FERMI SURFACE STUDIES OF ALUMINUM AIND DILUTE ALUMINUM—MAGNESIUM ALLOYS USING THE MAGNETOTIIERMAL OSCILLATION. TECHNIQUE Thesis for the Degree of Ph. D. MICHIGAN STATE UNIVERSITY JOHN C. ABELE 196.8 1-H“ I‘: This is to certify that the thesis entitled FERMI SURFACE STUDIES OF ALUMINUM AND DILUTE ALUMINUM - MAGNESIUM ALLOYS USING THE MAGNETOTHERMAL OSCILLATION TECHNIQUE presented by John C. Abele has been accepted towards fulfillment of the requirements for PhoDo degree in PhYSiCS 6/ / fl/AH/ 0-169 ABSTRACT FERMI SURFACE STUDIES OF ALUMINUM AND DILUTE ALUMINUM-MAGNESIUM ALLOYS USING THE MAGNETOTHERMAL OSCILLATION TECHNIQUE by John C. Abele The third zone Fermi surface of aluminum and dilute aluminum - magnesium alloys has been measured using the magnetothermal oscillation (MTO) technique. Measure- ments for pure aluminum.are found to be in good agree- ment with the results of Gunnerson, Gordon, Bohm and Vol'skii. These results can all be interpreted on the basis of a pseudopotential model due to Ashcroft. For aluminum alloys with up to 0.4 at.% magnesium the extremal cross-sectional areas of the Fermi surface were found to decrease by as much as 10%. This effect can be accounted for by a simple rigid band valence model. The so-called Dingle temperatures, which represent the collision broadening of the Landau levels, have also been measured for the alloys. A comparison is made of the lifetimes calculated from the Dingle temperatures (via A.D. Brailsford's theory) with those obtained from the electrical resistivity. FERMI SURFACE STUDIES OF ALUMINUM AND DILUTE ALUMINUM-MAGNESIUM ALLOYS USING THE MAGNETOTHERMAL OSCILLATION TECHNIQUE BY John C. Abele A THESIS Submitted to Michigan State University in partial fulfillment of the requirements for the degree of DOCTOR OF PHILOSOPHY Department of Physics 1968 ACKNOWLEDGMENTS I am indebted to Professor Frank J. Blatt who provided both guidance and encouragement during the course of this research. Support from the National Science Foundation, the National Aeronautics and Space Administration, and the Michigan Institute of Science and Technology is also gratefully acknowledged. ii TABLE OF CONTENTS ACKNOWLEDGMENTS. . . . . . . . . . . . . . . . . LIST OF TABLES . . . . . . . . . . . . . . . . . . . LIST OF FIGURES . . . . . . . . . . . . . . . . . . LIST OF APPENDICES . . . . . . . . . . . . . . CHAPTER I CHAPTER II CHAPTER III INTRODUCTION TO FERMI SURFACE STUDIES. 1.1 Introduction . . . . . . . . . 1.2 The Worth of Fermi Surface Measurements . . . . . . . . 1.3 Experimental Fermi Surface Studies 1.4 Theoretical Methods for Determining the Fermi Surface. . 1.5 Comparison of Theory and EXperiment . . . . . . . . THE THEORY OF OSCILLATORY QUANTUM EFFECTS . . . . . . . . . . . . . . . 2.1 Introduction . . . . . . . . 2.2 History of Landau Diamagnetism . 2.3 Lifshitz - Onsager Theory. 2.4 The General Result . . . . . . THERMDDYNAMIC ANALYSIS OF THE MAGNETO- THERMAL EXPERIMENT . . . . . . . . . . 3.1 Introduction and Working Hypothesis. 3.2 Thermodynamic Calculation. . . iii Page 10 10 10 12 15 19 19 20 CHAPTER IV CHAPTER V CHAPTER VI CHAPTER VII CHAPTER VIII BIBLIOGRAPHY iv THE EXPERIMENTAL ARRANGEMENT USED TO STUDY MTO. . . . . . 4.1 Introduction. . . . . . . . 4.2 The Experimental Cryostat . . 4.3 The Measurements of Small Diff- erential Temperatures . . . . 4.4 Magnetic Field Measurement. . 4.5 Field Sweep Techniques. . . . . 4.6 Data Acquisition and Reduction. SAMPLE PREPARATION. . . . . . . . 5.1 Introduction. . . . . . . . . 5.2 Necessary Precautions ... . . . 5.3 Crystal Growth. . . . . . . . 5.4 Resultant Crystals. . . . . . THE FERMI SURFACE OF PURE ALUMINUM. 6.1 Introduction. . . . . . . 6.2 Existing Fermi Surface Models and Data . . . . . . . . . EXPERIMENTAL RESULTS FOR AL-MG ALLOY S O O O O O O O O O O O O O O 7.1 Introduction. . . . . . . 7.2 Changes in the Aluminum Fermi Surface Induced by Alloying . . 7.3 Amplitude Dependence. . 7.4 Amplitude Comparisons . . . . . GENERAL CONCLUSIONS . . . . Page 28 28 28 33 4O 41 47 58 58 58 59 65 69 69 69 75 75 76 81 94 98 102 LIST OF TABLES Table Page 5.1 . . . Sample Information . . . . . . . . . . 68 7.1 . . . Dingle Temperature Results . . . . . . 87 7.2 . . . Scattering Results . . . . . . . . . . 92 7.3 . . . Amplitude Comparison . . . . . . . . . 98 LIST OF FIGURES Figure 2.1 Landau Levels and the Fermi Surface. 3. 4. 4. 4. 4. 4. 4. 4. 4. 4. 4.10 4.11 4.12 5. 5. 5. 6. l 1 2 3 4 5 6 7 8 9 l 2 3 1 Thermodynamic System . . . . . . . . Vacuum System Rotatable Sample Holder. Temperature Dependence of Resistance of Carbon Resistors . . . . . . . . . Thermal Bridge and Associated Electronics. D.C. Equivalent Circuit. Single Amplifier Sweep Control . . Manual Integrator Sweep Control. . . . . Automated Sweep Control. Dependence of Ca upon Magnetic Field . Hyperbolic Dependence of MTO and deA Amplitudes upon T/H. . . . . . . . . Steady Field Rotational Techniques . Field Mbdulation Electronics . AluminumrMagnesium Phase Diagram . Magnesium Concentration after Single Pass Zone Refining . . . . . . Sample Mounting. . . . Nearly Free Electron Construction for Aluminum 0 O O O O O O O O O O O O 0 vi Page 14 19 29 32 35 37 39 42 42 44 50 52 55 57 61 64 66 71 vii Figure 6.2 6.3 7.1 7.2 7.3 7.4A 7.4B 7.5 7.6 7.7 7.8 7.9 A.l B.1 C.1 D.l E.1 F.1 Ashcroft's Model for the Third Zone Surface of Aluminum. . . . . . . . . . . . . . . . . Comparison of Data with Ashcroft' 3 Model in {110} Plane. . . . . . . . . . . . . Angular Variation of [S Orbit near (110) in {100} Plane . . . . . . . . . . . . Variation of [3 Orbit Area along (110) with Mg Concentration . . . . . . . Variation in [3 Orbit Area along<100) with 'Mg Concentration . . . . . . . . . . . . Angular Variation of 3‘ Orbits near (110) in the {110} Plane . . . . . . . . . . . . Variation in ‘6‘ Orbit Area along (110) with Mg Concentration . . . . . . . . . Angular Variation of X‘ Orbits in {100}P1ane . Amplitude Dependence in the {100} Plane. Dingle Plots along (110) . . . . . . . . . Results of Brailsford's Scattering Calcula- tion 0 O O O O O O O O C 0 Temperature Dependence of the MTO Amplitude. Extraneous Heating Effects . . . . . . . . Crush-Type Lead O-Ring Seal. Differential Thermal Bridge Schematic. Magneto-resistance Probe . . Harvey-Wells Electromagnet Field Characteristics. . . . Squaring Circuit for-% Sweep . Page 73 74 77 79 80 82 83 84 85 87 90 93 107 110 112 114 115 117 viii Figure G.1 Least Squares Program for Finding Frequencies. . . . . . . . . . . G.2 Least Squares Program for Finding Frequencies, cont. . . . . . . G.3 Least Squares Program for Finding Frequencies: Typical Output. . H.1 Filter Circuits. H.2 Example of Application of Narrow Band Filter using 1/H Sweep . . . . . . . H.3 Low Frequency Data . . . . . . . H.4 High Frequency Data . Page 119 120 121 122 123 124 125 LIST OF APPENDICES Appendix A Heat Input via the Rotating Gear Mechanism . B C Crush-Type Lead O-Ring Seals . Differential Thermal Bridge Schematic. ‘Magneto-resistance Probe . . . Harvey-Wells Electromagnet Field Character- istics . . . . . . . . . . . . . . . . . . 1 Squaring Circuit for‘fi Sweep . Least Squares Program for Finding Fre- quencies . . . . . . . . . . . Filter Circuits. ix Page 107 110 112 113 115 116 119 122 lllll‘wllll. CHAPTER I INTRODUCTION TO FERMI SURFACE STUDIES 1.1 Introduction Over the last ten years an enormous amount of effort by both experimental and theoretical solid state physicists has been directed toward the determination of the Fermi surface of a large number of metal and alloy systems. The purpose of this first chapter is to relate some of the reasons for such an extensive study of Fermi surfaces and to summarize the progress, both eXperimental and theo- retical, that has been made. As the nature of Fermi sur- face measurements is unraveled it will become apparent that the techniques have become diversified as well as sophisticated. This is to say that many various types of measurements utilizing different physical phenomena can be used to probe the Fermi surface. On the theoretical side there have been some new ideas but much of the work has been the adaptation of the earlier methods to high Speed computer calculations. 1;2_ The Worth of Fermi Surface Measurements The reSponse of metallic elements as well as many other solids to their environment depends in many interesting 1 2 cases on the nature of the electron distribution. One way to characterize the distribution is by plotting surfaces of constant energy in a wave number or‘k Space. Many of the important prOperties of the carriers can be related to such surfaces. at 1 (e.g. mc* =i—1rg-é , v =5(—3—%).... ) AS the temperature of a Fermi Dirac system is reduced, the low-lying energy states become filled up to some fixed energy Ef and higher energy states are unfilled. A well known butvery important preperty of such a system is that the usual excitations which result in the trans- port of energy are largely limited to those states whose energy is very near Ef. Thus the contours of energy in '3 Space having energy near Ef are of extreme importance to the understanding of electronic processes in solids. The physically interesting parameters such as mg, v, etc. previously mentioned are to be evaluated at Ef. This then is briefly the motivation for Studying the Fermi surface of metals. 1.3 Experimental Fermi Surface Studies There are many methods for determining Fermi surface parameters. Some of the methods currently in use will be briefly surveyed here and references to much more complete descriptions given. 3 First, there are the oscillatory effects due to the Landau diamagnetism. These effects fall roughly into two categories: those related to equilibrium phenomena and those which require some kind of additional excita- tion mechanism (e.g. electric field, thermal gradient, etc.) and are thus non-equilibrium phenomena. Examples of the first type are the deHaas-van Alphenlu7 and magnetothermal oscillationsa'lo. The deHaas-van Alphen measurement, which is perhaps the most common of all the Fermi surface measurements, has undergone quite a series of improvements from the old "point by point" susceptibility balance to the field modulation (i.e. derivative) technique of the present. Those included in the second category are oscillatory electrical resis- tivityll’12 (Shubnikov-deHaas effect), oscillatory thermal resistance, and oscillatory thermopower13’14. The frequency of the oscillations observed in all of these eXperiments is proportional to the extremal cross- sectional areas of Fermi surface in a plane perpendicular to the applied field H. From the temperature and field dependence of the amplitude of these oscillations one should be able to obtain information about the scattering of the carriers as well as their effective masses. The amplitude measurements are probably more difficult to 4 interpret in the nonequilibrium phenomena because the amplitude of the one set of oscillations is not indep- endent of other parts of the Fermi surface. Another important class of eXperimentS is the caliper type measurements using geometric resonances. Among them are the Gantmakher r.f. size effect16 and ultra- sonic attenuation17-20. Both of the experiments measure the caliper or extremal diameters of the Fermi surface in a plane perpendicular to the applied field H. Since r.f. size effect resonances are produced by the relation between the diameter of the carriers‘orbits and the width of the sample, the preparation of smooth plane samples is critical. It Should in principle be possible to deduce some information about the boundary Scattering using this eXperiment. Yet another important type of measurement is the cyclo- tron resonance eXperimentZI. This is a temporal resonance effect in.which conduction electrons pursuing helical paths under the influence of a magnetic field H applied parallel to the surface are intermittently brought into the skin depth of a metal where they are acted upon by the microwave electric field. A resonance can occur when the component of the microwave electric field in the plane of the surface undergoes an integral number of 5 cycles during the time it takes a carrier to make one orbit. This experiment gives the average value of the effective mass over the electron orbit. The last class of Fermi surface measurements to be mentioned is magnetoresistance22’23. At low fields it is difficult to separate Fermi surface anisotrOpies from relaxation time anisotrOpies. In the high field region the behavior of the magnetoresistance is largely dependent upon existence or non-existence of open orbits. Thus the method can be used as a t0pologica1 check of prOposed Fermi surfaces or to choose between alternative models. There are other techniques which can be used to shed light on the Fermi surface of a particular material but these are the ones most commonly being used. In addition to the relatively straight-forward eXper- iments on pure materials, one can try to alter either the band structure or the Fermi energy. The alterations are made in the nature of perturbations of the usual Fermi surface. One possible alteration is to introduce an impurity which can affect the scattering, the electron 24,25 concentration, or the lattice structure . Another way to manipulate the surface would be to apply hydro- 26,27 static pressure . One would hope that changes due 6 to such effects could be accounted for within the frame- work of the current theories, although sometimes this process is muddled because of the limited amount of knowledge available about the physical changes that accompany alloying. Much effort (both experimental and theoretical) has been focused on the problem of magnetic breakdown in 28-30. Magnetic breakdown can give the last few years information about the nature of the band gaps in various directions and is an interesting effect on its own but it has not been used as a general tool to probe the Fermi surface. 1.4 Theoretical Methods for Determining the Fermi Surface At present there exist several methods by which one may calculate the band structure and hence infer the Fermi surface for a given material. The applicability of a given method depends largely upon the type of electronic states the valence electrons occupy. The methods most commonly used are the tight binding method, the cellular method, the augmented plane wave (APW) method, the orthogonalized plane wave (OPW) method, the pseudopotential method and the Green's function method. The applications of these methods are described very briefly below and references to much more complete expositions are given. The tight binding method is best applied to core States and localized outer electrons such as one finds in the transition metals. The cellular method dates back to the work of E. P. Wigner and F. Seitz. The APW method is based upon the cellular method, which assumes a Spherical potential inside non-overlapping Spheres centered on each lattice point and a constant one outside the Sphere331’32. If there is directional bonding the simple APW method will provide unsatisfactory results. There are many materials whose energy bands can be classified as nearly free electron (NFE). Among these materials are the alkali and alkali-earth metals; the Simple polyvalent metals A1, Cd, Zn, Mg, etc., as well as semi-metals and semiconductors. For many of these materials a tolerably good approximation to the actual Fermi surface can be obtained by the one OPW or NFE 33 . . The accuracy 13 increased construction of Harrison when more OPW's are included, eSpecially near the zone boundaries. The pseudOpotential method is based on the OPW method, although it could be based on an APW-type calculation. The OPW method requires that electrons be classified as either core or itinerant electrons. Conse- quently for materials containing partially-filled d 8 bands the OPW or OPW-based pseudOpotantial cannot be expected to yield a good description. The Green's function method is, like the APW, based on the muffin- tin crystal potential model34. In the Green's function method the coefficients in the reciprocal lattice vector expansion are Specified and coefficients in the atomic orbital expansion are determined variationally, This is just the reverse of the APW method and is use- ful in that the secular equation is usually much smaller than in the APW method. The Similarity between these two methods has been eXplored by Ziman35. Relati- vistic corrections become important as the atomic number becomes greater than about 55 to 70. 1.5. Comparison of Theory and Experiment The Fermi surfaces for the simple metals have by this time been fairly well determined, both experi- mentally and theoretically. These are the metals whose outer shells contain only S and p type electrons and are thus amenable to OPW or OPW-based pseudopotential methods. Although these methods have a few variable parameters which are adjusted to fit the experimental data the agreement of the angular variation of the extremal cross-sectional areas is remarkable. The experimental results on the noble metals are 9 well accounted for by the APW calculations. The transition metals are of current interest. The problem of obtaining good samples is rapidly being overcome. The computer APW calculations (some relativ- istic) which can be easily adapted for different mater- ials are producing models which agree well with eXper- iment for both these elements and associated intermetallic compounds. The rare earths are still relatively unexplored because of their complicated metallurgy?6 In addition to completing measurements of Fermi sur- faces the next few years will witness the measurement of the parameters ’C and mi and their anisotrOpy over the Fermi surface. As will be shown later these quantities can be determined from Studies of the amplitude varia- tion with temperature and field using the techniques presently available. Such values are not averaged over pieces of Fermi surface but are averaged over only the extremal orbit causing the oscillations. The effect of impurities upon these quantities and upon the Fermi surface itself will also involve much study. CHAPTER II THE THEORY OF OSCILLATORY QUANTUM EFFECTS 2.1 Introduction In this chapter a short historical Sketch of Landau diamagnetism is given. This is followed by a brief derivation of the Onsager - Lifshitz relation and a presentation of the formal result of Lifshitz and Kosevitch for the oscillatory free energy. The exten- sions of this theory as well as some interesting side effects are presented. 2.2 History of Landau Diamagnetism The oscillatory effects which are periodic in recip- rocal applied field have a common historical origin. In Leiden in 1930 W. J. deHaas and P. M; van Alphen37’1 first observed the oscillatory behavior of the magnetic susceptibility of a Single crystal of bismuth. This effect, which bears their names and will hereafter be referred to as the deA effect, was at first thought to be a particular prOperty of bismuth. It had been shown by Bohr38 in 1911 that the diamagnetic susceptibility 39 in of a classical free electron gas is zero. Landau 1930 showed that Bohr's result is not valid when one 10 11 applies quantum mechanics to the motion of the electrons. By 1939 the early work of D. Shoenberg4O had shown that the deA effect could provide detailed information about the electron energy Spectrum near maxima or minima in the energy bands as well as the number in each part. In a supplement to this article Landau, using the effective mass approximation, enumerated the eigenvalues and eigenfunctions for electrons in a magnetic field which obey a quadratic diSpersion relation. Apart from the region around a band edge there is little justifica- tion for the use of a quadratic diSpersion relation. By the time that Onsager41 had related the 1/H per- iodicity of the deA oscillations to the extremal cross- sections of Fermi surface normal to the field direction, the effect had been seen in many materials: Bi, Sb, Mg, Hg, Cd, Zn, Be, C, Ga, In, Sn, T1, and Al. The central result of the Onsager relation is that even though the energy may be quantized in a complicated manner the orbital areas of the charge carriers in momentum Space can be quantized in a simple way. Shortly thereafter, IgM. Lifshitz and A.M. Kosevitch42 used the quasi- classical Bohr-Sommerfeld quantization condition to quantize the areas and obtained the grand canonical potential for charged quasi-particles obeying a general 12 diSpersion law 8 = 8 (kx, ky, kz). This result forms the basis of the presently accepted result. 2.3 Lifshitz - Onsager Theopy Consider the motion of a charged quasi-particle in the state k under the arbitrary diSpersion relation 5 = g (kx, ky, kz) (2.1) From the Lorentz equation, k ‘2 v x H 2 2 -— _ tic — -— ( ‘ ) it is easily seen that since changes in‘k are normal to §,the quasi-particle's k-Space trajectory remains in a plane normal to H. Since 3 is normal to surfaces 1 of constant energy ()5 = " VkE ) we see that the 'fi quasi-particle trajectory in k-Space is along the surface of constant energy in a plane normal to E. It follows from.Eqn. (2.2) that the projection of the real Space orbit has the same Shape as the k-Space orbit though it is scaled by the factor -EE and rotated by' Tf/Z. In a magnetic field the momentum is generalized to s. =fis+ A film It is convenient to direct the magnetic field along the z axis and use the vector potential ‘A = (0, Hx, 0). 13 In this case the Bohr-Sommerfeld quantization relation {2'3 becomes 12% feds so that the k-Space orbit along a line of constant (n +'r )h, n = 0,1,... , (n +II')h . energy encloses an area A normal to the field H and quantized by ZZTeH fie (n +79) , n=0,1,2,... (2.3) A(E, kz) = This is the Onsager result. Eqn. (2.3) can be inverted to yield E = gn(kz,H). As a simple example consider an ellipsoidal Fermi sur- face. Cylinders with the allowed cross-sectional area are Shown in Fig. (2.1)A. Fig. (2.1)B Shows that E is not a constant for a given Landau tube but varies with kz. At T=0 the occupied States are those with energy equal to or below the Fermi energy, but the quasiparticles are restricted to orbits with enclosed area given by Eqn. (2.3), the Onsager relation. Thus as H is increased the number of quasi-particles on the outermost cylinder with k < kf must decrease as its area 14 mommunm Heuom one pom mam>mq downed Aa.mv .wwm Lit 15 surpasses that of the Fermi Sphere. The degeneracy of the Landau tubes is very high and the density is pro- portional to the field H. The Fermi energy does depend upon the field but this is a second order effect and of little importance unless one is in a region where only a few quantum levels are left inside the Fermi surface (i.e. the quantum limit). In addition to substantiating these assertions the theory of Lifshitz and Kosevitch shows that by far the major contribution to the oscill- atory free energy comes from an extremum in the cross- sectional area of the Fermi surface. One would expect this Since in this region a large number of particles must simultaneously make the transition to lower levels. From Eqn. (2.3) we can infer the frequency of the oscillations. We will bring the j th level up to the Fermi level when H is such that h. AF c = j +\“ 21-reH The oscillations are thus periodic in l/H ‘with frequency Aphc 2fre 2.4 The General Result The result of Lifshitz and Kosevitch for the oscill- l6 atory part of the free energy is: lhc ___. - fl’ eH 3/ E - ZHTF '— ZWTCEE) C°S(6H Aext( F) + 4) F " 2 X osc IOZACEF’R ) [QB/2833111217 lkT hmbz l a kz2 ext - 1r]: Mr smc* “was 1: cos e (2.4) 2m where V = volume k = Boltzmann's constant T = absolute temperature in 0K L32A1EF,kz) % curvature of the Fermi surface I 3 k 2 = along the field direction 2 ext evaluated at the extremum m*= cyclotron effective mass = E 2.2.. 217' 36 Ef’ext eH wc*= —- m*C r'= phase constant, = 1/2 for quadratic diSper- sion relation g = Spectrosc0pic Spin Splitting factor [Ts lifetime of a state on the extremal cross- section of Fermi surface following Brails- 17 For Eqn. (2.4) to be valid it is sufficient that we*"“ EF: k'I‘(( EF, and f/H )> 1. The e-” 1 /u.) c*’E' term in Eqn. (2.4) accounts for collision broadening and was derived for lifetime independent of energy and kz, for particles having quadratic diSpersion relation by Dingle43. This cal- culation has Since been generalized by Williamson44 for an arbitrary diSpersion relation and by Brailsford45 for arbitrary Landau level line shape. The cos-Agifgfif term46, modified for arbitrary g 47 value , is due to the Spin of the particles. From this term we can see that when gmc*/mo = 1,3,5.... , the amplitude of the fundamental frequency will be zero. Since mc*/mo can be determined from the temperature dependence of the amplitude, anisotropic values of g can be determined. Several workers have noted departures from g = 2 of as much as 30% 48. The effective mass mc* used in the Lifshitz and Kosevitch calculation has been shown to be enhanced by the electron-phonon and electron-electron inter- actions49'51. A calculation of such an enhancement has been discussed by Harrison in the pseudopotential formalism” l8 Eqn. (2.4) does not take account of magnetic break- down effects since they are greatly dependent upon the band Structure of a given material. The result also does not include the additional harmonic dependence seen in the so-called B-H effect. This effect has been discussed at length by Pippardsz, Shoenberg53, and Condon54. CHAPTER III THERMODYNAMIC ANALYSIS OF THE MAGNETOTHERMAL EXPERIMENT 3.1 Introduction and Working Hyppthesis In this chapter the formal result of Lifshitz and Kosevitch for the oscillatory free energy is used to gain an expression for the oscillatory temperature of a Single crystal. The calculation is made for the simplified but practical system seen in Fig. (3.1). Thermodynamic System / ”7v 0 Bath ’ do 50m”'"°'b°" ‘7’” JM 0"" 4_+ rumor. (Md ~—>— eddy curnnt (thermal , beat. leak support hcatm puma”); hmP. =7; ‘9 W7. . ‘Ha'I Fig. (3.1) In this calculation the Specific heat of the carbon resistor mounted on the sample, together with that of the associated wire and graphite support, is added to the Specific heat of the sample. It is also assumed that 19 20 changes in the sample temperature are Small relative to the average sample temperature. Due to the power dissipation in the sample resistor and eddy current heating arising from changing the mag- netic field strength, the temperature of an adiabatically isolated sample will gradually increase without bound. A thermal contact or heat leak.with conductivity K and CHL K11 to maintain the average sample temperature constant. The exponential time constant ’tq = is thus necessary effect of this heat leak has also been included in the analysis. 3.2 Thermodynamic Calculation For a magnetic system the first law of thermo- dynamics dQ dU + aw becomes dQ dU + dw' - HdI (3.1) By analogy with the chemical system one replaces P by ~H, and V by I. Considering U = U(H,T) and I = I(U,T) we have _ 19. 112 (ill - OH)T dH '1" 3T)H (1T 21 and d1 = '3‘ng d'I‘ +%__)T dH (3.2) For this system the ”energy equation” bu _ 31’ 537M” ‘ T 3T)V " becomes _ 3H )T - -T '55)]: + H Multiplying both Sides by'4§%)T we have 93 3;; 3H 3: H31 31".1‘ 3H)T T T)I BH>T+ HaH)T (3’3) Applying Bx L bz = _ TY>z n'xa x'r 1 to the first term on the right Side of (3.3) we have 311 T 113—156°“ Upon substitution of Eqns. (3.2) into (3.1) we find, - .= LU - a1 22 - aI dQ aw [3T)HH 5T>H:IdT + [3H)T H SENT] dH (3.5) From the modified energy equation, Eqn. (3.4), the second term on the right side of Eqn. (3.5) is obviously 22 ...?Jl 3.! CP - 3T)P + P 3T>P so that in this system ECU b1 CH = T)H ' H'ST)H With these definitions Eqn. (3.5) becomes .. . _ 21. where dQ is positive for heat flow into the System dW' is positive for work done by the System dW' has been reserved for joule heating of the carbon re- Sistors, eddy current heating due to sweeping the field or mechanical vibration of the sample relative to the field as indicated in Fig. (3.1). The sources of the temperature difference between the sample and the bath T - TB are the dissipative effects dW' and the Landau S diamagnetism. Now the rate at which heat flows between the bath and the sample is 99.. ° _ - =- = 41's 21 d3 £W__'.(3.6) where ,K = % , and AT = TS'TB In order to continue this calculation one needs an expression for €%%)H . Using I = % jLEM , Eqn. (2.4) is rewritten in the form, -b X l D 2m’f ———-1 H FOSC . VA,m3/2 “3‘ H + I! ) e (3.7) sinh b1 T/H where ‘ °' 1 F...= 2 Fosc =| 3/2 gm" 2K(h-ea) coal mo A‘ = 32A 35 3/2 Z ext 8‘ = 1.47x105 gauss/OK fl = -21r£r ; Tr/4 XD =n/zrr K1: fic f1 = l—é—Aexth) = If Thus .1 _. _1 )F _ - .1. 3ngc _ 1 Iosc — V‘Tfigfic )T " V 3H )T — Iosc 1. 1 2m: “2331 1" = _A Tlfl' [H3/2COSC-_Lj1 + Y1) e 08C ' 3 sinh bflT/H This result may be simplified since for all cases discussed 21rf here ‘71—'37) bIT/H and EXJH' Thus in taking deriva~ tives the slowly changing exponential can be ignored relative to the trigonometric terms. 24 Thus 277’f ..b X /H I. ATzwf SinLH£+VQ)e1D 03° — - l H sinh bLT/H so that I BI S -A221Tf£ . 21Tf _b X 3T0 C)H=_T—H2 S1n('—fi”¢'+fil ) e .9 D/H x ( l-b’pT/H coth byT/H ) (3.8) sinh be/H Thus Eqn. (3.6) becomes 1 _ dAT 3108c 5111 dW' where it is assumed that TB = constant, so dt dt dt To solve Eqn. (3.9) in the general case is a diff- icult problem, but fortunately one can make some well- justified simplifying assumptions. The magnitude of the oscillations is a few millidegrees at most, and a heat leak is used to insure the equilibrium value. Thus AT/TS << 1 so that TS IV To, a constant. The separation in field between adjacent peaks at the fundamental ( fl = 1) frequency is at most 5% of the field, so since the dominant terms in Eqn. (3.8) change very Slightly 25 over a few cycles of oscillations, Eqn. (3.9) is solved with the parameter evaluated at some arbitrary field HO. One can make the following explicit assump- tions for the oscillatory temperature evaluated at mean temperature T and mean field H0. 0 HO-+¢K t :13 ll CH = constant K 3 LA = constant L awl '5;- = -P, a constant and not necessarily zero since we will use this later to calibrate the heat leak Zng H + 71 is eXpanded as 21rf (——1— + ——J~ (1-%—+ 3.10 “6 (with error ((‘é—E) 2) Ho 26 where YI=Y-_2_1T._f.l and w gglr—f-L— l 1 H ’ 1 H2 0 Thus Eqn. (3.9) can be written as <1A1?_dw' co 0 I CH—dt+1°AT=dt - E B181n(btit- fl) (3.11) 13/ where 2 B = ("”511 2c )3/ <2osflzqrrmo * 431E, 1 __9__z_ 2A 3/2 H035 1 3K2 '54 l-bgTQ/HO coth bLTO/HO ) and the other symbols have their previous definitions. The general solution of Eqn. (3.11) is ‘ 00 AT 2+c-1€Ht+1EV-1r§——B = e — x 10 CHI, (Cfi)+%2 . l . C 00 8111((031: -Y’ - tan 1 "Hi—A) Thus the final expression for the oscillatory temper- ature dependence (including addenda due to thermal leaks) of a single crystal upon the magnetic field expanded about T = TO and H = H0 is, TS'TB = AT =AT 27 3/2 E 3/2 +ATp= -_2_KBTQH0 ( he ) OSC 2 I b A(gF,KZ) % CH I F K22 ext 00 21113 - 21ft ' sin[——L “2771» -T- W -tan 1( ...—.9. H I Tosc ) cos(11rgm3) 2 3 2 2mo 13' V1 + (Tosc/ZWIQ ) fl / -b X 44H 1-b,*1~0/H0 coth bgTO/HO P "E:- e - -- ) +"+Ce 9‘ (3.12) where KB = Boltzmann's constant ’hc f2 = I? Aext(EF) Z‘N'ZK *c 5 1%" b2 = BmQ 1 = 1.469x10 fig" gauss/OK eh tosc = period of oscillations ’UQ = CHL/KA = thermal time constant XD = Dingle temperature = ’h/Z TrKB’l' Z = lifetime of State on extremal cross-section of Fermi surface ATosc = oscillatory temperature change due to the Landau diamagnetism ATP = temperature change of the sample due to dissipative heating effects X CHAPTER IV THE EXPERIMENTAL ARRANGEMENT USED TO STUDY MTO 4.1 Introduction In this chapter the design and operation of the low temperature cryostat used in the present MTO Studies is presented and discussed. The techniques necessary for the measurement of small differential temperatures are given. Various methods of data acquisition and the subsequent data reduction techniques for each method are also discussed. The chapter closes with a discuss- ion of some new methods that were tried and suggests further improvements. 4.2 The Experimental Cryostat There were actually two cryostats designed and built for this Study. The second design includes all of the features found in the original cryostat; hence only it will be discussed in any detail. A schematic of this cryostat and pumping facilities is shown in Fig. (4.1). 4 bath type. A large The cryostat is a single He mechanical pump, pumping on this bath, provides temp- eratures down to 1.1°K. The pressure is regulated by 28 29 to mov to back line try cartcsmn mamstat Pump ":9 -, i a I 3.?" rc gauge ' - I ll . 90m ? e S: F % Walker mmostac 29"“, deg/or meshangz , a”? as}? #— * fin _ 00! 00’ and ’9 WP manqmws . wad. 14006 PUMP Pg“ raga bunsan, «macho» or v23. 9° ,‘ f I A Sample chombcr Fig. (4.1) Vacuum System 30 either a Walker-type condom manostat or a cartesian manostat. The bath pressure is measured by conventional methods using either mercury or oil manometers except for the lowest temperatures where it is determined using a Universal Todd type MCLeod gauge. The pressure in this pumping line can also be conveniently read on a U.S. f 30 inch vacuum gauge and at low pressures monitored by a thermocouple gauge. In order to observe the MTO effect it is necessary to have the sample thermally isolated. The degree of isolation necessary depends on the time period of the oscillations. In most cases this requires that the pressure as read on the ionization gauge in the sample vacuum line be < 5x10'4mm Hg. Since fluctuations in this pressure would greatly influence amplitude measure- ments and are difficult to control, the sample chamber was evacuated to pressures of ( 10'5 mm Hg. A water- cooled oil diffusion pump provided this pressure, which was monitored by a Veeco ionization gauge. The water- cooled pump was chosen Since an air-cooled model was found to introduce vibrations in the cryostat via their common supports. The second apparatus has a rotatable sample holder. This holder is rotatable about two mutually perpen- 31 dicular axes and is pictured in Fig. (4.2). Because it is difficult, if not impossible, to make a rotary vacuum seal which works reliably at He temper- atures, the control rods pass up through the sample chamber vacuum line to a pair of rotary Veeco seals at room temperature. The control rods are made of 3/16 inch diameter Stainless steel tubes having a wall thick- ness of 0.016 inches. Even so, enough heat passed down them to make the sample holder heat up to about 100K in about a two hour period while the bath remained at 4.2°K. The problem was really that these rods passed directly from room temperature to the sample holder which.was fairly well isolated from the bath. This was overcome by wrapping a bare #22 Cu wire several times around each rod and bolting it to the brass O-ring flange. In addition, an approximately 8 inch section of Glastic rod is used in place of the stainless tubing near the room temperature flange because it has a much lower thermal conductivity near room temperature. Because turning the gears in the rotating device produces frictional heating effects (calculation in Appendix A), it was also necessary to solder a pillbox 3 of about 5 cm capacity onto the bottom of the sample holder. This is filled through a curled lflb inch dia- thermal Sinking lead 0- ring fl' seal Samp/Cb vac uum —-’ Chamber term nal board d spiral 9¢or set helium bath 1‘s ‘ tailor) bush/n s and kupqcrs Siam/ass Cont rol rods m (a chamber /— sa p vacuum can tqflon bushings \\ and keep 2r: /— detachable lo war umt ,—— worm gear -— pinion gear b¢v¢l g¢ar liamd /— [ml/um [bi/lb“ lead o-rmg scal Fig. (4.2) Rotatable Sample Holder pi. 33 meter stainless steel tube from the helium bath. Near the lower end of this tube a brass flange and lead 0- ring arrangement was used to maintain the sample chamber vacuum. The general type of O-ring seal used throughout these apparati was suggested by M. Garber and is briefly discussed in Appendix B. The electrical leads for the carbon resistors and other additional probes were twisted in pairs, encased in teflon Spaghetti, and routed down the sample vacuum line. The leads used are #36 Manganin wire with a nearly temperature independent resistance of about 31 {I/foot. These leads, eight in number, are connected to a terminal board a few inches above the sample, facilitating easy changing of carbon resistors, etc. 4.3 The Measurements of Small Differential Temperatures To study the MTO effect one needs a technique which is able to measure differential temperatures of about lO'SOK relative to a background temperature of 1°K to 40K. In order not to damp the oscillations, such a sensor must also have a heat capacity which is small relative to that of the sample. A differential thermal bridge utilizing ordinary carbon resistors which satisfies both these criterion is described below. 34 The use of carbon resistors as thermal sensors has become quite common Since their introduction around 1950. The temperature dependence of their resistance is usually fairly well represented by the equations p dR B' A/T logeR ='T + B and '5; = :2 (4.1) Thus as the temperature is reduced the resistance as well as dR/dT increases quite markedly. Plots obtained for the various resistors used in this study are shown in Fig. (4.3). The choosing of resistors for use in a given temperature range will be discussed after the bridge circuit and its sensitivity considerations have been presented. The resistors to be used are modified in the follow- ing fashion. A large number of resistors are glued to a flat metal block and lapped on fine emery paper. After this is done to both sides of the resistors the metal leads are cut back as far as possible and twisted pairs of #31 Manganin wire are soldered to each resis- tor. Since two resistors are used in the differential technique it is worthwhile to attempt some matching procedure. In principle one should match the resistors for thermal and magneto-resistance characteristics; however, a simple matching of room temperature resis- 35 30,0000 10m § 4000' Re SIS tance (cums) 300. l I l l .2 .4- .6' .8 [.0 Reciprocal Tcmpcraturc ( °K” ) Fig. (4.3) Temperature Dependence of Resistance of Carbon Resistors 36 tances after grinding has proved satisfactory. Electri- cal insulation between the resistor and sample is provided by first gluing a small piece of cigarette paper to the sample and then gluing the resistor to this paper. The glue used is G.E. 7031 varnish. The resistors are placed so that they both have the same orientation ' relative to the magnetic field. After several (5-10) thermal cyclings between 4.2°K and room temperature the resistors tend to become noisy and are replaced. This is probably due to mechanical strains in the resistors as well as degradation of the glue bonds. In addition to having greater thermal conductivity than most glues the G.E. 7031 withstands thermal cycling far better than the more quick-drying varieties such as Duco Cement. A block diagram of the electronics associated with the differential thermal bridge is Shown in Fig. (4.4). The differential bridge with lock-in detection is essentially the same as the method developed by Garber and LePageSS. The a.c. method is used to reduce the effect of thermal emf's in the leads as well as enabling lock-in detection to be used. The low operating frequency (20 to 60 Hz) of the bridge is chosen so that the capacitive off-balance remains small and can either be balanced out in the bridge or neglected. The lock- 37 {attenuator [-— calibration rtsnwons J:_2, I nfc rmcz l‘ j‘ cryostat mfcmcc samp It low mm. IVI'afifla output lock-In “PM" I J 41 (NU/(JOIN! and L— post -d¢t¢c£I0fl . 5 “VP -chart Anglo - {Hans recorder mum field Fig. (4.4) Thermal Bridge and Associated Electronics 38 in detection scheme reduces both the electrical pickup and the effects of the sample vibrating in the magnetic field. Lock-in detection at the fundamental bridge frequency 00 eliminates the IZR self-heating effects of the carbon resistors since these occur at 2a). A complete schematic of the bridge circuit itself is given in Appendix C. The simple d.c. equivalent circuit Shown in Fig. (4.5) can be analyzed to yield the voltage across the detector input due to a small resistive change A.. The result is Vdetector = A 85/) [(2+} /R) r+}>][r+R+A] + AR However in practice A((r,f) ,R, so that Ydetector 1; A8 P (4'2) [(2+ P/R)r+fl [1+9] From Eqn. (4.1) A T Thus Eqn. (4.2) yields ==£Llsplrctr iv— detector T2 E2+P /R) r+})][r+lg EELJ) Rr dT T2 Er+R)}) +2rlgE+lg Hence the voltage output of the detector is propor- (4.3) 39 detector Fig. (4.5) D.C. Equivalent Circuit 40 tional to the temperature change of the sample. To determine the absolute temperature changes one must calibrate both the sample resistor to determine A and the electronics using the Simple Stepping calibration resistor which takes the place of A in Eqn. (4.2). The power dissipation in the sample resistor is typically around 10"11 watts. For the 33I1, 1/8 watt resistors at 1.2°K a temperature change of l/HOK correSponds to a voltage input to the detector (with 50K input impedance) of .005/1V. This figure represents the practical lower limit of observation. 4.4 ‘Mggnetic Field Measurement The accuracy with which one can determine the frequency of the MTO oscillations and hence the cross- sectional areas of the Fermi surface ultimately depends upon the measurement of the magnetic field. The mag- netic field was measured by three methods in these Studies. Initially a rotating coil gaussmeter (Rawson model 720) calibrated with an NMR probe was used. A magneto-resistance probe (American AeroSpace Controls, Inc. model MRA-ll) was also calibrated with the idea of using it in a high field solenoid. The resistance of the probe was found to be quite dependent on its orientation relative to the field. While this is not ‘ I I II 41 desirable for field calibration work it could be used for accurate orientation in a magnetic field. The effects of thermal cycling and temperature dependence in the l0 to 4°K range were less than .3%. A direct reading calibration circuit was designed for use with this probe and is presented together with the trans- verse calibration curve in Appendix D. A digital hall probe gaussmeter (F.W. Bell Inc. model 660) was also used. The error of this device when used with the NMR factory calibration curve was reputed to be less than .22 . The output of either of these devices was recorded concurrently with the thermal oscillations on either a 2 pen Varian or a 3 pen Texas Instruments (Servo/riterII) strip chart recorder. 4.5 Field Sweep Techniques During the course of these measurements a very useful adaptation of the sweep unit originally designed by J. LePage was made56. The LePage circuit shown in Fig. (4.6) is based on the fact that the Harvey-Wells electromagnet control will produce a current through the magnet preportional to an applied reference voltage. Since the H(I) curve for the iron electromagnet is not linear (Appendix E) one cannot simply make I=constant 42 ./ F’fi f .1” magnet to magnd} :rcfcrma power sum/y Fig. (4.6) Single Amplifier Sweep Control magnet 1'" "”9”“ “'1 reference power supply Fig. (4.7) Manual Integrator Sweep Control 43 to get a linear field sweep. In the LePage circuit dfi /dt was compared with a constant voltage and the error signal used as a reference for the magnet control. In order to make a very linear device with one amplifier stage it was necessary to use very high gain () 104) for which the circuit would oscillate. In order to eliminate this problem the output of an operational integrator was also added to the magnet reference as shown in Fig. (4.7). The voltage which was integrated could be varied manually in such a manner as to keep the output of the error amplifier minimized. This sweep unit was automated by Simply using a part of the error Signal to drive the integrator. One then has a quick reSponding error amplifier and a longer time constant electronic servo-integrator operating together in a closed loop. Since the loop is closed the accuracy of the control does not depend upon the linearity of the integrator and its rate of integration can be adjusted to minimize the output of the error amplifier. A modified sweep unit utilizing these principles has recently been constructed. A simplified schematic of this revised circuit is shown in Fig. (4.8). 44 Volta} 3171711)“ Val! Samwtr’ ' L/’ l for : for 7' 6 1fi“f§ : l/‘IS V «P5997 6 coast Va% '0’”\ 1r / a I “I L.\, '5 / \ 6‘7 I / __ may/m t ( 02339:: V “fiance and is magnet) _ Power supply Fig. (4.8) Automated Sweep Control 45 The versatility of this sweep control becomes apparent when one considers the possibility of non- linear sweep modes. The voltage reference with which dyi/dt (or H) is compared by the error amplifier clearly determines the sweep mode. For example, if Vref=CH, then (CH-bH) is minimized so dH/H =N3/b)dt, which results in a sweep which is exponential in time. In studying oscillatory effects which are periodic in l/H (i.e. sin 21rf/H) it would be very useful to have l/H proportional to time. Since the time separation of two adjacent oscill- ations is (n+1) - (n) = f/H1 - f/H2 =(f/H1H2)(H2-H1) thus H2 - H1 = AH = Hle/f or AH”H2/f Thus for a sweep rate H the time between successive peaks will be _ '= 2 ’ ’L'OSC - AH/H H /fH . (4.4) So for time periodic oscillations we set HZ/fH = A (a constant) Thus for the above sweep control the reference with - 2 which H must be compared is simply proportional to H . Time-based l/H sweeps have been described in the 46 literaturezo’57 . The conditions necessary for their operation can be obtained from Eqn. (4.4). dH/H2 = dt/f tosc so that l/H = -t/f EOSC + C or H = f tosc/ [(f tosc/H0)'€I ° But since tosc = HOZ/HOf 9 HQZHO (Ho'fiot)2 where H0 = H)t=0' _ 2 ' ° _ H — HO / (HO-Hot) or H — Thus direct or differential comparison of the field with a time-based reference requires adjustment of the initial sweep rate HO relative to H0. For this reason the time-based sweep, whether mechanically or electron- ically driven, is inherently more difficult to adjust initially for the l/H characteristic. In the differen- tial H method described above the time between oscill- ations can be changed in the middle of the sweep by merely adjusting the amount of H2 reference voltage which the error amplifier compares with H. It should be noted that this technique is not limited to electromagnets but is in fact more directly 47 applied to superconducting solenoids. The field in a solenoid is very nearly prOportional to the current I. The voltage drop across a superconducting solenoid, being almost entirely inductive, is LI which is propor- tional to H - the correct pickup for the differential l/H sweep. The reference with which to compare this can be obtained by squaring the current I. In practice the magnetic field is sampled by the rotating coil gaussmeter and this signal is then squared. The squaring circuit first takes the log of H, then multiplies by 2, and then takes the antilog. As the accuracy of the log and antilog functions are crucial, a series of about thirty transitors were tested to determine which ones had the best logarithmic prOperties. Appendix F contains the relevant circuits and notes on operation. More accurate squaring and logarithmic devices with greater voltage range can be obtained from the George A. Philbrick Co.58. Their units are heartily recommended for the construction of future sweep units. 4.6 Data Acqpisition and Reduction In this section the various conditions under which data is recorded are considered. Data analysis techni- ques are discussed concurrently with each method. 48 Additional methods that were tried as well as suggest- ions for modifications are also presented. To obtain the frequency of a set of oscillations periodic in 11H (i.e.a(sin 2fl'f/H) is in principle a simple task. One merely plots peak numbers versus 1/H and determines the frequency from the SlOpe. A linear least squares program to do this has been.written and is listed in Appendix G. A typical output complete with statistical parameters, errors for each peak and a 95% confidence interval for the period is also given there. The error intervals are to a large degree in- dependent of linear errors in the magnetic field calibration and really reflect only the statistical uncertainty in locating oscillation maxima (or minima). To seperate out simultaneously occurring frequencies, use can be made of the high pass filter characteristic which the thermal leak introduces. (1//\/1+(tosc/21rtQ)2) Examples of data taken using this technique are Shown in Appendix H in Fig. (H.3) and Fig. (H.4). Two filters designed to be used with the l/H sweep unit are also shown in Appendix H with an example of data output. For the more dilute alloys the amplitude of the axis along the X-ray beam axis using a convenient goniometer arrangement and a{100}face Sparkplaned with the crystal still mounted in the goniometer. The samples were then glued by this{100}plane to an accurately machined graphite holder. (Fig. (5.3)) Using this method it was possible to estimate the initial sample orientation to within about 2 degrees about one axis and to within 4 degrees about a perpendicular one. Samples prepared in the above fashion were weighed and their residual resistivity ratios (RRR) measured 66 {act of Samp/c spark - planed J, (100) ('9') rotation plane ,2) oral/cl {ace 9 Fig. (5.3) Sample Mounting 67 between 4.20K and room temperature. These data as well as the physical dimensions of the samples are given in Table (5.1). Using the data of B. Serin6O for the contribution to the resistivity due to impurity scattering as a function of magnesium concentration, one arrives at the calculated values of magnesium concentration as listed in the final column of Table (5.1). This cal- culation assumes that the low temperature resistivity is due to impurity scattering. The correlation between the impurity concentration before mixing and that calculated from the resistivity ratio is reassuring. Table (5.1) Sample Information sample at.% Mg before Residual Resis-* at.% Mg number zone refining tance Ratio(RRR) from RRR l .13 108 .08 2 .40 22 .39 7 .22 66 .13 pure Al 6-9's oriented single crystal These samples including the pure Al sample were roughly in the form of cubes; the masses ranged from .3 to .5 grams. * RRR = J03oooK 4,0 4.20K CHAPTER VI THE FERMI SURFACE OF PURE ALUMINUM 6.1 Introduction One of the reasons for undertaking a dilute alloy study in aluminum is that the Fermi surface has been relatively well established by a wide variety of tech- niques. In this chapter the agreement between the experimental data and various theoretical calculations is discussed and a presentation of the relevant data obtained in this study is also made. 6.2 Existing Fermi Surface Models and Data The early work of Heine61 (1957) showed that the valence wave function in aluminum is well represented by a single orthogonalized plane wave (OPW) except near the Brillouin zone boundary. A nearly free electron (NFE) construction in which the contours of constant energy are Spherical was first used by A. V. Gold62 to interpret his deA data in lead. In a magnetic field the effect of the lattice is to reflect the orbiting charge carriers at the Bragg reflection planes and to thus separate the carriers of one zone from those of another. By translating the correSponding 69 70 pieces of each zone back into the central zone Gold was able to form the Fermi surfaces corresponding to carriers of a given zone. The remarkable thing is that this naive model was able to explain the lead deA results. This reduced zone remapping procedure is eSpecially tedious in three dimensions. In 1959 63 greatly Simplified the method when W. A. Harrison he realized that instead of considering only one Sphere and the Bragg reflection planes, the same reduced surfaces could be obtained directly from the inter- section of Fermi Spheres centered on each lattice point. Thus since Heine's work had shown that aluminum is a good NFE metal it was selected by Harrison for the first trial of the method. The Harrison construct- ion, Fig. (6.l), was quite successful in interpreting Gunnerson's preliminary results64 for the third zone surface. More recently (1963) Ashcroft65 has used an OPW pseudo-potential with coefficients adjusted to fit the third zone results of Gunnerson and also those of Gordon66. Although Ashcroft's ”final model" confirms the Harrison construction in general, it predicts a different connectivity near the W point of the zone. This is, of course, where one would expect the one OPW calculation to fail. The Ashcroft model showing the -o‘“‘~o'2' A: 0x ‘3‘ ‘~-*.o'. \‘ I x : \K I, I ‘ l t ‘ w o - L l, 3 I o I )\ : ' I, “ U I r. \ * L- ”’ \‘\ ‘0‘ x ' ' : T‘ 4, ‘r' I . ‘\‘ I, ' 1‘ ‘. I ) ‘ \ I I o‘ \ I ’I \ Y I, ‘ I \‘ : ’ \s g ‘0 / s~*” Ist ZONE-FULL 0”-~~ H.2: 0r ::J\ ’ ~?o‘ “ I ‘\ ’Iol "\ I . .W I | l. 7, U K. r I ”19;; w ' I- V‘. l ‘ I x ' ’fl I ‘ " I . \ 1’ l \ I \‘ ’1 \ ‘ ’ I, \“ ‘ ’I’ \\ : ’/ --- i ." ‘QL"' 3td ZONE-REGIONS 0F EL'NS Fig. 71 --- .. --- —‘ ’ f s. ” 20d ZONE-POCKET OF HOLES 1"“~~ 0“." I T s I u \‘ I, ' ‘ ,‘ w I s I ' ‘ I ' ' l D l ' I*\ ' I V ’I \‘ 3 . ’I O s‘ C t.“ I, L ¢ ') I “-< y”’ ' ' \ I . ‘, Q I I l ‘ ’ G ‘ I, a, ‘\ or \ I I ‘ I I . v ,r \ I ’ \‘ . ” 0 ~‘+”’ 4th ZONE-POCKET?) OF EL'NS X (6.1) Nearly Free Electron Construction for Aluminum 72 dismemberment of the third zone ”monster” into “rings of four” is shown in Fig. (6.2). The Ashcroft model which agrees quantitatively with Gordon's data is shown in Fig. (6.3). The pure aluminum data taken in the present study is also shown. These measurements are not intended to repre- sent a Fermi surface determination but instead, a check of the experimental method being used. The an- 67 as well as omalous skin effect results of Vol'skii the ultrasonic attenuation measurements of Kamm and Bohm68 are in good agreement with this model. The existence of the /3 orbits is not consistent with Harrison's model but is predicted by Ashcroft's, thus confirming the latter model. 73 0( ORBIT \ IRBFT 2! (man Fig. (6.2) Ashcroft's M del for the Third Zone Surface of Aluminum 74 90‘ H «I {no} gal —— Asbcrofb model . Present study ‘6‘ of." 2 {$21 35 u C o H. I I I l I I 1 I on) m. 20‘ ad 40‘ séznlbw 70° arm!» Fig. (6.3) Comparison of Data with Ashcroft's Model in {110} Plane CHAPTER VII EXPERIMENTAL RESULTS FOR AL-MG ALLOYS 7.1 Introduction Experimental data has been taken with the intention of analyzing it to determine the shape and size changes of the Fermi surface caused by alloying. One might expect the effects to be small for dilute alloys with solute concentration less than l/2 at.% . It is found, however, that changes in extremal cross-sections in the small third zone electron surface of Al can be as large as 10%. The amplitude of the oscillations has also been studied as a function of temperature, field, and angle. From these measurements one can determine Dingle scattering factors. When the magnetic field is rotated away from a symmetry direction the analysis becomes more difficult due to the larger number of frequencies present. This difficulty is eSpecially apparent for the more concen- trated alloys where the amplitude of the signal_has been greatly reduced via the Dingle factor. Throughout the following discussion the oscillations 7S 76 are divided into high (8‘) and low (M andfi) frequency groups as indicated in Fig. (6.2). Rotation angles from (110) in a {100} or a {110} plane are denoted by 6 and ¢ reSpectively. 7.2 Changes in the Aluminum Fermi Surface Induced by Alloying The angular variation of the /3 orbit near4 in a {106} plane has been studied for pure Al and three alloys. The results are shown in Fig. (7.1). A system- atic decrease in extremal cross-sectional area with increasing Mg concentration is apparent. The theoretical prediction for the angular variation of frequency in a {100} plane shows four frequencies converging toward a common value at . Because these branches could not be resolved near in the most concentrated sample it is difficult to put much emphasis on changes in the structure of the angular variation curves. Since the cross-sections of the third zone electron surface are decreasing as di-valent Mg replaces tri- valent Al, one is tempted to try interpreting these changes in terms of a rigid valence band model. By analogy with the NFE Harrison construction, changing the electron concentration scales the radius of the Fermi Sphere. Since the third zone surface is formed by an 78 overlap of such Spheres it should be quite sensitive to changes in kF' Consider a simple model which assumes that the Fermi surface cross-sections scale quadratically with the amount that the Fermi ”radius" overlaps the zone boundary. Thus along (llO) A 2 A 2 'Xo = (kF‘kw> and '50 = (kF-kK) l/3 where kF o( Z . This model has been used successfully by Gordon et al66 to interpret their Al-Zn alloy data. In Fig. (7.2) the <110>I30rbit data for Al-Mg is presented. The solid line correSponds to the above-mentioned calculation. This simple model agrees with the present data to within the eXperimental error although it is not applicable to all alloy systems.* A similiar plot is shown in Fig. (7.3) for the .08 at.% alloy along (led). The amplitude of the high frequency oscillations is only about 20% of that of the low frequency, and consequently their analysis presented difficulty. The only simplifying fact is that since the nearly cylin- drical ”arms” lie along (11d) there is very little * Higgins and Marcus30 found that in Zn alloys changes in the axial c/a ratio were at least equally as important as the valence effect described above. 79 cowumuucoocoo w: 953 AOHHV macaw woman. uwnuo m.\ mo cowumwum> 3.3 .wfim Ao\o .90» 22 not. «to 230 m3 2‘. Mn. 0...... us. on. m... 2. .3. o I b p L p p a 3" 02:0 IV 'und fa % Aozv : I .8 8O cofimuucoocoo wz £9.26 AOOHV macaw mound. v0 CH nonhuman”; 3.3 .wfim A0}. "5% tosvoxutuucou ms .2. 2. Mo. 0 p b .2. .1 0‘ m as 9’40 [V and fa % 0‘ Q 0 \ «92V 2 l 81 beating of these X oscillations when the field is within 200 of this axis. The frequency of these oscill- ations near (110) in a {110} plane for pure Al and the two most dilute alloys is shown in Fig. (7.4)A. In steady field rotations in a {100} plane the oscillations come principally from the low frequency 3‘ oscillations. The variation of the ‘8 frequency with magnesium concentration along (110) is shown in Fig. (7.4)B. This frequency correSponds to the extremal cross- sectional area when the magnetic field is aligned with the axis of arms. Steady field rotation plots, described in Section (4.6), were obtained for the two lowest concentration alloys. For the .08 at.% alloy it was possible to obtain good data throughout the {106} plane. In the .13 at.% alloy the signal was smaller and its interpretation was difficult for 69 greater than about 15°. Plots of these frequencies versus 9 are compared with the pure Al data in Fig. (7.5). 7.3 Amplitude Dependence As the field is rotated away from the amplitude of both the high andlow frequencies decreases. Rough measurements of this decrease were made for all of the samples studied and are shown in Fig. (7.6). As the 82 .No. .o I .N oNN a 00W .2 02 0 h - o * . or A02V 1N ¢\Q\ \c e\c\ oo\ oolll «2% S I o\o emu \ .\| on Wigwam? o :m Eo\o.pom\. d o s? 93¢. . \ an». .3 ( 950/ x j 5 902 néuj 83 3 69 one + % ofpure 4/ arm [/~2.9x/a‘) 9 >3 :2 2 a? 3 ._§—. o .64 .68 .I'2 .I's .25 .2;- .258 352 M5 concmtratzon (at.%) Fig. (7.4)B Variation in 3‘ Orbit Area along (110) with Mg Concentration 84 434 42‘ 83 I S "'2“ C) C) a“, u. ‘3 u 9‘ 3: eylmdcr Frequcncy (I056) C» ‘1'}: 33- I0 /o 32 ./o . [I L Ashcroftémodcl 3’ ° (Pun Al) l OL' .Oaat.% My 30; 29. f..“"\—.13 at. 0/0 m] .O (no) 5" 15' 1'5“ 56' 23' 50‘ 55‘ $0“ 4? (I00) Fig. (7.5) Angular Variation of 3‘ Orbits in {100} Plane 8S Amplitudo (Orbifrary units ) o O —' Fig. (7.6) Amplitude Dependence in the {100} Plane upper: High Frequency 3‘ Orbits lower: Low frequency o( and f3 Orbits 86 angular dependence of the amplitude is due to aniso- tropies in g, m*, t and I4, it could not be simply accounted for. In principle the effect of each of these parameters could be sorted out, though this would be a very difficult series of experiments to perform. Field plots to obtain the Dingle temperatures as described in Section (4.6) were made for both the f3 and '3‘ oscillations near (110). For some of the samples the Dingle temperature was determined at a series of temperatures between 1 and 20K. Examples of the Dingle plots for high and low frequencies are shown in Fig. (7.7) The beating of the 3‘ oscillations by the higher amplitude /3 ones is manifest in Fig. (7.7)A. The effect of the 2:1 beating of the /3 by the o( oscillations is apparent in Fig. (7.7)B. Since in both cases the oscillations were followed over several cycles of the beat pattern this should have little effect upon the value of XD, which was measured. The results of the Dingle temperature measurements are shown in Table (7.1). The measured Dingle temperature can be related to the lifetime ’6 via XI, = h/anBt. (7.1) The €7as determined from Eqn. (7.1) is really very Specific. It is the lifetime of a state correSponding 87 —’*-- Q‘. . f"1 5' >5” 3‘ '3; 4B 530 5'2 5'4 .51 5Y8 " )fi (:6 G") ~§ 1: *2 30. E q 20‘ l_...l :3” (0+ 84 fl 34 Z. 5 is 9 I 8 5 4! 06‘6") Fig. (7.7) Dingle Plots along (110) upper: High Frequency 3‘ Oscillations lower: Low Frequency Oscillations 88 Table (7.1) Dingle Temperature Results approximate frequency of temperature alloy oscillations and * for measure- sample orientation XD(°K) ment(°K) #1 .08 at.% Mg sxlo5c 2.88 2.03 (llQ) 2.62 1.73 2.91 1.49 2.80 1.41 2.22 1.24 3x106G 2.69 1.46 (110) #2 5 .39 at.% Mg 5x10 C 4.65 1.21 (110) #7 5 .13 at.% Mg 5x10 C 2.30 1.89 (119) 2.37 1.72 2.6 1.60 2.5 1.45 3x106 3.2 1.89 (110) 3.1 1.72 3.8 1.61 4.2 1.42 * using m*/m = .118 for the 5x105G (110) osc. and .130 for the 3x106G’l(110> osc. 89 to an extremal orbit at the Fermi energy. Thus the 3’ as measured gives very Specific information about the scattering from one part of the Fermi surface. We can also calculate TI}; from the electrical resistivity/D . Z); = m/nezf (7.2) This is of course not the same C as has been measured. '9) of Eqn. (7.2) is the "average” lifetime of all the conduction electrons. It is composed not only of third zone states but also those states of the large second zone. The masses of these zones are reSpectively ~0.12 andAIl.3 free electron masses. Thus in consid- ering an "average” m to use in Eqn. (7.2) it is probably not a bad approximation to use m = m the free electron 0, mass. Having measured the .PBOOOK /f4.2°K resistance ratio it is then a simple matter to calculate 8'} . 4 In the above-mentioned paper Brailsford calculated 7" Z‘ £p(9)(1-cose)sin9 d9 _._._.__. 71’ ' de 3}) f0 (9)81n9 P(e) is the probability of scattering through an angle 9 . Considering a simple shielded coulomb potential -qor e W— I' he obtained the result of Fig. (7.8). The results of these calculations are compared with 90 j o I' 2 ?o/2 kF"—" .m- Fig. (7.8) Results of Brailsford's Scattering Calculation 91 the experimental values in Table (7.2). The increase of ”CI/1?}, for high alloy concentrations shows that a more SOphisticated scattering theory is probably necessary.* By comparing the amplitude of the oscillations in a given field range at several temperatures we can study the temperature dependence of the amplitude. After correcting for the simple temperature dependence of the amplitude (i.e. T/ CHfiJ1+E;%g%§)2 ) we would expect from Section (4.6) that AT -bXD osc a< 1-bT/H coth bT/H ( 8 —1T—-) H3/2 (7.3) amp sinh bT7H Thus for fixed field we would expect the temper- ature to vary as l-bT/H coth bT/H sinh bT/H A family of constant field curves showing this temperature dependence of the amplitude is shown in Fig. (7.9) for the .08 at.% Mg sample. As we go suc- cessively to curves of higher field we would expect (from Eqn. (7.1)) the temperature of the maximum to increase proportionally. This behavior is seen in i If 57$}: 4 .7 (the Thomas-Fermi value) then the 1% Al-Zn deA results of Gordon must have their amplitude at 17 KG reduced by a factor of «ae'lz relative to pure A1. 92 Table (7.2) Scattering Results (110) ‘approximate fre uency XD 333 1%; ‘gy at.%Mg (10 G) (0K) (10 sec) RR (10 sec) ’L} .08 5 2.8 4.3 106 7.4 .58 30 2.7 4.5 7.4 .61 .13 S 2.5 4.8 66 4.6 1.07 30 3.7 3.3 4.6 .72 .39 5 4.7 2.6 22 1.53 1.44 93 — theoretical ..... expmmcntol _____....--o 20.9 as ’ "O' ’ 6’ (e-bn )f/a/Z Smh bk, .( /- bhicothbp” \3JkG o-- - "' - - -o “.3“. ~ ‘ was“. amp/I t udc k \ I I I 5 I O T I I I I j r U j u n I: 1.4 I": I. 6 n l.8 L9 2.0 7'1 Tcmpcrot on C 0K ) Fig. (7.9) Temperature Dependence of the MTO Amplitude 94 Fig. (7.9) although the maxima appear sharper than one would expect from the theory. Since the temperature of the amplitude maximum for a given field curve depends only upon the effective mass and fundamental constants we can obtain a value of mfi/m from each curve. m*/m determined in this fashion varies from .104 to .121 with a mean of .113 . This value compares very favorably with m*/m :: .118 calculated by Gordon66 from the temperature dependence of the amplitudes (from deA data). 7.4 Amplitude Comparisons From the theoretical expression for the MTO effect we can calculate the absolute amplitude of the fund- amental oscillation, -bXD 3/2 3/2 +_ ATosc = ZKBTOHo (e/hc) e (1-1r—coth'fi— (7.4) 32A 35 4’ 1+(Z' /2wZ’ )Zsin H ext CH osc Q ha— akzz We make the initial assumptions: CH is mainly electronic (i.e.“XT, 987. isin A1 at 10K), 1711-?- coth 131-1: bT is in the constant region and Sinh-EF therefore g .31, tosc e: ZIrCQ so 1/’\/1+(toso/27TZ’Q)2 2,71 95 Thus -bx 3/2 D H "H -14 AT = ‘3 2.21x10 0K osc TP/A 32A 32 bkzz ext where H is in gauss Xis in ergs/mole deg2 fis the mass density in gm/cm3 A is the atomic weight (e.g.l” 27 for A1) For Al using m*/m = .118 and H = 17KG, 3 62xlo-40K e"XD ATOSC_ . a 2A 32' (7.5) 2 3k2 ext To evaluate the denominator in Eqn. (7.5) we can use the angular variation of frequency data. Consider a piece of Fermi surface having cylindrical symmetry about some axis determined by the magnetic field. The radius of an orbit tipped at an angle 9 with reSpect to this axis is expanded as r = r0(1 +049 2) . The area A(e )ext= 7Tr02(1 + «92) (7.6) At a distance rsina along kz from the extremal orbit at €3= 0 A = 7T(rcosg)2¢.' 1-92 + 2 0(62 It then follows that 96 a 1 a -/\]41rla<- 7| (7.7) IH Since for a cylinder X = 2 we have A<9>7A we can calculate a(- i g .097. Thus from Eqn. (7.7) 2 b A %’\/---417'(. 097)= l. 10 at; For these orbits there are two equivalent pieces of Fermi surface per Brillioun zone and thus 2(3.62x10'40K)e’XD " 1.10 xfilm The corresponding measured amplitude for pure Al was ..XD ATosc = 6.6x10'40K e 6.5 if 1 x10'40K. The [3 and 0( orbits arise from regions of the Fermi surface near the junction of the arms. Since these pieces do not lie alongl<110> it is difficult to evaluate the Shape factor 32A 36 Bkzz We would expect 97 1 92M; kzz [35 to be greater for these sections than for a Sphere where 1 1 IDZA/Ibkzz [a = afihr' = '4 We thus find for the 5x105 G frequency along<<110) a» 1.75x10“3°x . 04,3 The correSponding measured amplitude is 4.35x10’30K. ATOSC We can also compare the relative amplitudes of the alloys as determined from their measured Dingle temperatures. This comparison, made at fixed temper- ature and field, is shown in Table (7.3). 98 Table (7.3) Amplitude Comparison <110> Dingle ratio of approximate factor amplitude frequency measured XD amplitude to pure A1 at.%Mg (105G) A TOSCPK) (OK) reduction amplitude pure 5 4.35x10'3 0 l l 30 .65x10'3 0 1 1 -4 2 .1 .1. .08 5 3.65x10 .8 17 13 30 .4x10”4 2.7 l- -l 2 1 l 6 .13 5 4.6x10'4 2.5 .l .1 1 2 9 .5 - 1 1 30 1.5 10 5 3.7 —- ‘— x 64 (I5 -4 l .1. .39 5 1.2x10 4.65 105 36 CHAPTER VIII GENERAL CONCLUSIONS These measurements of the third zone Fermi sur- face of pure aluminum and dilute aluminum-magnesium alloys show that the extremal cross-sectional areas along (110) and (100) decrease as the concentration of magnesium is increased. The electron nature of this surface is thus verified. A simple free electron perturbation of the model proposed by Ashcroft can be used to explain these changes. In particular the cross-sectional areas correSponding to a frequency of about 5x105G where a fairly substantial decrease in area is observed (~10%) fit the model quite well. (Fig. (7.2)) The higher frequency ‘3 oscillations appear to be more dependent upon the alloying than would be expected from the model. Uncertainties in the high frequency pure aluminum frequencies of about 2% could account for most of this discrepancy. The MTO technique has been used to study the variation in both the amplitude and frequency as the magnetic field is rotated relative to the crystal. Although the amplitude variation is difficult to 99 lOO interpret it was possible to measure the angular variation of the ‘8’orbit very thoroughly. The variation of the amplitude of the oscillations with both temperature and magnetic field was also studied. The different hyperbolic dependence of the MTO and deA oscillations enables one to determine the effective mass more directly with the deA measure- ment. A technique which enables the MTO effect to be used to measure Dingle temperatures has been deve10ped. This technique takes advantage of the relatively small dependence of the MTO amplitude upon the hyperbolic T/H term. Dingle temperatures determined using this method agree qualitatively with those obtained from the electrical resistivity. The effective mass measured along <110> for the low frequency (5x105G) was found to be m*/m = .113 f .008 , in agreement with the value measured by Gordon of .118. The absolute amplitude,which could be calculated quite accurately for the X oscillations, was found to agree with the measured value to within the experimental error of about 15%. A crude amplitude calculation for the low fre- quency oscillations also agreed with experiment. 101 The latter comparison cannot be considered a rigorous test of the theory because of the difficulty involved in evaluating the shape factor for this part of the Fermi surface. The absolute amplitude of the alloys was found to Scale approximately as expected from the Dingle factor. The actual reduction in amplitude was in all cases less than would be expected from the Dingle theory. Effective Dingle temperatures determined from the scaling of the amplitudes of the alloys relative to pure A1 are 10 to 20% less that the actual Dingle temperatures measured for each alloy. 10. 11. 12. 13. 14. BIBLIOGRAPHY W. J. deHaas and P. MI. van Alphen, Leiden Comm. 208d, 212a (1930), 220d (1933). J.H. Condon and J.A. Marcus, Phys. Rev. 134, A446 (1964). D. Shoenberg and P.J. Stiles, Proc. Roy. Soc. 281A, 62 (1964); Phys. Letters 4, 274 (1963). D. Shoenberg, Phil. Trans. Roy. Soc. (London) A255, 85 (1962). L.R. Windmiller and M.G. Priestly, Solid State Comm. _3_, 199 (1965). R.W. Stark, The Simon Fraser University Lectures on Solid State Physics I, edited by J.F. Cochran, R.R. Haering (Gordon and Breach, New York, 1968). A. Goldstein, S.J. Williamson, and S. Foner, Rev. Sci. 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I'll- APPENDIX A Heat Input via the Rotating Gear Mechanism The heat input to the sample holder via the rotating gear mechanism is the result of two different effects: heat conducted down the control rods and frictional heating during the turning of the gears. Because the sample holder is located in a vacuum chamber and ther- mally isolated from.the helium bath these heating effects are particularly troublesome. The situation is shown in Fig. (A.l). mmdml Gountcr ' tampcraturt control rod —\ .oté” wall, 15¢.”dm. 5.5. tub/n] W [:_ .2241 L flange. W . «b l.:cn;::f}76wym: rt in“ F‘s-010'?“ "View. ,-— ~5on mm VOCUUW7 49 Ms: sample Mr 64:»? 15 344ch JK— samplc. can Rig. (A.l) Extraneous Heating Effects ‘ 107 108 For each of the control rods Operating between 3000K and 40K the heat flow per second is about 2.5x10"2 watts. If we consider a c0pper wire thermal leak of length L, cross-sectional area A and conductivity K the temperature rise is about P L L AT 2 w— 3 5x10'3 X cm°1< RA To turn the control rods requires a torque of about 1 inch-ounce or 7x10"3 newton-meters. Thus for one complete revolution of these shafts, correSponding to 2 joules a few degree change in the gears, about 4x10- of work must be done. If this energy all goes into frictional heating of the gears during a period of 15 seconds the temperature rise will be, PL 2 L A. _ ~ " — 0 where K ~ .5 joules/cm sec OK . The time constant for returning to the equilibrium temperature is C L L =‘EX‘ 2.2x10‘3‘K sec-cm Since the length L is about 30 cm and a reasonable A is about 1x10"2 cmz (i.e. #17 wire), L/A is about 3x103 cm'l, giving AT ~'15°K. It became obvious in 109 early experiments that another type of heat leak was necessary. A helium pillbox was soldered to the bottom of the sample holder thus reducing L to about 2 cm. Since glastic rod has a much lower thermal conductivity 1 ) a 100 30 cm section of this was incorporated in the higher than stainless steel at room temperature ( temperature regions of each control rod. The control rods were brought in thermal contact with the bath at the helium flange by wrapping copper wire around each and attaching this wire to the flange. With these mod- ifications the conduction heating effect is less than 10'30K as measured using the carbon resistors with either M100 microns of helium exchange gas in the sample can or a good vacuum. The thermal time constant from rotating the gears is about 1 sec. . APPENDIX B Crush-Type Lead O-Ring Seals This particular type of lead seal was introduced to our laboratory by M. Garber. A possible seal is shown in Fig. (B.l). [and (.0014 Fig. (B.l) A lead wire of diameter ~ .02 inches is greased lightly with Apiezon M 1ubricant,wrapped around the flange and twisted tightly. When the flanges are clamped together a simple but very reliable vacuum seal is formed. When these seals were used in the present 110 111 apparatus no failures were encountered even upon re- peated thermal cycling between 1 and 3000K. APPEND IX C owumEmsom mwcwum HmEuw£H ammucwpmmmwa AH.UV .t.4~h ...: ‘74". L.‘ .54.: ...: #..1u¢8~.!~ $14.26 0-5 ...v 1n u ...: 1:. ...: ‘I on. :98 1t~..« (yo~..u 422. .3 ‘:~ .-~ 5“ “5 out (.0: . .u (Raf-C ‘Xflae a $3.»! a! t tun 9?. .5. Q “35% .‘ k... .8. .J. m. 831% 422.3 34.} v? n. J A- 1.: _ P: -- tilt- 7 1.1!. am- _.J D L .v D}! P 5" ’9} ..1 wlalm- L2‘ in“ i“ ..uhl *‘k‘2-:u A...“ V 2...... .. ..w Kat: ..J .Q‘v ..~ . :35 a!» 2(15 “\K...» ...w «2...! 1...... ...: .....e an .... ..83 ..u n x h. .8 u). "a. ..2 .8... 9 .8... “\\.8v ...u .68. ....u wKKo-on ..C t.‘ 33 ...u I... I l touF .vtn.‘ g “a.“ b‘\\ ‘m 30 h I o : C .— 9 ® @ -® ® .39: >1}: .qotm \o . u ‘“\u ..W C {m 2: L29 ..1 a ...-J .1 t . . . . .1. t ® tn. @ ’50 {Stncrk 41.1.. . ....I\~ \QQKU I?!“ . 3e Ly!“ .9.» as: ”2 ..v ,. ... a some 53%. $1 il‘. 4 m g ... z .53....» it... ...: ..t 3...... .. an .3... .v e a . 4.x... 3 h 4.4!. LCOIl‘ ‘.sC-za.b‘ >c1yat .“tm . ..oL ...(J . hm wi‘... ..U r . “we... \K‘a . -9 C .. ~. .452: \thu A": in m tk‘ Gd .0 S aw 3...: ...?- ..,.\ s :1 u ..w .3 s o! I . II ..III «tofgw e “ifbg‘hfi. d -.I~L.ham g 10 .1 r v B a" 1 H II. o A m H 4 S W 1.34 O r O m a a -" filoc T . 1 a .1 t e r e f f .1 D .J- -32.-.- .. 1+ l L»- in. it.» 1:4. {.0 [w v: _ .- _ u- — o- J JA J on « 4 4 1 > 1,51 é... Q‘s ‘QQQ\F 112 APPENDIX D Magneto-resistance Probe The magneto-resistance probe which was referred to in Sec. (4.4) was examined as a means of monitoring the magnetic field. Since it is useful to have contin- uous measure of the field available a simple power supply to accomplish this was built. This circuit is shown in Fig. (D.1)A. The current through the probe varies by up to 2% when the resistance of the probe changes from 100:1 to SKSl. This is unimportant however, since the magneto-resistance is not linear anyway. Once a cal- ibration has been made the circuit can be re-zeroed by maintaining the voltage across the 4.7K resistor constant. The drift in this voltage is only a few parts in 104 during an 8 hour period. The bias circuit is used to buck out thermal voltages which also amount to a few parts in 104 for the magnetic fields of interest. A calibration of this probe is shown in Fig. (D.l}B. 113 114 ? N 9 Magnetic Field (*6) 3: I2- 3. 4, 0 u T v u u 0' I 2 £3 4‘ 5' Resistance. (RA) Fig. (D.l) Magneto-resistance Probe upper: Power Supply Circuit lower: Magnetic Field Calibration APPENDIX E Harvey-Wells Electromagnet Field Characteristics “1 w '8‘ cut Flt/d E- ? 3 may: ‘3 3 ob ioddoa'ooiommmmaio Current (amps) ‘2’". 2t6k6—\ w car/bl who '2' K—I£u:6 30‘ % o 0 -3 .s :75 Lb L's i0 5.2: Out on¢¢ mm C Onttr {IO/J (In/ms) Fig. (E.l) Harvey-Wells Electromagnet Field Characteristics upper: Field versus Current Relationship lower: Field Profile Perpendicular to Field Axis and Equidistant from.Pole Faces 115 APPENDIX F l Squaring Circuit for-E Sweep 1 For the magnetic sweep control to maintain g o( t 2 is necessary. A circuit which an external reference 0( H provides arbitrary powers between about 1 and 5 of an input voltage over three decades of output is described. This circuit is shown in Fig. (F.1). Approximately thirty transistors were checked to determine their logarithmic properties. For the present studies the field reference was obtained from a rotating coil gaussmeter*. Because the reference voltage for the sweep must be floating it is necessary to keep from grounding the tip of the gauss- meter on magnet pole faces or connecting the power common of the amplifiers and their power supply to any fixed grounds (e.g. racks or chassis). For the transistors currently employed in the 1 l .( t sweep circuit an error of less than 1/2% in‘fi H was measured for sweeps between 9 and 22 KG. The cir- cuit parameters were initially adjusted as follows: i) using the meter mode switch all amplifiers 9: Rawson-Lush model 720 116 @695 m How 35936 woaumovm 3.5 .mfim .quM “Q S\$\.§K 8&6 H Vuhtsogm rug??? \okzuoxuko xxo uum KG. 523! A...» - in . - as V5.95 meuowu 6 +2me s as ... a 3.3.5 .2 u... Bari who: save! 1 62 <: z>¢ V: con 0 «to 7 v0 n OKUN 92 ~ «an .O 0n. 2. £35 as 93m .> u$\ 0 lb.‘ <8 H A533.» ..h h n... x n o emote; 2m x. yams Z _ 8.959% 118 are zeroed and returned to their "Operate” positions (a zeroing error of .lv correSponds to 100 nanoamps ) ii) with the adder off, the multiplier output is set to 2.370 v output for 1.000 v input using the calibration source and the mult- iplier potentiometer(s) iii) with the calibration source off the adder is adjusted so that the multiplier output reads -.190v The amount of H2 signal being supplied to the error amplifier of the sweep control determines the-% sweep rate. Thus for a given set of deA oscillations with frequency f their time period can be set by adjusting the input attenuator potentiometer of the sweep control. The experimentally determined relation connecting these quantities is: tosdsec) = 3°86X107 gauss Sec f (gauss) N where N is the potentiometer setting (0 +10). APPENDIX G Least Squares Program for Finding Frequencies PR3GRAY LIMFIT . ‘TTIST snag LIN QFGRESS ' PERIOD’HNCERT'IS‘§§“fi7E”CT DIMPW3IO\ A(80)o8(80\oH(3) ‘8 PEA) 1300.KMAK,(H(J) J= 1 3) 1000 FOQ4AT(110 3A8) H PRIJT 1001. (H(J).J=1a3) 1001 F0914T(1H1 20X, 5A8) ,- _,,1,Lweiiii, 1111, _ —_WU_1170 J=1.RMA{_ -"_ “_‘pA READ 1002. K, N 1002 FORWAT (215) 7 READ 1003.(A(I).I=1.N) 1003 FORAAT (8F10.3) D0 1130 1311-” ___, '113UmRTTTW?UTTU7ATI1Mflflfiu'”*17W”77m HAW” CPR—"7 " AN 2 ’ XSJ1 : . YSJW = . XSQR : . YSQR : . “‘”“““13€T"T[1[1rtr 'T””Ef‘3I":BQ”" “"“‘ ""‘ "”““’ ' " I’ " ”““'“"Pf'*”"_‘“_"_'P"' l L [ocacno RI 2 XSJM 1140 YSJM YSUM + 9(1) . XMEAM : (XSU81/AN WNW” YMEAM = (YSUM)/A~ " XSUM + RI f7“' XVAHN : XVARN 4 (B! 7 XMEAN)t*2 ___.... '—'YVWP_E_'VV7§RT\1“¥ ‘ ’1 ‘HT‘TT"'-—YME‘A‘N"" in?” 7 ‘ F"'"—‘"M“ — 1150 XYPRODN = XYPROUN + 81*B(I) xvaw = XVAQH/AM YVAQ = YVAnN/AN XYPRflD = xvppnnN/AM SL3PF = (XYPRHD - YMFAthMEAN)/XVAR -— flmnrrrmsn 0.78tUP1-‘"' PRINT 1004. K 1004 FORMAT (ll/l/lOX.*FRFQ. IDENT. Nn.v. 110) PRINT 1007 1007 FORMAT (llflX.wPEAK Nn.*.15X.¢YERR-IJ VARYN = 0. —‘_————1N77113TU—1—'E”IjJV__ ""““*“*—m"“"*—W'——'- i- — RI 2 I . Ytau = SLopE~(HI—XMEAN> + YMFAN . 8(1) VAQYN = VARYN + YERRtt? ”Effiv = VARVN/AN* . a Fig. (G.1) Program Listing 119 11160 PRINT 1008.1. YERR . 11008 FORWAT_(13¥,12;18x,E11;4)” 1 — W *“*“"“ “'“- ”-‘-' W*“_r-~ PRINT 1035 . AREAS _ '1005 FORMAT (/1nx.~FRFQ. n? 080. «.E11.4.v GAUSS*) ‘ TCOEFF = SQRTF((AN - 2.)*XVAR/VAQY) Pt?) = SLOPE/100000. FRR = 2.1/( TCOEFFtIHOOOO.) ““———’PRTNT'1150;"DERD;“:Rw “ ‘ ‘ ’ 1"“ “hr * ‘“*‘“‘“"‘—*"' 1100 FDQMAT (I10X.*PERIOD OF USE. «LE11.4.9 + - *.E9,2,* G-lt) _fl—"TPRINT"1006{mVARY, V H‘“w__-""_m_“fl""vm_"“mm_kmm"”_”w‘_w_ 1006 FO?MAT(/10Y.*VARIAMCF = *. E11.4 . //. ‘1 10X,tNUMB:R 0F pEAKS = *IIS) 1110 CONTINJE ENn Fig. (G.2) Program Listing, Continued 120 121 FREQ. IUFHT. No. 10 PEAK N3. YFRR 1 4.1554-003 2 7,8527-004 3 9,8808-003 --*-——4'_“"-*"fi4~~r~WLe-'ww.5473-003 -"***~~**t * _1 *v* 5 9.5532-005 6 1.2968-003 7 “1.1189‘003 a -7.0539-004 9 -7.2902-0n4 1U"*—“"‘—*“*"“—“*“““21;1813-003 '"*~ '““*‘*—‘ ““““““ ’ 11 -9.0558-003 12 -x.3434-0n3 13 -9.0330-003 14 ~1.1964-on3 15 9.0990-003 . 16 ~0.0811-on4 . _i___17_"__1__0 '*‘*‘ “'-1;4386-003 " ‘i ‘“ -1111111111 18 -9.4075-003 19 -3.8063'003 an -9,8845-on3 21 7.5505-004 22 -?.4864-003 ‘“ "23““ “M” "*“"’*"“"“-‘x.5958-004 ' ‘*‘**"’***"“‘” "* M‘“ 24 1.2385-003 25 9.3191'003 26 9,8932-003 27 9,9713-0n3 28 2.5637-003 ”""_”29*“‘“”““"”m"“_—“‘”“1:6806-003 "'*"""“r“”‘""fi'r*“ so 9,7146-003 61 3.2255-003 32 0.0982'004 33 4.4114-004 34 -9.7698-003 *———"35 —"*"“+4:1781:un3“-*"'“-*“"”*”'““”*Wrr‘ FREQ. or 090. ~2.8606+006 Gauss PERIOD 0F OSC. -3.4957-007 + - 8.08-010 G-l -VARiANCE“:~—r—-4;9229.onn-m-"~v~--w~—~m""—-w~w&w~~J“J—r NUMBER OF DEAKQ = x5 Fig. (G.3) Typical Output APPENDIX H Filter Circuits 5),:de coo VnP TANTALEX "—"4I __.v5.___ 3744 °_—_i}————A::r__L_::>\\\\\\\\ m 5.6 / o ([— R’s zzthcr 5'60 K ~ I.” ~16 sec. or 390K ~t~IZsta 30m éfll 944 " 5M! —1% :1— 50K "n hflh O—_w" \ In 'C :- 113/7V— 5“- N : lbw/got scum, 0‘10 13 l:—:L/////,/' OUt Fig. (H.l) Filter Circuits upper: Wide Band Integrator-Differentiator Filter lower: Narrow Band Bridged-tee Filter 122 123 {i/tcnd l H 1‘ n / \— unfnltzmd o( magnetic {m /a’ .6 .'7 :8 |/H ( Ié‘d') Fig. (H.2) Example of Application of Narrow Band Filter using l/H Sweep I .s' 124 .mpamww uofiwwfi um monosooum awnwwfi mnu mo mocwmmua wsu muoz .wumh aowBJ CHE\ooon . puma mocmsomuh 304 Am.mv .wwm N90. .ox mofi. on... a c—SChOQ v. 1 3!“. ‘ on" g a, <193‘fi’r EC’ zgao '0‘.- 125 . thh~\omopv+H 3 $33 Hmfimf wsu ww> scamnomum 5mg: mnu ou o>wumamu econooum 30H msu mo wafiaEmv msu wuoz. . wfiwu am03m .cHE\oom~ . puma uocwaomum swam Aq.mv .me . _ .mvx Nw.m_ .Vm.¢_ QC-l‘cfi I C I > .0. u’ «whiz. fixil