Orientador: Carlos José Leopoldo Constantino / Banca: Henrique de Santana / Banca: Ruth Kunzli / O Programa de Pós-Graduação em Ciência e Tecnologia de Materiais POSMAT, tem caráter institucional e integra as atividades de pesquisa em materiais de diversos campi da UNESP / Resumo: Neste trabalho foram estudadas amostras do Centro de Museologia, Antropologia e Arqueologia da FCT - UNESP de Presidente Prudente, o qual é coordenado pela professora Dra. Ruth Kunzli. As amostras foram caracterizadas por espectroscopia vibracional via espalhamento micro-Raman e a absorção no infravermelho com transformada de Fourier (FTIR), análise térmica por termogravimetria (TG) e energia dispersiva de raio-X (EDX). O objetivo principal do trabalho foi identificar os pigmentos utilizados na fabricação dos artefatos cerâmicos encontrados no sítio arqueológico Lagoa São Paulo - 02, Presidente Epitácio, SP, bem como os aditivos incorporados ao corpo cerâmico para entender como os arteftos foram confeccionados. Para o pigmento vermelho os resultados de Raman, FTIR, EDX e TG sugerem a utilização de hematia, um óxido de ferro consistente com o que podia ser encontrado nas rochas avermelhadas das encostas dos rios que eram desgastadas pela água. O pigmento preto apresenta bandas Raman características do carvão, provavelmente, este pigmento era encontrado na natureza como o produto da queima de material orgânico, possivelmente de origem vegetal. Para o pigmento branco, os espectros de FTIR e as curvas de TG sugerem o uso de caulim pela presença das bandas de absorção e do pico endotérmico em 550ºC aracterístico da caulinita, o que é consistente com os dados arqueológicos. Os aditivos identificados foram o carvão e o quartzo, sendo este último encontrado nas rochas presentes na região do sítio arqueológico. Tais aditivos são adicionados na confecção das cerâmicas para evitar o rachamento quando do cozimento, facilitar uma secagem homogênea e, ao mesmo tempo, reduzir a porosidade e a plasticidade. O processo de queima das amostras foi investigado via TG revelaram que todas elas passaram por processos de queima. Entretanto, os resultados sugerem que a amostra ... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: In this study samples from the "Centro de Museologia, Antropologia e Arqueologia (CEMAARQ)" of the "UNESP Unip Estadual Paulista" in Presidente Prudente, São Paulo State, Brazil, coordinated by professor Dra. Ruth Künzli, were investigated. The samples were characterized by vibrational spectroscopy via micro-Roman scattering and Fourier transform infrared absorption (FTIR), thermal analysis by termogravimetry (TG) and energy dispersive X-ray (EDX). The main objective was to identify the pigments used in the manufacture of ceramic artifacts found in the archaeological site "Lagoa Sao Paulo - 02", Presidente Epitácio, SP, and the additives incorporated to the ceramic body to understand how the artifacts were made. For the red pigment of the results of Raman, FTIR, EDX e TG suggested the use of hematite, an iron oxide consistent with that found in the red rocks of the river banks eroded by water. The black pigment has Roman bands characteristic of charcol, probably, this pigment was found in nature as the product of burning organic material, possibly from vegetable. For the white pigment, the FTIR spectra and TG curves suggest the use of Kaolin by the presence of the absorption bands and the endothermic peak at 550ºC, characteristic of kaolinite, which is consistent with the archaeological data. The additives were identified as charcoal and quartz, the latter being found in rocks present in the archeological site. These additives are added in the manufacture of ceramics to prevent cracking when buring, to promote a homogeneous drying and to reduce porosity and plasticity. The burning process of the samples was investigated by TG and revealed that all of them were submitted to burning processes. However, the results suggest that the sample ... (Complete abstract click electronic access below) / Mestre

Made available in DSpace on 2014-06-11T19:30:19Z (GMT). No. of bitstreams: 0 Previous issue date: 2010-07-08Bitstream added on 2014-06-13T20:20:42Z : No. of bitstreams: 1 cavalheri_as_me_bauru.pdf: 1802164 bytes, checksum: 698a9c21192120139e25ee0dcbb758fa (MD5) / Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) / Neste trabalho foram estudadas amostras do Centro de Museologia, Antropologia e Arqueologia da FCT - UNESP de Presidente Prudente, o qual é coordenado pela professora Dra. Ruth Kunzli. As amostras foram caracterizadas por espectroscopia vibracional via espalhamento micro-Raman e a absorção no infravermelho com transformada de Fourier (FTIR), análise térmica por termogravimetria (TG) e energia dispersiva de raio-X (EDX). O objetivo principal do trabalho foi identificar os pigmentos utilizados na fabricação dos artefatos cerâmicos encontrados no sítio arqueológico Lagoa São Paulo - 02, Presidente Epitácio, SP, bem como os aditivos incorporados ao corpo cerâmico para entender como os arteftos foram confeccionados. Para o pigmento vermelho os resultados de Raman, FTIR, EDX e TG sugerem a utilização de hematia, um óxido de ferro consistente com o que podia ser encontrado nas rochas avermelhadas das encostas dos rios que eram desgastadas pela água. O pigmento preto apresenta bandas Raman características do carvão, provavelmente, este pigmento era encontrado na natureza como o produto da queima de material orgânico, possivelmente de origem vegetal. Para o pigmento branco, os espectros de FTIR e as curvas de TG sugerem o uso de caulim pela presença das bandas de absorção e do pico endotérmico em 550ºC aracterístico da caulinita, o que é consistente com os dados arqueológicos. Os aditivos identificados foram o carvão e o quartzo, sendo este último encontrado nas rochas presentes na região do sítio arqueológico. Tais aditivos são adicionados na confecção das cerâmicas para evitar o rachamento quando do cozimento, facilitar uma secagem homogênea e, ao mesmo tempo, reduzir a porosidade e a plasticidade. O processo de queima das amostras foi investigado via TG revelaram que todas elas passaram por processos de queima. Entretanto, os resultados sugerem que a amostra... / In this study samples from the Centro de Museologia, Antropologia e Arqueologia (CEMAARQ) of the UNESP Unip Estadual Paulista in Presidente Prudente, São Paulo State, Brazil, coordinated by professor Dra. Ruth Künzli, were investigated. The samples were characterized by vibrational spectroscopy via micro-Roman scattering and Fourier transform infrared absorption (FTIR), thermal analysis by termogravimetry (TG) and energy dispersive X-ray (EDX). The main objective was to identify the pigments used in the manufacture of ceramic artifacts found in the archaeological site Lagoa Sao Paulo - 02, Presidente Epitácio, SP, and the additives incorporated to the ceramic body to understand how the artifacts were made. For the red pigment of the results of Raman, FTIR, EDX e TG suggested the use of hematite, an iron oxide consistent with that found in the red rocks of the river banks eroded by water. The black pigment has Roman bands characteristic of charcol, probably, this pigment was found in nature as the product of burning organic material, possibly from vegetable. For the white pigment, the FTIR spectra and TG curves suggest the use of Kaolin by the presence of the absorption bands and the endothermic peak at 550ºC, characteristic of kaolinite, which is consistent with the archaeological data. The additives were identified as charcoal and quartz, the latter being found in rocks present in the archeological site. These additives are added in the manufacture of ceramics to prevent cracking when buring, to promote a homogeneous drying and to reduce porosity and plasticity. The burning process of the samples was investigated by TG and revealed that all of them were submitted to burning processes. However, the results suggest that the sample ... (Complete abstract click electronic access below)

This thesis presents results of the corrosion layers removal which could be found on the archaeological artefact surfaces. The low pressure low temperature plasma reduction was used for this purpose. Brass samples were chosen for this study. Two different ways have been used to form model corrosion layers. Several sets of corrosion layers were prepared in laboratory in two different corrosion atmospheres, namely ammonia atmosphere and atmosphere of hydrochloric acid. These samples were placed into desiccator. Small quantities of sand were added to some sets of samples so samples with sandy incrustation were prepared. The corrosion layers had been usually formed during four weeks. The second way, which was used to prepare model corrosion layer, was the natural corrosion in soil or compost. In this case, the corrosion layers had been formed approximately 2 years. The samples were treated in the low pressure (150 Pa) cylindrical Quartz reactor (90 cm long and 9.5 cm in diameter) with a pair of external copper electrodes connected via the matching network to a radiofrequency generator (13.56 MHz). The flows of working gases were set by independent mass flow controllers. Whole system was continuously pumped by the rotary oil pump which was separated from the discharge reactor by liquid nitrogen trap with aluminium chips eliminating dust and reactive species from the gas flow. Each sample was placed on a glass holder at the reactor center. Plasma was generated in pure hydrogen or in mixture of hydrogen and argon. Total flow of working gas was 50 sccm. Different ratios of gas mixture were tested, the ratio 30 sccm hydrogen and 20 sccm argon flows was the best. RF discharge was used in a continuous and pulsed regime. Pulsed mode was carried out with various duty cycle at the frequency of 1000 Hz. There were two ways of temperature monitoring. The sample temperature during the treatment was monitored by a K-type thermocouple installed inside the sample in the first case. Thermometer optical probe was connected to the sample surface by a small stainless plate and allowed continuous sample temperature monitoring in the second way. Safe object temperature for copper and copper alloys is 100–120 °C. To avoid exceeding this temperature, power control or the duty cycle in pulse mode were automatically controlled if thermometer optical probe was used. Plasma chemical treatment is based on generation of reactive atomic hydrogen in plasma discharge. The main reactions during reduction were reactions between oxygen and chloride contained in the corrosion layer and the hydrogen ions and neutral atoms generated in the plasma. These reactions create an unstable OH radical, which emits light in the region of 306–312 nm. This radiation was detected by the optical emission spectroscopy using Ocean Optics HR4000 spectrometer with 2400 gr/mm grating. Data obtained from this method were used to calculate rotational temperatures and integral intensity of OH radicals that were used for the process monitoring. Corrosion layer was not completely removed during the reduction, but due to the reactions which occur in the plasma corrosion layer became brittle and after plasma chemical treatment can be removed easily. The SEM-EDS material analyses were carried out before and after treatment of some samples. Some samples were analysed by XRD analysis. EDS analysis showed that amount of oxygen and chloride was decreased, mainly at 400 W pulse mode.