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THE BEHA VIOR of Tac and Tac+AI ELECTRODES in Ticl4 PLASMA GASES THESIS by Department of Chemical Engineering

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THE BEHA VIOR of Tac and Tac+AI ELECTRODES in Ticl4 PLASMA GASES THESIS by Department of Chemical Engineering THE BEHA VIOR OF TaC AND TaC+AI ELECTRODES IN TiCL4 PLASMA GASES A THESIS BY Department of Chemical Engineering -- McGill University Under the supervision of Dr. R. J. Munz and Dr. P. Tsantrizos Submitted to the Faculty of Graduate Studies and Research of McGill University in partial fulfillment of the requirernents for thl~ de!Ç'ee of MasteT of Engineering McGill University 1 Montreal, C~mada December 1990 , To my parents and my sister's family • ACKNOWLEDGEMENTS My sincere appreciation is expressed to my supcrvisors Dr. R. J. Munz and Dr. P. TSlmtrizos for their guidance and help throughout aIl the phases of this work. Special thanks to G. LeBlanc, Dr. R. N. Szente, Dr. K. Shanker, G. Q. Chen and M. Habelrih for their friendly help, and to tpe plasma group supervisors: Dr. D. Berk, Dr. 1. L. Meunier, and Dr. W. Gauvin for their valuable input. A lot thanks to Mr. J. Dumont, Mr. A. Krish, Mr. A. Gagnon, Mr. D. Leishman and Mr. C. Dolan, Mr. L. Cusmich, and Mr. N. Habib for ail their greal J assistance. To the plasma group member: Murray, Bogdan, Muftah, Mario, Chico, Mike, and to my fiends: Yonghao, Jian, Biao, Lijie and many others, thank ail of them very much. Many thanks to P. Fong, Mrs. A. Prihoda, Louise Miller and Valerie IlubbanJ for their help. ,. Abstract An experimental study was carried out to identify a suitable electrode material for the treatment of TiC4 in a plasma arc. The behavior of the arc voltage, velocity and rate of electrode erosion were examined in a OC pI.l;:.,ma torch using concentric cylindrical eIectrodes and arc rotation by an axial magnetic field. The re~ults of the expcriments and analyses showed that pure TaC was not suitable as an electrode materia! because of its mechanical failure under themlal stress. A new composite matenal, TaC infiltrated with Al proved to he successful. Stable plasmas were produced containing up to 30 % titanium tetrachloride in argon at a CUITent of 100 amperes, an interelectrode gap of 4 mm, and a magne tic field strength of lOOO Gauss. The cathode erosion rate was less than 30 micrograms/C at a ùtanium tetrachloride concentration of 14.3 %. , 1 CONTENTS Abstract Resume Acknowledgement Contents List of Figures 5 List of Tables 7 Chapter 1. Introduction 1.1 Background Infonnation X 1.2 Objectives 10 1 Chapter 2. Literature Review 2.1 Plasma Phenomena A. The Definition of Plasmas U B. Categories of Plasma 14 2.2 The Approaches to Producing Plasmas A. Plasma Generation 14 B. Electrical Discharge 15 2.3 Plasma Deviees A. Electrodeless Deviees 1<) B. Electrode Deviees 20 2.4 Phenomena of Electrode Erosion A. Introduction 25 1 B. Parameters Affecting Electrode EroSIon 25 Resumé Une étude expérimentale fut enterprise afin d'identifier un materiau d'électrode permettant le trai tment de TiC14 dans un plasma d'arc. Le comportement de la tension et de la vitesse de rotation de l'arc ainsi que du taux d'érosion de l'électrode ont éte etudie sur une torche n plasma munié d'electrodes cylindriques concentriques. Un champ magnetique axial imposait une rotation de l'arc entre les électrodes. Les resultats expérimentaux indiquent qu'un cathode de TaC pure ne peut supporter les stress thermiques, provoquent ainsi une defaillance méchanique rapide de l'électrode. Une noveau materiau composite formé de TaC avec infiltration d'aluminium a éte développe et teste avec sucees comme materiau d'electrode. Des plasmas stables on été produits avec des pourcentages allant jusqu'a 30% de tetrachlorure de titane dans l'argon a un courant d'arc de 100 amperes, une espacement interelectrodes de 4 mm et une champ magnetique de 1000 Gauss. Le taux d'érosion de la cathode mesure à une concentration de tetrachlorure de titane de 14.3 % etait inferieur à 30 X 10-6 g/C. 1 C. Improwment of Electrode 1~roslon 2.5 Plasma Containing TICLI Chapter 3. Experimental Ar,paratus 3.1 Introduction ,' , 3.2 The DC-Pla~ma Arc Torch l, , A. The Configuration of the Elcctllldc" ~( 1 B. The Exten,,\on of the Rcactor l,1l C. The Viewing Window ,~ D. The Rc]ocatlon of the OplH.:aJ Flber l,S E. P]a~ma Ga:.. Fred LlIlcs l,S 3.3 The Fccdmg Sy~tem ~s 3.4 The Scrllbblllg Sy:-.tC11l ~I) 1 3.5 The Heatlllg/Cooltng Sy..,tCJ11 12 3.6 The Data Recordlng Sy:-.tem 12 3.7 Power Supphc:-. l , 3.R The Hlgh Freqllency Unit 1 \ Chapter 4 Kxpcrimen(al Procedures 4.1 1n troduction 11 4.2 Preparation of Expenmentl, A. Prcparation of Electrode 1 1 B. Cleanmg Procedure of the .... y..,tem 1') C. As:-.cmbling Procedure 1') D. Pre-Check Procedurc 1') 4.3 Operation of Expcnmcntl, A. Startmg Procedure 1(l - 3 B. Operating of Tests 46 4.4 PO\t-Treatments 47 Chapter 5 Pioneering Analysis 5. ] Thermodynamic Considerations A. Ba~ c Thermodynamic Analysis 48 B. Conclusion 51 ., 5.2 Preliminary Experiments A. Preparation of Pure TaC Cathode Rings 51 B. Experimental Condirions 55 C. Results of Experiments 55 5.3 Basic Failure Analysis A. Temperature Cycling and Gradient 60 B. Them1o-Mechanical Failure of the Electrode Ring 61 C. Conclusion 62 Chaptcr 6 Experiments with TaC+AI Electrodes 6.1 The PreparatIon of TaC+AI Electrodes A. Fabncation of TaC+AI Electrode 63 B. The Propenles of TaC+A! Materia! 63 6.2 TaC+Al Electrode ;n Argon Plasma Gas A. Results 66 B. DiscussIOn 66 6.3 TaC+AI Electrodes ln TICI4 + Argon Plasma Gases A. Experimental Conditions 70 B. The Features of the Arc Voltage 70 ·1 C. Weight Loss and Erosion Rate 75 ! d1 ·1 ~ D. Arc Velocity XJ E. Effect of Arc Velocity on Erosion Rate Xl) F. SEM Analysis 91 G. The Behavior of the Anodes 97 H. Conclusions 9X Chapter 7 Conclusions and Recommendations 7.1 Conclusions 100 7.2 Recommendations lOI References IO::! J J 5 1 LIST OF FIGURES Figures Caption j - 1 Tnanium Production - the KroH Process Il 2-1 Voltage vs. CUITent for Neon at 40 mm Hg 16 2-2 Characteristics of Arc Dl~harges 18 2-3 Schcmatlc OI<!WlI1g of RF Plasma Torch 20 2-4 Schcmatlc Drawll1g of Transferred Arc Torch 22 2-5 Schcmatic Drawing of DC Pla~:ma Torch 2.4- 2-6 Arc Voltage Vanatlons with Tlme for TiCl4 -Rich Arcs U.,lI1g a Thuriated Tungsten Cathode 31 2-7 Arc Voltage Vanatiom. wlth Time for TiCI4 -Rich Arcs Using a Thonated Tantalum Carbide Cathooe 32 1 3-1 Schematlc DlawlI1g of the Overall Expenmental Set-up 34 3-2 Schcmauc Drawmg of the Reactor Assembly 35 3-3 SchematIc Drawing of the Anode and the Calhcxle 37 3-4 Schematlc Orawing of the Feeding System 40 3-5 Schematlc DrawlI1g 0f the Scrubbing System 41 5-1 The Flow ChaI1 of Fabncatmg TaI'": Cathode Ring 53 5-2 The RlIlgs in Different Stages of Fabrication 54 5-3 The Ml(:rmtructure of the Ring (SEM) 55 5-4 The Photograph of a Cathode Ring and a Copper Anode After Testing 58 5-5 The Fractured Parts {,f the Pure TaC Cathode Ring 59 6-1 The Flow ChaI1 of TaC+Al Electrodes Fabrication 64 6-2 The Micrograph of a TaC+Al Electrode 65 1 6-3 The Photograph of a Ring and a Tip After a One Hour Test 69 0-4 The Microstructure of TaC+Al After a One Hour Test 69 b .., 6-5 Average Arc Voltage vs the Concentration ofTleL) 72 6-6 The Features of Average Volt:lge v~ Opcratlng TIJllC 7·1 6-7 The Response of Voltage Dunng 14% TI('!.1 Gas Testlllg 76 6-8 The Welght Loss of TaC-r Al Cathode III 'l'1Cl, Pla~111a 79 6-9 The Welght Loss of TaC+Al Cathode v.., the Conccrllration of TrCL, ~o 6-10 The Erosion Rate of TaC+AI Cathode III TICl.1 Plasma X2 6-11 Erosion Rate as a Function of TICl4 ConcentratiOn at Different 'l'lInc.., X·I 6-12 Arc Velocity vs TICl4 Concentration Xh 6-13 Arc Velocity as a Function of TiCI4 Concentration XX 6-14 Effeet of Arc Velocity on Erosion Rate of Electrodes 90 6-15 The Micrograph of the Cathode In~ide Surface !)2 6-16 The Micrograph of the Cathode Owslde Surface 93 6-17 The Comparison of Element Mapp1l1g on the Cathode Surface 9·1 ~ 6-18 The Deposit'i ofTnanium on the Cathode Surface 9.') 6-19 The Analysis of the Compo~ition on the Cathode Surface % 6-20 A Tantalum Carbide Anode Tip After Te~tll1g l)l) 6-21 A Photograph of the l\rc in TiCl4 Gas 99 7 1 LIST OF TABLES Tables Caption 1-1 Economies of Titanium Production 9 2-1 Experimental Data on Cathode Erosion 30 5-1 The Results of Chemieal Reaction Analysis 50 5-2 The Results of Equilibrium Analysis at 2000 K 50 5-3 The Composition of TaC Powder 52 5-4 The Experimental Conditions 57 6-1 The Properties of TaC+AI Material 65 6-2 Experimental Conditions for TaC+AI Electrodes in Argon Plasma 67 6-3 The ResuIts of TaC+Al Cathode Rings in Argon Gas 68 1 6-4 Operating Conditions for TiC4 + Argon Plasma Gases 70 6-5 The Arc Voltage vs TiC4 Concentration 71 6-6 Reproducibi.lity of the Arc Voltage 73 6-7 Weight Loss and Erosion Rate of Electrodes 77 6-8 The Arc Velocities in Different Conditions 85 1 CHAPTER 1.
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