Microscopia Eletrônica de Varredura (MEV) acoplada a

O MEV permitiu observar a formação de partículas relativamente simétricas (Figura 59) e estruturas assimétricas (Figura 60). O resultado das análises por EDS comprovaram a presença da camada de apatita para ambas.

Figura 59 – Fotomicrografia, por meio de MEV/EDS mostrando a morfologia de partículas presente na superfície e a composição química, de amostras após 7 dias de imersão em

SBF.

Fonte: Elaborada pelo autor.

Ti Ti-H

036

Ti-H

927

Ti-H

1818

Ti-H

279

Ti-H

360 0

2 4 6 8 10 12

Área oculpada por partículas(%)

Figura 60 – Fotomicrografia, por meio de MEV/EDS mostrando a morfologia de partículas presente na superfície e a composição química, de amostras após 7 dias de imersão em

SBF.

Fonte: Elaborada pelo autor.

As superfícies de 𝑇𝑖𝑂₂ são conhecidas por promoverem a nucleação de apatita, por conter grupos funcionais que são carregados negativamente. O que explica o comportamento observado na condições 𝑇𝑖 − 𝐻₃₆⁰ condição de maior fluxo de oxigênio. Entretanto, uma superfície de 𝑇𝑖𝑂₂ dopada com nitrogênio (considerada carregada positivamente) também pode induzir efetivamente a formação de apatita(HASHIMOTO; KASHIWAGI; KITAOKA, 2011). Para Piscanec e colaboradores, isso ocorre devido à presença de estados de valência mista dos átomos de Ti superficiais que levam à localização de cargas negativas nos oxigênios superficiais, promovendo a adsorção dos íons 𝐶𝑎²⁺ favorecendo as fases superficiais dos oxinitreto (𝑇𝑖𝑂𝑥𝑁𝑦) (PISCANEC, 2004), o que explica o comportamento observado na condição 𝑇𝑖 − 𝐻₉²⁷. Nas condições intermediárias mesmo com a presença do oxigênio na atmosfera de tratamento não foi observado esse comportamento, para essas condições experimentais observou-se comportamento semelhante a amostra controle (𝑇𝑖) e a condição sem fluxo de oxigênio (𝑇𝑖 − 𝐻₀³⁶).

4.3.3 Difração de raios-X com incidência rasante (GIXRD)

Analisando os difratogramas apresentados na Figura 61, verifica-se que as condições (𝑇𝑖 − 𝐻₀³⁶) e (𝑇𝑖 − 𝐻₂₇⁹ ), são as que apresentaram maior intensidade dos picos referente ao composto hidroxiapatita 𝐶𝑎₅𝐻𝑂₁₃𝑃₃(COD: 00-087-0629), isso pode ter ocorrido devido à baixa cristalinidade ou pouco material nas demais amostras como mostrou as análises de microscopia óptica.

Figura 61– (a) Difração de raios-X amostras tratadas e padrão, após 7 dias de imersão em SBF, (b) caracterizarão das amostras 𝑇𝑖 − 𝐻₃₆⁰ .

5 CONCLUSÕES

Com os resultados obtidos durante a realização deste trabalho pode-se concluir que:

O fluxo de 24sccm do gás hidrogênio provocou alterações na cinética do plasma favoráveis para etapas de limpeza e tratamento, através da redução dos picos de nitrogênio 𝑁₂⁺(𝐵 − 𝑋), 𝑁₂(𝐶 − 𝐵), e inibição da linha 𝑂(3𝑝⁵𝑃 → 3𝑠⁵𝑆).

A modificação de superfície por tratamento termoquímico assistido por plasma em diferentes proporções de fluxos de gases N2-O2 e H2(24sccm) fixo, permitiu produzir superfícies com características diversificadas e possibilitando ampliar as aplicações do Titânio Cp II.

Foi possível obter basicamente duas estruturas de oxinitretos, estrutura hexagonal e cúbico. Entretanto, a sobreposição de picos das fases de estrutura hexagonal (TiN0,26 e TiO0,325), dificultaram indicar a composição predominante (TiN0,26(O) ou TiO0,325(N)). Todavia, a presença da estrutura cubica TiNx(O) ficou bem evidenciada na condição 𝐻₉²⁷.

Nas condições de máxima concentração de gases oxigênio (𝑇𝑖 − 𝐻₃₆⁰ ) ou nitrogênio (𝑇𝑖 − 𝐻₀³⁶), observa-se majoritariamente a oxidação e a nitretação da superfície respectivamente. Fato corroborado pelas análises de difração de raios-X em ângulos rasante, espectroscopia Raman e XPS. Na condição experimental 𝑇𝑖 − 𝐻₉²⁷, a espectroscopia Raman e a difração de raios-X sugeriram a presença de uma estrutura não estequiométrica para o nitreto de titânio, ou seja o TiNx, estrutura que favoreceu a formação do oxinitreto TiNx(O) .

Para molhabilidade e tensão superficial os dados demostraram a influência da razão entre fluxo de gás nitrogênio e oxigênio na modificação da molhabilidade e tensão superficial das superfícies. Observa-se uma relação entre o acréscimo do fluxo de nitrogênio e redução do oxigênio no aumento do ângulo de contato e redução da coordena polar e tensão superficial.

Nas proposições de tensão interfacial para os hemoderivados fibrinogênio e albumina, observa-se igualmente uma relação entre o fluxo nitrogênio e oxigênio.

Nota-se que o aumento de nitrogênio e redução do oxigênio na atmosfera de trabalho

resultou na elevação da tensão Interfacial para fibrinogênio e albumina.

Comportamento coerente com o aumento da hidrofobicidade.

Os resultados das amostras imersas por 7 dias em solução SBF foram positivos no que se refere ao ensaio de bioatividade, observou-se dois níveis de bioatividade uma composta pelas condições experimentais 𝑇𝑖 − 𝐻₃₆⁰ , 𝑇𝑖 − 𝐻₂₇⁹ de alta bioatividade e outra com a bioatividade reduzida amostra controle (𝑇𝑖), 𝑇𝑖 − 𝐻₂₇⁹ , 𝑇𝑖 − 𝐻₁₈¹⁸ e 𝑇𝑖 − 𝐻₀³⁶. A difração de raios-X em ângulo rasante e EDS fora de fundamental importância para caracterizar a partículas presente na superfície após o ensaio de bioatividade.

Logo, as condições mais promissoras para acelerar o crescimento de cristais de apatita óssea após a nucleação inicial (aplicações para ósseo integração) são as condições experimentais 𝑇𝑖 − 𝐻₃₆⁰ e 𝑇𝑖 − 𝐻₂₇⁹ . Os demais tratamentos são condições sugestivas para aplicações que exijam baixo grau de bioatividade como por exemplo os stents.

6 SUGESTÕES PARA FUTUROS TRABALHOS

1. Realizar o ensaios em solução SBF com maiores tempos de imersão;

2. Realizar ensaios de coagulação sobre as superfícies tratadas por plasma;

3. Realizar ensaios de adsorção de proteínas (fibrinogênio e albumina) sobre as superfícies tratadas por plasma;

4. Avaliar a atividade osteogênica sobre as superfícies tratadas por plasma;

5. Exame da topografia superficial através da microscopia de força atômica (AFM);

6. Analises de nanoindetação nas superfícies tratadas.

7. Avaliar a concentração dos intersticiais por reação nuclear ressoante (NRA)

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