Brock University

Physics Department

St. Catharines, Ontario, Canada L2S 3A1

PHYS 3P91 Laboratory Manual

Physics Department

Copyright c Brock University, 20062007

Contents
1 X-Ray Diraction 1.1 The X-Ray Emission Spectrum of Copper . . . . . . . . . . . . . . . . . . . . . . . . 1.2 The X-ray diraction pattern of MgO . . . . . . . . . . . . . . . . . . . . . . . . . . 1.3 The XRD pattern of an unknown substance . . . . . . . . . . . . . . . . . . . . . . . 2 X-ray uorescence 2.1 X-ray uorescence . . . . . . . . . . 2.2 X-ray Diraction . . . . . . . . . . . 2.3 Apparatus . . . . . . . . . . . . . . . 2.4 Energy Dispersive X-ray Diraction 2.5 Objective . . . . . . . . . . . . . . . 2.6 Operation . . . . . . . . . . . . . . . 2.6.1 Energy Calibration . . . . . . 2.7 Analysis of powdered samples . . . . 3 Electron Diraction 4 Preparation of a thin lm by vacuum evaporation 4.1 Vacuum Evaporator . . . . . . . . . . . . . . . . . . 4.2 Exercise . . . . . . . . . . . . . . . . . . . . . . . . . 4.3 Procedure for Operating the Vacuum Evaporator . . 4.4 Thickness Measurement . . . . . . . . . . . . . . . . 4.5 Procedure for measuring d. . . . . . . . . . . . . . . 5 Resistivity and Hall eect of a thin Bismuth lm . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 2 3 4

5 . 5 . 5 . 6 . 7 . 8 . 9 . 9 . 10 11 15 15 17 17 18 18 21

6 The gamma-ray Scintillation Spectrometer 25 6.1 Calibration Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27 7 The Compton eect 8 Plancks ConstantMethod 1 9 Plancks ConstantMethod 2 29 31 35

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Experiment 1

X-Ray Diraction
Before starting this experiment, you must be familiar with the concepts of: crystal lattice, unit cell, lattice spacing, Miller indices, X-ray spectrum, crystal diraction and Bragg diraction (references 1-4).

Introduction
) encounter atoms, they When X-rays (electromagnetic waves, wavelength order-of-magnitude 1 A are diracted (changed in direction of propagation, with a dierent amplitude and phase, but unchanged in wavelength) by the electron clouds of the atoms. If the atoms are arranged in a crystalline lattice (an array which is periodic in three dimensions), and the incident X-ray wave is a monochromatic parallel beam, then the waves diracted by the = 1023 atoms in the crystal will interfere in such a way that only in a few directions constructive interference will take place, and a non-zero intensity diracted beam will result. The directions of the diracted beam can be constructed as follows: Slice the crystal into planes of atoms, called lattice planes. Each set of lattice planes (two are sketched in gure 1.1) is characterized by its orientation in the crystal (given by the Miller indices h, k and and its lattice spacing d ). Each lattice plane, when hit by an incoming X-ray beam (direction ) acts as a mirror, producing a reected beam as well as a straight-through beam which impinges on the next lattice plane. Only when the reected beams from successive lattice planes interfere constructively, that is, when AB + BC AD = n (1.1)

then the crystal as a whole will produce a diracted beam with non-zero intensity. The angle between the incident and diracted beams is then 2 . This is called Bragg diraction, and from the geometry of gure 1.1 it can be seen that it will occur when: 2d sin = n (1.2)

Often the order number n and d are combined in a quantity d, given by d = d /n, so that Braggs Law is written as: 2d sin = (1.3)

Figure 1.1: X-rays striking a crystal lattice

1.1

The X-Ray Emission Spectrum of Copper

You will determine the wavelength of some of the sharp lines of the Cu X-ray emission spectrum. The diractometer geometry is shown if gure 1.2. The X-rays emitted by the copper target in the X-ray source are ltered, so that only the spectral lines labelled Cu-K1 , Cu-K2 and Cu-K1 (with very low intensity) are present in the X-ray beam. The beam is incident on a single crystal of MgO. Its (h, k, ) = (1, 0, 0) lattice planes will be used; they are parallel to the cleaved front face of the crystal. The intensity I of the diracted beams (at a direction 2 with respect to the incident beam) is measured by the X-ray counter; the chart output is a graph of I as a function of 2 . CAUTION: The instructor will demonstrate the diractometer. Under no circumstances is the apparatus to be used, or adjusted, without prior permission of the instructor. X-rays are a radiation hazard, so you must observe all safety instructions listed next to the experiment. Mount the MgO crystal in the sample holder, so that its (100) face is accurately parallel to the sample plane. For the (100) lattice planes the d spacing is d(100) = 4.205 A The 2nd order (n = 2) Bragg reection for the CuK doublet occurs in the 2 range 42 44 ; the n = 4 reection occurs in the range 93 95 . The n = 2 reection of the K1 line can be seen around 2 = 38 39 with low intensity. Record the I (2 ) curves in these ranges, and calculate the wavelength of the observed spectral lines. Compare the experimental results with the literature values. The wavelength separation of the K1 - K2 doublet can be determined quite accurately, in the following way: Let the wavelength of the two lines in the doublet be 1 and 2 and = 2 1 , the separation of the recorded lines on the I (2 ) chart is measured as 2 (in radians). By dierentiating Braggs Law show that: 2 = . 2 tan 2

Figure 1.2: Diractometer geometry Calculate / for the CuK doublet directly from the measured 2 at 2 = 43 and 2 = 94 ; compare your experimental results with the calculated values of 2(2 1 ) = , (2 + 1 ) where 1 and 2 are taken from one of the references, or from the Handbook of Chemistry and Physics.

1.2

The X-ray diraction pattern of MgO

Replace the single crystal MgO plate by a sample consisting of a thin layer of MgO powder. In the powder the individual crystals (grains of approximately 103 cm size) are oriented totally at random. Of the millions of grains only a few will, accidentally, lie such that their (100) planes are parallel to the plane of the sample holder. When the sample holder is therefore at an angle = 21.5 with respect to the incident beam, and the detector therefore at an angle 2 = 43 , these few grains can produce a Bragg reection. All the other grains will not give a Bragg reection, and therefore the I (2 ) graph will have a (relatively) weak peak at 2 = 43 . Similarly, there will be in the powder sample, grains with a dierent set of lattice planes, say with Miller indices (h, k, ) = (311), parallel to the sample plane; these grains will give a Bragg reection at an angle 2 satisfying Braggs Law with d(311) . The diraction pattern I (2 ) of a MgO powder will therefore consist of a set of peaks, each of which is characterized by its own value of d and of (h, k, ). Record the I (2 ) pattern of MgO powder in the range 28 2 64 . Calculate the d values of the reection, use an average value of = 1.5405 A. The possible sets of lattice planes have Miller indices: (111), (311), (331), (200) and (222). Calculate the d-value for each of these planes according to: a0 d= 2 h + k 2 + 2 and compare with the experimental values. with the lattice constant a0 = 4.205 A

1.3

The XRD pattern of an unknown substance

Each solid crystalline material has its own I (2 ) diraction pattern. In general, the position (2 ) of the diracted beams is determined by the size and shape of the unit cell of the crystalline lattice; the intensity I of a given beam is determined by the kind of atoms and their position inside the unit cell. The XRD pattern is therefore like a ngerprint for each crystalline substance, and can be used for identication. You will be given a powder of an oxide copper. Two copper oxides are known, with formulae Cu2 O and CuO. Record the XRD pattern of the powder in the range 28 2 64 , and calculate d-spacings and relative intensities for each diraction peak. Compare your results with the patterns for CuO and Cu2 O (patterns 5.0661 and 5.0667 of ref. 5) and determine which copper oxide you have.

References
1. B.D. Cullity, Elements of X-Ray Diraction, Chapters 1, 2, 3. 7. 2. E.W. Nueld, X-Ray Diraction Methods, Chapters 1, 2, 3, 5.2. 3. D.L. Livesey, Atomic and Nuclear Physics, Chapters 4.6 - 4.9. 4. R.T. Weidner and R.L. Sills, Elementary Modern Physics, Chapter 5. 5. Powder Diraction File, (Joint Committee on Powder Diraction Standards, 1968). In library as REF QC 482 P68.

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Experiment 2

X-ray uorescence
X-ray uorescence (XRF) and X-ray diraction (XRD) may be used to determine the constituent elements and the crystalline structure of materials.

Introduction 2.1 X-ray uorescence

where K is the kinetic energy of the photoelectron liberated from the atom and B is its binding energy to the atom. Subsequently, the ionized atom combines with an electron and undergoes a de-excitation to its electrically neutral ground state. X-ray photons, whose energies (hj ) are characteristic of the target atom (Z), are produced in the de-excitation. An energy level diagram is shown in gure 2.1. Each level corresponds to the excitation of the atom when a single electron is missing from the otherwise full subshell (nlj ). Zero energy corresponds to the ground state of the neutral atom. Level K, corresponds to the binding energy (BK ) of an electron in the K shell. There are three closely spaced L shell levels labelled LI , LII , LIII corresponding to slightly dierent L shell electron binding energies. If h0 > BK then all characteristic X-rays (K series, L series, etc.) are produced. If BL < h0 < BK , then the K series X-rays are not produced.

XRF refers to the absorption of incident X-rays (h0 ) resulting in the production of a set of X-rays whose energies (hj ) are characteristic of the absorber atom(s) (Z). The characteristic X-rays can therefore be used to identify the atom(s) present in the sample. The incident X-ray photon (h0 ) undergoes a photoelectric interaction with a target atom (Z) resulting in the annihilation of the photon and ionization of the target atom. The energy equation is K = h0 B

2.2

X-ray Diraction

X-ray diraction is used extensively to determine the structure of crystalline and also of noncrystalline and amorphous materials. For crystalline materials, the directions ( ) and wavelength() 5

Figure 2.1: A schematic diagram of the X-ray energy levels. of the diracted beams are given by Braggs Law; with reference to gure 2.2, this is 2d sin = n where n is the order of diraction from crystalline lattice planes of spacing d. The equation may be rewritten as 2dn sin = where dn = d/n and the equation now represents rst order diraction from planes d/n. Using Braggs Law, a measurement of and for a diracted beam enables the spacing dn to be determined. For cubic lattices, a d= 2 h + k 2 + l2 where a is the side length of the cubic lattice cell (the lattice constant), and h, k and l are the Miller indices of the lattice planes.

2.3

Apparatus

A diagram of the apparatus is shown in gure 2.3. The incident beam produced by the X-ray machine has its intensity continuously distributed over a range of X-ray photon energy up to a maximum value = eV , where V is the X-ray tube voltage. The incident beam strikes a crystalline powder; the X-rays diracted from the crystals and those uoresced from the target atoms are recorded by a Si semiconductor junction photon detector (which is sensitive to photons with energies in the range 1 50 keV) positioned at an angle 2 relative to the direction of the incident beam. The Si detector produces a single voltage pulse 6

Figure 2.2: Diraction geometry. for each photon detected; its amplitude is proportional to the energy of the photon detected. The energy (voltage amplitude) spectrum of X-ray photons produced from the target is recorded by a multichannel analyser (MCA). The spectrum I (E ) which is the variation of the number of photons detected, I , with photon energy, E , consists of a series of relatively narrow peaks superimposed on a smoothly varying background. The peaks arise from X-rays uoresced from the target atoms, X-rays diracted from the crystal lattice. The position of the peak centre on the MCA energy scale equals the corresponding photon energy.

2.4

Energy Dispersive X-ray Diraction

In this apparatus, the diraction is observed by measuring I (E ) keeping constant. Braggs Law may be rewritten in terms of the diracted beam photon energy, E , i.e., 2dn sin = = or, Ehkl = 1 hc . 2 sin dhkl (2.1) hc E

hkl are the Miller indices of the planes which produce diraction of photons of energy Ehkl . For a particular value of the diraction angle r (the detector is positioned at an angle 2 relative to the incident beam) diraction from planes with dierent dhkl values produce diraction peaks at 7

Figure 2.3: Schematic diagram of apparatus. energies Ehkl , given by equation (2.1). Diraction peak energies Ehkl are a function of (Eq. 2.1); XRF characteristic peak energies are independent of . In addition, the diraction peak intensities are normally much weaker than those produced by the characteristic X-rays uoresced from the target. Either of the above features may be used to distinguish the characteristic X-ray and the diraction peaks.

Experiment
CAUTION The instructor will demonstrate the operation of the X-ray machine, the Si photon detector and the multichannel analyser. Under no circumstances is the apparatus to be operated prior to instruction. Under no circumstances are adjustments to be made to the target arrangement with the X-ray beam on. The X-ray beam is a radiation hazard.

2.5

Objective

The objective is to identify the constituent elements (using XRF) of the powdered samples.

2.6

Operation

Si Photon Detector The detector is operated at liquid nitrogen temperature. The detector reverse bias must only be applied to a cold detector, otherwise irreversible damage to the detector will result. Normally, the reverse bias ( 1200 V) and the amplier are already switched on and preset, and no adjustments are necessary. However, if the reverse bias has to be switched ON or OFF, this must be done with the bias voltage potentiometer turned to zero. Do not make any adjustment without rst consulting the instructor. X-ray Machine The machine is normally operated at a tube voltage in the range, 20-30 kV, and a current up to a maximum of approximately 15 mA. These values are not at all critical; the voltage range provides an incident X-ray beam spectrum which is reasonably well-matched to that required both for XRF and diraction. Note: The X-ray beam port and shutter must be closed and the X-ray tube high voltage switched OFF prior to making any beam-target alignment changes. This requirement is MANDATORY. MCA The multichannel analyser (MCA) is normally left switched ON, ready for use. The computer monitor is switched OFF when not in use. The operation of the MCA is by selection from a menu which is displayed, together with the spectrum, on the monitor.

Procedure
2.6.1 Energy Calibration
1. Alignment (X-ray HV OFF; beam shutter CLOSED) Position, visually, the energy calibration target into the X-ray beam path (which is determined by the axis of the X-ray beam collimator) and set the Si detector rotatable platform somewhere in the range 2 = 45 60 , relative to the incident X-ray beam path. Check visually, but carefully, that the X-ray beam path strikes the target surface centrally and also that the target surface can be seen by the Si detector. The precise value of 2 is not required; the approximate value ( a few degrees) may be helpful in identifying features of the diraction spectrum. For the calibration, use samples of Zn, Mo and KBr. 2. Spectrum Accumulation (X-ray HV ON; beam shutter OPEN) Accumulate a smooth spectrum in which the peaks are clearly dened (that is, the peak centres can be determined by inspection to 1 channel). The XRF lines due to the main elements in the layer are normally signicantly stronger than any diraction lines. When the accumulation is completed, CLOSE the beam shutter and turn the X-ray current HV OFF. 3. Calibration analysis Record the channel number (n) for the centre of each XRF peak and identify the peaks with the characteristic energies (En ) corresponding to the known elements in the calibration target. The energy calibration of the MCA is accurately given by En = an + b.

The calibration constants (a and b) should be determined by a linear regression analysis and also the data should be plotted. This calibration may be used, without further check, throughout the experiment providing the gain of the Si detector amplier and the set-up of the MCS remain unchanged. Using the calibration, the energies of XRF and diraction peaks obtained in subsequent spectra may be determined. 4. Diraction peaks Use the d values, with largest intensity, of the calibration samples and an estimated 2 value, to calculate the Ehkl values from Eq. (2.1) where a diraction peak might be located. Inspect the I (E ) spectrum for such (weak) peaks. If one (or more) are found, redo a spectrum at a dierent ( a few degrees) 2 value and check that indeed the peak energy is a function of .

2.7

Analysis of powdered samples

1. Alignment (X-ray HV OFF; X-ray beam shutter CLOSED) Install the powdered crystalline target and repeat the beam-target-detector alignment described in section 2.6.1, item 1. 2. Spectrum accumulation (X-ray HV ON, X-ray beam shutter OPEN) Accumulate data and store the resulting spectrum; there should be strong XRF lines present and (maybe) much weaker diraction lines visible. Change the detector angle by a few degrees and repeat the accumulation; compare with the previous spectrum. The diraction peaks shift position in the spectrum, the XRF peaks do not. After this provisional classication into XRF and diraction lines, keep the detector angle xed and accumulate until a smooth spectrum is obtained. A smooth spectrum is a very qualitative term which simply means that the centres of the peaks of interest may be determined by visual inspection to approximately 1 channel. It is useful to keep an eye on the X-ray machine current and voltage readings during accumulation since occasionally the machine trips OFF; if this occurs, restart; if trips persist, call the instructor. When the accumulation is completed, CLOSE the X-ray beam shutter and turn the X-ray current and HV OFF. 3. Data Analysis (a) Determine the energies of the XRF and diraction peaks (if any). (b) Using the characteristics X-ray energy tables, identify the elements in the powdered sample.

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Experiment 3

Electron Diraction
Introduction
In 1924, de Broglie proposed that the motion of particles was described by a wave equation. He associated with each particle a wave, the de Broglie wave, whose wavelength depended on the momentum p of the particle according to h = (3.1) p where h is Plancks constant. In this experiment you will measure the de Broglie wave-length for fast moving electrons, and show that it is related to its momentum according to equation (3.1).

Theory
If an electron leaves a cathode with zero velocity, then its kinetic energy after traversing an accelerating potential V is given by: 1 mv 2 = eV (3.2) 2 where m is the electron mass, v is its speed after traversing the potential V , and e is its charge. The momentum p of the electron is then given by p = mv = 2meV and its de Broglie wavelength h . (3.3) 2meV If this electron strikes a crystal, its de Broglie wave will be diracted by the 3-dimensional periodic structure of the crystal. The electron will pass through the crystal only in those directions in which the de Broglie wave is diracted strongly by the crystal. These directions are given by Braggs Law: 2d sin = n (3.4) = Therefore, if we know the d-values for a crystal (and we can calculate these if the crystal structure is known), then the wavelength can be found by measuring the directions (2 ) in which the waves are strongly diracted. Consider now the situation where a parallel beam of waves is incident on many crystals, which are oriented in a completely random fashion with respect to the beam. In such a random aggregate of crystals there are always crystals with the same set of lattice planes in an orientation satisfying 11

Braggs Law. All these crystals will diract the incident beam strongly over the same angle 2 : the result is a diracted beam in the shape of a cone with top angle 4 . This is the powder method of diraction (Cullity, Chapter 3, p.96) and in eect is the technique used in this experiment to measure the wavelength . Our beam of electrons is incident on a polycrystalline foil of aluminum. The cones of diracted electrons strike a uorescent screen at a distance D , forming a set of uorescent rings of radius r . It is evident that diraction angle 2 is given by r (3.5) tan 2 = . D The Braggs Law 2d sin = n (3.6) may be rewritten as 2 d sin = n (3.7)

In equation (3.4) we refer to as the direction of the nth order beam diracted from the set of atomic planes with spacing d. In the alternative formulation (equation (3.6)) we may refer to as the direction of the 1st order beam diracted from a set of planes with spacing d/n. For cubic crystals the distance d between successive lattice planes in the set specied by the Miller indices hk is a d= 2 h + k 2 + 2 where a is the unit cell side length. Hence we may write d a a = = 2 2 2 2 n n h +k + H + K 2 + L2 (3.8)

where H = nh, K = nk, L = n are the Miller indices of a set of planes with spacing d/n. In the present experiment, the diraction angles are suciently small that tan 2 = 2 and sin = . Hence, combining equations (3.6), (3.7), and (3.8) gives an expression for the electron beam wavelength in terms of the radii of the diraction rings on the uorescent screen, namely = H2 r a . 2 2 +K +L D (3.9)

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Finally, by equating the expression for the diraction measurement of the electron beam wavelength (equation (3.9)) to the de Broglie expression for the electron beam wavelength written in terms of the electron tube accelerating voltage V (equation (3.3)) one obtains r= H 2 + K 2 + L2 D h a 2me 1 V (3.10)

Equation (3.10) gives an explicit expression for the radii of a set of diraction rings as a function of accelerating tube voltage and its validity rests on that of the de Broglie postulate.

Experimental

The instrument is a modied cathode-ray oscilloscope with a variable accelerating potential V . The electron beam can be deected with horizontal and vertical deection plates till it strikes an Al foil in the tube. The diraction pattern of the Al foil can be measured on the screen. Obtain a diraction pattern at V = 4000 V, following the instruction sheet supplied with the instrument. Measure the diameters of the diraction rings ve times with calipers. In order to minimize the eects of ring distortion, make the ve measurements on each ring in dierent directions. Repeat the measurements as a function of V up to V = 9000 V. DO NOT EXCEED 5 A BEAM CURRENT. From the data calculate average values of r for each ring, at each value of V . The value of D for this instrument is: D = 18.2 0.2 cm. The value of a for aluminum is: a = 4.05 A. Verify equation (3.10).

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Experiment 4

Preparation of a thin lm by vacuum evaporation

Before starting the experiment, you should be familiar with the basic concepts of vacuum technique (pumps, gauges).

Introduction
106 m, are important components of Thin layers (lms) of solid materials, with thicknesses = many modern electronic and optical devices. They are often produced by evaporating the material in a vacuum, and condensing the vapour on a cold substrate until the desired thickness is reached. A vacuum is used in order: to prevent a chemical reaction of the material with air, to lower the boiling/sublimation temperature, and, to deposit the material in a smooth, even manner on the substrate. In this experiment you will produce a thin lm of the metal bismuth on a glass substrate, and measure its thickness with a Michelson interferometer. The electrical properties of the lm will be measured in a subsequent experiment.

4.1

Vacuum Evaporator

The mechanical (rotary) pump evacuates the bell jar, via the bypass, to a pressure of = (10100) mTorr, and ejects the evacuated gas into the air. The Turbo pump can pump down to a limit of = (105 106 ) Torr . Units of pressure (force per area): Units of Pressure (force per area) Pa (for Pascal) 1 Nm2 Torr (for Torricelli) 760 Torr (1 standard atmosphere) mm of Hg (mercury): equal to 1 Torr atmospheric pressure: 760 Torr, or 1.013 105 Pa.

MKS unit Practical units

It only operates properly when rst evacuated by the rotary pump. The evaporation takes place in a glass bell jar, from a tungsten lament which acts as a boiling reservoir for a small 15

Figure 4.1: Diagram of a Vacuum Evaporator quantity of Bi. The pressure in the bell jar is measured with either a thermocouple gauge (range (103 100 ) Torr), or with an ionization gauge (range = = (103 106 ) Torr). Good lms can be produced when the atoms/molecules of the material, in our case Bi, travel from the hot lament to the substrate directly, without colliding with residual air molecules, and when the substrate is clean and has no layers of gas, grease, etc., absorbed on its surface. In this respect the following parameters are important and can be calculated from the kinetic theory of gases: 1. the number density of gas N0 ; this is the number of gas molecules per unit volume. It can be calculated from the ideal gas law as P N0 = , kT where P is pressure, T is temperature, k = Boltzmanns constant = 1.38 1023 JK1 . of the gas molecules: 2. the average speed V 8kT m

= V where m = mass of the gas molecule. of the molecules: 3. the mean free path L = L where d = diameter of molecule

1 2 d2 N0

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4. the rate at which gas molecules collide with a surface: 1 = N0 V 4 (collisions per unit area per unit time).

4.2

Exercise

,L and for P = 760 Torr, 76 Torr, etc., down Calculate, and plot versus P , the quantities N0 , V 6 to 7.6 10 Torr. Use nitrogen at room temperature as the gas: d = 3.73 1010 m. Use double logarithmic scales for your graph. At what values of P and T are: about equal to the distance from boiling reservoir to substrate. 1. L 2. the collision rate ((m2 s)1 ) about equal to the typical numbers of atoms per m2 of substrate surface ( = 3 1019 m2 )? It should be clear from your calculations that a vacuum of < 104 Torr is required for proper vacuum evaporation. Use the vacuum evaporator to produce a thin lm of Bi, in the shape of a cross suitable for electrical measurements. Follow the procedure outlined below; the instructor will be present to assist you.

4.3

Procedure for Operating the Vacuum Evaporator

(a) Wash the glass slide with detergent and water and rinse. (b) Rinse with distilled water. (c) Rinse with ethanol. These steps remove water and grease from the slide. Ethanol may dissolve grease from your ngers and leave it on the glass when it evaporates. Use gloves. (d) Dry the slide in air. Check that it is clean.

1. Preparation of substrate for lm deposition:

2. Deposition of the bismuth lm. (a) Check that the ion gauge is o. (b) Close the high vacuum valve. (c) Vent the vacuum chamber and lift the bell jar. (d) Put some bismuth into the lament basket. (e) Put the slide inside the mask and place it above the lament. (f) Put the bell jar back on, make sure that the vent valve is closed. (g) Use the roughing pump and pump down the bell jar to below 100 m Torr pressure via the by-pass.

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Figure 4.2: Diagram of a Michelson Interferometer (h) Turn on the turbo pump open high vacuum gate valve. The turbo pump will now start removing the low pressure residual air from the bell jar. After a few minutes the thermo-couple gauge will read 103 and the cold cathode gauge switches on automatically at the 104 Torr range. Wait until the pressure is 5 105 Torr. (i) Turn on the lament supply switch, increase the current until the lament starts glowing. Keep it like that for a minute to outgass it. Increase lament current, until bismuth starts evaporating. Hold lament current until all Bi has evaporated.

(j) Shut down the lament current; turn the lament supply o. (k) Repeat steps (2a)(2c). (l) Remove slide with bismuth lm on it, replace bell jar, evacuate chamber to high vacuum as in steps (2g) and (2h).

4.4

Thickness Measurement

Since the thickness is of the same order of magnitude as the wavelength of visible light, we will use a method based on wave interference, the Michelson Interferometer. When the optical paths 1 and 2 dier by k (k = 0, 1, 2, . . . ) the monochromatic waves (wavelength ) on their way to the observer are out of phase, and destructive interference produces a dark fringe in the eld of view. The glass substrate plus lm will form one mirror of the interferometer. The light reecting from the Bi lm travels a distance 2d less than the light reected from the glass slide, and therefore the fringe pattern over the Bi lm is shifted with respect to the pattern over the glass slide. From the shift the thickness d can be easily calculated. The actual instrument is a Michelson interferometer optically folded-up so that it ts over a microscope (10) objective. It contains the beam splitter and reference mirror (which can be tilted) and a means of controlling the distance 1 .

4.5

Procedure for measuring d.

1. The instructor will put the interferometer over the microscope objective, and adjust 1 . 18

2. Place your slide (lm up) under the microscope; turn the illuminator on; use white light. 3. Focus on a lm edge by adjusting the vertical position of the microscope stage. This sets the distance 2 . 4. Switch to monochromatic illumination by putting a Fabry-Perot interferometer lter in the light path. 5. Gently adjust the vertical position of the lm, until you see interference fringes. (Be patient). 6. Adjust the tilt screws of the reference mirror until the fringes are perpendicular to the lm edge. You should see a fringe pattern as shown in gure 4.3.

Figure 4.3: Fringe pattern 7. Estimate b (the fringe spacing) and a (the fringe shift) using a measuring eyepiece with a scale in it. The lm thickness is then: a d= . b 2 8. Repeat at dierent positions along the edge of the lm.

References
For vacuum techniques, books such as: J. Yarwood, High Vacuum Technique. J. F. OHanlon, A Users Guide to Vacuum Technology. For the Michelson Interferometer: H. Mark and N. T. Olson, Experiments in Modern Physics, Ch. 4.

E. Hecht and A. Zajac, Optics, Chapter 9.10.2 19

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Experiment 5

Resistivity and Hall eect of a thin Bismuth lm

Introduction
The conductivity of a solid depends on two parameters: one is the number of charge carriers (in metals, electrons of charge e) per unit volume, n. The other factor is the velocity with which the carriers will move through the solid when an electric eld is applied. The ratio of this drift velocity (in ms 1 ) to the applied eld (in Vm1 ) is called the mobility (in m2 V1 s1 ). The conductivity is given by = en (5.1) The conductivity (or its inverse, the resistivity ) can in principle be determined by measuring the resistance of a block of length and cross-section area A(= wxh). If a current i is passed through the block, and a potential dierence V is measured at two points apart then V wxh = (5.2) i In practice one rarely has (or can make) a sample in this ideal shape, and a number of techniques are available to determine from i V measurements on samples of irregular shape. We will use a method developed by van der Pauw, for homogeneous samples of constant thickness d, but otherwise of arbitrary shape. Four contacts, labelled A, B, C and D, are attached to the side of the at sample in arbitrary positions. A current iAB is passed from A to B, and the resulting voltage dierence VCD is measured between contacts C and D; call the ratio VCD /iAB a resistance; RAB,CD = R1 . Next, the current is passed from B to C, and the voltage VDA is measured: RBC,DA = R2 . Similarly, determine VAB /iCD , which equals R1 , and VBC /iDA which equals R2 again. Now van der Pauw showed that R1 and R2 are related to the sample resistivity and thickness d by: exp dR1 + exp dR2 =1 (5.3)

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Equation (5.3) cannot be solved for in closed form, but it can be rewritten as: = d (R1 + R2 ) f ln 2 2 R1 R2 (5.4)

where the van der Pauw function f of the argument R1 /R2 satises cosh ln 2 (R1 /R2 ) 1 ln 2 1 = exp f (R1 /R2 ) + 1) 2 f (5.5)

Values of f (R1 /R2 ) have been tabulated; therefore after measuring R1 and R2 and calculating R1 /R2 for the sample its resistivity can be calculated from equation (5.4). Notice that the van der Pauw method requires the measurement of only one dimension (d) of the sample; the standard method requires three measurements of sample dimensions. The Hall eect is the sideways deection of the moving charge carriers in the sample due to a magnetic eld B perpendicular to the current i. The electron owing in the (negative) x-direction experiences a Lorentz force q V B in the (negative) z -direction due to a B eld in the (positive) y -direction; the result is a potential dierence, the Hall voltage VH , developing between the top and bottom face of the sample, (positive) z -direction. The Hall coecient RH is now dened as: RH = VP Q w iB 1 eRH (5.6)

It is related to the carrier concentration n from equation (5.1) by n= (5.7)

Once n is known, the mobility of the charge carriers can be calculated (from equation (5.7)): = RH (5.8)

The van der Pauw method allows an easy determination of RH for a at sample: Pass a current iAC between opposite contacts; it gives a voltage VBD . Now put a B eld perpendicular to the sample; VBD changes to a new value VBD + VH . The Hall coecient is related to VH by RH = VH d iAC B (5.9)

Procedure
To determine , n and for a thin Bismuth lm: 1. Place the lm in the sample holder and attach the four contacts A, B, C and D to the lm. 2. Connect a circuit from a current source, a voltmeter and ammeter to measure iAB and VCD . Do the measurements, and calculate R1 . Reverse the direction of the current leads and determine R1 again. The two values of R1 should be identical unless you have bad(rectifying) contacts. 3. Similarly determine R2 = IBC /VAD ; also check that indeed R1 is also equal to iCD /VAB and R2 to iAD /VBC . Calculate average values of R1 , R2 and R2 /R1 . 22

4. From the graph of the van der Pauw function f (R1 /R2 ) determine the appropriate f value for your sample, and calculate . 5. Place the samples between the poles of the electromagnet, and measure iAC and VBD . Switch the B -eld on, and measure the Hall voltage VH . Reconnect the leads to measure iBD , and VAC , and measure VH again. Reverse the current leads to check for non-Ohmic contacts. Reverse the direction of the B -eld, and check that VH changes sign. 6. Calculate RH from the average VH value, and calculate n and for Bismuth. Compare n (the number of free electrons per unit volume) to the number of Bi atoms per unit volume.

References
1. D. Halliday and R. Resnick, Fundamentals of Physics, Chapters 28, 30-4 2. K. Seeger, Semiconductor Physics, Chapter 4.3 3. E. H. Putley, The Hall Eect and Semi-conductor Physics, Chapters 1-2 and 2-1.

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Experiment 6

The gamma-ray Scintillation Spectrometer

The spectrometer is designed to record and display the spectrum of gamma-rays emitted by radioactive sources. The energies cover the range from about 10 KeV (X-rays) to nearly 10 MeV. The use of energy units, rather than the wavelength or frequency of the EM waves, for the classication of the emissions from radioactive materials emphasises the particle-like interaction of the gammarays with matter. There is no dispersive element, such as a grating or a prism, in the spectrometer. There are no slits, lenses or mirrors. The detector is a crystal of thallium-doped sodium iodide. When radiation, in the form of an X or gamma-ray photon, or energetic electrons, interacts with the crystal a certain fraction of the energy deposited in the crystal is transferred to the thallium activation centres and subsequently emitted as visible light. Other fractions of the energy deposit are dissipated as heat or by radiation in the invisible portions of the spectrum. The energy deposit is itself proportional to the incident gamma or X-ray photon energy. The number of visible light photons emitted by the centres is directly proportional to the amount of energy deposited and, hence, to the energy of the radiation. The group of photons emitted by the centres appears as a short ash of light, or scintillation. The photons are detected by a photomultiplier tube (PMT) which produces a voltage pulse with height proportional to the number of photons that entered the tube. Hence, the height of the voltage pulse is proportional to the energy deposited in the crystal. If the dimensions of the crystal are such that the incident radiation is completely absorbed (i.e., the probability of absorption approaches 1), the height is proportional to the energy of the radiation. By means of electronic circuits the number of voltage pulses per second with heights lying between V and V + dV (a channel) is counted and recorded for channels having voltage V (proportional to energy) between pre-set limits. The channels are numbered in order of increasing energy. The device that performs the counting and recording function is called a multi-channel analyzer (MCA). The MCA, the detector crystal and the photomultiplier form the gamma-ray spectrometer. If a source of monoenergetic gamma-rays, such as Cs137 , is examined with the spectrometer it is found that the recorded spectrum consists of a fairly well dened peak at some channel number, and a broad continuum with some smaller peaks that extends from the main peak towards lower channel numbers. The origin of these features of the spectrum is found in the nature of the interactions of the gamma-ray with the crystal. The gamma-ray interacts with the crystal in one of three ways described below. 1. Photoelectric Absorption. The gamma-ray is annihilated and the energy of the photon is transferred to an electron bound to an atom or ion of the crystal. The kinetic energy of the electron (KeV or MeV), plus its binding energy to the atom or ion (eV), is equal to the energy of the gamma-ray photon. This photoelectron then transfers, on average, a certain fraction 25

Figure 6.1: Spectrum recorded with Cesium137 sources of its energy to the thallium activation centres as it moves through the crystal. In crystals of the sizes used in practice the photoelectron loses all its kinetic energy within the crystal. The number of photons emitted by the thallium centres is proportional to the gamma-ray energy. The voltage pulse at the output of the PMT that collect the light from the NaI(Th) crystal is proportional to the gamma-ray energy. 2. Compton Scattering. The gamma-ray transfers momentum to an electron and is thereby scattered with lower energy and momentum. The scattered electron will excite some thallium centres and cause a voltage pulse to appear at the PMT output. The scattered gamma photon may interact by mechanism (1) and produce a PMT voltage pulse. The height of this pulse, as well as that produced by the interaction of the scattered electron with the crystal, will be less than that produced when the gamma photon energy is deposited as in (1). Since the loss of energy by the gamma photon depends on the scattering angle, there will be a range of pulse heights detected. 3. Pair Production. When a photon of energy greater than or equal to twice the rest energy of an electron interacts with matter it may be annihilated. The photon energy appears as a positron electron pair. When the positron meets another electron a gamma photon (annihilation radiation) appears. For our purposes this eect may be ignored because the gamma sources used do not have sucient energy. The spectrum recorded for a Cesium137 source with the equipment to be used is shown in Figure 6.1. The large peak at the high end of the pulse height (gamma energy) axis arises from mechanism (1). It is called the Full Energy Peak. The energy corresponding to the channel of the maximum height is the energy of the gamma photon. The step to the lower energy side is the Compton Edge. It is produced by the most energetic electrons arising from the Compton scattering process. The secondary peak at still lower energy arises from the full energy peak of the back-scattered photons in the Compton process. Other lower energy peaks may arise from x-rays produced in the PMT shielding or from background eects. The recognition of the full energy peak and its channel number provides a means to calibrate the apparatus.

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6.1

Calibration Procedure

The scintillation crystal and PMT are housed in a protective shield. The anode voltage of the PMT has been set to +1000 V. The gain of the amplier that follows the PMT has been adjusted to give about 6 volt pulses for the full energy peak of the cesium. If the gain setting or the PMT voltage is altered your calibration will be invalidated and will have to be repeated. The MCA electronics are mounted on a card in an Apple computer. The program that runs the analyzer and permits various display options for the data, as well as recording on disk, is loaded and set for 256 channels. This setting is sucient for the energy resolution of the detector. (Read the instruction manuals or ask for help.) Place the cesium source near the crystal end of the detector and record the spectrum until you have a clean looking spectrum. Note the channel for the full energy peak. Print out a spectrum and a channel count around the peak. Identify the backscatter peak and the Compton edge and verify that the energy value of the feature corresponds to theory in each case. Repeat the measurements for the sodium22 , barium133 and cobalt57 sources. The energies are: Source Cs137 Na22 Ba133 Co57 may measure other gamma energy values. Energy 0.662 MeV 0.511 MeV 0.356 MeV 0.1222 MeV

Plot a graph of Channel Number vs. Energy in MeV and determine the slope so that you !

? Why is the full energy peak not sharp?

References
A discussion of the scintillation detector is given in: Radiotracer Methodology in Biological, Environmental and Physical Sciences, C. H. Wang, D. L. Willis and W. D. Loveland (Prentice-Hall), Chapters 4, 6, 7, 12. Call Number QC 795.42 W36 1975. The electronic equipment described is obsolete. The physics of the processes is the important part.

Computer and Printer Commands

Equipment activation procedure
1. Turn on AC toggle switch on Regulated High Voltage Power Supply 2. Turn dial from HV O to 1000 3. Turn on CI Power Supply (lower far right) toggle switch 4. Turn on Oscilliscope 5. Turn on printer and set to Draft mode (see section Printer Commands on page 28).

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6. Turn on Apple monitor followed by the Apple computer which computer will display: Dos Version 3.3 Apple II Plus alternate slot? (Y/N) alternate slot #(3 or 5) printer slot # type y type 5 type 1

(DO NOT TOUCH ANY OTHER DIALS !) Multi-channel Analyser commands: Key(s)
f h1, h2 q1, q2, q3, q4 , a d c + [return] [esc] <,> p

Function
full screen display (spectrum broken into 2048 channels) half screen display quarter screen display continous scrolling of spectrum (left, right) accumulate halt accumulation clear screen quit change (decrease, increase) vertical scale print

For use with paddle: (halt accumulation rst) r paddles control two pointers, the total counts between pointers and the channel numbers are displayed

Printer Commands
Draft Mode with the printer on, press ON LINE to take the printer oine (the light next to ON LINE should now be o) press PRINT MODE twice (until only the HS (High Speed) light is on) to set the printer to draft mode press ON LINE to put the printer online Line Feed/Form Feed press ON LINE to take the printer oine to perform a line feed, press and release LF/FF to move the paper forward one line to perform a form feed, press and hold LF/FF to eject the page to put the printer online, press ON LINE

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Experiment 7

The Compton eect

The Compton eect can be studied and the scattering formula veried. The apparatus has been set up as shown if Figure 7.1. Measure the energy, E , of the scattered gamma photons as a function of their scattering angle .

Figure 7.1: Compton scattering arrangement S Cs137 gamma source; Energy 0.661 MeV; Strength 25 millicuries. E Direction of the collimated gamma photon beam of energy E. Note: The 25 millicurie source produces an intense collimated beam. DO NOT stand in the direct line E. T Aluminum target that contains the free electrons from which the gamma rays will be scattered. E Direction of the scattered photons of energy E . D NaI gamma ray detector. Both S and D are well shielded with lead. The source shielding minimizes the radiation intensity in all directions except within a small solid angle centred on the beam direction, E. The detector shielding is designed to admit the scattered photons, E , and to exclude entrance to photons incident from other directions. The scattering angle, , is varied by rotating the source assembly, S , about

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the target position, T. To measure E use the energy calibration that you made earlier. Check it out if there has been an interval between laboratory sessions! Accumulate the pulse height spectrum of the scattered photons as a function of the scattering angle and so determine E ( ). The Compton formula is usually given in terms of incident wavelength and scattered wavelength : h = (1 cos ). m0 c Show that in terms of photon energies E and E this formula becomes 1 1 1 = (1 cos ) E E m0 c2 Plot your experimental data as 1/E versus (1 cos ) and from the results determine E and the electron rest mass energy m0 c2 . The minimum value of the scattering angle at which the Compton scattering energy shift is observable will be determined by the energy resolution of the detector and the eectiveness of the lead collimator which denes the solid angle of emergence of the cesium photon beam. If the scattering angle is made too small, the direct shine of the cesium gamma photons into the detector will completely mask the small Compton energy shift. Only a small fraction of the photons are scattered in the target. The intensity of the scattered beam is much less than that of the incident beam. The recording time required to obtain a satisfactory spectrum may be many minutes. If there is any direct shine into the detector the recording time will be seconds rather than minutes!

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Experiment 8

Plancks ConstantMethod 1
Introduction
The constant h (= 6.62559 1034 Js) was introduced by Planck in 1900 when he provided the rst satisfactory theoretical basis for the temperature and wavelength dependence of the radiation from a black body. A black body, by denition, absorbs all the radiation that falls upon it. The rate of energy emission by the body summed over all wavelengths is proportional to the fourth power of the thermodynamic temperature T. The spectral distribution of the radiation depends on the temperature. There is a maximum in the emission versus wavelength curve so that the product of the wavelength of the maximum emission and the temperature is a constant. These relations are known as Stefans Law and Wiens Law, respectively. In 1893, W. Wien showed from thermodynamic considerations that the form of the radiation curve was given by E = 1 f 5 1 T

where E is the energy emitted in range d at wavelength and f is some function to be determined. The experimental data were obtained by Coblentz, who examined the spectral distribution of the body maintained at temperature T. Such a system provides an excellent approximation to a black body because radiation that enters the hole from outside has an exceedingly small chance to escape before it is absorbed at the walls of the cavity. The form of the radiation curve is shown in Figure 8.1. The curves are independent of the nature of the material that forms the walls of the cavity. Today, for convenience, the cavity is a hollow metal cylinder, blackened inside, and completely closed except for a narrow slit in one end. At the temperatures available in the laboratory the shortest wavelength radiation of measurable intensity is in the near ultra-violet. In 1900, Planck introduced the assumption that each mode of vibration of frequency of the electromagnetic eld in the cavity could change its energy by a denite amount h (where h was a constant to be determined) rather than by continuously variable amounts. He was then able to derive the explicit form of the radiation curve and to show that Stefans Law and the Wien Law followed from his form. Moreover, the form was identical to that determined by Coblentz if the constant h was given a value close to that quoted above. Plancks assumption was the rst use of the idea of quantization in the radiation eld and, later, in the interaction of radiation with atoms. Some years later, Einstein introduced the idea of light quanta in the explanation of the photo electric eect. The electromagnetic wave of frequency that is the light beam gives energy to the electrons in the material in units of h . The kinetic energy of the emitted electron is h W , where W is the energy required to remove the electron from the material. The constant h appeared again in the Bohr theory of the hydrogen atom in 1912 and eventually became an essential part of modern quantum mechanics. Its value is important and much eort 31

Figure 8.1: Temperature dependent energy emission by a blackbody has been devoted to the measurement. In two experiments you will obtain estimates for h. The rst method is based on the black body radiation curve. The second is a direct experimental examination of Einsteins photo electric equation introduced above.

Method
Plancks formula for the power radiated by a black body at frequency and temperature T is P = 2 c
2

h exp
h kT

where P is the energy radiated per unit area of surface per second per unit frequency range at frequency , k is Boltzmanns constant and c is the velocity of light. If a body is not a black body radiator, so that it does not absorb all radiation that falls upon it, the power radiated is less than the formula value. If the absorption coecient at is independent of the temperature P will be reduced by a constant factor for all temperatures. If the frequency and temperature are such that exp(h/kT ) 1 then P is proportional to exp h kT .

Thus a graph of ln P versus 1/T should be a straight line of slope h/k. The frequency is determined by the experimental conditions and k is known independently of this experiment. Thus a value of h can be obtained. In the experiment we use an oven cavity as a black body radation source which uses MoSi2 as a heater element. This oven can reach temperature as high as 1500 C . The Temperature of the oven 32

will be measured using two dierent methods. In the rst method the temperature is measured directly using S-type thermocouple inside the oven. In the second method you use the Infra red technique to measure the temperature of the oven. Determination of h Increase the current to the oven heater until a noticeable light output P is registered on the detector output meter. Measure and record the temperature of the oven when it is stable as well as the light output power P . Correct, if necessary, P for the zerolight-output, and plot ln P versus 1/T. Repeat at ten dierent temperatures, by increasing current to the oven. The data points (ln P, 1/T ) should fall on a straight line, with slope h/k. Calculate h from the slope; the Fabry-Perot lter passes only wavelengths in a narrow band at = 650 nm or as indicated by the instrument.

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Experiment 9

Plancks ConstantMethod 2
The Einstein photoelectric equation relates the kinetic energy K of the emitted electron to the frequency of the radiation falling on the emitter and the energy required to extract the electron from the material K = h eV0 , where the extraction energy is written as the product of the magnitude of the electron charge and a potential V0 known as the work function of the material. Unless h > eV0 no electrons will be emitted. If the emitter is used as the cathode of a vacuum cell and connected to the other electrode, or anode, a current will exist in the circuit as long as light of suciently short wavelength falls on the cathode. If a retarding potential is applied between anode and cathode in the external circuit the current will be reduced. The current will be zero if the retarding potential is set at the value K/e. In the experiment you will measure the retarding potential required to stop the photoelectric current as a function of frequency, or reciprocal wavelength. A value of h will be calculated from the graph of the stopping potential versus reciprocal wavelength. The photocell has a potassium cathode and a ring anode set so that light can reach the cathode without striking the anode. The cell is connected to a low leakage small value capacitor so that the capacitor charges as the photo current is generated. The potential dierence between the capacitor plates approaches the stopping potential, the photo current is reduced by the electric eld between anode and cathode, and eventually the voltage across the capacitor reaches a steady value. This value is the stopping potential plus any contact EMFs arising from the connections between circuit elements. These unknown voltages only aect the intercept of the graph and can be ignored. The incident light is provided by a microscope illuminating lamp and condensing lens. The frequency is selected with a narrow band pass Fabry-Perot lters. Care must be taken to ensure that the light does not strike the anode and cause the emission of electrons from its material or from small amounts of potassium acquired in the manufacturing of the cell. The cell must also be shielded from room light. The steady potential reached by the capacitor is measured by an electrometer rather than a voltmeter. The input impedance of the electrometer is so high that it does not provide any signicant drain for the charge on the capacitor. Such is not the case for everyday voltmeters. The potentials measured will lie in the range 0.3 to 1.2 volts (approximately). Use lters for wavelengths 650, 600, 550, 500, 450 nm with the microscope lamp. Then substitute a mercury lamp without lter to get the stopping potential for the 404.7 nm line. (The glass lenses prevent the ultraviolet lines of mercury from reaching the cell.) Plot a graph of stopping potential versus reciprocal wavelength and determine Plancks constant and the apparent work function of potassium. Record 35

the stopping potential for the microscope lamp without any lters and use your other results to determine the short wavelength limit of the emission from the lamp.

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