NNR IN RAPIDLY ROTATED METALS By - Nottingham eTheses ...

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- 104 - the corresponding values of d (T1Z/T1D). The errors quoted again refer to the distribution of values obtained in each case. Using the same technique Tunstall and Brown (72) measured T1D and 6 in samples of pure filed annealed powder over the temperature range 1.3-295 K. Although their measured 6 value at room temperature was 2.25 they interpreted the recorded temperature dependence as indicating a contribution due to a quadrupolar thermal reservoir and concluded that the value of 6 relating the true dipolar relaxation time to Tlz was in fact 2.15 ± 0.07. From room temperature measurements of the spin-lattice relaxation in the rotating frame 113 (Tlp) Fradin and Rowland(d ) measured 6 as 2.65. Pifer a CW slow passage saturation method and obtained a value of (114) used 2.07 ±'0.02 at 273 K. At liquid helium temperatures experimental values of 6 have been consistently greater than 2.5(18'72,115) The measurements reported here indicate that the method of sample preparation contributes to the measured values of T1D and hence Ö. The recorded 6 value for the filed powder (c) is somewhat lower than Tunstall and Brown's uncorrected value from a similar sample at 295 K. On the other hand the value for powder (a) agrees with their corrected value to within experimental error and is in excellent agreement with that reported by Pifer. Such an occurrence may well be fortuitous, however, because no details of Pifer's samples are included. With the simplifying assumption of a spherical Fermi surface the theoret- ical value for 6 is 2.06(72). The experimental value for the pure sprayed powder therefore fits present theory very well. It remains to be seen whether this value is independent predicts. of temperature as theory
T10 ms 3. O 2.5 2'C H 1"C o.. v 23456 ROTATION RATE kHz FIGURE 7.4 : The variation of IT WI with rotation rate about an axis inclined at 900 to H0
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NNR IN RAPIDLY ROTATED METALS By R.
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I wish to express my thanks to: ACK
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quadrupole relaxation. However theo
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2.3.5 Quadrupole Relaxation 26 (i)
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5.9 Sample Preparation 71 5.9.1 Cup
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1.1 BASIC THEORY -i- CHAPTER 1 INTR
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-3- Transforming to the rotating fr
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-5- lattice and T2 is the spin-spin
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and -7- Vd(t) f(w1)cos w't dw Sao -
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-9- where the terms represent the Z
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- 11 - If rii = nrij = (Xli + X2j +
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- 13 - In powdered samples a weak i
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- 15 - This contact term manifests
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- 17 - where 0 is the angle between
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- 19 - termed pseudo-dipolar. It is
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- 21 - the non-secular terms of the
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- 23 - to the lattice directly via
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- 25 - (2.25), can then be assumed
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- 27 - quadrupole moments to produc
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- 29 - where En are the Zeeman ener
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3.1 INTRODUCTION - 31 - CHAPTER 3 N
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Aý T. B a A"T"B " - 33 - It is a g
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(-Ur Ho FIGURE 3.1. : Co-ordinate s
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D, (t) = 331 2 + 3YI2 sin 2a 4 - 36
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- 38 - X (t) = cos a cos ßp + sin
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- 40 - 3.7 THE EFFECT OF ROTATION O
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- 42 - observations are inconsisten
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- 44 - that it apparently offered n
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- 46 - bearings suffer from instabi
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SI FIGURE 4.1 SCALE il cm : The con
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N to 9 . ýC 8 Ü7 Z w D 06 w ax U.
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- 50 - The rotors used in this work
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Ip IJýi O 1 t - 1 - 1 p OI ý I ý
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- 52 - at rotation speeds around 4
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- 53 - the manufacture of which was
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PTFE Tape_ FIGURE 4.7 rotors SCALE
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4.4.4 COMMENTS - 55 - For completen
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Clamp Pf-£-- SECTION II SECTION 11
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5.1 EQUIPMENT - 58 - CHAPTER 5 EXPE
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- 59 - the range ±1 V are digitise
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SCALE 3 cm j Cooling Gas ; tainiess
Page 83 and 84: Trensmitter EXL, FIGURE 5.3 : The s
Page 85 and 86: FIGURE $. 4 s The spectrometer prob
Page 87 and 88: Gas Tuning ransmi tter Input Receiv
Page 89 and 90: - 64 - phase can then be set so tha
Page 91 and 92: -66- The transient nuclear signals
Page 93 and 94: - 68 - 5.7.1 THE SOLID ECHO PULSE S
Page 95 and 96: - 70 - sequence may be repeated. In
Page 97 and 98: a° P/'rvu - 72 - p is the resistiv
Page 99 and 100: - 74 - combined with a low viscosit
Page 101 and 102: 6.2 RESULTS AND DISCUSSION - 76 - A
Page 103 and 104: IC 1 I. FIGURE 6.2 : Measured T1 va
Page 105 and 106: - 78 - TABLE 6.1. DEBYE TEMPERATURE
Page 107 and 108: - 80 - TABLE 6.2. RATIO OF TI VALUE
Page 109 and 110: - 82 - TABLE 6.3. DEPENDENCE OF T1
Page 111 and 112: - 84 - provides further evidence th
Page 113 and 114: - 86 - CHAPTER 7 EXPERIMENTAL RESUL
Page 115 and 116: - 88 - Lorentzian NMR lineshape of
Page 117 and 118: - 90 - at the top with epoxy glue.
Page 119 and 120: - 92 - (c) Bulk Susceptibility Effe
Page 121 and 122: - 94 - aluminium nuclei in the meta
Page 123 and 124: FIGURE 7.1 : 27A1 F. I. Ds and corr
Page 125 and 126: - 97 - TABLE 7.1. COMPUTED SECOND A
Page 127 and 128: - 99 - and Slichter(104) reported t
Page 129 and 130: - 101 - of this value would be requ
Page 131 and 132: N JL I F- 0 z J I0 0123456789 ROTAT
Page 133: -103- results obtained at a tempera
Page 137 and 138: 0 - 106 - CHAPTER 8 MEASUREMENTS ON
Page 139 and 140: - 108 - process for vanadium the me
Page 141 and 142: - 109 - in the same way to the prec
Page 143 and 144: Qv == , 2 28 kHz -111- which is sli
Page 145 and 146: - 113 - from Cerac Inc. (USA). The
Page 147 and 148: - 115 - 8.4.3 SPIN-LATTICE RELAXATI
Page 149 and 150: tv D Xm =o N O Ul- X- z N O FIGURE
Page 151 and 152: which gives K=0.048 an ± 0.002 - 1
Page 153 and 154: - 118 - Lifetime broadening alone g
Page 155 and 156: - 120 - cannot be spun at low tempe
Page 157 and 158: - 122 - 11. L. E. Orgel, J. Phys. C
Page 159 and 160: - 124 - 59. P. J. Randall, Ph. D. T
Page 161 and 162: - 126 - 101. H. R. Khan, J. M. Reyn
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