Dr. Andreas Diegeler Director Center for Device Development Fraunhofer ISC, Germany. Fraunhofer

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1 Thermo-Optical Measuring method (TOM) - A high efficient tool for the analysis and optimization of coal firing process and characterization of slag behavior Dr. Andreas Diegeler Director Center for Device Development Fraunhofer ISC, Germany

2 Outline Brief introduction Fraunhofer ISC Characterization of coal com bustion and slag behavior using TOM Application of Therm o-optical-measuring m ethod Optim ization of firing process through in-situ characterization of ash/slag behavior and the interaction with environm ental m aterial Characterization of wetting on refractory m aterial and corrosion process Analysis of slag com ponents View to degasing process via IR-spectroskopy Sum m ary Fraunhofer lines

3 Finance volume Contract Research The Fraunhofer-Gesellschaft at a Glance The Fraunhofer-Gesellschaft undertakes applied research of direct utility to private and public enterprise and of wide benefit to society. 24,500 staff 2.1 billion 1.9 billion Major infrastructure capital expenditure and defense research Almost 30% is contributed by the German central and federal Governments 69 institutes and research units 2017 More than 70% is derived from contracts with industry and from publicly financed research projects.

4 Fraunhofer-Institut für Silicatforschung ISC Locations ISC Stadt Würzburg Alzenau/Hanau ISC Stadt Bayreuth

5 Fraunhofer ISC overview It s a material world Material-based solutions Materials Chemistry Inorganic Sol-gel-materials Hybrid materials Barrier coatings Particles Application Technology Micro-optics/ Electronics Specialty glass Dental/ Micromedicine Services Applied Analytics Device Development Cultural Heritage Center for Applied Electrochemistry Battery materials and components Testing Post mortem analysis Center Smart Materials Adaptive Materials Sensors Energy harvesting 423 Employees (2017) 29.8 Mio Budget (2017), including Mio venue from contract research approx m² labs and technical space 5 sites centrally located within Germany Fraunhofer- Center HTL High temperature lightweight materials, energy efficient heat treatment Bayreuth Project Group IWKS Materials recycling, substitution, and ressource strategies Alzenau/ Hanau

6 Characterization of coal combustion and slag behavior using Thermo-Optical-Measuring method - TOM CSIRO

7 Why using TOM for the optimization on coal fired plants? Online view to the real process in the lab furnace boiler/gasifier Monitoring of efficient conditions through the firing process Decrease temperature Decrease cost Detection of flow behavior of ash/slag to avoid/control slagging in the boiler/gasifier Characterization of wetting on refractory material to avoid corrosion process and increase lifetime of the environmental material Analysis of slag components for quality control View to gasification process via IR-spectroskopy to improve CO 2 capture (CCS) Higher efficiency + less emission + less cost Fraunhofer lines

8 Application of Thermo-Optical Measuring procedures (TOM) In-situ optical investigation of slag and ash behaviour Continuous monitoring of sample silhouette by CMOS camera during heat treatment up to 2400 C Full automatic control of gas atmosphere Additional modules for creep, TGA, viscosity and gas analysis (my physical lab in a furnace ) Dimension change Viscosity Creep Wetting

9 Application of Thermo-Optical Measuring procedures (TOM) THE TOM - PRINCIPLE optical axis probe PC base light source CMOS-camera furnace window balance balance gas analysis/ viscosity IR/GC load force

10 Application of Thermo-Optical Measuring procedures (TOM)

11 Application of Thermo-Optical Measuring procedures (TOM) Sample size up to 60 mm Temperature range RT 2400 C Resolution ca. 0.3 µm Detection of: Sample height, width, area, curvature, contact angle Thermal expansion of Al 2 O 3 TOMMI Literature data L/L Temperature [ C] CTE of Al 2 O 3

12 Application of Thermo-Optical Measuring procedures (TOM) Investigation of oxide, non oxide ceramics and powder metals In situ measurement of sintering kinetics and warping Detection of high temperature reactions Investigation of wetting and infiltration processes Determination of thermophysical data Wetting of SiO 2 Infiltration of Si to Carbon

13 Application of Thermo-Optical Measuring procedures (TOM) on various coal, ashes and slag TOM-AC at the IEC (Department of Energy Process Engineering and Chemical Engineering) in use to optimize firing process in the boiler/gasifier and determine slag behaviour Investigations on various coal and biomass ashes within the projects Virtuhcon and DER (density, wetting behaviour, surface tension, degasing, interaction with refractory, ) Detection of high temperature reactions experimental investigation of surface tension: C C C C View to slag wetting at high temperatures

14 Width in mm Slag-refractory interactions TOM-AC Investigation of wetting behavior C C C C new developed refractories of different ceramic systems test with different ashes/slags (acid, intermediate, basic) experimental conditions: - up to 1450 C - 10 K/min - reducing atmosphere (5 vol.-% H2 in Ar) Slag A (short melting interval) start of sintering (shrinking) 10 -B -A Temperature in C Slag A Slag B different slags on same refractory Seggiani, M.: Modelling and simulation of time varying slag flow in a Prenflo entrained-flow gasifier. Fuel, Vol. 77, No. 14, 1998

15 Investigation of slag flow behaviour at refractory walls (entrained flow gasifier) Aim: validation experiments for numerical simulation Observed Phenomena: diffusion of slag into refractory and transition into gas phase (deposition at windows) test with different ashes/slags (acid, intermediate, basic) Experimental setup: - 3-component slag (Al2O3-10 at.%, CaO - 45 at.%, SiO2-45 at.%), - melting point 1275 C - maximum temperature 1300 C, inert conditions (N2 purge gas) -900 C C C C(cooling) Pictures at different temperatures

16 Investigation of the release of volatiles Release of volatile ash components: temperature of degasing and degasing intensity pretest for other high temperature investigations within sensitive devices (prevention of over boiling, spattering) degasing, over boiling, spattering

17 Behaviour of slag during heat treatment with different refractory material

18 Slag-compound analysis (1) SEM analysis with EDX analysis of heterogeneous slag compounds embedded with EPO 4 different locations on polished cross section additional analysis of IR- spectra of slag at high temperature (>1600 C) TU Freiberg SEM with 4-point EDX

19 Slag-compound analysis (2) SEM analysis with EDX Element Gewichts% Gewichts% σ Atom% Komponente n% Formel Kohlenstoff CO2 Natrium Na2O Magnesium MgO Aluminium Al2O3 Silizium SiO2 Phosphor P2O5 Chlor Kalium K2O Kalzium CaO Titan TiO2 Eisen FeO Sauerstoff

20 Slag-compound analysis (2) SEM analysis with EDX Element Gewichts% Gewichts% σ Atom% Komponenten Formel % Kohlenstoff CO2 Phosphor P2O5 Eisen FeO Sauerstoff

21 Slag-compound analysis (3) SEM analysis with EDX Element Gewichts% Gewichts% σ Atom% Komponente n% Formel Kohlenstoff CO2 Magnesium MgO Aluminium Al2O3 Silizium SiO2 Phosphor P2O5 Schwefel SO3 Chlor Kalium K2O Kalzium CaO Eisen FeO Kupfer CuO Zink ZnO Sauerstoff

22 Slag-compound analysis (4) SEM analysis with EDX Element Gewichts% Gewichts% σ Atom% Komponente n% Formel Kohlenstoff CO2 Natrium Na2O Magnesium MgO Aluminium Al2O3 Silizium SiO2 Phosphor P2O5 Schwefel SO3 Chlor Kalium K2O Kalzium CaO Titan TiO2 Eisen FeO Kupfer CuO Sauerstoff

23 Transmission [a.u.] Slag-compound analysis (5) IR-Spectra analysis gas analysis IR/GC IR-analysis of heterogeneous slag 100 C-H compounds during melting- degassing at high temperature (>1600 C) first steps O-H CH 2, CH 3 Si-H C-H TU Freiberg 40 C=O Si-CH 3 C-H C-Cl 20 Si-O-CH 3 C=C-H 0 Schlacke-1-LD-Schlacke Si-H Wellenzahl [cm -1 ] different bonds/double bonds of Si, C, O, H

24 Summary Versatile tool for investigation of heating processes up to 1750 C/2400 C to help to understand how to increase efficiency of coal firing process and slag behavior In situ measurement of sintering, shrinkage and warping of various coal, ashes and slag Determination of creep, mass change, wetting and crack properties Determination of viscosity character of melts, slag TU Freiberg ISC

25 Acknowledgement ZIK Virtuhcon Department of Energy Process Engineering and Chemical Engineering

26 Batterien in PKW - Ausblick Standard-PKW 88,5% Micro 10% HEV 1,5% EV/ PHEV 2010 Thank you for your Standard Bleibatterie attention! Moderne Bleibatterie LiB Standard-PKW nach C. Pillot (Avicenne Développement), Batteries International, Spring 2014 Microhybrid 50% 2020 Dr. Andreas Diegeler 44% Fraunhofer-Institute for S ilicate Research IS C Bronnbach Wertheim -Bronnbach Ultra/ Hybrid Germ Zukunft any Bleibatterie andreas.diegeler@isc.fraunhofer.de LiB HEV 4% EV/ PHEV 2% Li/S, Li/air, PEMFC A. Schollenberger für Fraunhofer ISC