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Master's Dissertation
DOI
https://doi.org/10.11606/D.85.2019.tde-16092020-141451
Document
Author
Full name
Geraldo de Lima Carezzato
E-mail
Institute/School/College
Knowledge Area
Date of Defense
Published
São Paulo, 2019
Supervisor
Committee
Martinez, Luis Gallego (President)
Bock, Eduardo Guy Perpétuo
Linhares, Horacio Marconi da Silva Matias Dantas
Title in Portuguese
Desenvolvimento, construção e aplicação de acessórios para difratometria de raios X
Keywords in Portuguese
spinner
cimentos Portland
difração de raios X
orientação preferencial
trocador programável de amostras
Abstract in Portuguese
No presente trabalho, um conjunto de acessórios foi projetado e construído para ser usado em um difratômetro de raios X, modelo Ultima IV, Rigaku. Um dos dispositivos, conhecido como spinner, projetado para girar a amostra em torno do eixo normal de sua superfície durante a medição, permite reduzir a orientação preferencial dos cristalitos no material, que pode ocorrer durante a preparação da amostra. Outro dispositivo projetado e construído foi um trocador programável de amostras, acoplado ao spinner, permitindo que até cinco medidas sejam agendadas sequencialmente, sem a intervenção do operador. Os protótipos foram construídos com materiais e componentes eletrônicos de baixo custo e apresentam inovações como o acoplamento magnético, sem contato entre o motor de passo e os porta-amostras. Embora existam dispositivos similares produzidos pelo fabricante do equipamento como acessórios opcionais, o desenvolvimento de tecnologia e o treinamento técnico e profissional para o desenvolvimento de instrumentação científica automatizada, destaca a relevância do projeto. Para demonstrar a aplicabilidade desses acessórios e sua eficácia na redução dos efeitos de orientação preferencial, foram feitas medidas de difração de raios X, em diferentes difratômetros, em amostras de cimentos Portland, que são especialmente suscetíveis a esses efeitos, e foram realizadas quantificações de fases cristalinas pelo método de Rietveld. As medidas e os resultados de análises quantitativas de fases, empregando os dispositivos desenvolvidos, foram comparados aos resultados das medidas realizadas em equipamentos de difração de raios X de outros laboratórios, com e sem o spinner. Os resultados demonstraram que, em 58,33% dos casos, o uso do spinner reduziu a dispersão dos valores de quantificação de fases.
Title in English
Development, construction and application of accessories for X-ray diffractometry
Keywords in English
spinner
automatic sample-changer
Portland cement
preferred orientation
X-ray diffraction
Abstract in English
In the present work, a set of accessories were designed and built in order to be used in an Ultima IV model Rigaku X-ray diffractometer. One of the devices, known as spinner, is intended to spin the sample around the normal axis to its surface during the measurement. This device allows reducing the preferred orientation of crystallites in the material that can occur during the sample preparation. Another device designed and built was a programble sample changer coupled to the spinner, allowing to schedule up to five samples measurements sequentially without operator intervention. The prototypes were built with low-cost materials and electronic components, and present innovations such as the non-contact magnetic coupling between the stepper motor and the sample holders. Although there are similar devices produced by the equipment manufacturer as optional accessories, the development of technology and the technical and professional training for the development of automated scientific instrumentation highlight the project relevance. To demonstrate the applicability of these accessories and their effectiveness in reduction or elimination of preferred orientation effects, in different diffractometers were performed X-ray diffraction measurements on Portland cements, which are especially susceptible to these effects, and were performed crystal phase quantifications by the Rietveld method. The measurements and results of quantitative phase analyses performed using the devices were compared to other measurements performed in X-ray diffraction equipment from other laboratories, with and without the use of spinner. Results demonstrated that the use of spinner reduced the dispersion of phase quantification values in 58.33% of cases.
 
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Publishing Date
2020-09-22
 
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