Debye-Scherrer Diffraction PDF
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This document details an experiment on electron diffraction in a polycrystalline lattice, also known as the Debye-Scherrer method. It provides the principles, objects, and details for carrying out the experiment. The experiment involves the diffraction of electrons on graphite and the determination of wavelengths and lattice plane spacings.
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LD Atomic and Nuclear Physics Physics Introductory experiments Leaflets P6.1.5.1...
LD Atomic and Nuclear Physics Physics Introductory experiments Leaflets P6.1.5.1 Dualism of wave and particle Diffraction of electrons in a polycrystalline lattice (Debye-Scherrer diffraction) Objects of the experiment g Determination of wavelength of the electrons g Verification of the de Broglie’s equation g Determination of lattice plane spacings of graphite Principles Louis de Broglie suggested in 1924 that particles could have wave properties in addition to their familiar particle properties. He hypothesized that the wavelength of the particle is in- versely proportional to its momentum: h λ= (I) p λ: wavelength h: Planck’s constant D1 p: momentum His conjecture was confirmed by the experiments of Clinton Davisson and Lester Germer on the diffraction of electrons at crystalline Nickel structures in 1927. In the present experiment the wave character of electrons is demonstrated by their diffraction at a polycrystalline graphite lattice (Debye-Scherrer diffraction). In contrast to the experi- ment of Davisson and Germer where electron diffraction is observed in reflection this setup uses a transmission diffrac- tion type similar to the one used by G.P. Thomson in 1928. From the electrons emitted by the hot cathode a small beam is singled out through a pin diagram. After passing through a focusing electron-optical system the electrons are incident as sharply limited monochromatic beam on a polycrystalline D2 graphite foil. The atoms of the graphite can be regarded as a space lattice which acts as a diffracting grating for the elec- trons. On the fluorescent screen appears a diffraction pattern Bi 0206 of two concentric rings which are centred around the indif- fracted electron beam (Fig. 1). The diameter of the concentric Fig. 1: Schematic representation of the observed ring pattern due to rings changes with the wavelength λ and thus with the accel- the diffraction of electrons on graphite. Two rings with diame- erating voltage U as can be seen by the following considera- ters D1 and D2 are observed corresponding to the lattice tions: plane spacings d1 and d2 (Fig. 3). LD Didactic GmbH. Leyboldstrasse 1. D-50354 Huerth / Germany. Phone: (02233) 604-0. Fax: (02233) 604-222. e-mail: [email protected] by LD Didactic GmbH Printed in the Federal Republic of Germany Technical alterations reserved P6.1.5.1 -2- LD Physics leaflets From energy equation for the electrons accelerated by the voltage U e ⋅U = 1 m ⋅ v2 = p2 (II) n λ = 2d sinϑ 2 2⋅m U: accelerating voltage e: electron charge m: mass of the particle ϑ ϑ v: velocity of the particle ∆1 ∆2 the momentum p can be derived as d p = m ⋅ v = 2 ⋅ e ⋅m ⋅U (III) Substituting equation (III) in equation (I) gives for the wave- length: h λ= (IV) Fig. 2: Schematic representation of the Bragg condition. 2 ⋅ m ⋅ e ⋅U In 1913, H. W. and W. L. Bragg realized that the regular ar- If we approximate tan 2⋅ϑ = sin 2⋅ϑ = 2⋅ sin ϑ for small angles rangement of atoms in a single crystal can be understood as we obtain an array of lattice elements on parallel lattice planes. When D we expose such a crystal lattice to monochromatic x-rays or 2 ⋅ sin ϑ = (VII) 2⋅L mono-energetic electrons, and, additionally assuming that those have a wave nature, then each element in a lattice The substitution of equation (VII) in (V) leads in first order plane acts as a “scattering point”, at which a spherical wave- diffraction (n = 1) to let forms. According to Huygens’ principle, these spherical D wavelets are superposed to create a “reflected” wave front. In λ = d⋅ (VIII) 2 ⋅L this model, the wavelength λ remains unchanged with respect to the “incident” wave front, and the radiation directions which D: ring diameter are perpendicular to the two wave fronts fulfil the condition L: distance between graphite and screen “angle of incidence = angle of reflection”. Constructive interference arises in the neighbouring rays d: lattice plane spacing reflected at the individual lattice planes when their path differ- ences ∆ = ∆1 + ∆2 = 2⋅d⋅sinϑ are integer multiples of the wavelength λ (Fig. 2): 2 ⋅ d ⋅ sin ϑ = n ⋅ λ n = 1, 2, 3, … (V) d: lattice plane spacing ϑ: diffraction angle d1 This is the so called ‘Bragg condition’ and the corresponding diffraction angle ϑ is known as the glancing angle. In this experiment a polycrystalline material is used as diffrac- tion object. This corresponds to a large number of small sin- gle crystallites which are irregularly arranged in space. As a result there are always some crystals where the Bragg condi- tion is satisfied for a given direction of incidence and wave- d2 length. The reflections produced by these crystallites lie on a cones whose common axis is given by the direction of inci- dence. Concentric circles thus appear on a screen located perpendicularly to this axis. The lattice planes which are im- portant for the electron diffraction pattern obtained with this setup possess the lattice plane spacings (Fig. 3): -10 d1 = 2.13⋅10 m -10 d2 = 1.23⋅10 m From Fig. 4 we can deduce the relationship Fig. 3 Lattice plane spacings in graphite: D d1 = 2.13⋅10-10 m tan 2 ⋅ ϑ = (VI) d2 = 1.23⋅10-10 m 2 ⋅L LD Didactic GmbH. Leyboldstrasse 1. D-50354 Huerth / Germany. Phone: (02233) 604-0. Fax: (02233) 604-222. e-mail: [email protected] by LD Didactic GmbH Printed in the Federal Republic of Germany Technical alterations reserved LD Physics leaflets -3- P6.1.5.1 Apparatus 1 Electron diffraction tube......................................555 626 L 1 Tube stand.........................................................555 600 1 High-voltage power supply 10 kV.......................521 70 1 Precision vernier callipers...................................311 54 1 Safety Connection Lead 25 cm red....................500 611 F2 1 Safety Connection Lead 50 cm red....................500 621 2ϑ D 1 Safety Connection Lead 100 cm red..................500 641 1 Safety Connection Lead 100 cm blue.................500 642 F1 2 Safety Connection Lead 100 cm black...............500 644 C X A 100 kΩ U Fig. 4: Schematic sketch for determining the diffraction angle. Due to equation (IV) the wavelength λ is determined by the L = 13.5 cm (distance between graphite foil and screen), accelerating voltage U. Combining the equation (IV) and D: diameter of a diffraction ring observed on the screen equation (VIII) shows that the diameters D1 and D2 of the ϑ: diffraction angle concentric rings change with the accelerating voltage U: For meaning of F1, F2, C, X and A see Fig. 5. 1 D = k⋅ (IX) U with k= 2 ⋅L ⋅ h (X) Setup d⋅ 2⋅m⋅ e The experimental setup (wiring diagram) is shown in Fig. 5. Measuring Diameters D1 and D2 as function of the accelerat- - Connect the cathode heating sockets F1 and F2 of the ing voltage U allows thus to determine the lattice plane spac- tube stand to the output on the back of the high-voltage ings d1 and d2. power supply 10 kV. - Connect the sockets C (cathode cap) and X (focussing electrode) of the tube stand to the negative pole. - Connect the socket A (anode) to the positive pole of the 5 kV/2 mA output of the high-voltage power supply 10 kV. - Ground the positive pole on the high-voltage power supply 10 kV. Safety notes A F1 F2 When the electron diffraction tube is operated at high volt- X C ages over 5 kV, X-rays are generated. F1 F2 g Do not operate the electron diffraction tube with high 6.3 V~ / 2 A voltages over 5 keV. The connection of the electron diffraction tube with groun- ded anode given in this instruction sheet requires a high- A voltage enduring voltage source for the cathode heating. F1, F2 C g Use the high-voltage power supply 10 kV (521 70) for supplying the electron diffraction tube with power. Danger of implosion: the electron diffraction tube is a high- vacuum tube made of thin-walled glass. kV 0...max. 0...5V g Do not expose the electron diffraction tube to mechani- cal stress, and connect it only if it is mounted in the tube - 0...5kV max.100 µ A + - 0...5kV max.2 mA + stand. g Treat the contact pins in the pin base with care, do not 521 70 bend them, and be careful when inserting them in the tube stand. The electron diffraction tube may be destroyed by voltages Fig. 5: Experimental setup (wiring diagram) for observing the elec- or currents that are too high: tron diffraction on graphite. Pin connection: F1, F2: sockets for cathode heating g Keep to the operating parameters given in the section C: cathode cap on technical data. X: focusing electrode A: anode (with polycrystalline graphite foil see Fig. 4) LD Didactic GmbH. Leyboldstrasse 1. D-50354 Huerth / Germany. Phone: (02233) 604-0. Fax: (02233) 604-222. e-mail: [email protected] by LD Didactic GmbH Printed in the Federal Republic of Germany Technical alterations reserved P6.1.5.1 -4- LD Physics leaflets Carrying out the experiment Table 2: Measured diameter D1 of the concentric diffraction rings as function of the accelerating voltage U. The wave- - Apply an accelerating voltage U ≤ 5 kV and observe the lengths λ1 and λ1,theory are determined by equation (VIII); and diffraction pattern. equation (IV), respectively. Hint: The direction of the electron beam can be influenced by U D1 λ1 λ1,theroy means of a magnet which can be clamped on the neck of kV cm pm pm tube near the electron focusing system. To illuminate an another spot of the sample an adjustment of the magnet might be necessary if at least two diffraction rings cannot be 3.0 seen perfectly in the diffraction pattern. 3.5 - Vary the accelerating voltage U between 3 kV and 5 kV in 4.0 step of 0.5 kV and measure the diameter D1 and D2 of the diffraction rings on the screen (Fig. 1). 4.5 - Measure the distance between the graphite foil and the 5.0 screen. Table 3: Measured diameter D2 of the concentric diffraction rings as function of the accelerating voltage U. The wave- Measuring example lengths λ2 and λ2,theory are determined by equation (VIII); and Table 1: Measured diameters D1 and D2 (average of 5 meas- equation (IV), respectively. urements) of the concentric diffraction rings as function of the U D2 λ2 λ 2,therory accelerating voltage U. kV cm pm pm U D1 D2 kV cm cm 3.0 3.5 3.0 4.0 3.5 4.5 4.0 5.0 4.5 5.0 Distance between graphite foil and screen: L = 13.5 cm b) Verification of the de Broglie’s equation The de Broglie relation (equation (I)) can be verified using e = 1.6021 ⋅ 10 -19 C m = 9.1091 ⋅ 10 -31 kg Evaluation and results h = 6.6256 ⋅ 10 -34 J⋅s in equation (IV). The results for the wavelengths determined a) Determination of wavelength of the electrons by equation (IV) are λ1,theroy and λ2,theory. They are listed for From the measured values for D1 and D2 and the lattice plane the diameters D1 and D2 in Table 2 and Table 3, respectively. spacings d1 and d2 the wavelength can be determined using The values λ1 and λ2 determined from the diffraction pattern equation (VIII). The result for D1 and D2 is summarized in agree quite well with the theoretical values λ1,theroy and λ2,theory Table 2 and Table 3, respectively. due to the de Broglie relation. Note: Rewriting equation (VIII) as 2 ⋅L d = λ⋅ D c) Determination of lattice plane spacings of graphite shows that the diameter D of the rings (Fig. 1) is inversely In Fig. 6 the ring diameters D1 and D2 are plotted versus proportional to the lattice plane spacings d (Fig. 2). This in- 1 / U. The slopes k1 and k2 are determined by linear fits formation is necessary for the evaluation of the wavelength from the lattice plane spacings (here assumed as known) through the origin according equation (IX) to the experimental according equation (VIII). The lattice plane parameters are data: derived directly in part c) using equations (IX) and (X). k1 = 1,578⋅m V k2 = 2.729⋅m V The dominant error in the measurement is the determination of the ring diameters D1 and D2. For an accuracy of reading Resolving equation (X) for the lattice plane spacing d about 2 mm the error is approximately 5% for the outer ring 2⋅L ⋅h and approximately 10% for the inner ring. d= k ⋅ 2⋅m⋅e LD Didactic GmbH. Leyboldstrasse 1. D-50354 Huerth / Germany. Phone: (02233) 604-0. Fax: (02233) 604-222. e-mail: [email protected] by LD Didactic GmbH Printed in the Federal Republic of Germany Technical alterations reserved LD Physics leaflets -5- P6.1.5.1 0,06 0,05 D2 0,04 D/m 0,03 0,02 0,01 D1 0,00 0,000 0,005 0,010 0,015 0,020 -1/2 -1/2 U /V Fig. 6: Ring diameters D1 and D2 as function of 1 / U. The solid lines correspond to the linear fits with the slopes k1 = 1.578 m V and k2 = 2.729 m V , respectively. gives -10 d1 = 2.10⋅10 m -10 d2 = 1.21⋅10 m which is within the error limits in accordance of the parame- ters depicted in Fig. 3. Supplementary information After the experiment of Davisson and Germer further experi- ments with particle wave effects due to particles confirmed the de Broglie relation and thus the wave-particle dualism. In 1930, for instance, O. Stern and I. Esterman succeeded in demonstrating the diffraction of hydrogen molecules and in 1931 they diffracted Helium atoms using a Lithium Fluoride crystal. Experimental results which can be described by quantum theory only have the Planck constant h in their basic formula. In this experiment, for instance, the Planck’s constant can be determined from equation (X) if the lattice spacings d1 and d2 of graphite are assumed to be known e.g. from x-ray structure analysis: d⋅k ⋅ 2 ⋅m ⋅ e h= 2⋅L Using the values k1 and k2 obtained by the linear fit to ex- perimental data (Fig. 6) gives -34 d1: h = 6.724⋅10 J⋅s -34 d2: h = 6.717⋅10 J⋅s h = 6.6256 ⋅ 10 -34 Literature: J⋅s LD Didactic GmbH. Leyboldstrasse 1. D-50354 Huerth / Germany. Phone: (02233) 604-0. Fax: (02233) 604-222. e-mail: [email protected] by LD Didactic GmbH Printed in the Federal Republic of Germany Technical alterations reserved