves
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Softening under load
0 200 400 600 800 1000 1200 1400 1600 1800
P res
sur e
/ e x
ten s
ion
(%)
- 2
- 1
0
1
2
3
Temperature o C
magnesia zirconia
magnesia spinel
Magnesia chromate
dolomite
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Creep measurement of various high alumina refractories under 25 psi load at 2600 O F for 0 - 100 hours
L in e
a r s
u bs i
d en c
e-p e
rce n
t
54
32
1
0-1
-2-3-4
-5-6
-7
-8-9
-100 10 20 30 40 50 60 70 80 90 100
Time(hrs)
60 % alumina - low alkali
70 % alumina
50 % alumina
85 % alumina
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Linear expansion (Permanent linear change)High temperature reheat test maybe used to reveal
1) if a brick has been fired long enoughor at a high temperature
2) whether a brick has adequaterefractoriness and volume stabilityIt is expressed as a percentage , preferably by the ratio of the length of the test piece after heating andthe original value of the length
Equipments used to determine
Thermal expansion
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20 deg c
1000 deg c
2000 deg c
L= 1000 mm
L= 1013 mm
L = 1026 mm
Magnesia : Thermal expansion = + 1.3 % at 1000 degc
Alumina oxide : Thermal expansion = + 0.8 % at 1000 degc
Fire clay Thermal expansion = + 0.5 % at 1000 degc
Thermal expansion or refractory materials
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Thermal expansion curves
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Thermal expansion is important in service , as the effect of expansion hasto be taken into account during refractory installation and construction oflarge installations ( expansion joints). The expansion curves of most of refractories is more or less linear with increasing temperature or reversible.
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Thermal shock resistance( spalling resistance)
Thermal spalling results from stresses caused byunequal rates of expansion and contraction in different parts of brick and usually associated with rapid changes of temperature.
In cement rotary kiln the brick lining needs to bespalling resistant as the lining is subjected tocontinuation variation of temperature because of rotary motion of kiln.
TSR ( thermal shock resistance ) is given in cycles.Quenching is done by air or water
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Equipments for thermalshock resistance test
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Thermal conductivityThe coefficient of thermal conductivity is defined as the quantity ofheat that flows across unit area in unit time if the temperature gradient across this area is unity.
Thermal conductivity K is given ask ( T1 - T2 ) At Kcal / hr - m - O C or BTU / hr -sq.ft - O F
Q = d Q = amount of heat
T1 = hot face temperatureT2 = cold face temperatureA = area cross sectiont = timed = thickness
Thermal conductivity of a refractory decreases with increase in porosity.Increase and decrease of thermal conductivity at elevated temperature also depends on amount of glass, liquid and crystallinity of the material.
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12
346
578
9 10
11
12
13 14
200 400 600 800 1000 1200 deg c
2
4
6
8
10(w
/ k
m)
Thermal conductivity offired refractory bricks
1. Insulating refractory bricks2. Zirconia3. Dry- pressed fire clay4. Fused silica5. Forsterite6. Chromite7.Corundum 90 %8. Magnesia- chrome9.Zircon silicate.10. Corundum 99 %11. Carbon12.Silicon carbide 40%13. Magnesia14. Silicon carbide
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Thermal conductivity depends on temperature , chemical and mineralogical, composition of the brick , porosity, pore size and brick firing temperatureMaterial Thermal conductivity
at 1000 O C (W/(m.K)
Magnesia 4.4Magnesia chromite 2.5Magnesia –spinel 2.8Magnesia hercynite 2.6Alumina 3.0Insulating brick 0.6Iron 28.0
Thermal conductivity
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The bending strength can be calculated by means of the equationσ bending = 3.F.l / (2.b.h2)l = distance between bladesb = width of sampleh= height of sample
In order to determine the magnitude of the rupture stress ofrefractoies , the resistance to deformation under bending load is measured.
F Pressure load
Tensile load
Determination of modulus of rupture
sample
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Determination of hot modulus of rupture (HMOR)
Structural configuration of the refractory material as well as the amount and properties of occurring melts characterize the HMOR
HMOR (N /mm2)
Testing temperature (deg C) 1200 1400 1500
Magnesia , low iron content > 14 11 8
Magnesia , high iron content > 12 5 1
Magnesia – Chromite > 10 5 3
High alumina > 25 18 7
Zirconia > 25 > 25 > 18
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Modulus of rupture
MOR test
The resistance to bending stress of refractory products provideinformation on their deformation behavior at high temperature.
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Hot MOR Test
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Principle of wedge splitting test
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Wedge splittingmachine
Groovedsplit
The specific feature ofthis method of testing is thedetermination of fracture mechanical parameters athigher temperatures , up to
1200 deg C
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Influence of of the aggregates on the secondaryload bearing capacity of the softening behavior
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Chemical composition
By quantifying all the constituents present in refractory, it ispossible to assess the chemical properties and melting behaviorof a given refractory.As it is important to know the % Al2O3 inhigh alumina brick, % MgO in magnesite brick , and % SiO2 in silica brick etc.,the determination of minor constituents hasalso been recognized as controlling factors in the performanceof many refractories. The chemical composition is of greatimportance with respect to attack by slag , glass melts , flue dusts and vapors. In general the principle applies that a brick ismore resistant the lower the rate of chemical reaction gradientbetween the slag and brick is. Therefore, where the acid slagis expected , acid bricks are preferably used , and basic brickswhere basic slag is expected.
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According to the behavior during contact reaction ,the following groups of bricks can be differentiated.
Acid group - fused (99% SiO2), Silicon carbide bricks,Zircon crystobalite . Zircon silicate
Basic group - dolomite, magnesia, magnesia chrome, chrome magnesia ,forsterite
Inert or neutral - carbon , high alumina chromite group
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Cup corrosion test
Alkali test of a high alumina brickwith K2CO3
Alkali test of a sic containing high alumina brick with K2CO3
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Mineralogical investigations by X-ray diffractionDetermination of the mineral phases composition of material
X-ray diffraction diagram of a used magnesia –spinel brick grade ,salt infiltrated
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Microscopically techniques ( micrologies)
• Light micoscopy ( transmitted light and reflected light microscopy
• Microprobe analysis ( WDS, EDS)
• Scanning electron microscopy
Advantages of these micrlogies opposite other investigationmethods
• Diagnosis of mineral phases composition in raw materials , refractory products etc and their configuration
( textural/ structural criterions, pore shape and size etc
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Mineralogical investigationsReflected light microscopy
Pictures of magnesia - spinel brick grades with different raw material composition
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Microprobe Analysis
Chemical – mineralogical composition in m mBoundary between slag and corundum brick
Polished section image (reflected light microscope)
Back scattered electron image(microprobe)
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Mineralogical investigationsScanning electron microscopy (SEM)
Hydration of Magnesia .crack formation ,caused byformation of brucite(Mg(OH)2
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Minerological investigations
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Cont...
Refractory Bricks PropertiesChem. Comp. Bulk
DensityApp.
porosity CCS PCE Therm exp.
Therm. Condct. TSR (air)
(%) (gm/cm3) (%) (N/mm2)ta
(°C) tb
(°C) s.cat 1200
OC %
(W/mK)at 1000
OC
(cycles at 950
OC)
Ankral S 65-(Mg
chrome)
M = 77- 80Cr = 7 - 9 Al = 2 - 4 F= 7 - 10C= 1 - 2 S= 0.4 - 1
3.00 < 21 35 >1650 >1700 > 42 1.04 2.1 > 150
Perilex - 83 (Mg chrome)
M=80 - 85Cr = 3 - 5 A= 1 - 3F= 7 - 9C =2.5S = 1.5
2.9 - 3.05 17 - 19 55 1600 >1700 42 1.7 2.8 80
Bazal Z extra (Mg
chrome)
M = 77 Cr = 8A= 3 F= 9.5 C =1.6 S = 0.6
3 19 55 1720 1.6 2.4 100
Rexal S extra
(Spinel bricks)
M = 87 Cr = 0 A= 11 F < 0.5C < 1 S < 0.3
2.93 17 50 >1740 1.7 2.9 >120
RUL
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Cont...
Chem. Comp.Bulk
Density
App. porosity CCS PCE T herm
exp.Therm. Condct. TSR (air)
(%) (gm/cm3) (%) (N/mm2)ta
(°C)ta
(°C) s.cat
1200 OC %
(W/mK)at 1000
OC
(cycles at 950
OC)
Al mag - 85
(Spinel bricks)
M = 85 - 89Cr = 0A= 9 - 12F < 0.5C < 1S < 0.5
2.85 - 3 16 - 18 50 >1700 >1700 > 42 1.4 2.8 >100
Al mag - 85 SLC
(magnesia fused spinel bricks)
M = 85 - 90 C r = 0 A= 9 - 12 F < 0.5 C < 1.4 S < 0.9
0.9 17 55 >1700 >1700 42 1.4 2.7 100
Ankral R - 19
(Spinel bricks)
M = 94Cr = 0A= 5 F = 0.2C = 0.9 S = 0.2
3 16 40 >1700 >1750 42 1.5 3 >101
Ankral R - 17
(Spinel bricks)
M = 86 Cr = 0A= 12F = 0.5C = 0.7S = 0.2
2.95 16 >40 >1700 >1750 >42 1.49 2.6 >100
RUL
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Cont...
Chem. Comp. Bulk Density
App. porosity CCS PCE Therm
exp.Therm. Condct. TSR (air)
(%) (gm/cm3) (%) (N/mm2)ta
(° C ) tb (° C ) s.cat
1200 OC %
(W/mK)at 1000
OC
(cycles at 950
OC)
AS - 90 (Spinel bricks)
M = 91- 94Cr = 0 A= 5 - 7F = 0.5 C = 0.8S = 0.2
2.9 17 >40 1700 2.9 >100
Mag Pure - 93
(Spinel bricks)
M = 89-93A= 5 - 8 Cr= 0F = 0.5C = 2S = 1
2.9 16 - 18 50 >1700 >1700 >42 1.5 2.9 100
Mag Pure - 95
(Spinel bricks)
M = 93-96A= 3 - 5Cr= 0F =0.5C = 1S < 0.7
2.9 17 - 18 50 >1700 >1700 >42 1.6 3 100
Refra Mag -85 (Spinel bricks)
M =84-89A= 9 -12 Cr= 0F =0.8C = 1.4S =0.9
2.9 17 -19 45 >1700 >1700 >42 1.4 2.7 100
RUL
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Chem. Comp.
Bulk Density
App. porosity CCS PCE Therm
exp.Therm. Condct. TSR (air)
(%) (gm/cm3) (%) (N/mm2)ta
(° C)tb
(° C) s.c at 1200 OC %
(W/mK)at 1000
OC
(cycles at 950
OC) Ferro Mag
-90 (Magnesia- hercynite)
(Spinel bricks)
M =87 - 92A= 4- 6Cr= 0F =3-5C = 1.5S =0.5
2.9 18 - 20 50 1600 >1600 42 1.5 2.6 100
R -63 (Magnesia- hercynite)
(Spinel bricks)
M =86A= 2.5Cr= 0F =8.2C = 1.8 S =0.9
3.1 17 > 50 >1600 >1700 42 1.5 2.7 > 100
Ankral X2 (Magnesia-galaxite)
M =91A= 3.5Cr= 0F =0.7C = 0 MnO =2.6
2.98 15 90 > 1700 2.7 > 100
VRW-70 A = 70 % Fe2O3 = 3.5 2.65 23 > 55 1460 37 2 1.9 30
VRW- Lofal 70
A = 70 % Fe2O3 = 2.5 2.65 23 > 55 1500 36 2.5 1.9 30
RUL
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