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RAW MATERIALS BATCHING MELTING FORMING ANNEALING Glass Defects Jean Louis HEITZ, CRITT Matériaux Alsace PRIMARY CONTAMINATION raw material production delivery media (boats, cars) raw materials storage in the glass plant CONTAMINATION FROM BATCHING REFRACTORY WEAR CONDENSATE DRIPPING BATCHING ERROR CONTAMINATION FROM CONTACT WITH TOOLS ATMOSPHERE CONTAMINATION PROCEDURE Cullet : metals, porcelain, vitroceramics Lead oxide : corundum, sillimanite, metal lead CONTAMINATION FROM : corundum, sillimanite, chromite corundum, SiC, iron oxides Unmelted silica, Cords Cords Metals, Conveyor belt Black speck (press-blow sodalime glass, SEM ) Annealing bloom Tin oxide condensates (float glass) Silica batch stones HANDLING Sand, dolomite : heavy minerals redox contaminants Miscellaneous : Ni -> NiS Silicon ball from metallic aluminum Porcelain Vitroceramic Corundum (ruby) Nickel sulfide Reduced lead balls (lead crystal glass) Andalousite Chromite Corundum (saphir) POOR BATCH HOMOGENEITY Temperature, pull-out FURNACE MANAGEMENT Diopside b - wollastonite (sodalime glass) Unmelted silica Devitrification stones Volatilization Volatilization cords (lead crystal glass) Silica : air surface devitrification (borosilicate glass) Fused cast, sintered, silica, electrodes, refractory metals Cat scratches Vitreous knots Top view (PLM) Section (SEM) AZS superstructure with secondary zirconia (sodalime glass) AZS glass contact in a dead water zone with secondary wadeite (lead crystal glass) Iron oxide flake stuck on the inner side of vessel –> revealed by acid polishing (lead crystal glass) Primary AZS stones (lead crystal glass, sodalime glass, SEM) Primary silica from superstructure (sodalime glass, PLM, SEM) Primary tin oxide + secondary potassium tin silicates (lead crystal glass - PLM, SEM) Ceramic fibres (sodalime glass, PLM, SEM) the core of the Al – Zr enriched cords is 10 µm under the surface 1. Collection of data and samples in collaboration with glasswork production staff 2. Sample in-situ examination using PLM (polarizing light microscope) 3. SEM+EDX(+WDX) analysis of selected samples Defect sorting by categories Representative defects selection for SEM analysis Optional analyses : XRD, XRF, TOF-SIMS, ICP, etc. 5. Discussion of results with glasswork production staff Defect reference samples Dismantled furnace reference samples 4. Synthesis Comparison with proprietary database Frictive damage on top of knurl : smeared metal and crecsent crack www.critt.fr

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  • RAWMATERIALS

    BATCHING

    MELTING

    FORMING

    ANNEALING

    Glass Defects Jean Louis HEITZ, CRITT Matriaux Alsace

    PRIMARYCONTAMINATION

    raw materialproduction

    delivery media(boats, cars)

    raw materials storage in theglass plant

    CONTAMINATION FROM BATCHING

    REFRACTORY WEAR

    CONDENSATEDRIPPING

    BATCHING ERROR

    CONTAMINATION FROM CONTACT WITH TOOLS

    ATMOSPHERECONTAMINATION

    PROCEDURE

    Cullet : metals, porcelain, vitroceramics Lead oxide :corundum,sillimanite,metal lead

    CONTAMINATION FROM :

    corundum,sillimanite,chromite

    corundum,SiC,iron oxides

    Unmelted silica, Cords Cords Metals, Conveyor belt

    Black speck(press-blow

    sodalime glass, SEM )

    Annealing bloom

    Tin oxide condensates (float glass)

    Silica batch stones

    HANDLING

    Sand, dolomite :heavy minerals redox contaminants

    Miscellaneous :Ni -> NiS

    Silicon ball from metallic aluminum

    Porcelain Vitroceramic

    Corundum (ruby) Nickel sulfide Reduced lead balls(lead crystal glass)

    Andalousite

    Chromite

    Corundum (saphir)

    POOR BATCH HOMOGENEITY

    Temperature, pull-outFURNACE MANAGEMENT

    Diopsideb - wollastonite(sodalime glass)

    Unmelted silica

    Devitrification stones

    Volatilization

    Volatilization cords(lead crystal glass)

    Silica : air surface devitrification(borosilicate glass)

    Fused cast, sintered, silica, electrodes, refractory metals

    Cat scratches Vitreous knots

    Top view (PLM) Section (SEM) AZS superstructure with secondary zirconia

    (sodalime glass)

    AZS glass contact in a dead water zone with

    secondary wadeite(lead crystal glass)

    Iron oxide flake stuckon the inner side of vessel

    > revealed by acid polishing(lead crystal glass)

    Primary AZS stones(lead crystal glass,

    sodalime glass, SEM)

    Primary silica from superstructure

    (sodalime glass, PLM, SEM)

    Primary tin oxide + secondary potassium tin

    silicates (lead crystal glass - PLM, SEM)

    Ceramic fibres(sodalime glass,

    PLM, SEM)

    the core of the Al Zr enriched cords is 10 m under the surface

    1. Collection of data and samples in collaboration with glasswork production staff

    2. Sample in-situ examination using PLM (polarizing light microscope)

    3. SEM+EDX(+WDX) analysis of selected samples

    Defect sorting by categories Representative defects selection for SEM analysis

    Optional analyses : XRD, XRF,TOF-SIMS, ICP, etc.

    5. Discussion of results with glasswork production staff

    Defect reference samples Dismantled furnace reference samples

    4. SynthesisComparison with proprietary database

    Frictive damage on top of knurl :

    smeared metal and crecsent crack

    www.critt.fr