Prosiding Pertemuan llmiah Ilmu Pengetahuan dan Teknologi Bahan 2002 Serpong, 22 -23 Oktober 2002

lSSN 1411-2213

RESEARCH AND DEVELOPMENT PROGRAM FOR CATALYTIC CONVERTER MATERIALS IN BATAN Gunandjar, P. Untoro, Syahril and Wuryanto NationalNuclear EnergyAgency MampangPrapatan, Kuningan Barat,Jakarta12710

ABSTRACT Researchand Development Program tor Catalytic Converter Materials is coordinated researchprogram in tour main areas toward the development of catalytic converter systems over the next five fiscal years. The four areas are: concept development, human resources development, researchtools & supporting development, and demonstration & technology base development. In order to meet the program mission and goals. research must be conducted on the sinergize of the intire catalytic converter system, including integration into the market applications. The total system must be designed properly to work together efficiently and reliability. To conduct systems studies and develop promising designs for succest"ullplan, it will be necessaryto coordinate the technical of various subsystemsand components continously included the syntesis of catalyst and base materials, surtace treatments, modelling and simulation, testing and characterizations

INTRODUCTION The researchand developmentprogram described in this paper is designed to facilitate and encourage research communities in the related field to make use of the research facilities in Batan. By doing this we hope that the communities can make a concerted effort to address a specific issue; which in this case is the researchand development of materials for catalytic converter. This program, which was begun in 1999, is one of the continuously funded materials development programs ever undertaken at BAT AN and International Buero from Ministry of Education and Research,Federal Republicof Germany in the frame of bilateral cooperation research in science and technology for Development ofMaterials for .4utomotive Catalytic Converter IDN 99/004. The Aachen University of Technology (GFE Rwth Aachen) and Juelich ResearchCenter (RC Juelich) has provided facilities and consumable materials to this program and expertise of the research cooperation. The various researchthemas from syntesis until prototipe production step are examined in detail and for their adequacy to meet percieved future demands. Someexamples of the developmentsemerging from our reserchcenters include the following: .Syntesis and development of metalic substrate based on Fe, Al through casting, mechanical alloying, and powder technology. .Surface treatments and deposition technique used to modify and improve the metal or ceramic subtrate. .Structural Characterization with SEM/TEM (Scanning/Transmission Electron Microscope) and XRD (X Ray Diffraction) to monitor and analyse processes in materials on time scales so short that

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the various stagesin atomic rearrangementsand chemicalreactionscanbe distinguished. .High TemperatureCorrosionto testthe material at operatingconditions. .Modelling and simulation to study physical and mechanicalpropertiesof the carrier.

PROGRAM MANAGEMENT The Batan materials research program for catalytic converterhas beena succesfulscienceand technology development program for a number of reasons. These include consistent and continuous funding, effective coordinated research program, flexibility to orient and refocusthe researchefforts in responseto promising results or identified needs of every center,and establishmentof partnershipsand collaborationswith otherinstitutions.(Figure 1). The coordinationresearchin the nationalfield will be connectedwith the national planning from ministry of researchand technology and also with industriesto identifytheir needsand establishpractical goals for technologydevelopment. The program management strategy will be forwardedto reflect a newcommitmentto increasethe commercialimpactof this program.BATAN's research and developmentmanagementstrategywas changed from a technology push strategy to a market pull strategy.

Researchand DevelopmentProgram/or CataLyticConverterMaterialsin BATAN (Gunandjar)

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Figure 1. Program management of the cooperation research

TECHNICAL PROGRAM The technical research program has made significant technicaladvancessinceits inceptionfrom basicresearchandapplications.The early decissionto focus on sinergiesall of diciplines in researchcenters and their relationships are shown schematically in Figure2 in the form of a tetrahedron. The field of catalytic converter researchhas involved along many parallel and intertwined paths associated with wide ranges diciplines and R&D laboratories.It is theseelements-syntesis andprocess,

perfonnance,and modelling & simulation and properties and the strong interrelationship among them- that define the field research work synergies. The technical program should be well managed, with effective integration of the program elements from basic research through prototipe production demontrations and effective coordination of program goals and responsibilities among participating research institutions.

Figure 2. A tetrahedron synergism program tor materials research and development

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Pro.~iding Pertemuan lbniah lbnu Pengetahuan don Teknologi Bahan 2002 .s'erpong,22 -23 Oktober 2002

ISSN1411-2213

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Figure 3.1. Calculated stress distribution after cooling from 1200oC in the case of irregular oxide/metal interlace given in Figure 3.11 a) for alumina scale on PM 2000 a) Stress in X direction; b) Stress in Y direction

Figure 3.2. Calculated stress distribution after cooling from l200oC in the case of convoluted scale morphology given in Figure 3.11 b) tor alumina scale on PM 2000 a) Stress in X direction; b) Stress in Y direction

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Figure 5. TEM-image from cross section and EDX analysis after lOOh isothermal oxidation at 1200.C in air

Technicalaccomplishmentsin the syntesisand developmentof subtrateinclude: .The identification of processingtechnology .The determination of physical and mechanical properties .The improvementof ductility by nricroalloyingwith reactiveelements .The improvementof elevatedtemperaturestrength and processibility using standard alloying techniques,including solid solutionstrengthening, dispersion strengthening, weldability, and castability. The preparing a catalyst is one important processand shouldemphasizelow costprocesses\\"ith big effort from nationalresourcesin Indonesia: .Metal e:\.1raction .Chemical reactions .Process optimation Surfacetreatmentusing nucleartechnique\\"ith ion beamand coatingtechnique: .Vacuum Coating,PlasmaCoating and Sputtering

technique .Pack

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.Ion Implantationtechnique .Ion Beam Mixing technique using cambination betweencoatingand ion bombardement technique Characterization for physical, chemical and mechanical and also microstructure with electron microscopytechnique: .Stress-strain behaviour in atmosphereand also during heating .Thermal behaviour .High TemperatureO.xidationattemperature< 1100 °C in isothermalandzyclic conditions .SEMffEM coupledwith crystallographyanalysis Modellingand Simulation .Mechanical Modeling .Thermal modelling

FACILITIES AND SUPPORT The main facilities for the program responsibilities include facilities from various centers in BATAN or from other institutions. The facilities that had been supported from BMBF in the frame of cooperation will be used and optimized for further

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[4]. [3].

Pro.siding Pertemuan Ilmiah lbnu Pengetahuan don Teknologi Bahan 2002 .\'erpong. 22 -23 Okt()ber 2002

researchtools connected with the program participating centers. Some results that has been produced using thesefacilities will be also be presented in this seminar. The support facilities are .MSBTGA : Mass Suspension Balance Thermogravimetry Analyser .Software ANSYS 6.0 lite version .Dironond wire saw maschine .PIPS: Precision Ion Polishing System Financial support will be obtained from BATAN and other sources. However, it seemsto me that a great deal of comnritment can be found on internal centers in BATAN. and also especially in connection with the activities of RISTEK in the frame of Indonesian International Joint ResearchProgram (RUTI). Another assetis the sustaining financial support from German government in the frame of bilateral cooperation in the science and technology.

PROGRESS Technical activities started with a group from alumni who have trained at GFE Rwth Aachen and RC Juelich. A working group, called "inteffiletalik" has been founded includ: to design and . execute ti}e program. Activities .Finite Element Modelling .Material syntesis .High TemperatureCorrosion, including the activities with nuclear technique monitoring for corrosion of TLA (Thin Layer Activation), surface treatmentand corrosion testing with theffilogravimetry technique (The result will be also presented in this seminar). .Characterization, a routine training or practical works in the field of newest characterization methods. Some expermental results in Figure 3 [5] shows the calculation of the stress distribution during cooling of oxidized commercial alloys from 1200°C to 20 °C for 5 ~m thick oxide scale on 100 ~m thick subtrate with ANSYS. The stress distribution in X direction points out the tensile stress at the valleys and compressive stress at the ridges. In the Y direction the oxide stress is tensile with a value, which seems to the author too low to cause initially oxide failure. Much higher tensile stress value is featured by the convoluted scale. Both in X and Y direction, there are tensile stress areas with significant values of 0.5 -I GPa. Due to the oxide roughness the tensile stress areas appeared at ridges, but also in the oxide valleys. Therefore, the possibility of oxide failure is greater by convoluted scale that by the scale with an irregular oxide/metal interface. The result of high temperature corrosion measurement with TGA measurements in Figure 4 shows that the implanted sample with yttrium has the lower oxidation rate [6].

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Microstructural examination with TEM-EDX with FIB (FocussedIon Beam) cross section preparation (Figure 5) were used to study scale structure and more precisely locate the trace amount of elements in the oxide layer. The scale appeared to consist of columnar grains near the scale alloy interface and equiaxed grains near the oxide surface. The TEM investigations not only allowed to locate grains of spinel (MgAI2O 4)at the top of the oxide layer, but also magnesium at the grain boundaries of the alumina, whereas magnesium could not be identified within the alumina grains [7].

FUTURE FOCUS PROGRAM Throughout the BAT AN material research program, interaction with industrial participants will be critical to identify needsand priorities. Interactions with local industry will help BATAN to focus on optimizing alloy modifications and developing process technologies to meet industrial needs. Future structure program in material research should be included 4 catagories of activities: .Human resources development and mobility in contribution to national mobility programmes open to other institutions and support for teams of the highest level of excellence. .Research integrated infrastructures should be usable to support cross acces communication infrastructure and support for the development of new infrastructures/teams. .Synergism and Networking in long-term and multidisciplinary objectives implemented by ajoint programme of activities. .Science and people wellfare to bring the reserch closer to people with a new form of dialogue, knowledge of science by citizens and young scientist interesrt in spesific thema of material research.

REFERENCES [1). JAKSTRA. PUNAS Ristek [2]. MATECK, Material Research Program from German Ministry of Education and Research,

(1.998) Materials Program from Departemen of Energy USA, (2001.) H. BODE, Materials Aspects in Automotive Catal)1ic Converters,Wiley- VCH, (200 I) SUN.ARDI, Report during research in Institutfor Materials and Processesin Energy System,(200 I. ) [6J. W AGIYO, Jndonesian-GermanySeminar Report IDN99/004, (2002) [7). P. UNTORO et.al., Coluerence on Material Aspects in Automotive Catalytic Converters,Muenchen,2001. [5].

Researchand DevelopmentProgram/or CatalyticConverterMaterialsin BATAN (Gunandjar)

TANYAJAWAB Evvy Kartini, P3ffi -BATAN Pertanyaan

1. Penelitian catalytic converter materials yang dilakukan antar pusat daD antar instansi telah berjalan, apakah dapat memicu topik penelitian lainnya Jawaban

I. Penelitian catalytic converter materiaL\"berjalan karena didukung oleh para peneliti, sedangkan pejabatstruktural hanya memfasilitasisaja.Tentu saja pola yang sarna dapat diterapkan untuk penelitianyanglain.

Ke Daftar Isi 9