HI ‘ MIMI” IN! I I MI]! W I f “1 THE fimmmuae aspammcz 3:: w FERRQMAGNEHC RESC iii-1N {.LE 2.! .‘3‘ ‘15 M“ \MDTH {N ELECTRQPLATED CGEAJ Mshefimbemaffivi.5. MlCHiGAR H.533 COLLEGE Davié Lymm Kéngsma €955 i HUIHIUIWHIHIIHHUIHHHHIlllllHIIIIHHHIIIIHII 1 3129301771 190 This is to certify that the thesis entitled 71-: Tmfu‘zu.‘ 77b/amcl-wa. /7X-. 0......“ / presented by has been accepted towards fulfillment 'of the requirements for AL degree in m E D. 5&2. a . Majo ' professor 0-169 THE TEMPERATURE DEFENDENCE OF THE FERRUMAGNETIC RESONANCE LINE WIDTH IN ELECTROPLATED COBALT by David Lyman Kingston A THESIS Submitted to the School of Graduate Studies of Michigan State College of Agriculture and Applied Science in partial fulfillment of the requirements for the degree of MASTER OF SCIENCE Department of Physics 1955 1:1:0'. ILE (3.3117223: The author wishes to extend his deepest gratitude to Dr. Robert D. 5301108 who directed this research. His ad- fl vice, helpful suggestions, end continue nteres t made the work very enjoyable. The author also wishes to thank Walter 6. Meyer who worked side by side with him for many months. “350 <3) £3 (a 7’“ Tim. FEFBOI-IAGITE‘T IC WIDT Submitted to the State Colleg in partial A 3roved *d ”5 0 mm 'DTT‘ID 'I T Y?“ Tfi—Z‘ 1" fi‘?”"‘ .L 1—13..“ LLB-51‘ DALI-L ELVDL‘IVAL on 1‘": ..~ ‘ [J .44.“. 4- in.“ FEES OI-TAITC E LII‘TE H IN E ECTROPLATED COBALT by David Lyman Kingston School of Graduate Studies of Hichigsn of Agriculture and Applied Science fulfillment of the requirements for the degree of PM? Did MASTER OF 80133 Department of Physics 1955 73% D s;vid L. Kin5ston Thesis Abstract This thesis reports a study of the temperature dependence of the ferroma5netic resonance line width in electroplated cobalt. At a frequency of 9300 megacycles per seconds, the resonance was found at fields between 400 and 500 gauss, depen in5 on the temperature. The resonance line width in electro- plated cob: lt is much broader than that found in electroplated nickel and considerably broader than that found in electroplat- *5 ed iron. The line width may be expressed in terms of a e ip- c an ~v-n [T1 '1 9 rocal relei tion time, l/T2° -he value of l/T is 31 X i0 1 2 9 seconds— at room temperature, decreases to 17 X 10 se econds-l at 300 de5rees centi rede and re ins ne early const: nt up to 600 de5rees centi5rade which was the hi5hest temperature at which data wel -e taken. This is to be constrasted with the behavior of electroplated nickel and for electroplated iron. - 9 -1 For nickel ,l/T2 is 3.1 x 10 seconds at room temperature and remains fairly constant up to 250 degrees centigrade. At this point it re. see very sharply and reaches a value of q -1 '9 ‘ ‘I § 5.9 x 109 seconds at 370 de5rees centi5rade wnicn is tne Curie tem erature for nickel. For electrOplated iron, l/T2, l C)- .. at room t mperature, is 15 x 10’ seconds . It decreases -l nearly line Hrl to 72109 seconds at 600 de5rees centigrade. TABLE OF CONTENTS I. INTRODUCTION II. THEORY A. FERROMAGNETIC RESONANCE ABSORPTION IN AN ISTROPIC MEDIUH I B. THEORX OF THE USE OF THE RESONANT CAVITY III. EXPERIMENTAL APPARATUS AND PROCEDURE A. MICROWAVE APPARATUS B. HEATING THE SAMPLE C. MAGNET D. PREPARATION OF SAMPLE IV. REDUCTION OF DATA V. RESULTS APPENDIX BIBILOGRAPHY CO Figure l. {‘0 Figure Figure 3 Figure 4. 5 Figure Ch Figure “I Figure Figure 8. Figure 9. LIST OF FIGURES Motion of the Magnetization Vector in Ferromagnetic Resonance Equivalent Circuit of Resonant Cavity Picture of Apparatus Block Dia5ram of Apparatus Cavity Assembly Magnet Calibration Method of Finding HO and H0 From the Experimental Curve R(H) Typical Resonance Curve for Electroplated Cobalt Temperature Dependence of l/T2 for ElectrOplated_Cobalt Page THE TEMPERATURE DEPENDENCE OF THE FERROMAGNETIC RESONANCE LINE WIDTH IN ELECTROPLATED COBALT I. INTRODUCTION Ferromagnetic resonance was discovered by Griffithsi in 1946. In his eXperiment a thin film of ferromagnetic material was placed on one end of a cylindrical microwave resonant cavity. An external magnetic field was applied parallel to the surface of the film. With a constant mi— crowave magnetic field of fixed frequency parallel to the film, but perpendicular to the applied field, it was found that a maximum power absorption occured for a parf ticular value of the external field. In l9u8 Kip and Arnold2 investigated the ferromagnetic resonance in an iron single crystal as a function of the orientation of the crystal in the applied field. The tem- perature dependence of the width was first examined by 3 who worked Vvith polycrystalline nickel and Bloembergen supermalloy. His work on the temperature dependence of the line width was extended by Healyh who studied ferro- magnetic resonance of nickel ferrite as a function of 5 temperature. In 1953 Spence and Cowen6 examined the temperature dependence of the resonance line width in single crystals of iron and nickel, and electrOplated iron and nickel. A ferromagnetic may be visualized as consisting of a great number of electron spin magnetic moments coupled to- gether by exchange forces to give a resultant magnetic moment. If the applied magnetic field and the r-f field have the correct magnitude and orientation, the ferromagnetic will absorb energy from the r-f field. Quantum mechanically the applied magnetic field splits the degenerate energy levels into a set of Zeeman levels designated by the magnetic quantum numbers ms. If the selection rule Zlnk==il is satisfied, the r-f field can induce transitions between these levels. Since the most papulated level is the lowest energy level the result is an absorption of energy from the r-f field. The absorption continues because the spins give up energy to the crystalline lattice tending to maintain an excess of electrons in the lower state. At.the present time it appears that a satisfactory the- oretical explanation of the temperature dependence of the line width has not been given. Bloembergen presented a means of representing the line width by using spinspin re- laxation times and spin-lattice relaxation times. Kittel 7 and Abrahams calculated the temperature dependence of the Spin-lattice relaxation. No calculation of the dependence of Spin-Spin relaxation times have been made. It is a com— mon belief that the Spin-Spin terms make the major contribut— ion to the line width. Kittel and Abrahams8 have suggested that at temperatures below one-half the Curie temperature the Spin-spin terms predominate, and above one-half the Curie temperature the spin-lattice terms predominate. II. THEORY A. FERROMAGNETIC RESONANCE ABSORPTION IN AN ISOTRUPIC MEDIUM A thin sheet of ferromagnetic material, lying in the xy plane, is subjected to a static magnetic field in the z direcxion and a r-f field in the x direction. The mag— netization will consist of a large constant component, M2 and a varying “X and My. The magnetization E and the total angular momentum 3 are related by =7" ’ (1) where )z, the magneto-mechanical ratio is _ 99 Warm-5, g is the spectroscopic splitting factor, e is the charge of the electron, m is the mass of electron, c is the velocity of light. The classical equations of motion are, d_Mxy=7[MXHeff]x _ MU. , (2a) xy T2 dM — .. M2. M0 ——2 = _. _— d' Y[MXHEff]Z TI (2b) In the case of an isotrOpic ferromagnetic material M X Heff is the total torque. Hei‘f is the effective field inside the material, and is given by neff =H ’Nx 2M+fionis+ ova-M. : ext y (3) where Nx is the demagnetization factor. The third term yz on the right of equation (3) is due to ferromagnetic anis- tropy. Since, in this case, the medium is isotrOpic (see appendix) this term will be dropped. The last term on the right is due to exchange interactions. The exchange effects9 will be small for pure metals such as cobalt in the temper- ature range in question. Since this term will have little effect on the effective field, it will be drOpped. The damping terms in equations (2) involve T1 and T2. T1 is the spin-lattice relaxation time, and T2 is the rel- axation time for all effects disturbing the epin system from within. T1 and T2 may depend on the frequency of the applied field and on the temperature. In general T1 and T2 are not equal. 3 Following Bloembergen we obtain expressions for the ferromagnetic frequency permeability and resonant frequency. A solution of equations (2) can be obtained by letting M =Mx e'wt . Combining equations (2), (3) and xy Y ext _ iw'r ext_ ext__ we get expressions for Mx’ My, and M2. In these calculations terms involving products such as MxMy, which are small (see figure 1) are dropped. Letting M3 3 M0, the last term of 5 FIGURE l MOTION OF THE MAGNETIZATION VECTOR IN FERROMAGNETIC RESONANCE 6 equation (2b) becomes zero. Hence Tl drops out of the final equations. Using the relation for the susceptibility, Il'L—|=ll'Ll—l—'/L2=C4’—HMX ' (5) where H1 is the r—f magnetic field, we get 47ry2Mo£rh+(Ny—N2)Mo](w§— mg) l 2 Z 2 4w?! , , (0)0 -a)) +- ’/EE (6) __ 47f] 2M0[Ho +( Ny- N ZIMO] Zea/T? ’U'Z- (w:— w 7) + 4071-2 ’ (7) where (u: , the resonant frequency is w: = y2[Ho + (Nx- NZ)M0] [Ho+ (Ny - NZ)MO]+% ' , 2 I8) T2 is the quantity to be evaluated in this experiment. B. THEORY OF THE USE OF THE RESONaNT CAVITY A microwave resonant Cavity is a dielectric filled re— gion completely surrounded by conduction walls, except for an iris which couples the cavity to the rest of the micro- wave system. The boundary conditions are satisfied by par- ticular configurations and frequencies of electromagnetic field solutions. These normal modes correspond to the res- onant frequencies of the cavity. In this experiment we are interested only in those which have linear dimensions of the cavity of the order of the wave length in the wave guide. For convenience, the cavity may be represented by an equivalent circuit made up of lumped elements. The cavity and coupling iris may be replaced by parallel resonant cir- cuit which is coupled to the transmission line by a trans- former (see figure 2) R nTV R ' :1J__ C I I FIGURE 2. EQUIVALENT CIRCUIT OF RESONANT CAVITY Zo (_— T v I It is assumed that the transmission line is terminated by its characteristic impedance Z0 and the line sees an effect- ive resistance R. The turns ratio of the transformer is n. It is assumed that no energy is lost in the transformer. With the Cavity at resonance, conservation of energy gives _\_/_2=n2V2 R R' (9) hence R'=n2R , and (I0) .- 2 20— n ZO The absorbed power is then 2 2 2 P =_v_=_<_!-I:_V_ri=Vu2<'+‘"), O R I? R . (ID where ,r', the voltage reflection coefficient, is _. VF F Vi (l2) At cavity resonance F=Jiii R+IZo ’ (I3) and £9: I—F , R |-+1" (I4) V2 2 V2 2 V2 V-2 pO-—|-R(I+T )..-Z—'O(I ELF} 20,8 ZOI", (I5) where P1 and Pr are the incident power and the reflected power. They are related to the absorbed power by a=P—e (I6) At resonance, the reflection coefficient I1 is real and may be positive or negative since R and 20 are real. l/n is a measure of the coupling between the guide and the cavity. In this experiment all the data was taken with an undercoupled cavity. Therefore only the case of the under- coupled cavity will be considered. For the undercoupled case, l/n is small compared to Zo/R', I. is negative and Vr is negative. Thus ,Vrnax :: Vi —vr ’ (I7) Vmin =Vi+vr The voltage standing wave ratio is ___Vmcm= Vi-Vr= I_P__Zp_ P me va+V. I+F R ' (IS) The Q of the cavity will now be defined and related ‘to quantities which can be measured, namely p, Irw , PT. The total Q is 10 energy stored in cavity :: 277' ' Q TOTOI energy lost per perIOd ('9) The total losses of the cavity are made up of the losses of the unloaded cavity and the external losses. These losses are prOportional to the reciprocals of the total Qt, unloaded Q,L1 and the external Q8, reSpectively. I I I = — + -— . Qt Q" Qe (20) The unloaded Qu is made up of all of the losses in the cavity proper, QC, the losses in the c0pper walls of the cavity and Qfer' losses in the ferromagnetic sample. The external Q6 is the energy lost by the cavity to the guide. Qfer . (2I) The Qfer' is due to the magnetic losses in the sample, and losses due to eddy current and dielectric losses. However, the magnetic losses in the sample are predominate. The fundamental quantity measured in a ferromagnetic re- sonance experiment is the ratio of the external Qe to the unloaded Qu. This is defined as a. =.___.'+T‘ Q" ’0 I-F' (22) .93- Qe(SB_ [[sz 0-)somple+( 17H 0mm . 0., (17qu d1, m of “my (23) ll where we ewe- Therefore we can express the ratio as to Qu as Qe '6} = A fl-tEB . (24) EXperimentally a quantity p, which is prOportional to reflected power, is measured. 2 p = CB ==CHW R (25) This equation assumes that the amplifier used is linear. Therefore I {1:9}, (I where a = w/cPi (I may be determined by measuring the standing wave ratio f) at one value of p. For the undercoupled case I + NW . I - NW (26) In the case of an overcoupled cavity f) is the same as above. . —I LF| 73777 ' (27) Then (28) 12 Hence Afi+s=p=l_|fl. (29) I “ DZ, (30) " 95 (am where A and B involve Q,c and Qu and are constants for a given cavity at a given temperature. Thus, a quantity pro- portional to the effective permeability can be obtained from measurments made on the cavity. 13 III. EXPERIMENTAL APPARATUS AND PROCEDURE A. MICROWAVE APPARATUS The apparatus is the conventional microwave apparatus as shown in the block diagram (Figure 4). The klystron is a 723AB low power oscillator operating at about 9000 mega- cycles per second. It is modulated with a 1000 cycles per second square wave which, along with necessary DC voltages, is isolated from the lOad by a flap attenuator. The klystron and attenuator are matched with a Hewlett-Packard E-H tuner to the H-arm of a magic T. The E-arm is matched with another E-H tuner. The output of the matched detector is read on a Browning TAA-l6 twin-tee tuned amplifier peaked to match the frequency of the square wave. The two side arm of the T feed the energy to a matched load coupled to one arm and through a standing wave detector to the resonant cavity, coupled to the other arm. Energy from the klystron is coup- led into the two side arms but not into the E-arm of the T. That portion of the energy which goes into the arm with the matched 10ad is completely absorbed. The portion which goes in to the arm with the cavity is reflected from the cavity and partially coupled into the E-arm. Only power that is re- flected from the cavity goes into the E-arm. This is the power that is measured by the detector, and the meter read- ing is pr0portional to this reflected power. The matching devices prevent any multiple reflections in any of the arms of the T. The overall matching of the system is to a volt- 1h FIGURE 3 APPARATUS m3knaa2m _ mmBOQ, mmijazq moeomemo l 823 I A II m>§> mdo COO. 02.024Hm < a . I _ I mosomemol $23 $23 EB: .2954 W 8:02.). A. :Im s :3”. 4 due“. aadxzoEm5¥ I _ a neon _ _e curve/us. l 6 age standing wave ratio of about 1.05 except in the arm con- taining the resonant cavity. In this arm, the standing wave ratio is determined by the type of cavity used. A mica win- dow was cemented in the guide to prevent leakage of the hy— drogen gas which was used as a reducing atmosphere. The mica introduced so little reflection that it was not necess- ary to match these reflections out. The resonant cavity used was three half wave lengths long. It was coupled to the guide with a symmetrically placed circular iris. An iris with a diameter less than 5/16 inch resulted in an undercoupled cavity. An undercoup- led cavity was used throughout the experiment.‘ The cavity was assembled with silver solder. Silver solder was used because of its high melting point. Oxidation was removed from inside the guide by polishing with a fine grade of carborundum and then washed with a 10% solution of nitric acid. The sample was plated on a brass disks(copper disks were also used). The disk was then silver soldered on the end of the cavity, thus completing the cavity. The preparation of the sample will be discussed later. 17 F LANGE—< I X-BAND ' WAVEGUIDE TI MICA WINDOW FLANGE 4 F T 3:34—H2 INLET 4—WATER INLET _[::I*—WATER OUTLET --— IRIS RE SONANT CAVITY L— / SAMPLE mfg.— H2 OUTLET DISK —- I:_l__m_ FIGURE 5 CAVITY ASSEMBLY l 8 B. HEATING THE SAMPLE The heating coil had resistance of approximately 9 ohms and was fabricated of .112 inch by .005 inch Nichrome ribbon wound on the cavity in a non-inductive manner. The coil was Operated on AC supplied by a Variac. The coil was wound on a layer of asbestos on the cavity and was held in place by a layer of baked potters clay. An insulating layer of glass wool was wrapped on the clay. This oven was cap- able of temperatures up to 800 degrees centigrade with a power input of 500 watts. The temperature was measured with a calibrated Chromel-Alumel thermocoupheinserted in disk on which the sample was plated. Thus making it possible to read the temperature at a point adjacent to the sample. The 5 thermocouple was checked by Cowen and was found to be accur- ate to 2 degrees centigrade from room temperature up through the range needed. The output of the thermocouple was read on a Leeds and Northrup type K potentiometer. The hydrogen gas in the cavity prevented oxidation of the sample at high temperatures. The gas entered above the cavity and paSsed out the bottom where it was burned. A water cooled section of the guide was placed above the cavity to prevent excessive heating of the rest of the microwave apparatus. 19 C. MAGNET The magnet was constructed on SAE 1020 low carbon steel in the form of a square box 22 inches by 22 inches by 9 inches. The sides of the box which are 3% inches thick were machined and bolted together with 2 inch bolts. The pole pieces are 7 inches in diameter. They were machined to slip fit holes bored in the box, and were threaded and held in place with retaining rings 1 inch thick. Because the ferromagnetic res- onance line is Very wide no special treatment of pole faces to insure a homogeneous field was undertaken. The copper wire used in the winding was .072 inches square formvar in- sulated wire which was wound on four cOpper bobbins. The bobbins were made of 3/16 inch thick capper sheet and were designed so that the finished spool was 15 inches in diameter and 1 3/A inches thick. Each coil had a resistance of approx- imately 5 ohms. The wire was insulated from the bobbin with a layer of .010 inch asbestos paper. After winding,the coils were dipped in formVar and wrapped in linen. The two coils on each pole were connected in series. The windings on one pole were connected on parallel with those on the other pole. The magnet was cooled with 6 water coils made of t inch square cOpper tubing. It was found that the magnet itself did not heat up to any great extent. However, the cooling was nece essary because of the high temperature to which the cavity was heated. The power source was a bank of 12 marine batter- ies with a 300 ampere hour capacity. The magnet was control- 20 led with a water cooled rheostat. The current was read on a Westinghouse Type PX—h ammeter to an accuracy of approx- imately 25 milliamperes in the range 0—5 amperes. Since the hysterysis of the magnet is approximately 65 gauss, care was taken in always taking readings with increasing current. The magnet was calibrated with a Sensitive Research Company model F. M. fluxmeter. D. PREPARATION OF SAMPLE The cobalt was plated on brass and copper disks. The disks measured 1 l/h inches in diameter by 1/8 inch thick. The disks were polished with various grades of emery paper. The final polish.was done with.Jewdu$ rouge until a near mirror finish was obtained. After polishing, the disks were thoroughly cleaned, first by washing with a detergent and then electrolytically in a Special cleaning solution. The cleaning solution consisted of 23 grams of sodium carbonate, 23 grams of sodium triphosphate, 15 grams of sodium hydroxide, and 8 grams sodium meta silicate dissolved in one liter of water. The sample to be cleaned was used as cathode. The current density used was of the order of 5 amperes per square inch. The disks were then plated in a solution containing cobalt sulphate, magnesium sulphate and ammonium sulphate. The current density used was .012 amperes per square inch. Oxidation at room temperature was unimportant with cobalt plates. For this reason it was possible to plate several 21 20_._.m30 woz._. mmmwdzd. l _ QM Oh 9N O.N . m._ O._ 1 a m6 m wmaoi OBBHOSBV HBMOd 3.2 N H ._..._ove (2) After substituting 2fl'7T I; ngo‘“ K,sIn29+Kzsin48)sIn8'd9'd8 = (Ek>ove. The coordinate axes can be picked such that 9 = 9' (3) 3H Hence ove= O (u) Therefore the average anisotropy energy in electroplated cobalt is zero. B5 ‘0 a) ‘0 0‘ Kn c- u: no I4 a, (3 CI <3 LI :n t: :z p BIBLIOGRAPHY . H. E. Griffiths, Nature lig, 670 (1946) F. Kip and R. D. Arnold, Phys. Rev. 21, 1556 (1949) Bloembergen, Phys. Rev. IQ, 572 (1950) W. Healy Jr., Phys. Rev. Qé, 1009 (1952) D. Spence and J. A. Cowen, 0. O. R. Report (195A) A. Cowen, Ph.D. Thesis, Michigan State College (1954) Kittel and E. Abrahams, Rev. of Mod. Phy. 35 233 (1953) Kittel and E. Abrahams, Phys. Rev. 20, 238 (1953) Kittel and C. Herring, Phys. Rev.‘zz, 725 (1950) 36 mm. 9n w HICHIGQN STQTE UNIV. LIBRQRIES Ill! 1 312930177 llll 1908