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The Formation and Reactivitt of Some Transition Metal

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The Formation and Reactivitt of Some Transition Metal University of Plymouth PEARL https://pearl.plymouth.ac.uk 04 University of Plymouth Research Theses 01 Research Theses Main Collection 1970 THK FORMATION AND REACTIVITY OF SOME TRANSITION METAL NITOIDES ALI, IRSHAD http://hdl.handle.net/10026.1/1878 University of Plymouth All content in PEARL is protected by copyright law. Author manuscripts are made available in accordance with publisher policies. Please cite only the published version using the details provided on the item record or document. In the absence of an open licence (e.g. Creative Commons), permissions for further reuse of content should be sought from the publisher or author. THE FORMATION AND REACTIVITT OF SOME TRANSITION METAL NITRIDES A' Thesis presented for the Research Degree of DOCTOR OF PHILOSOPHY of the COUNCIL FOR NATIONAL ACADEMIC AWARDS London by IRSHAD ALI Department of Chemlstryp Plymouth Polytechnicp PLYI^OUTH, Devon May, mo I ST Lz-fj <<^-L y 0^ r^^o T200fi5 3H1R33 S33HnOS3B 9HirjB»31 3IUU3aui0d HinOliiAld ACKNOWLEDGMENTS T!he author wishes to express his sincere gratitude to DTC Dfl R« Glasson for his supervision, guidance and encouragement throughout the course of this work„ He is grateful to Dr. A. B, Meggy9 Head of Chemistry Departanent, Plymouth Polytechnic, for the \ise of facilities and the supply of materials. His thanks are also due to the Polytechnic Governors for the award of a Research Assistantship, Further acknowledgement is made to the follofwing? Hargaret Sheppard for her technical assistance5 lecturers of the Chemistary Department for their help and useful discussions; the Polytechnic Library Staff for their co-operation and to Hiss Vivienne Colwill^ who typed the mamscripto (2) ABSTRACT The fonnation of transition metal nitrides is ^«^^.ev7ed oritically with special reference to newer production mechods and fabrication techniqueso Crystal structures and types of bonding arc dircussed in relation to those of other nitrides and refractory hard metals generally, cf»>» borideSp carbides and sllicidea. Information so far available on the sintering of materials is summarisedo Por nitrides (as witii borides and carbides),, the sintering is influenced by additives and irapi^ritles sueh as oxides forDed by partial hydrolysis and oxidationo F.esista:kce to oxidation is increased by sintering and hot-x>xo3sing the refractoriesc The kinetics and products of oxidation of nitrides so fai' scadied depend mainly on the intrinsic reactivity of the material and available surface at which oxidation can occur^ In the present research, changes in phase composi tion^, surface area, crystallite and aggregate sizes are correlated wiirii oxidation time and temperature conditions for nitrides of sone transition metals, viz., Ti,Zr, V, Nhy Ta., Cr and Mo^Kinetics and rates of oxidation are influenced by the crystallite and aggregate sise& of the nitrideSp by differences in tjrpe of crystal structujre and in molecular volume of the oxide productsc Sintering of the newly-formed oxide is an additional factoro The nitrides were milled to increase their s\irface activity and to examine changes in the micros trueture caused by the comminutiono The milled nitrides apparently have greater 3UT*face heterogeneity and tend initially to give linear rather than parabolic oxidation rates until sufficient oxide of rational crystallite size composition i.3 formed to give stable oxide layerso The sintering of the oxides is controlled by surface diffusion promoting grain-boundary penetration at lower temperatures (above about y niopD oxide m k) and cr-ystal lattice diffusion at higher temperatures (above r,ne Tammann Temperature, about -J- m^po oxide in K)„ Comparison of the oxidation of n.\trided and free metals indicates that oxide sintering is inhibited sometimes by removal of nitrogen but accelerated oceoiSiouallv by the remaining metalo (3) CONTENTS Cha£t©r^ Page. I Introductory Survey and Review Ul Classification of Nitrides «^S 1o2 Transition Hetal Nitrides oo oo o* 9 K3 Relationship between Bonding and Crystal Structure of Binary Compounds oo o.: oo i4 10301 Hagg°s P^ile of Radius Ratio Lixiit oo V4 10302 Paulinfe-Rundle Theory oo o. oo 15 10303 Application of Band Theory oo 16 10304 Ubbelohdo - Samsonov Theory oo I8 1o4- Relationship between Bonding and Crystal Struouire of Ternary Compounds oo DO- O« ' O 2t 1„5 Production of Nitrides oo oo co 21 1o5o1 Methods of Production o« oo 2t U5o2 Thermodynamics of Nitride Px^oduction 25 1„6 Kinetics of Metal Nitridation oo o 29 1e6„1 Rate of Nitridation oo .o 29 1o6.2 Factors Affecting the Rate of Reaction oo 30 ^o6,3 Innic Diffusion s Parabolic Relationship ^5 I06.4 Linear Growth Rate 00 ' 3^ l,6o5 Nature of Nitride Scale 00 00 5? I0606 Kinetic Studies of Nitride Formation with Ammonia o 00 00 00 a a .,0 or> 41 1„6,7 Effect of Gas Pressure on Nitildation KintticSp ©o 00 co k-o 00 -^'t. ^ol ReactivityvOf Nitrides 00 00 - ^ 42 U7c1 Sintering of Nitrddes ^3 Oxidation and Hydrolysis of NitrioeQ o„ ^-T 1.8 Titanium Nitride .0 00 o. ... 49 1o8,1 Formation 00 00 00 00 cn ^9 Io8o2 The System Titanium-Nitrogen . ^.9 Zirconium Nitride „v 00 .-^o ^ <- 5^ U9o1 Pomation 1o9^2 The System Zirconium-Nitrogcrj 00 5^ 1.10 Vanadium Nitride OP 00 or ^ 54 101001 Formation or 00 00 r.« 54 101002 The System Vanadium-Nitrogen 55 Niobi\un Nitride 00 o^ ^no co 5^- 1o11»1 Formation o ^ 00 ^ I0II.2 The System Niobi-'im-Nitrogen co 57 CONTENTS Chapter Pfi£o I U12 Tantalum Nitride oo oo oo oo oo 57 1e12e1 Formation. oo oo oo uo oo 57 1o12o2 The System Tantalum-Nitrogen oo oo 59 K13 Chromium Nitride oo oo oo oo oo 59 1o13o1 Formation oo oo oo oo oo 59 1ol3-2 The System Chromium-Nitrogen oo oo 60 1 o 14 Molybdenum Nitride «o o« cr e o 6t] 1o14.1.Formation oo oo oo oo 61 1 o 14«2 The System Molybdenum-Nitrogen «o 62 n Eyperlmentar Techniques 2ol- X-Ray Diffraction*" oo oo oo oo oo 64 2o1o1 Theory of X-ray Diffraction o <> oe 64 2o1 •2oX-ray Generators oo oo oo oo 64 2.1o3 Debyo-Scherrer Powder Diffraction Camera 67 20104 The Counter Diffractometer oo oo 68 20105 X-ray Line Broadening oo oo oo 71 2o1.5(a) Broadening due to Small Crystallite size* oo 00 oo eo oo 7^ 2.lo5(b) Broadening due to Lattice Distortion 72 2o 1.6 Measurement of IntirLnsic Broadening oo 72 2.1 o7 The Interpretation of Intrinsic Bromiening 74 2c2 Electron Microscopy and Diffraction oo oo 75 2o2Jl Theory of Electron Microscopy and Diffraciiion oo oo oo oo o« 75 2.2o2 The Equipment .o oo oo 79 20203 Preparation of Samples oo oo 80 20204 The Replica Tischnique and Shadow casting 62' 23 Optical Microscopy oo oo oo oo 83' 2o4 Surface Area Measurement by Gas Sorption oo ^ 2.4o1 BoE.T, Procedure oo oo oo oo 84 20402 The Apparatus oo oo oo oo 87 20403 Measurement of Sorption Isotherms oo St 2c5 Thermoanalytical Techniques g oo oo -o 89 2.5.1 Thermal Balance . oo oo oo 89 2o5o2 Hi^ Temperature Vacuum Furnace oo 91 2,5.3 Analysis of Materials oo oo 93 206 Ball«-^lilUng .o. .o oo co oo 9? 207 Computation . oo oo oo oo oo 96 (5) CONTENTS Chanter Page III. Titaniim and Zirconium Nitrides 3.1 Titanium Nitride 3.1.1 Nitridation of Titanium c- 97 3.1.1(a) Compactness of Titanium Nitride Pil^- 1.15 3.1.2 Milling of Titanium Nitride : 17 3.1.3 Oxidation of Titanium Nitride t]. 3.1.3(a) Comparison i/ith oxidation of TitaniUjVi metal. ,, ,. .. .. .. , , i.^jii 3.1.3(b) Comparison with oxidation of Titaniv.r.i Boride and Carbide. izS 3.2 Zirconium Nitride «. .. .. I3o 3.2.1 Nitridation of Zirconium .. l30 3.2.2 Milling of Zirconium Nitride 131 3.2.3 Oxidation of Zirconium Nitride 136 IV. Vanadium, Niobium and Tantalum Nitrides 4-1 Vanadium Nitride , 2k5 4.1.1 Nitridation of Vanadium .. 145 4.1.2 Hilling of Vanadium Nitride 145" 4.1.3 Oxidation of Vanadium Nitride 25-i 4.2 Niobium Nitride .. 136 4.2.1 Nitridation of Niobium >9o 4.2.2 lailing of Niobium Nitride . 157 4.2.3 Oxidation of Niobium Nitride .. .'.61 4-2.3(a) Comparison with oxidation of NiobinT", metal. IM 4.3 Tantaltim Nitride 170 4.3.1. Nitridation of Tantalum .. 170 4.3.2 Hilling of Tantalum Nitride 171 4.3.3 Oxidation of Tantalum Nitride .. 176 4.3.3(a) Comparison with oxidation of Tantalum Metal. 181 4.3.3(b)' *^xidation of Tantalum and its Nitride at higher temperatures 195 V. Chromium and Molybdenum Nitrides 5»1 Chromium Nitride ..' - -.* IS^ 5.1.1 Nitridation of Chromium -. l85 5.1.2 Milling of Chromium Nitride .. 187 5.1.3 Oxidation of Chromium Nitride 192 5.1.3(a) Comparison with Oxidation of Chromiun Metal. 194 (6) C 0 NbT E N T S Chapter Pa^ T. • 5.2 Molybdenum Nitride oo o. ^i'fJ9 502.1 Nitridation of Molybdenum 209 5.2.2 Mlling of Molybdenum Nitride ?lp 5.2o3 Oxidation of Molybdenum Nitride 217 5o2o3(a) Comparison with Oxidation of Molybdenum Metalo o. 222 VI. Concluding Summary ^o «• .o - ^ Zt6 REFERENCES ^ 230-24r APPENDICES 24^-25J (7) Chapter I INTRODUCTORY SURVEY AND REVIEV Nitrides are the nitrogen compounds formed generally at elevated temperatures when nitrogen reacts with other elements especially the more electropositive elements. Transition el^ents such as those of sub groups HA', "SAf and VIA of the Periodic Table, form nitrides which have high melting points and great hardness approaching that of diamond (tfhittemore, 1968).
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