Nanopartículas aciculares metálicas de 'Fe', 'Fe''Co', 'Fe''TR' e 'Fe''Co''TR'('TR'='La'-'Tb') para tecnologia avançada de gravação magnética
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Data
2003
Autores
Varanda, Laudemir Carlos [UNESP]
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Editor
Universidade Estadual Paulista (Unesp)
Resumo
Neste trabalho, nanopartículas metálicas (NPM) aciculares e monodispersas de FeCo, FeTR (TR = Nd, Eu, Sm e Tb) e FeCoTR (TR = La-Tb), com ~60 nm de comprimento, razão axial de ~6 e estáveis frente à oxidação e sinterização foram obtidas pela redução em atmosfera de hidrogênio de NP de goetita contendo Co ou Co/TR e recobertas com alumina. O precursor na forma de NP de goetita monodispersas (60±5 nm de comprimento e razão axial de ~6) foi obtido por uma nova rota sintética baseado na hidrólise alcalina de íons Fe(III) em solução na presença de íons carbonato em três estágios: (i) formação de ferrihidrita, (ii) dissolução da ferrihidrita e nucleação de goetita, e (iii) crescimento dos núcleos de goetita. Duas temperaturas distintas foram utilizadas para a nucleação e o crescimento das partículas de goetita e o mecanismo de formação das NP monodispersas de goetita pode ser proposto. NP aciculares e monodispersas de hematita (210±20 nm de comprimento e razão axial de ~5) também foram sintetizadas por reações de hidrólise ácida forçada, e o mecanismo de transformação de -Fe2O3 a -Fe foi avaliado. NP de hematita foram recobertas com agentes antisinterizantes (sílica ou alumina), reduzidas a metal em atmosfera de hidrogênio (450 °C/12 h) e passivadas utilizando uma nova metodologia de passivação: uma mistura de vapores de etanol e gás nitrogênio passada pela amostra durante 15-20 min (processo comercial: nitrogênio:oxigênio (1:1) durante 4-6 h). NP recobertas com sílica apresentaram pequenas partículas esféricas metálicas encapsuladas em um molde acicular de sílica, conduzindo a perda da forma elipsoidal da fase metálica. NP recobertas com alumina resultaram em partículas aciculares metálicas recobertas com uma fina camada do agente anti-sinterizante (alumina) e estabilizadas pela formação...
Acicular monodispersed, metallic nanoparticles (MNP) of FeCo, FeRE (RE = Nd, Eu, Sm and Tb) and FeCoRE (RE = La-Tb), ~60 nm in the length and axial ratio ~6, stabilized against oxidation and sintering, obtained by reduction of alumina-coated goethite NP containing either Co or Co/RE under hydrogen flow were reported. Monodispersed goethite NP precursor (60±5 nm in length, axial ratio ~6) was obtained by a new synthetic route based on the hydrolysis of alkaline Fe(III) solutions in the presence of carbonate ions by a three step-procedure: (i) ferrihydrite formation, (ii) ferrihydrite dissolution and goethite nucleation, and (iii) goethite nuclei growth. Two different temperatures to promote goethite nucleation and growth were used and the formation mechanism of monodispersed goethite NP was proposed. Monodispersed and acicular hematite NP (210±20 nm in length, axial ratio ~5) were also synthesized by forced acid hydrolysis reaction, and the transformation mechanism from -Fe2O3 to -Fe was evaluated. Hematite was covered with anti-sintering agents (silica or alumina), reduced to metal in hydrogen atmosphere (450 °C/12 h) and passivated using a new methodology: ethanol vapors and nitrogen gas mixture for 15-20 min (commercial procedure: nitrogen:oxygen (1:1) gas mixture for 4-6 h). Silica-coated NP showed small metallic spherical particles encapsulated in an acicular silica template, leading to ellipsoidal-shape metallic phase loss. Alumina-coated particle showed an acicular metallic particle with thin layer anti-sintering alumina agent stabilized by maghemite thin layer on particle surface. The influence of the temperature, hydrogen flows and reduction time on the magnetic properties, crystallite size, crystallographic structure and phases were also investigated. A topotatic ...(Complete abstract, click electronic access below)
Acicular monodispersed, metallic nanoparticles (MNP) of FeCo, FeRE (RE = Nd, Eu, Sm and Tb) and FeCoRE (RE = La-Tb), ~60 nm in the length and axial ratio ~6, stabilized against oxidation and sintering, obtained by reduction of alumina-coated goethite NP containing either Co or Co/RE under hydrogen flow were reported. Monodispersed goethite NP precursor (60±5 nm in length, axial ratio ~6) was obtained by a new synthetic route based on the hydrolysis of alkaline Fe(III) solutions in the presence of carbonate ions by a three step-procedure: (i) ferrihydrite formation, (ii) ferrihydrite dissolution and goethite nucleation, and (iii) goethite nuclei growth. Two different temperatures to promote goethite nucleation and growth were used and the formation mechanism of monodispersed goethite NP was proposed. Monodispersed and acicular hematite NP (210±20 nm in length, axial ratio ~5) were also synthesized by forced acid hydrolysis reaction, and the transformation mechanism from -Fe2O3 to -Fe was evaluated. Hematite was covered with anti-sintering agents (silica or alumina), reduced to metal in hydrogen atmosphere (450 °C/12 h) and passivated using a new methodology: ethanol vapors and nitrogen gas mixture for 15-20 min (commercial procedure: nitrogen:oxygen (1:1) gas mixture for 4-6 h). Silica-coated NP showed small metallic spherical particles encapsulated in an acicular silica template, leading to ellipsoidal-shape metallic phase loss. Alumina-coated particle showed an acicular metallic particle with thin layer anti-sintering alumina agent stabilized by maghemite thin layer on particle surface. The influence of the temperature, hydrogen flows and reduction time on the magnetic properties, crystallite size, crystallographic structure and phases were also investigated. A topotatic ...(Complete abstract, click electronic access below)
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Físico-química, Materiais magnéticos, Magnetic materials
Como citar
VARANDA, Laudemir Carlos. Nanopartículas aciculares metálicas de 'Fe', 'Fe''Co', 'Fe''TR' e 'Fe''Co''TR'('TR'='La'-'Tb') para tecnologia avançada de gravação magnética. 2003. 126 f. Tese (doutorado) - Universidade Estadual Paulista, Instituto de Química, 2003.