A determinação do estado de deformação de monocristais planos através da técnica pseudo-Kossel, combinada com o estudo do espalhamento difuso de raios X próximo a uma reflexão de Bragg, permite uma caracterização dos defeitos quanto a sua natureza, tamanho e simetria se houver poucas variedades de defeitos diferentes ou quando ocorrer a predominância de um deles. Estudamos monocristais de silício Czochralski dopados com antimônio ou com boro, e que também continham oxigênio e carbono devido ao processo de crescimento. Estas amostras apresentam aglomerados de defeitos pontuais com dimensões características em torno de 102 - 103 nm. Medidas de espalhamentos interplanares mostram que estas são mais fortemente influenciadas pela direção de crescimento que pela concentração de dopantes, e que as maiores alterações ocorrem à medida que 0 angulo entre a direção de crescimento e os planos diminuem. A partir das medidas dos espalhamentos interplanares podemos levantar 0 estado de deformação dos cristais através do tensor de \"strain\" e foi possível analisar a configuração \"stressstrain\". Desta análise obtivemos, além da variação do parâmetro de rede, 0 tensor de \"stress\" e dele 0 tensor momento de dipolo elástico P. 0 tensor P pode nos dar informações acerca da simetria do defeito &nos permitiu calcular 0 espalhamento difuso de raios X próximo de uma reflexão de Bragg. Vimos que algumas amostras estão deformadas numa configuração muito próxima daquela de cisalhamento simples e que a simetria do tensor P indica que em praticamente todas as amostras tem uma variedade grande de defeitos diferentes. Uma das amostras, Si com Sb (CSb= 8. 1018 dopantes/ Cm3)apresenta um tensor P pr6ximo daquele gerado por defeito que temsimetria ortorrombica e, para ela foram construidas curvas de isso intensidades em torno do ponto (004) da rede recíproca, calculados a partir das componentes de P, e que foram comparadas com as curvas de \"rocking\" experimentais. / The accurate determination of strain distributions in single crystals through the pseudo-Kossel technique together with the analysis of the diffuse X-ray scattering near a Bragg reflection permits the characterization (nature, size and shape) of predominant defects. Czochralski silicon single crystals doped by diffusion during growth with antimony and boron were studied. These samples presented clusters of 102 - 103 nm. Interplanar spacings determined by the pseudo- Kossel method showed a significant dependence on growth direction,planes parallel to growth direction were the most affected. From and the dipole tensor P determined. This dipole tensor was employed in the calculation of the diffuse X-ray scattering. For one of the samples Si:Sb P presents an orthorrombic simetry. The results for this sample were compared with experimental rocking.

A determinação do estado de deformação de monocristais planos através da técnica pseudo-Kossel, combinada com o estudo do espalhamento difuso de raios X próximo a uma reflexão de Bragg, permite uma caracterização dos defeitos quanto a sua natureza, tamanho e simetria se houver poucas variedades de defeitos diferentes ou quando ocorrer a predominância de um deles. Estudamos monocristais de silício Czochralski dopados com antimônio ou com boro, e que também continham oxigênio e carbono devido ao processo de crescimento. Estas amostras apresentam aglomerados de defeitos pontuais com dimensões características em torno de 102 - 103 nm. Medidas de espalhamentos interplanares mostram que estas são mais fortemente influenciadas pela direção de crescimento que pela concentração de dopantes, e que as maiores alterações ocorrem à medida que 0 angulo entre a direção de crescimento e os planos diminuem. A partir das medidas dos espalhamentos interplanares podemos levantar 0 estado de deformação dos cristais através do tensor de \"strain\" e foi possível analisar a configuração \"stressstrain\". Desta análise obtivemos, além da variação do parâmetro de rede, 0 tensor de \"stress\" e dele 0 tensor momento de dipolo elástico P. 0 tensor P pode nos dar informações acerca da simetria do defeito &nos permitiu calcular 0 espalhamento difuso de raios X próximo de uma reflexão de Bragg. Vimos que algumas amostras estão deformadas numa configuração muito próxima daquela de cisalhamento simples e que a simetria do tensor P indica que em praticamente todas as amostras tem uma variedade grande de defeitos diferentes. Uma das amostras, Si com Sb (CSb= 8. 1018 dopantes/ Cm3)apresenta um tensor P pr6ximo daquele gerado por defeito que temsimetria ortorrombica e, para ela foram construidas curvas de isso intensidades em torno do ponto (004) da rede recíproca, calculados a partir das componentes de P, e que foram comparadas com as curvas de \"rocking\" experimentais. / The accurate determination of strain distributions in single crystals through the pseudo-Kossel technique together with the analysis of the diffuse X-ray scattering near a Bragg reflection permits the characterization (nature, size and shape) of predominant defects. Czochralski silicon single crystals doped by diffusion during growth with antimony and boron were studied. These samples presented clusters of 102 - 103 nm. Interplanar spacings determined by the pseudo- Kossel method showed a significant dependence on growth direction,planes parallel to growth direction were the most affected. From and the dipole tensor P determined. This dipole tensor was employed in the calculation of the diffuse X-ray scattering. For one of the samples Si:Sb P presents an orthorrombic simetry. The results for this sample were compared with experimental rocking.

Die Arbeit beschäftigt sich mit zerstörungsfreien Untersuchungen von Kristalldefekten an kompakten Proben mittels röntgenographischer Kossel- u. Weitwinkel-Mikrobeugung im Rasterelektronenmikroskop. Das REM wurde durch ein neu entwickeltes Aufnahmeverfahren so erweitert, daß die äußerst intensitätsschwachen Kossel-Röntgeninterferenzen mittels Phosphorszintillator und hochauflösendem, extrem empfindlichen CCD-Flächendetektor registriert werden können. Das aufwendige Röntgenfilmverfahren wurde damit abgelöst. Die Aufnahme-Techniken wurden so kombiniert, daß die sich gegenseitig ergänzenden Methoden, v.a. die Kossel- u. Pseudo-Kossel-, aber auch die Rückstreu-Elektronen-Beugung, erstmals mit einem einzigen CCD-System im REM ausführbar sind. Die Aufnahme von Kikuchi-Bändern wurde so weit verbessert, daß diese erstmalig bei vertikaler Inzidenz des Elektronenstrahls auf der Probe beobachtet werden konnten. Durch Einsatz einer fokussierenden Polykapillarlinse in einem Röntgenfluoreszenzspektrometer konnte die Anregung von Kossel-Linien durch Bremsstrahlung und erheblich kürzere Belichtungszeiten sowie deutlich höhere laterale Auflösungen erzielt werden. Für die komplementären Mikrobeugungsmethoden wurde ein einheitliches Programm entwickelt, dessen neue Art der Simulation komplizierter Weitwinkel-Kurven 4. Ordnung die Lokalisierung von Gitterbaufehlern im kompakten Kristall ermöglichte. Entsprechende Simulationen und Verfeinerungen der Kanüle erlaubten in feinkörnigen Polykristallen, wie Bariumtitanat, eine Einzelkornanalyse mit der Weitwinkel-Beugung. Insbesondere wurden markante Erhöhungen der Versetzungsdichte nahe der Korngrenze einzelner Kristallite in FeAl festgestellt. An intermetallischen Fe-Al-Verbindungen wurden in Weitwinkel-Kurven Feinstrukturen gefunden, die sich durch Umweganregungen in Zusammenhang mit Überstrukturen erklären lassen. An zugverformten Ni-Kristallen wurden Kossel- u. Weitwinkel-Linienbreiten in Abhängigkeit des Azimuts im symmetrischen Bragg-Fall ausgewertet u. mit theoretischen Modellen verglichen. Anisotrope Linienverbreiterungen durch die Wirkung von Stufenversetzungen konnten quantitativ nachgewiesen werden. Erste Kossel- u. Weitwinkel-Untersuchungen an zyklisch verformten Ni-Einkristallen zeigten, daß beobachtete perlenkettenförmige Intensitätsanhäufungen an Weitwinkelreflexen die Konfiguration von Versetzungswänden aus Stufenversetzungsdipolen im Kristallvolumen widerspiegeln. Erstmals konnte der Einfluß von Stapelfehlern auf Weitwinkel-Linien, der sich durch linsenförmige Intensitätsaufspaltungen zeigte, experimentell nachgewiesen, theoretisch erklärt und quantitativ bestimmt werden. / The thesis deals with the nondestructive investigation of crystal defects by X-ray Kossel and Pseudo Kossel microdiffraction on compact specimens in the scanning electron microscope. The SEM was extended by means of a newly developed detection method in such a way that X-ray Kossel interferences, which are extremely faint in intensity, can be observed by a phosphor scintillator as well as a high resolution and ultra-sensitive CCD area detector. The demanding X-ray film method was thus replaced. The observation techniques were combined so that the mutually complementary methods, above all the Kossel and Pseudo Kossel, but also the electron backscattered diffraction, are made possible for the first time by using just one CCD system in the SEM. The detection of Kikuchi bands was improved to such a degree that these could be recorded even at vertical incidence of the electron beam on the specimen for the first time. It was shown that the lateral resolution of the Kossel technique under polychromatic X-ray tube excitation could be enhanced considerably and the exposure times strongly reduced by using a polycapillary lens in an X-ray fluorescence spectrometer. For the complementary microdiffraction methods a homogeneous simulation program was developed, whose novel way of simulating the complicated Pseudo Kossel curves of the fourth order enable the lattice defect localization in compact crystals. The corresponding simulations and refinements of the target tube allowed a single grain analysis also in fine-grained polycrystals like barium titanate with Pseudo Kossel X-ray diffraction. Particularly, a marked increase of the dislocation density was ascertained near the grain boundary of individual crystallites in FeAl. At intermetallic Fe-Al compounds Pseudo Kossel curves fine structures were found, which can be explained by umweg (detour) excitations in relation to superstructures. Kossel and Pseudo Kossel line widths were analyzed in dependence on the azimuth and compared with theoretical models at tensile deformed Ni-crystals in the symmetrical Bragg case. Anisotropic line broadenings through the effect of edge dislocations could be proved quantitatively. Conclusions could be drawn from the initial Kossel and Pseudo Kossel investigations of cyclically deformed nickel crystals with respect to the observed pearl-necklace-like intensity thickening at Pseudo Kossel lines reflecting the strong local variations of the dislocation density and, thus, the configuration of dislocation walls of edge dislocation dipoles inside the crystalline volume. For the first time, the effect of stacking faults on Pseudo Kossel reflections appearing by lens-shaped intensity splittings could be proved experimentally, explained theoretically and determined quantitatively.

Die Arbeit beschäftigt sich mit zerstörungsfreien Untersuchungen von Kristalldefekten an kompakten Proben mittels röntgenographischer Kossel- u. Weitwinkel-Mikrobeugung im Rasterelektronenmikroskop. Das REM wurde durch ein neu entwickeltes Aufnahmeverfahren so erweitert, daß die äußerst intensitätsschwachen Kossel-Röntgeninterferenzen mittels Phosphorszintillator und hochauflösendem, extrem empfindlichen CCD-Flächendetektor registriert werden können. Das aufwendige Röntgenfilmverfahren wurde damit abgelöst. Die Aufnahme-Techniken wurden so kombiniert, daß die sich gegenseitig ergänzenden Methoden, v.a. die Kossel- u. Pseudo-Kossel-, aber auch die Rückstreu-Elektronen-Beugung, erstmals mit einem einzigen CCD-System im REM ausführbar sind. Die Aufnahme von Kikuchi-Bändern wurde so weit verbessert, daß diese erstmalig bei vertikaler Inzidenz des Elektronenstrahls auf der Probe beobachtet werden konnten. Durch Einsatz einer fokussierenden Polykapillarlinse in einem Röntgenfluoreszenzspektrometer konnte die Anregung von Kossel-Linien durch Bremsstrahlung und erheblich kürzere Belichtungszeiten sowie deutlich höhere laterale Auflösungen erzielt werden. Für die komplementären Mikrobeugungsmethoden wurde ein einheitliches Programm entwickelt, dessen neue Art der Simulation komplizierter Weitwinkel-Kurven 4. Ordnung die Lokalisierung von Gitterbaufehlern im kompakten Kristall ermöglichte. Entsprechende Simulationen und Verfeinerungen der Kanüle erlaubten in feinkörnigen Polykristallen, wie Bariumtitanat, eine Einzelkornanalyse mit der Weitwinkel-Beugung. Insbesondere wurden markante Erhöhungen der Versetzungsdichte nahe der Korngrenze einzelner Kristallite in FeAl festgestellt. An intermetallischen Fe-Al-Verbindungen wurden in Weitwinkel-Kurven Feinstrukturen gefunden, die sich durch Umweganregungen in Zusammenhang mit Überstrukturen erklären lassen. An zugverformten Ni-Kristallen wurden Kossel- u. Weitwinkel-Linienbreiten in Abhängigkeit des Azimuts im symmetrischen Bragg-Fall ausgewertet u. mit theoretischen Modellen verglichen. Anisotrope Linienverbreiterungen durch die Wirkung von Stufenversetzungen konnten quantitativ nachgewiesen werden. Erste Kossel- u. Weitwinkel-Untersuchungen an zyklisch verformten Ni-Einkristallen zeigten, daß beobachtete perlenkettenförmige Intensitätsanhäufungen an Weitwinkelreflexen die Konfiguration von Versetzungswänden aus Stufenversetzungsdipolen im Kristallvolumen widerspiegeln. Erstmals konnte der Einfluß von Stapelfehlern auf Weitwinkel-Linien, der sich durch linsenförmige Intensitätsaufspaltungen zeigte, experimentell nachgewiesen, theoretisch erklärt und quantitativ bestimmt werden. / The thesis deals with the nondestructive investigation of crystal defects by X-ray Kossel and Pseudo Kossel microdiffraction on compact specimens in the scanning electron microscope. The SEM was extended by means of a newly developed detection method in such a way that X-ray Kossel interferences, which are extremely faint in intensity, can be observed by a phosphor scintillator as well as a high resolution and ultra-sensitive CCD area detector. The demanding X-ray film method was thus replaced. The observation techniques were combined so that the mutually complementary methods, above all the Kossel and Pseudo Kossel, but also the electron backscattered diffraction, are made possible for the first time by using just one CCD system in the SEM. The detection of Kikuchi bands was improved to such a degree that these could be recorded even at vertical incidence of the electron beam on the specimen for the first time. It was shown that the lateral resolution of the Kossel technique under polychromatic X-ray tube excitation could be enhanced considerably and the exposure times strongly reduced by using a polycapillary lens in an X-ray fluorescence spectrometer. For the complementary microdiffraction methods a homogeneous simulation program was developed, whose novel way of simulating the complicated Pseudo Kossel curves of the fourth order enable the lattice defect localization in compact crystals. The corresponding simulations and refinements of the target tube allowed a single grain analysis also in fine-grained polycrystals like barium titanate with Pseudo Kossel X-ray diffraction. Particularly, a marked increase of the dislocation density was ascertained near the grain boundary of individual crystallites in FeAl. At intermetallic Fe-Al compounds Pseudo Kossel curves fine structures were found, which can be explained by umweg (detour) excitations in relation to superstructures. Kossel and Pseudo Kossel line widths were analyzed in dependence on the azimuth and compared with theoretical models at tensile deformed Ni-crystals in the symmetrical Bragg case. Anisotropic line broadenings through the effect of edge dislocations could be proved quantitatively. Conclusions could be drawn from the initial Kossel and Pseudo Kossel investigations of cyclically deformed nickel crystals with respect to the observed pearl-necklace-like intensity thickening at Pseudo Kossel lines reflecting the strong local variations of the dislocation density and, thus, the configuration of dislocation walls of edge dislocation dipoles inside the crystalline volume. For the first time, the effect of stacking faults on Pseudo Kossel reflections appearing by lens-shaped intensity splittings could be proved experimentally, explained theoretically and determined quantitatively.