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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
21

Caracterização química multitécnicas de tintas artísticas brasileiras, um estudo de caso / Multi-technique chemical characterization of Brazilian artistic paints, a case study

Marcelo Miyada Redigolo 30 November 2018 (has links)
O presente trabalho apresenta a caracterização química de tintas artísticas brasileiras. Diferente de outras matrizes, os materiais de arte fabricados no Brasil não apresentam informações na literatura que auxiliem em sua conservação e restauração. Amostras de tintas acrílicas e a óleo, nacionais e importadas, foram analisadas pelas técnicas espectroscópicas Raman e infravermelho por transformada de Fourier (FTIR), pirólise acoplada a cromatografia a gás e espectrometria de massas (Py-GC/MS) e microscopia eletrônica de varredura acoplada a espectrometria de fluorescência de raios X (SEM-EDS). Resultados de análise indicam que tintas acrílicas brasileiras são compostas por poliestireno (PS), diferentemente das importadas, compostas por polimetilmetacrilato (PMMA). Enquanto as tintas a óleo apresentam composição semelhante (óleo de linhaça), brasileiras e importadas. Duas pinturas do acervo da Pinacoteca do Estado de São Paulo foram selecionadas para um estudo de caso. As obras apresentam a formação de exsudatos em sua superfície, o que demanda a caracterização química como etapa anterior ao desenvolvimento de uma metodologia de restauração. A obra \"Mandala da saudade\", de Sara Goldman-Belz, é composta por tinta spray (alkyd) e a obra \"Três pessoas\", de Marina Saleme, por tinta a óleo. Os resultados de análise apresentam um primeiro passo no estabelecimento de um banco de dados de materiais artísticos fabricados no Brasil para fins de restauração e perícia criminal de obras de arte. / The current work presents the chemical characterization of Brazilian artistic paints. Differently from other matrices, art materials produced in Brazil lack for information in literature that help in their conservation and restoration. Acrylic and oil paint samples, Brazilian and imported, were analyzed by Raman and Fourier transform infrared (FTIR) spectroscopies, pyrolysis coupled with gas chromatography and mass spectrometry (Py-GC/MS) and scanning electron microscopy coupled with x-ray fluorescence spectrometry (SEM-EDS). Results indicate that Brazilian acrylic paints are composed of polystyrene (PS), differently from imported ones, composed of polymethyl methacrylate (PMMA). Whereas, oil paints present similar composition (linseed oil), Brazilian and imported. Two paintings from the collection of Pinacoteca do Estado de São Paulo were selected for a case study. Both works of art present formation of exudates on their surface, which demands chemical characterization as a previous step to the development of a restoration methodology. The painting \"Mandala da saudade\", by Sara Goldman-Belz, is composed of spray paint (alkyd) and the painting \"Três pessoas\", by Marina Saleme, is composed of oil paint. Results presented in this thesis are the first step towards the establishment of a database for artistic materials produced in Brazil for purposes of art restoration and forensic science.
22

Caracterização química multitécnicas de tintas artísticas brasileiras, um estudo de caso / Multi-technique chemical characterization of Brazilian artistic paints, a case study

Redigolo, Marcelo Miyada 30 November 2018 (has links)
O presente trabalho apresenta a caracterização química de tintas artísticas brasileiras. Diferente de outras matrizes, os materiais de arte fabricados no Brasil não apresentam informações na literatura que auxiliem em sua conservação e restauração. Amostras de tintas acrílicas e a óleo, nacionais e importadas, foram analisadas pelas técnicas espectroscópicas Raman e infravermelho por transformada de Fourier (FTIR), pirólise acoplada a cromatografia a gás e espectrometria de massas (Py-GC/MS) e microscopia eletrônica de varredura acoplada a espectrometria de fluorescência de raios X (SEM-EDS). Resultados de análise indicam que tintas acrílicas brasileiras são compostas por poliestireno (PS), diferentemente das importadas, compostas por polimetilmetacrilato (PMMA). Enquanto as tintas a óleo apresentam composição semelhante (óleo de linhaça), brasileiras e importadas. Duas pinturas do acervo da Pinacoteca do Estado de São Paulo foram selecionadas para um estudo de caso. As obras apresentam a formação de exsudatos em sua superfície, o que demanda a caracterização química como etapa anterior ao desenvolvimento de uma metodologia de restauração. A obra \"Mandala da saudade\", de Sara Goldman-Belz, é composta por tinta spray (alkyd) e a obra \"Três pessoas\", de Marina Saleme, por tinta a óleo. Os resultados de análise apresentam um primeiro passo no estabelecimento de um banco de dados de materiais artísticos fabricados no Brasil para fins de restauração e perícia criminal de obras de arte. / The current work presents the chemical characterization of Brazilian artistic paints. Differently from other matrices, art materials produced in Brazil lack for information in literature that help in their conservation and restoration. Acrylic and oil paint samples, Brazilian and imported, were analyzed by Raman and Fourier transform infrared (FTIR) spectroscopies, pyrolysis coupled with gas chromatography and mass spectrometry (Py-GC/MS) and scanning electron microscopy coupled with x-ray fluorescence spectrometry (SEM-EDS). Results indicate that Brazilian acrylic paints are composed of polystyrene (PS), differently from imported ones, composed of polymethyl methacrylate (PMMA). Whereas, oil paints present similar composition (linseed oil), Brazilian and imported. Two paintings from the collection of Pinacoteca do Estado de São Paulo were selected for a case study. Both works of art present formation of exudates on their surface, which demands chemical characterization as a previous step to the development of a restoration methodology. The painting \"Mandala da saudade\", by Sara Goldman-Belz, is composed of spray paint (alkyd) and the painting \"Três pessoas\", by Marina Saleme, is composed of oil paint. Results presented in this thesis are the first step towards the establishment of a database for artistic materials produced in Brazil for purposes of art restoration and forensic science.
23

Utilização da técnica de fluorescência de raios X por dispersão em energia (EDXRF) na avaliação do material particulado em suspensão na cidade de Limeira - SP / Using energy dispersive X ray fluorescence (EDXRF) technique to evaluate the suspended particulate matter from Limeira city, State of São Paulo, Brazil

Liz Mary Bueno de Moraes 31 August 2009 (has links)
O objetivo principal deste trabalho foi avaliar a composição química do material particulado em suspensão na atmosfera na cidade de Limeira/SP, pela técnica de fluorescência de raios X dispersiva em energia (EDXRF). Um amostrador tipo stacker foi utilizado para coletar particulados fino (partículas com diâmetro aerodinâmico entre 2,5 e 10 \'mü\'m) e grosso (partículas maiores que 10 \'mü\'m), utilizando filtros de policarbmüonato de 47 mm de diâmetro e com diâmetros de poro de 0,4 e 8 \'mü\'m, respectivamente. As amostras foram coletadas em 2006 (de janeiro a dezembro), 2008 (de janeiro a abril e de julho a dezembro) e 2009 (de janeiro a março). Na excitação da técnica de EDXRF utilizou-se um tubo de Mo com filtro de Fe (análise sob vácuo) para a determinação dos elementos do Al ao Ca, e com filtro de Zr (análise sob ar atmosférico) para determinação do Sc ao Zn e também do Pb. Para a detecção dos raios X utilizou-se um detector semicondutor de Si(Li) acoplado a um analisador multicanal, com um tempo de aquisição de 300 s. Os espectros de raios X foram interpretados através do programa AXIL e a para a quantificação dos elementos químicos fez-se o uso da metodologia dos parâmetros fundamentais. Realizou-se também microanálises nas amostras utilizando-se um microscópio eletrônico de varredura acoplado a um sistema de fluorescência de raios X por dispersão em energia (SEM/EDS) para a caracterização química e morfológica das partículas coletadas no material particulado em suspensão. Determinou-se também a concentração de negro de fumo (black carbon) utilizando a técnica de reflectância. Embora a amostragem não tenha sido suficiente para indicar a contribuição de cada fonte de emissão, a metodologia de análise de agrupamento possibilitou a identificar duas principais fontes para o material particulado em suspensão: poeira de solo e resíduos de queima de cana-de-açúcar / The main objective of this work was to evaluate the chemical composition of the suspended particulate matter from the atmosphere of the city of Limeira, State of São Paulo, by energy dispersive X-ray fluorescence (EDXRF) technique. A stacker filter sampler was used to collect the fine (particles with aerodynamic diameter between 2.5 and 10 \'mü\'m) and the gross particulates (particles larger than 10 \'mü\'m) employing 47 mm polycarbonate filters, with 0.4 and 8 \'mü\'m pore diameters, respectively. Samples were collected in 2006 (from January to December), 2008 (from January to April and from July to December), and 2009 (from January to March). The EDXRF excitation was carried out using a Mo X-ray tube with Fe filter (analysis under vacuum) to determine elements from Al to Ca, and with Zr filter (analysis under air atmosphere) to determine from Sc to Zn and also Pb. A Si(Li) semiconductor detector coupled to a multichannel analyzer was used for X-ray detection, with 300 s acquisition time. The X-ray spectra were deconvoluted by the AXIL software, and fundamental parameters methodology was adopted for quantification. Samples microanalysis by scanning electron microscope, connected to an energy dispersive X-ray fluorescence system (SEM/EDS) was carried out for chemical and morphological characterization of collected particles in the suspended particulate matter. Black carbon content was also evaluated by reflectance. Despite the fact that the sampling was not enough to indicate the contribution of each emission source, grouping analysis statistical method allowed to identify two main sources of the particulate matter in suspension: dust soil and sugar cane burning residues
24

Efeito de três diferentes doses de radiação com raios-X na microdureza, morfologia superficial, espectrometria de energia dispersiva de radios-X (EDS) e resistência de união ao esmalte e dentina com dois diferentes sistemas adesivos / The effect of three different doses of radiation with x-rays in the microhardness, superficial morfology, energy dispersive X-ray spectroscopy (EDS) and bond strength of enamel and dentin with two adhesive systems

Sandra Ribeiro de Barros da Cunha 19 January 2015 (has links)
Este estudo teve como objetivo analisar dentina e esmalte irradiados com diferentes doses de radiação ionizante com raios-x (20, 40 e 70Gy), através da microdureza, morfologia superficial, conteúdo mineral e resistência de união com adesivo de condicionamento total de 2 etapas (Adper Single Bond 2) e um novo sistema adesivo, universal, com a técnica auto-condicionante (Universal Single Bond). Oitenta e quatro terceiros molares humanos foram cortados, separados e preparados para cada ensaio. Para os ensaios de microdureza e microcisalhamento as amostras foram incluídas em resina acrílica e polidas. Para a microscopia eletrônica de varredura (MEV) e espectrometria de energia dispersiva de raios-x (EDS), as amostras foram fixadas em solução de glutaraldeído 3%, lavadas em solução de cacodilato 0,1M e desidratadas em álcool etílico crescente. A microdureza (n=30) foi realizada pré e pós-radioterapia, com força de 50gf em esmalte cervical, médio e oclusal e 25gf em dentina profunda, média e rasa, por 30s. As amostras para o microcisalhamento foram divididas em 4 grupos (n=20) e 2 subgrupos (n=10) conforme o sistema adesivo. Foram construídos 3 corpos de prova cilíndricos com 1mm de diâmetro e altura em cada amostra. O teste de microcisalhamento foi realizado em máquina de ensaio universal com velocidade de 1mm/min. Os resultados indicam perda de propriedade de microdureza apenas em esmalte cervical em todas as três doses (20Gy pré-radioterapia: 298,04±11,80 e pós-radioterapia: 294,36±16,68; 40Gy pré-radioterapia: 285±19,45 e pósradioterapia: 275,3±36; 70Gy pré-radioterapia: 291,98±16,51 e pós-radioterapia: 283,68 ± 21,64) e em dentina em todas as profundidades (profunda: 20Gy préradioterapia: 57,79±1,96; pós-radioterapia: 55,37±1,30; 40Gy pré-radioterapia: 57,31±1,76; pós-radioterapia: 55,83±1,63; 70Gy não apresentou alterações; média: 20Gy pré-radioterapia: 58,05±1,79; pós-radioterapia: 55,36±1,20; 40Gy préradioterapia: 57,87± 2,04; pós-radioterapia: 55,65 ± 2,48; 70Gy não apresentou alterações; rasa: 20Gy pré-radioterapia: 56,60±12,17; pós-radioterapia: 55,18±2,57; 40Gy pré-radioterapia: 57,36±2,78; pós-radioterapia: 55,18± 2,57; 70Gy préradioterapia: 55,08±1,94; pós-radioterapia: 54,72±2,57). O teste de microcisalhamento não apresentou diferença significativa entre grupo controle e as 3 doses, tanto para esmalte (p=0,325) como para dentina (p=0,719), apresentando o adesivo Universal Single Bond, em dentina, a resistência de união mais satisfatória. A análise de padrão de fratura para dentina, indicou um maior número de rupturas coesivas em dentina na dose 70Gy quando comparada ao grupo controle. Em esmalte prevaleceram as fraturas do tipo adesivas. As eletromicrografias apresentaram alterações apenas em esmalte na dose 70Gy, com prismas de esmalte mais curtos e arredondados. O EDS mostrou que o conteúdo mineral permaneceu intacto em ambos substratos. Dentro das limitações de um estudo in vitro, conclui-se que a radiação ionizante apresenta maior interação preferencialmente em dentina, no entanto, o EDS mostra não haver modificação no conteúdo mineral em ambos substratos. Existe uma diminuição da microdureza em dentina, porém as alterações não são suficientes para interferir na resistência de união dos substratos irradiados, que mostraram resultados mais satisfatórios com o sistemas adesivos universal, utilizando-se a técnica auto-condicionante. / The aim of this study was to evaluate the effects of different doses (20Gy, 40Gy and 70Gy) of ionizing radiation with x-rays in the microhardness, superficial morphology, mineral content and bonding effectiveness with a 2 steps all-etch adhesive (Adper Single Bond 2) and the new generation of adhesive, the universal adhesive system, (Universal Single Bond), using the self-etch technique. Eighty-four third molars were cutted, separed and prepared for each assay. For the microshear-bond and microhardness the samples were included in acrylic resin and then polished. For the scanning electron miscroscopy (SEM) and energy dispersive x-ray spectroscopy (EDS), the samples were fixated in a 3% glutaraldehyde solution, washed in 0,1M cacodylate solution and dehydrated in increscent concentrations of ethyl alcohol. The microhardness (n=30) was held pre and post radiotherapy with 50gf on cervical, middle and occlusal enamel and 25kg on superficial, middle and deep dentin, both cases with 30s. The microshear-bond was divided in 4 groups (n=20) and 2 subgroups (n=10) according to the adhesive system. Three cylinders were built with 1mm in diameter and heigh in every sample. The assay were accomplished at an universal testing machine with 1mm/min. Results indicate loss of microhardness properties only in cervical enamel at all 3 doses (20Gy pre-radiotheraphy: 298,04 ± 11,80 and post-radiotherapy: 294,36 ± 16,68; 40Gy pre-radiotherapy: 285 ± 19,45 and post-radiotherapy: 275,3 ± 36; 70Gy pre-radiotherapy: 291,98 ± 16,51 and post-radiotherapy: 283,68 ± 21,64) and in all dentin depths (deep: 20Gy preradiotherapy: 57,79 ± 1,96; post-radiotherapy: 55,37 ± 1,30; 40Gy pre-radiotherapy: 57,31 ± 1,76; post-radiotherapy: 55,83 ± 1,63; 70Gy showed no alteration; Middle: 20Gy pre-radiotherapy: 58,05 ± 1,79; post-radiotherapy: 55,36 ± 1,20; 40Gy preradiotherapy: 57,87 ± 2,04; post-radiothetrapy: 55,65 ± 2,48; 70Gy showed no alteration; Superficial: 20Gy pre-radioterapia: 56,60 ± 12,17; post-radiotrapia: 55,18 ± 2,57; 40Gy pre-radiotherapy: 57,36 ± 2,78; post-radiotherapy: 55,18 ± 2,57; 70Gy pre-radiotherapy: 55,08 ± 1,94; post-radiotherapy: 54,72 ± 2,57). The microshearbond test did not show significant difference between the control group and the 3 doses, both enamel (p=0.325) and dentin (p=0.719), showing better bonding with Universal Single Bond adhesive in dentin. The fracture pattern analysis indicated a larger number of cohesive failure in dentine with the 70Gy dose when compared with control group. The micrographs showed changes only on enamel at 70Gy dose, with shorter and rounder prisms. EDS test indicated no changes in mineral content for both substrates. Knowing the limitations of an in vitro study, it were concluded that ionizing radiation shows deleterious effects preferentially in dentin, probably due to it\'s high organic content, since EDS showed no modifications both enamel and dentin. There is a reduction in microhardness on dentin, but the changes are not enough to interfere at bonding properties of irradiated substrates, showing better results when used the universal adhesive with the self-etch techniques.
25

La composition des thèques d'amibes xénosomiques : utilisation potentielle comme bio-indicateur des dépôts de particules d’origine atmosphérique / Xenomic testate amoebae shells composition : potential use as bio-indicator of atmospheric particle deposits

Delaine, Maxence 19 November 2016 (has links)
Les amibes à thèque, également appelés thécamoebiens, sont des micro-organismes unicellulaires, qui construisent une enveloppe rigide, appelée thèque (Adl et al., 2012). Ces thèques ont des tailles, formes et natures très variées (Ogden & Hedley, 1980). Les récentes études sur la composition des thèques ont conduit à émettre l’hypothèse que les amibes xénosomiques (constituées de particules exogènes), peuvent constituer des bio-indicateurs pertinents de la diversité particulaire de l’environnement minéral, organique et biologique dans lequel elles évoluent.L’objectif principal des recherches menées au cours de cette thèse vise donc à caractériser la composition des thèques d’amibes xénosomiques et à en évaluer leur utilisation potentielle en tant que bio-indicateurs des dépôts de particules d'origine atmosphérique. Pour cela, des thèques d’amibes ont été analysées in situ en conditions naturelles et après dépôts artificiels de particules minérales allochtones.Ces travaux permettent de dégager plusieurs conclusions majeures :(1) La taille des particules minérales intégrées dans la thèque xénosomique de Bullinularia indica est similaire à celle des particules minérales transportées dans l'atmosphère; (2) les particules minérales intégrées dans les thèques sont des silicates stables dans les conditions physico-chimiques régnant dans les tourbières, les bryophytes et les sols étudiés; (3) certains minéraux comme la phlogopite, même lorsqu’ils sont présents en de fortes concentrations, ne sont jamais intégrés par les amibes; (4) la combinaison des observations portant sur la taille, la forme et la nature des particules utilisées par des amibes xénosomiques permet de poser les bases de l'utilisation des amibes à thèques pour la bio-indication de la diversité particulaire atmosphérique récente ou ancienne. / Theca-like amoebae, also called thecaamoebius, are unicellular microorganisms, which construct a rigid envelope called theca (Adl et al., 2012). These themes have very varied sizes, shapes and natures (Ogden & Hedley, 1980). Recent studies on the composition of the themes have led to the hypothesis that xenosomal amoebae (constituted by exogenous particles) can constitute relevant bio-indicators of the particulate diversity of the mineral, organic and biological environment in which they evolve . The main objective of the research carried out during this thesis is therefore to characterize the composition of the xenosomal amoebae and to evaluate their potential use as bioindicators of deposits of atmospheric particles. For this purpose, amoeba theae were analyzed in situ under natural conditions and after artificial deposits of allochtonous mineral particles. Several major conclusions can be drawn from this work: (1) The size of the mineral particles integrated in the xenosomal theca of Bullinularia indica Is similar to that of mineral particles transported into the atmosphere; (2) the mineral particles integrated into the thecs are stable silicates under the physico-chemical conditions prevailing in the peatlands, bryophytes and soils studied; (3) some minerals such as phlogopite, even when present in high concentrations, are never integrated by amoebae; (4) the combination of observations on the size, shape and nature of the particles used by xenosomic amoebae forms the basis for the use of tea amoeba for bioindication of recent or former atmospheric particulate diversity .
26

Characterization of non-metallic inclusions according to morphology and composition : A comparison of two different steels before and after turning

Gram, Tove, Vickerfält, Amanda January 2015 (has links)
Investigation of non metallic inclusions in two different steels from Sandvik was made before and after turning. After dissolving the non-metallic inclusions by electrolytic extraction the particles were analysed manually or by INCA feature. This was referred to as 3D analysis. INCA feature analysis without extraction of particles was also performed, this was referred to as 2D analysis. The aim of the report was to a make a characterization of non-metallic inclusions with respect to chemical composition, aspect ratio, size and shape. The aim was also to compare different investigation methods. Samples were prepared and investigated. It was obtained that inclusions with sulphur content was elongated and crushed during the turning process. Broken sulphides were detected in one of the steels, and broken oxysulphides in the other steel in the electrolytically extracted chips created by turning. The first steel, steel 1, mainly contained sulphide and oxysulphide inclusions, and steel 2 mainly contained oxysulphides. The aspect ratio obtained by 2D analysis of the sulphide inclusions in steel 1 before turning showed similar results to the electrolytic extracted inclusions measured by hand. The aspect ratio increased with the length of the inclusion. However the deviation of data obtained by the 2D analysis was larger than deviation from the extracted particles measured by hand. The reason for this was assumed to be that the 2D method was not able to analyse the true shape of the inclusions e.g. if inclusions were partly concealed by metal matrix. In analysis of steel 2 the average aspect ratio decreased for oxides and increased for oxysulphides after turning. The chemical composition of inclusions did not change after the turning process for neither of the steels. Copper was detected in the electrolytic extracted inclusions, however not in the 2D investigation by SEM. This is an interesting topic for future research.
27

Precipitation Study in a High Temperature Austenitic Stainless Steel using Low Voltage Energy Dispersive X-ray Spectroscopy

Gharehbaghi, Ali January 2012 (has links)
Precipitation of second phase particles is a key factor dominating the mechanical properties of high temperature alloys. In order to control and optimize the precipitation effect it is of great importance to study the role of alloying elements in the formation and stability of precipitates. As a favored family of corrosion and creep resistant austenitic stainless steels the 20Cr-25Ni alloy was modified by addition of copper, molybdenum, nitrogen, niobium and vanadium. A set of alloys with similar matrix but varying contents of niobium, vanadium and nitrogen were prepared. Sample preparation process included melting, hot forging, solution annealing and finally aging for 500 h at 700, 800 and 850 ºC. Light optical and scanning electron microscopy revealed micron-scale precipitates on grain and twin boundaries as well as sub-micron intragranular precipitates in all samples. Characterization of precipitates was carried out by means of energy dispersive X-ray spectroscopy (EDS). Among micron-scale precipitates M23C6 carbide was the dominant phase at 700 ºC aging temperature; whereas silicon-rich eta phase (M5SiC) was the main precipitate in samples aged at 800 and 850 ºC. A few sigma phase particles were found in one of the niobium containing samples aged at 700 and 800 ºC. Sub-micron intragranular precipitates were analyzed using low voltage EDS. The spatial resolution of EDS microanalysis at 5 kV accelerating voltage was estimated as almost 100 nm which was at least eight times better than that using the ordinary 20 kV voltage. Also, low voltage EDS revealed the presence of light elements (carbon, nitrogen and boron) in the composition of sub-micron particles thanks to the less matrix effect in absorption of low energy X-rays of light elements. In samples aged at 700 ºC niobium-rich and vanadium-rich carbonitrides were found as the dominant precipitates; whereas they contained much less carbon in samples aged at 800 ºC and mostly became carbon-free nitrides with well-defined cuboidal shapes at 850 ºC aging temperature. This showed that niobium/vanadium-rich nitride phases are stable precipitates at aging temperatures above 700 ºC. The drawbacks of low voltage EDS were indicated as high detection limit (no detection of low- content elements), poor accuracy of quantitative analysis and high sensitivity to surface contamination. Some possible ways to improve the accuracy of low voltage EDS, e.g. longer acquisition time were examined and some other suggestions are proposed for future works.
28

Precipitation Study in a High Temperature Austenitic Stainless Steel using Low Voltage Energy Dispersive X-ray Spectroscopy

Gharehbaghi, Ali January 2012 (has links)
Precipitation of second phase particles is a key factor dominating the mechanical properties of high temperature alloys. In order to control and optimize the precipitation effect it is of great importance to study the role of alloying elements in the formation and stability of precipitates. As a favored family of corrosion and creep resistant austenitic stainless steels the 20Cr-25Ni alloy was modified by addition of copper, molybdenum, nitrogen, niobium and vanadium. A set of alloys with similar matrix but varying contents of niobium, vanadium and nitrogen were prepared. Sample preparation process included melting, hot forging, solution annealing and finally aging for 500 h at 700, 800 and 850 ºC.Light optical and scanning electron microscopy revealed micron-scale precipitates on grain and twin boundaries as well as sub-micron intragranular precipitates in all samples. Characterization of precipitates was carried out by means of energy dispersive X-ray spectroscopy (EDS). Among micron-scale precipitates M23C6 carbide was the dominant phase at 700 ºC aging temperature; whereas silicon-rich eta phase (M5SiC) was the main precipitate in samples aged at 800 and 850 ºC. A few sigma phase particles were found in one of the niobium containing samples aged at 700 and 800 ºC. Sub-micron intragranular precipitates were analyzed using low voltage EDS. The spatial resolution of EDS microanalysis at 5 kV accelerating voltage was estimated as almost 100 nm which was at least eight times better than that using the ordinary 20 kV voltage. Also, low voltage EDS revealed the presence of light elements (carbon, nitrogen and boron) in the composition of sub-micron particles thanks to the less matrix effect in absorption of low energy X-rays of light elements. In samples aged at 700 ºC niobium-rich and vanadium-rich carbonitrides were found as the dominant precipitates; whereas they contained much less carbon in samples aged at 800 ºC and mostly became carbon-free nitrides with well-defined cuboidal shapes at 850 ºC aging temperature. This showed that niobium/vanadium-rich nitride phases are stable precipitates at aging temperatures above 700 ºC.The drawbacks of low voltage EDS were indicated as high detection limit (no detection of low- content elements), poor accuracy of quantitative analysis and high sensitivity to surface contamination. Some possible ways to improve the accuracy of low voltage EDS, e.g. longer acquisition time were examined and some other suggestions are proposed for future works.
29

Re-evaluating the Exercise Dependence Scale-Revised and the prevalence of exercise dependence in Sweden

Isaacson, Joseph January 2023 (has links)
The purpose of this study was to investigate the prevalence of exercise dependence, as well as conducting a re-evaluation of the Exercise Dependence Scale-Revised (EDS-R) through a confirmatory factor analysis. The study was based on three Swedish data collections (N = 1101), collected through online questionnaires answered by physically active adults. The study found a prevalence of exercise dependence between 3.6-9%, primary exercise dependence between 1.7-2.2%, and a prevalence of primary exercise dependence with anxiety management as motivation of 1.8% across the three data-collections. The confirmatory factor analysis revealed that the hypothesized 21-item 7-factor structure of the EDS-R contributed to a tolerable fit of data with good psychometric properties, although a poor factor loading of item 19 in the factor ‘Reduction in other activities’ was found. This study concludes that the EDS-R is a valid measurement of exercise dependence, but further research is needed to evaluate the relation between primary exercise dependence and anxiety management, as well as the construct validity of the individual items. / Syftet med denna studie var att undersöka prevalensen av träningsberoende, samt utföra en omvärdering av träningsberoendeskalan-reviderad (EDS-R) genom en konfirmatorisk faktoranalys. Studien baserades på tre svenska datakollektioner (N = 1101), insamlade genom online-enkäter besvarade av fysiskt aktiva vuxna. Studien fann en prevalens av träningsberoende mellan 3.6-9%, primärt träningsberoende mellan 1.7-2.2%, och en prevalens av primärt träningsberoende med ångesthantering som motivation på 1.8% över de tre datakollektionerna. Den konfirmatoriska faktoranalysen avslöjade att den hypotiserade 21-objekt 7-faktor strukturen av EDS-R bidrog till en tolerabel passform av data med goda psykometriska egenskaper, även om en dålig faktorladdning av objekt 19 i faktorn 'Reduktion i andra aktiviteter' hittades. Denna studie drar slutsatsen att EDS-R är ett giltigt mått på träningsberoende, men ytterligare forskning behövs för att utvärdera relationen mellan primärt träningsberoende och ångesthantering, samt konstruktionsvaliditeten för de enskilda objekten.
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Characterization of Secondary Carbides in Low-Alloyed Martensitic Model Alloy Tool Steels

Jubica, Jubica January 2020 (has links)
The development of tool steels for making and shaping other materials requires a better understanding of the material's properties during manufacture. These high-quality steels include many alloying elements, which give increased hardness during tempering. For producing hardened microstructures, austenite generation is essential. The martensite formed by rapid quenching of austenite followed by tempering helps develop high strength steels. Studying carbide precipitation is a challenge as they are very small in size, present only in small volume fractions and high number densities. The carbide reactions are complicated due to so-called metastable carbides, which are only present as part of the precipitation process. This work focuses on model alloys with two main elements in addition to iron and carbon, molybdenum, and vanadium, to clarify and simplify the carbide characterization. This is done to determine the effect of molybdenum and vanadium carbides on the overall hardness. In this work, two model alloys, A and B, are tempered at 550°C and 600°C with the same vanadium content but different molybdenum contents. The hardness of the materials is evaluated and compared at these temperatures. A more detailed characterization work is done for material A with Scanning Transmission Electron Microscopy-Energy Dispersive Spectroscopy (STEM-EDS) to understand the microstructure and analyze the precipitates. Simulations are performed with Thermo-Calc Prisma (TC-Prisma) to support the experimental work, which includes the simulation of the secondary carbide precipitation, mainly molybdenum carbides in material A tempered for 24h at 600°C, and predicts the carbide precipitation behavior in this steel. The results from STEM-EDS and TC-Prisma for material A, show that the small secondary carbides in the martensite contribute to the increased strength of material A. Due to the overaging of the carbides at 600°C, the hardness at 550°C is higher than at 600°C for material A. The given thesis work is an attempt to interpret the development of secondary carbides of Mo and V in the martensitic matrix and their role in the overall hardness. / Den ständiga utvecklingen av högpresterande stål för transport, konstruktion och energisektorn kräver bättre förståelse för materialets egenskaper vid tillverkning. Dessa martensitiska stål inkluderar många legeringselement vilket ger ökad hårdhet vid härdning och anlöpning. Att studera utskiljning av karbider är en utmaning eftersom de är närvarande endast i liten volymsfraktion. Karbidreaktionerna är komplexa till följd av så kallade metastabila karbider vilka endast är närvarande vid en del av utskiljningsförloppet. För att tydliggöra och förenkla karbidkarakteriseringen fokuserar detta arbete på modellegeringar med två huvudelement utöver järn och kol, molybden och vanadin. Detta görs för att fastställa effekten av molybden och vanadinkarbider på den totala hårdheten. I detta arbete studeras två modellegeringar, A och B, härdade och anlöpta vid 550 °C och 600 °C med samma vanadininnehåll men olika molybdeninnehåll. Materialens hårdhet utvärderas och jämförs vid dessa temperaturer. Ett mer detaljerat karaktäriseringsarbete görs för material A med hjälp av STEM-EDS för att förstå mikrostrukturen och analysera utskiljningarna. Simuleringar görs med TC-PRISMA för att stödja det experimentella arbetet, vilket inkluderar simulering av den sekundära karbidutskiljningen och predikterar karbidstrukturen i dessa stål. Resultaten visar att de små sekundärkarbiderna i martensiten bidrar till den ökade styrkan hos material A. Hårdheten vid 550 °C är högre än vid 600 °C för material A eftersom både utskiljningen av karbider är sker långsammare och även dislokationsåterhämtning.

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