Difrao dos raios-X

- Para avaliar uma estrutura cristalina, necessrio usar as figuras de difrao produzidas por ondas que interagem com os tomos e que possuem comprimentos de onda ( ) comparveis (da ordem ou menores) com a ordem de grandeza das distncias interatmicas. - A estrutura cristalina pode ser estudada atravs da difrao de ftons, eltrons de alta energia e neutrons. - A difrao depende da estrutura cristalina e do comprimento de onda da radiao. - Because X-rays have wavelengths similar to the size of atoms, they are useful to explore within crystals.

Aplicao dos raios-X

- Os raios-X podem afetar um filme fotogrfico assim como a luz visvel. - Raio-X uma radiao eletromagntica exatamente com a mesma natureza da luz visvel mas de comprimento de onda muito pequeno. - Os raios-X so mais penetrantes que a luz visvel e podem facilmente atravessar o corpo humano, madeira, metal e outros objetos opacos.

Resoluo da tcnica: 10-3 mm

Resoluo da tcnica: 10-7 mm

Espectro de raios-X

Caractersticas dos raios-X

- Os raios-X se encontram na regio entre os raios-gama e raios ultravioleta no espectro eletromagntico. - A difrao pode indiretamente mostrar detalhes de estrutura interna dos materiais da ordem de 10-7 mm de tamanho. Luz visvel = 6000 Raios-X usado em difrao - = 0.5 - 2.5 1 = 10-10 m 1 nm = 10-9 m = 10
X-rays are electromagnetic waves of very short wavelength (of the order of 0.1 nm). It would be impossible to construct a grating having such a small spacing by the cutting process. However, the atomic spacing in a solid is known to be about 0.1 nm.
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Espectro de ondas eletromagnticas

Energia dos raios-X

A energia ( ) de um fton de raio X relacionada com o seu comprimento de onda segundo a equao de Einstein:

= h = hc/
onde: = energia h = constante de Planck = 6,63 x 10-34 Joule.s = frequncia c = velocidade da luz = 3,0 x 108 m/s = comprimento de onda 1 eV = 1,602 x 10-19 joule

Em unidades mais usadas no laboratrio:

() = 12,4 / (keV)
Para o estudo dos cristais, os ftons devem possuir energias no intervalo entre 10 e 50 keV. Logo, como os raios-X possuem menor comprimento de onda do que a luz visvel, eles possuem energia mais elevada. Devido a sua elevada energia, os raios-X podem penetrar mais facilmente no material do que a luz visvel. Esta capacidade depende tambm da densidade do material.

Comprimento de onda versus energia da partcula, para ftons, eltrons e neutrons.

Para os eltrons:

() = 12 / [ (eV)]1/2

Difrao dos raios-X

Raios atmicos e estrutura cristalina para diversos metais. FCC face-centered cubic HCP hexagonal close-packed BCC = body-centerd cubic

Comprimento de onda versus energia da partcula, para ftons, eltrons e neutrons.

Difrao dos raios-X

There are various diffraction techniques currently employed which result in diffraction patterns. These patterns are records of the diffracted beams produced.

From diffraction patterns we can: measure the average spacings between layers or rows of atoms; determine the orientation of a single crystal or grain; find the crystal structure of an unknown material; and measure the size, shape and internal stress of small crystalline regions.

Produo dos raios-X

Os raios-X so produzidos quando uma partcula carregada com suficiente energia desacelerada rapidamente. Raios X podem ser produzidos quando eltrons so acelerados em direo a um alvo metlico. X- ray tube consist of: - On evacuated chamber with a tungsten filament at one end of the tube, called the cathode, and a metal target at the other end, called an anode. - Electrical current is run through the tungsten filament, causing it to glow and emit electrons. A large voltage difference (measured in kilovolts) is placed between the cathode and the anode, causing the electrons to move at high velocity from the filament to the anode target. - Upon striking the atoms in the target, the electrons dislodge inner shell electrons resulting in outer shell electrons having to jump to a lower energy shell to replace the dislodged electrons. These electronic transitions results in the generation of X-rays. The X-rays then move through a window in the X-ray tube and can be used to provide information on the internal arrangement of atoms in crystals or the structure of internal body parts.

Tubo para produo dos raios-X 8

Produo dos raios-X

A estrutura do tubo de Rntgen

Na figura est representada esquematicamente a estrutura de um tubo eletrnico de Rntgen. O ctodo C uma espiral de volfrmio, que emite eltrons graas emisso termoeletrnica. O cilindro Cl foca o feixe de eltrons que depois colidem com o eletrodo metlico (nodo) A. Durante este processo, formam-se os raios X. A diferena de potencial entre o ctodo e o nodo atinge vrias dezenas de quilovolts. No tubo forma-se um alto vcuo; a presso do gs neste tubo de 10-5 - 10-7 mm Hg.

Continuous and Characteristic X-ray Spectra

When the target material of the X-ray tube is bombarded with electrons accelerated from the cathode filament, two types of X-ray spectra are produced. The first is called the continuous spectra. O choque do feixe de eltrons (que saem do catodo com energia de dezenas de KeV) com o anodo (alvo) produz dois tipos de raios X. Um deles constitui o espectro contnuo, e resulta da desacelerao do eltron durante a penetrao no anodo. O outro tipo o raio X caracterstico do material do anodo. Assim, cada espectro de raios X a superposio de um espectro contnuo e de uma srie de linhas espectrais caractersticas do anodo.

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Espectro Contnuo

The continuous spectra consists of a range of wavelengths of X-rays with minimum wavelength and intensity (measured in counts per second) dependent on the target material and the voltage across the X-ray tube. The minimum wavelength decreases and the intensity increases as voltage increases.

SWL short-wave-length limit

Espectro de raios-X do Molibdenio em funo da voltagem aplicada.

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Espectro Caracterstico
The second type of spectra, called the characteristic spectra, is produced at high voltage as a result of specific electronic transitions that take place within individual atoms of the target material. This is easiest to see using the simple Bohr model of the atom. In such a model, the nucleus of the atom containing the protons and neutrons is surrounded by shells of electrons. The innermost shell, called the K- shell, is surrounded by the Land M - shells. When the energy of the electrons accelerated toward the target becomes high enough to dislodge K- shell electrons, electrons from the L - and M - shells move in to take the place of those dislodged.
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Espectro Caracterstico
Each of these electronic transitions produces an X-ray with a wavelength that depends on the exact structure of the atom being bombarded. A transition from the L shell to the K- shell produces a K X-ray, while the transition from an M - shell to the K- shell produces a K X-ray.

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Espectro Caracterstico
Each of these electronic transitions produces an X-ray with a wavelength that depends on the exact structure of the atom being bombarded. A transition from the L - shell to the K- shell produces a K X-ray, while the transition from an M - shell to the K- shell produces a K X-ray. These characteristic X-rays have a much higher intensity than those produced by the continuous sprectra, with K X-rays having higher intensity than K X-rays. Very important point - the wavelength of these characteristic x-rays is different for each atom in the periodic table (of course only those elements with higher atomic number have L- and M - shell electrons that can undergo transitions to produce Xrays). A filter is generally used to filter out the lower intensity K X-rays.
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Espectro Caracterstico

Modelo de Bohr

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Espectro Caracterstico
K Wavelength ( ) 0.7107 1.5418 1.7902 1.9373 2.2909

Element

Mo Cu Co Fe Cr

X-rays wavelengths for commonly used target materials in X-ray tubes.

Espectro de raios-X do Mo para voltagem aplicada de 35 kV.

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Produo dos raios-X

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Produo dos raios-X

FILTERS Many x-ray diffraction experiments require radiation which is as closely monochromatic as possible. However, the beam from an x-ray tube operated at a voltage above V, contains not only the strong K line but also the weaker K line and the continuous spectrum.

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Tubo de raios-X
The x-ray tube must contain: (a) a source of electrons, (b) a high accelerating voltage, and (c) a metal target. Furthermore, since most of the kinetic energy of the electrons is converted into heat in the target, the latter is almost always water-cooled to prevent its melting. The x-ray tubes contain two electrodes: - an anode (the metal target) maintained, with few exceptions, at ground potential, - a cathode, maintained at a high negative potential, normally of the order of 30,000 to 50,000 volts for diffraction work. X-ray tubes may be divided into two basic types, according to the way in which electrons are provided: -gas tubes - in which electrons are produced by the ionization of a small quantity of gas (residual air in a partly evacuated tube), - filament tubes - in which the source of electrons is a hot filament.
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Tubos de raios-X
Gas Tubes These resemble the original x-ray tube used by Roentgen. They are now obsolete. Filament Tubes These were invented by Coolidge in 1913. They consist of an evacuated glass envelope which insulates the anode at one end from the cathode at the other, the cathode being a tungsten filament and the anode a water-cooled block of copper containing the desired target metal as a small insert at one end.

Esquema da seco transversal de um tubo vedado de raios-X

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Conceitos de Max von Laue - 1912

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Difrao de luz em uma fenda

Difrao em duas fendas

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DIFRAO - Espalhamento coerente + Interferncia

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Interferncia e Espalhamento

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X-ray Diffraction
Since a beam of X-rays consists of a bundle of separate waves, the waves can interact with one another. Such interaction is termed interference. If all the waves in the bundle are in phase, that is their crests and troughs occur at exactly the same position (the same as being an integer number of wavelengths out of phase, nl, n = 1, 2, 3, 4, etc.), the waves will interfere with one another and their amplitudes will add together to produce a resultant wave that is has a higher amplitude (the sum of all the waves that are in phase. If the waves are out of phase, being off by a non-integer number of wavelengths, then destructive interference will occur and the amplitude of the waves will be reduced. In an extreme case, if the waves are out of phase by a multiple of 1/2l (n/2l ), the resultant wave will have no amplitude and thus be completely destroyed.

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William Henry Bragg

July 2, 1862 - March 10, 1942

William Henry Bragg was born at Westward, Cumberland, on July 2, 1862. He was educated at Market Harborough Grammar School and afterwards at King William's College, Isle of Man. Elected a minor scholar of Trinity College, Cambridge, in 1881, he studied mathematics under the well-known teacher, Dr. E. J. Routh. He was Third Wrangler in the Mathematical Tripos, Part I, in June 1884, and was placed in the first class in Part II in the following January. He studied physics in the Cavendish Laboratory during part of 1885, and at the end of that year was elected to the Professorship of Mathematics and Physics in the University of Adelaide, South Australia. Subsequently he became successively Cavendish Professor of Physics at Leeds (1909-1915), Quain Professor of Physics at University College London (1915-1925), and Fullerian Professor of Chemistry in the Royal Institution. His research interests embraced a great many topics and he was an adept at picking up a subject, almost casually, making an important contribution, then dropping it again. However, the work of Bragg and his son Lawrence in 1913-1914 founded a new branch of science of the greatest importance and significance, the analysis of crystal structure by means of X-rays. If the fundamental discovery of the wave aspect of X-rays, as evidenced by their diffraction in crystals, was due to von Laue and his collaborators, it is equally true that the use of X-rays as an instrument for the systematic revelation of the way in which crystals are built was entirely due to the Braggs. This was recognized by the award of the Nobel Prize jointly to father and son in 1915.

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William Lawrence Bragg,

March 31, 1890 / July 1, 1971

William Lawrence Bragg, son of William Henry Bragg, was born in Adelaide, South Australia, on March 31, 1890. He received his early education at St. Peter's College in his birthplace, proceeding to Adelaide University to take his degree in mathematics with first-class honours in 1908. He came to England with his father in 1909 and entered Trinity College, Cambridge, as an Allen Scholar, taking firstclass honours in the Natural Science Tripos in 1912. In the autumn of this year he commenced his examination of the von Laue phenomenon and published his first paper on the subject in the Proceedings of the Cambridge Philosophical Society in November. In 1914 he was appointed as Fellow and Lecturer in Natural Sciences at Trinity College and the same year he was awarded the Barnard Medal. From 1912 to 1914 he had been working with his father, and the results of their work were published in an abridged form in X-rays and Crystal Structure (1915). It was this work which earned them jointly the Nobel Prize for Physics in 1915, and from this year to 1919, W. L. Bragg served as Technical Advisor on Sound Ranging to the Map Section, G.H.Q., France, receiving the O.B.E. and the M.C. in 1918. He was appointed Langworthy Professor of Physics at Manchester University in 1919, and held this post till 1937.

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