BR112014012123B1 - Sistema de camada de casca, métodos para a preparação de superfície de vários substratos de compósito e para formar uma estrutura de compósito ligada - Google Patents
Sistema de camada de casca, métodos para a preparação de superfície de vários substratos de compósito e para formar uma estrutura de compósito ligada Download PDFInfo
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- BR112014012123B1 BR112014012123B1 BR112014012123-0A BR112014012123A BR112014012123B1 BR 112014012123 B1 BR112014012123 B1 BR 112014012123B1 BR 112014012123 A BR112014012123 A BR 112014012123A BR 112014012123 B1 BR112014012123 B1 BR 112014012123B1
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Abstract
1 / 1 resumo âsistema de camada de casca, mãtodos para a preparaãão de superfãcie de vãrios substratos de compãsito e para formar uma estrutura de compãsito ligadaâ uma camada de casca rica em resina (11) que nã£o deixa para trã¡s fibras residuais apã³s desprendimento e pode funcionar bem com diferentes substratos de compã³sito baseados em resina (10). a camada de casca rica em resina (11) ã© composta de um pano tecido (11b) impregnado com uma matriz de resina (11a) diferente da matriz de resina do substrato de compã³sito (10). a camada de casca (11) ã© projetada de tal modo que, apã³s remoã§ã£o manual da camada de casca (11) da superfãcie do substrato de compã³sito (10), um filme fino da resina de camada de casca permanece na superfãcie do substrato de compã³sito para criar uma superfãcie ligã¡vel capaz de ligar com outro substrato de compã³sito (12), porã©m nenhum material fibroso do pano tecido permanece na mesma superfãcie.
Description
[0001] A presente revelação se refere genericamente a camadas de tecido poroso para preparação de superfície de substratos de compósito, mais particularmente a substratos de compósito baseados em resina, antes da ligação.
[0002] Lixamento com a mão, jateamento com areia e remoção de camada de casca são métodos convencionais para preparar superfícies de substratos de compósito à base de resina para ligação de adesivo em indústria aeroespacial. A ligação de adesivo por remoção de camada de casca é a mais comum das três técnicas porque economiza quantidades significativas de mão-de-obra e cria superfície mais uniformemente tratada. A remoção de camada de casca envolve normalmente aplicar um material de pano texturizado, seco sobre a superfície de ligação do substrato compósito baseado em resina seguido por cura. Após cura, a camada de casca é removida, isto é, desprendido, para revelar uma superfície de ligação áspera ou texturizada. Entretanto, peelplies secos tendem a deixar fibras quebradas residuais na superfície de ligação após desprendimento. Isso leva a propriedades ruins de ligação de adesivo porque as fibras residuais podem atuar como defeitos que evitam que o adesivo umedeça totalmente a superfície de ligação do substrato de compósito, desse modo resultando em falha de adesivo. A experiência geral na indústria é que o processo de camada de casca não tem confiabilidade e capacidade de predição com relação ao desempenho de ligação.
[0003] A presente revelação provê uma camada de casca rica em resina que não deixa fibras residuais para trás após desprendimento e pode funcionar bem com diferentes substratos de compósito baseados em resina. A camada de casca rica em resina é composta de um pano tecido impregnado com uma matriz de resina diferente da matriz de resina do substrato de compósito. A camada de casca é projetada de tal modo que, após remoção manual da camada de casca a partir da superfície do substrato de compósito, um filme fino da resina de camada de casca permanece na superfície do substrato de compósito para criar uma superfície ligável, porém nenhum material fibroso a partir do pano tecido permanece na mesma superfície. Essa camada de casca rica em resina é capaz de modificar a superfície de vários compósitos para ligação segura com uma variedade de adesivos. Consequentemente poderia ser considerada como uma camada de casca “universal”.
[0004] A presente revelação também provê um método de preparar uma superfície para ligação de compósito utilizando a camada de casca discutida acima. Também é revelado um método para formar uma estrutura de compósito ligada que inclui: aplicar uma camada de casca sobre uma superfície de um primeiro substrato de compósito composto de resina reforçada com fibra; curar em conjunto a camada de casca e o primeiro substrato de compósito; remover a camada de casca a partir do primeiro substrato de compósito deixando para trás uma camada fina de resina de camada de casca na superfície do substrato de compósito; aplicar um filme adesivo sobre pelo menos uma da superfície modificada do primeiro substrato de compósito e uma superfície de um segundo substrato de compósito; contatar a superfície modificada do primeiro substrato de compósito com uma superfície do segundo substrato de compósito com o filme adesivo entre as mesmas; e curar para ligar os substratos.
[0005] A figura 1 mostra esquematicamente o mecanismo de trabalho da camada de casca rica em resina de acordo com a presente revelação.
[0006] A figura 2 mostra a linha de fratura que ocorre quando a camada de casca é removida de um substrato de compósito.
[0007] A figura 3 é uma imagem de microscópio eletrônico de varredura (SEM) de um pano de poliéster exemplar que pode ser utilizado para a camada de casca rica em resina.
[0008] A figura 4 é uma imagem de microscópio eletrônico de varredura (SEM) de um pano de vidro exemplar que pode ser utilizado para a camada de casca rica em resina.
[0009] A figura 5 é uma imagem de microscópio eletrônico de varredura (SEM) de uma superfície tratada após a camada de casca rica em resina ser removida.
[0010] A figura 6 mostra os dados de tenacidade de fratura (Gic) para vários prepregs adesivamente ligados em um Exemplo.
[0011] As figuras 7A e 7B são imagens de microscópio óptico mostrando a condição de falha coesiva de prepregs coligados após teste de tenacidade de fratura (Gic) de acordo com um Exemplo.
[0012] Foi descoberto que uma vantagem que pode ser realizada no tratamento de um substrato de compósito de resina reforçada com fibra com uma camada de casca rica em resina para modificar a superfície do substrato de compósito tratada de modo a facilitar e promover ligação de duração mais longa e mais forte entre a estrutura de compósito tratada superficialmente e um segundo substrato de compósito. A superfície do substrato de compósito (10) é modificada por um filme de resina fina (12) que resta sobre a mesma após a camada de casca rica em resina (11) é desprendida (figura 1). O mecanismo de trabalho da camada de casca é ilustrado pela figura 1. A espessura da resina restante após a camada de casca ter sido removida é aproximadamente 2% - 15% da espessura original da camada de casca antes de desprendimento. Essa camada de resina de camada de casca restante provê uma camada de superfície compatível para ligação de adesivo, incluindo ligação em conjunto e ligação secundária. A ligação em conjunto na indústria de ligação de compósito significa ligação de um prepreg curado com um prepreg não curado utilizando adesivo. Ligação secundária significa ligação de um prepreg curado com outro prepreg curado utilizando adesivo. A reologia e cinética de cura da resina de camada de casca são controladas para minimizar intermistura entre a resina de camada de casca e a resina do substrato de compósito durante cura, pelo que a formulação de resina de camada de casca tem uma cinética de cura substancialmente mais rápida do que a formulação de resina do substrato de compósito. Como a camada de casca rica em resina pode ser utilizada com vários substratos de compósito de resina reforçada com fibra, pode ser considerada como uma camada de casca “universal”.
[0013] Os substratos de compósito de resina reforçada com fibra discutidos aqui incluem prepregs ou layups de prepreg convencionalmente utilizados na fabricação de partes estruturais aeroespaciais. O termo “prepreg” como utilizado aqui se refere à folha ou lâmina de fibras que foi impregnada com uma resina de matriz. A resina de matriz pode estar presente em um estado não curado ou parcialmente curado. O termo “layup de prepreg” como utilizado aqui se refere a uma pluralidade de camadas de prepreg que são camadas adjacentes entre si em uma pilha. As camadas de prepreg no layup podem ser posicionadas em uma orientação selecionada em relação mútua. Por Exemplo, layups de prepreg podem compreender camadas de prepreg tendo arquiteturas de fibra unidirecional, com as fibras orientadas em 0o, 90°, um ângulo selecionado 0, e combinações dos mesmos, com relação à maior dimensão do layup, como o comprimento. Deve ser adicionalmente entendido que, em certas modalidades, prepregs podem ter qualquer combinação de arquiteturas de fibras, como unidirecionais e multidimensionais.
[0014] A camada de casca rica em resina (11) da presente revelação é composta de um pano tecido (Ha) impregnado por uma matriz de resina (11b), como ilustrado na figura 1, e tem um teor de resina de pelo menos 20% em peso com base no peso total da camada de casca, dependendo do tipo específico de pano tecido sendo impregnado. Em certas modalidades, o teor de resina está compreendido na faixa de 20% - 50%. A formulação de resina e a construção de pano são selecionadas de tal modo que nenhuma fibra quebrada seja deixada na superfície do substrato de compósito após a camada de casca ter sido removida. A linha de fratura (13) durante desprendimento está compreendida na matriz de resina (11b) ou na interface de resina-fibra, porém não no pano (11a), como ilustrado na figura 2. A camada de casca rica em resina é facilmente removida da superfície do substrato de compósito após cura. Para essa finalidade, apresenta uma resistência de desprendimento não maior do que 10 pol-lb/polegada de largura - de acordo com o Teste de desprendimento de tambor ASTM D1781.
[0015] O pano da camada de casca rica em resina é composto de uma pluralidade de fios tecidos em um padrão de tecedura. Cada fio é composto de uma pluralidade de filamentos fibrosos contínuos (fibras únicas) torcidos juntos. O pano tecido tem um peso de pano compreendido na faixa de 50-250 gsm (gramas/m2), preferivelmente 70-220 gsm, e uma espessura compreendida na faixa de 50-250 pm, preferivelmente 100-200 pm. espessura é principalmente uma função de peso e tipo de fibra, porém também depende da tecedura. O tipo de fibra para o pano tecido pode ser selecionado de vários materiais sintéticos incluindo poliésteres (tereftalato de polietileno, tereftalato de polibutileno, tereftalato de politrimetileno, ácido poliláctico, e copolímeros dos mesmos), polietileno, polipropileno, náilon, materiais elastoméricos como LYCRA®; fibras de alto desempenho como as poliaramidas (por Exemplo, Kevlar), poliimidas, polietileno imina (PEI), polioxazol (por Exemplo, Zylon), polibenzimidazol (PBI), poliéter éter cetona (PEEK) e vidro. As exigências principais para o material de fibra são: o material não é quebradiço e tem a resistência à tração exigida. Além disso, o pano pode ter um acabamento de endurecimento a calor ou outros acabamentos convencionais.
[0016] O tamanho de fio pode ser expresso em termos de unidades de densidade de massa linear de denier. Denier é igual ao peso em gramas de 9000 metros de fio. Quanto mais baixo o número, mais fino o fio. Para um rolo de pano, os fios que estendem na direção do rolo e são contínuos para o comprimento inteiro do rolo são os fios de urdidura. Os fios curtos que estendem no sentido transversal à direção de rolo são chamados os fios de enchimento. Para a camada de casca rica em resina, o pano é selecionado com base nas seguintes características: fios de urdidura com densidade de massa linear na faixa de 50-250 deniers, preferivelmente 70-230 deniers, e fios de enchimento com densidade de massa linear na faixa de 50-250, preferivelmente 70-230 deniers, resistência à tração de urdidura de pelo menos 70 Ibf/pol. (1,23 x 104 N/m), preferivelmente > 80 Ibf/pol. (1,40 x 104 N/m); resistência à tração de enchimento de pelo menos 40 Ibf/pol. (7,00 x 103 N/m), preferivelmente > 50 Ibf/pol. (8,76 x 103 N/m). O padrão de tecedura não é limitado e pode ser tecedura lisa, tecedura entrançada, tecedura de cesto, tecedura acetinada e similar. A densidade de tecedura não deve ser demasiadamente elevada para pano à base de polímero (isto é, tecedura de aperto) de tal modo que impregnação baixa de resina e impregnação incompleta dos fios resultaria.
[0017] A figura 3 é uma imagem de microscópio eletrônico de varredura (SEM) de um pano de poliéster exemplar que pode ser utilizado para a camada de casca rica em resina. Esse pano específico tem um peso de 110 gsm e fios com densidade de massa linear de 125 deniers. Como pode ser visto a partir da figura 3, esse tipo de pano de poliéster não é apertadamente tecido e contém aberturas minúsculas na tecelagem. Quando a camada de casca contendo esse tipo de pano de poliéster é desprendida da superfície de compósito, um filme de resina com uma superfície áspera e nenhuma fibra quebrada é produzido. Tal superfície áspera é desejável para ligação. Panos apertadamente tecidos como panos de vidro também podem ser utilizados para formar a camada de casca rica em resina para criar uma aspereza superficial desejável para ligação de compósito. A figura 4 mostra um pano de vidro exemplar que pode ser utilizado para a camada de casca rica em resina. Esse pano de vidro é mais apertadamente tecido e mais espesso do que o pano de poliéster mostrado na figura 3; tem um peso de 205 gsm e uma espessura de 175 pm.
[0018] A matriz de resina da camada de casca é formada de uma composição de resina curável que inclui: pelo menos uma resina novolac epoxidada tendo funcionalidade de epóxi de pelo menos 2; resina de epóxi difuncional selecionada de éteres de diglicidil de fenóis poliídricos; resina de epóxi trifuncional selecionada de éteres de trigliclidil de aminofenois; partículas de enchimento inorgânicas (por Exemplo, sílica coloidal); e um agente de cura. A resina novolac epoxidada é composta de pelo menos 40% em peso com base no peso total da composição, preferivelmente 50-70% em peso. A resina de epóxi difuncional está presente em quantidade de 10-35%, preferivelmente 15-25% em peso, a resina epóxi trifuncional está presente em uma quantidade de 10-30%, preferivelmente 10-20% em peso, com base no peso total da composição de resina.
[0019] Os exemplos de resinas novolac epóxidadas incluem aquelas obtidas por reagir fenóis como fenol, o-cresol, m-cresol, p-cresol, p-terc- butilfenol, p-nonil fenol, 2,6-xilenol, resorcinol, bisfenol-A, α e β-naftol, e naftalenodiol com aldeídos como acetaldeído, formaldeído, furfural, glioxal e p-hidroxi benzaldeído na presença de um catalisador de ácido.
[0020] Resinas novolac epoxidadas apropriadas incluem resinas novolac de epóxi fenol e resinas novolac de epóxi cresol representadas pela seguinte estrutura I: (I) em que n é um número inteiro de 0 a 8, R = H ou CH3. Quando R=H, a resina é uma resina novolac de fenol. Quando R=CH3, a resina é uma resina novolac de cresol. Resinas novolac de epóxi fenol são comercialmente disponíveis como DEN 428, DEN 431, DEN 438, DEN 439, e DEN 485 da Dow Chemical Co. Resinas novolac de epóxi cresol são comercialmente disponíveis como ECN 1235, ECN 1273, e ECN 1299 da Ciba-Geigy Corp.
[0021] Outra resina novolac epoxidada apropriada é resina novolac de epóxi de hidrocarboneto tendo uma espinha dorsal de diciclopentadieno representada pela seguinte Estrutura II: em que n é um número inteiro de 0 a 7. Exemplos comerciais de tais resinas novolac de epóxi de hidrocarboneto incluem Tactix® 71756, Tactix® 556, e Tactix® 756 da Vantico Inc. Em uma modalidade, a resina novolac da Estrutura I é utilizada em combinação com resina novolac contendo diciclopentadieno da Estrutura II.
[0022] Resinas de epóxi difuncional apropriadas incluem éteres de diglicidil de bisfenol A ou bisfenol F, por Exemplo, Epon™ 828 (resina de epóxi líquida), D.E.R. 331, D.E.R. 661 (resina de epóxi sólida) fornecidas pela Dow Chemical Co.
[0023] Éteres de triglicidil de aminofenois são comercialmente disponíveis como Araldite® MY 0510, MY 0500, MY 0600, MY 0610 da Huntsman Advanced Materials.
[0024] Agentes de cura apropriados para a resina de epóxi na composição de resina de camada de casca incluem uma classe de agentes de cura conhecidos como Acido Lewis; trifluorboreto (BF3), tricloreto de boro (BCI3) e complexos dos mesmos, como complexos de BF3-Amina e complexos de BCls-Amina. Os exemplos de complexos de BF3-Amina incluem BF3-MEA da Ato-Tech, Anchor 1040 (BF3 complexado com benzil amina e isopropil amina) da Air Products, Anchor 1115 (BF3 complexado com aducto de isopropil amina) da Air Products, e Anchor 1170 (BF3 complexado com clorobezenil amina) também da Air Products. Os exemplos de complexos de BCh-Amina incluem Omincure™ BC-120. Os complexos são feitos para fornecer formas líquidas ou sólidas sob condições de uso normal. Muitos prepregs baseados em epóxi comercial mente disponíveis incluem agentes de cura baseados em amina como 3,3’-diaminodifenil sulfona (DDS) e diciandiamido (DICY), que mostram cinética de cura substancialmente mais lenta do que aquelas de uma formulação de resina de camada de casca contendo os agentes de cura cima, por Exemplo, BF3 líquido. Como resultado, a formulação de resina de camada de casca pode curar rápido 0 bastante para minimizar a intermistura com a resina de prepreg durante 0 processo de cura em conjunto.
[0025] Materiais de enchimento inorgânicos em forma de partículas (por Exemplo, pó) são adicionados à composição de resina de camada de casca como um componente de modificação de reologia para controlar 0 fluxo da composição resinosa e evitar aglomeração no mesmo. Materiais de enchimento inorgânicos apropriados que podem ser utilizados na composição de filme de superfície incluem sílica coloidal, talco, mica, carbonato de cálcio, alumina. A quantidade de material de enchimento inorgânico pode estar compreendida na faixa de 1-10% em peso, preferivelmente 1-5% em peso, com base no peso total da composição de filme de superfície.
[0026] Em uma modalidade, a composição de resina da camada de casca pode incluir, em percentagens em peso com base no peso total da composição de resina: aproximadamente 45-55% de resina de epóxi novolac de fenol; aproximadamente 5-15% de resina de epóxi novolac contendo diciclopentadieno, aproximadamente 20-30% de éter de diglicidil de bisfenol A; aproximadamente 15-25% de éter de triglicidil de aminofenol; aproximadamente 5-15% de agente de cura de BF3 e aproximadamente 1-5% de material de enchimento inorgânico.
[0027] Além disso, um ou mais solventes orgânicos também podem ser adicionados à composição de resina descrita acima, como necessário, para facilitar a mistura dos componentes. Os exemplos de tais solventes podem incluir, porém não são limitados a, metil etil cetona (MEK), acetona, dimetil acetamida e N-metil pirrolidona.
[0028] A camada de casca rica em resina pode ser formada por revestir a composição de resina descrita acima sobre 0 pano tecido de modo a impregnar totalmente os fios no pano utilizando processos de revestimento de fusão a calor ou solvente convencionais. A camada de casca úmida é então deixada secar se necessário para reduzir 0 teor volátil, preferivelmente, até menos do que 2% em peso, a secagem pode ser feita por secagem a ar em temperatura ambiente durante a noite seguido por secagem em fomo a 140°F - 170°F, ou por secagem em forno em temperatura elevada, como necessário, para reduzir 0 tempo de secagem. Subsequentemente, a camada de casca rica em resina seca pode ser protegida por aplicar papeis de liberação removíveis ou filmes sintéticos (por Exemplo, filmes de poliéster) em lados opostos. Tais papeis de liberação ou filmes sintéticos devem ser removidos antes do uso da camada de casca para ligação de superfície. A camada de casca seca é aplicada sobre uma superfície de um substrato compósito baseado em resina não curada (ou parcialmente curada), por Exemplo, prepreg baseado em epóxi. A seguir, a camada de casca juntamente com o substrato de compósito é submetida à cura em conjunto. A camada de casca é então removida para deixar um filme de resina fina no substrato de compósito, desse modo formando uma superfície modificada pronta para ligação de adesivo com outro substrato de compósito.
[0029] Para ligação em conjunto e ligação secundária de dois substratos de compósito, um filme adesivo curável é aplicado sobre pelo menos uma da superfície modificada de um primeiro substrato de compósito que já está curado e uma superfície de um segundo substrato de compósito. A superfície modificada do primeiro substrato de compósito curado é colocada em contato com uma superfície do segundo substrato de compósito de tal modo que o adesivo esteja entre os substratos. A cura é então realizada para formar uma estrutura de compósito ligada. Os termos “cura” e “curar” como utilizado aqui se referem à polimerização e/ou processo de reticulação que pode ser realizado por aquecimento, exposição à luz ultravioleta ou radiação.
[0030] A cura em conjunto da camada de casca rica em resina e o substrato de compósito baseado em resina (por Exemplo, prepreg baseado em epóxi) podem ser realizadas em temperaturas maiores do que 230°F (110°C), mais especificamente, compreendidas na faixa de 250°F - 375°F (121°C - 190°C). Foi descoberto que uma vantagem da camada de casca rica em resina descrita aqui é que a camada de casca pode ser curada em conjunto com a maioria dos prepregs comercialmente disponíveis compreendidos na faixa de cura acima. Tais prepregs incluem panos e/ou fitas pré-impregnados com resina comercialmente disponíveis como CYCOM 997, CYCOM 977-2, CYCOM 934, CYCOM 970, CYCOM 5317-3, CYCOM 5320-1 e CYCOM 851 da Cytec Industries Inc.; Hexply 8552 da Hexcel Corp.; e Toray 3900-2 da Toray Industries Inc. Após cura em conjunto, a camada de casca rica em resina apresenta uma temperatura de transição vítrea (Tg) > 140°C, em algumas modalidades, 140°C -200°C, como medido por método de Calorimetria de Varredura Diferencial Modulada (DSC).
[0031] Os seguintes exemplos são ilustrativos de algumas modalidades da camada de casca rica em resina revelada aqui e sua aplicação, e não devem ser interpretados como limitando o escopo da presente revelação.
[0032] Uma camada de casca rica em resina foi preparada por impregnar um pano de poliéster com uma formulação de resina compreendida, em percentual em peso: 45% de resina de epóxi novolac de fenol-formaldeído; 11% de resina de epóxi novolac contendo diciclopentadieno; 23% de éter de diglicidil de bisfenol A; 14% de éter de triglicidil de aminofenol; 5% de BF3 líquido e 2% de sílica coloidal. O pano de poliéster tinha as seguintes propriedades: Pano Tecedura lisa, fibras de poliéster Peso 85 g/m2 Densidade de massa linear urdidura 150 denier; enchimento 150 denier Resistência à tração urdidura 155 Ibf/ pol (2,7 x 104 N/m); enchimento 120 Ibf/pol (2,1 x 104N/m) Espessura ~ 0,005 pol
[0033] A formulação de resina foi misturada utilizando um processo de fusão a calor seguido por um processo de adição de solvente. Após uma mistura de fusão a calor ser feita, solvente de metil etil cetona (MEK) foi adicionado à composição de resina para formar uma suspensão sólida a 82%. A composição de resina úmida foi revestida sobre 0 pano utilizando processo de revestimento de solvente e deixada secar durante a noite em temperatura ambiente seguido por processo de secagem em fomo para reduzir 0 teor volátil a menos de 2%. A camada de casca seca tinha um teor de resina de aproximadamente 43% em peso e uma espessura de aproximadamente 140 pm.
[0034] Altemativamente, a formulação de resina também pode ser misturada com MEK em um processo auxiliado por solvente em temperatura ambiente. A mistura de resina úmida obtida em 82% de teor sólido pode ser revestida sobre o pano do mesmo modo como descrito acima.
[0035] A camada de casca seca como discutido acima foi utilizada para preparar a superfície de um prepreg baseado em epóxi reforçado com fibra, fita CYCOM 997 (da Cytec Industries Inc.). após cura em conjunto a 177°C, a camada de casca foi desprendida deixando para trás uma superfície modificada pronta para ligação. Um teste de Desprendimento de Tambor (ASTM D1781) foi realizado para avaliar a Resistência de desprendimento da camada de casca. O resultado de teste indicou 11,1 Newton (2,5 pol- lb/polegada de largura). Isso mostra que a camada de casca foi facilmente desprendida. A análise de superfície por ATR-FTIR (Reflexo total atenuado) foi realizado para estudar a superfície tratada do prepreg após cura e remoção da camada de casca. Verificou-se que uma camada fina de aproximadamente 3-10 pm de resina de camada de casca foi deixada no topo do prepreg. A figura 5 é uma imagem de microscópio eletrônico de varredura (SEM) da superfície tratada após a camada de casca rica em resina ser removida, que mostra que nenhuma fibra quebra do pano permanece.
[0036] Uma camada de casca rica em resina foi fabricada por impregnar um pano de poliéster com uma formulação de resina compreendida, em percentual em peso: 45% de resina de epóxi novolac de fenol-formaldeído; 11% de resina de epóxi novolac contendo diciclopentadieno; 22,5% de éter de diglicidil de bisfenol A; 13,5% de éter de triglicidil de aminofenol; 6% de BF3-MEA; e 2% de sílica coloidal. O pano de poliéster tinha as seguintes propriedades: Pano Tecedura lisa, torcido, fibras de poliéster Peso 110 g/m2 Densidade de massa linear urdidura 126 denier; enchimento 126 denier Resistência à tração urdidura 105 Ibf/pol. (1,8 x 104 N/m); enchimento 105 Ibf/pol. (1,8 x 104N/m) Espessura ~ 0,0045 pol.
[0037] A formulação de resina foi misturada, revestida sobre o pano, seca e testada do mesmo modo que no Exemplo 1. Resultado similar foi visto - uma camada fina de aproximadamente 3-10 pm de resina de camada de casca foi deixada no topo do prepreg após a camada de casca rica em resina ser removida, porém nenhuma fibra quebrada do pano permanece.
[0038] Uma camada de casca rica em resina foi preparada por impregnar um pano de poliéster com uma formulação de resina compreendida, em % em peso: 44,5% de resina de epóxi novolac de fenol- formaldeído; 9% de resina de epóxi novolac contendo diciclopentadieno; 22% de éter de diglicidil de bisfenol A; 18% de éter de triglicidil de aminofenol 4,7% de BF3 líquido e 1,8% de sílica coloidal. O pano de poliéster tinha as seguintes propriedades: Pano Tecedura lisa, fibras de poliéster Peso 85 g/m2 Densidade de massa linear urdidura 150 denier; enchimento 150 denier Resistência à tração urdidura 155 Ibf/pol. (2,7 x 104 N/m); enchimento 120 Ibf/pol. (2,1 x 104N/m) Espessura ~ 0,005 pol.
[0039] A formulação de resina foi misturada, revestida sobre o pano, seca e testada do mesmo modo que no Exemplo 1. Resultado similar foi visto - uma camada fina de aproximadamente 3-10 pm de resina de camada de casca foi deixada no topo do prepreg após a camada de casca rica em resina ser removida, porém nenhuma fibra quebrada do pano permanece.
[0040] Uma camada de casca rica em resina foi preparada por impregnar um pano de poliéster com uma formulação de resina compreendida, em % em peso: 44% de resina de epóxi novolac de fenol- formaldeído; 9% de resina de epóxi novolac contendo diciclopentadieno; 22% de éter de diglicidil de bisfenol A; 17% de éter de triglicidil de aminofenol; 6% de BFa-MEA e 2% de sílica coloidal. O pano de poliéster tinha as seguintes propriedades: Pano Tecedura lisa, torcido, fibras de poliéster Peso 110g/m2 Densidade de massa linear urdidura 126 denier; enchimento 126 denier Resistência à tração urdidura 105 Ibf/pol. (1,8 x 104 N/m); enchimento 105 Ibf/pol.(1,8 x 104N/m) Espessura ~ 0,0045 pol.
[0041] A formulação de resina foi misturada, revestida sobre o pano, seca e testada do mesmo modo que no Exemplo 1. Resultado similar foi visto - uma camada fina de aproximadamente 3-10 pm de resina de camada de casca foi deixada no topo do prepreg após a camada de casca rica em resina ser removida, porém nenhuma fibra quebrada do pano permanece.
[0042] Uma camada de casca rica em resina foi preparada por impregnar um pano de poliéster com uma formulação de resina compreendida, em % em peso: 45,5% de resina de epóxi novolac de fenol- formaldeído; 11,4% de resina de epóxi novolac contendo diciclopentadieno; 22,8% de éter de diglicidil de bisfenol A; 13,7% de éter de triglicidil de aminofenol; 4,8% de BF3 líquido e 1,8% de silica coloidal. O pano de poliéster tinha as seguintes propriedades: Pano Tecedura lisa, torcido, fibras de poliéster Peso 110 g/m2 Densidade de massa linear urdidura 126 denier; enchimento 126 denier Resistência à tração urdidura 105 Ibf/pol.(1,8 x 104 N/m); enchimento 105 Ibf/pol.(1,8 x 104N/m) Espessura ~ 0,0045 pol.
[0043] A formulação de resina foi misturada, revestida sobre 0 pano, seca e testada do mesmo modo que no Exemplo 1. Resultado similar foi visto - uma camada fina de aproximadamente 3-10 pm de resina de camada de casca foi deixada no topo do prepreg após a camada de casca rica em resina ser removida, porém nenhuma fibra quebrada do pano permanece.
[0044] Uma camada de casca rica em resina foi preparada por impregnar um pano de vidro com uma formulação de resina compreendida, em % em peso: 44,5% de resina de epóxi novolac de fenol-formaldeído; 8,9% de resina de epóxi novolac contendo diciclopentadieno; 22,3% de éter de diglicidil de bisfenol A; 17,8% de éter de triglicidil de aminofenol; 4,7% de BF3 líquido e 1,8% de sílica coloidal. O pano de vidro tinha as seguintes propriedades: Pano Tecedura lisa, fibras de vidro Peso 207 g/m2 Resistência à tração urdidura 350 Ibf/pol. (6,1 x 104 N/m); enchimento 260 Ibf/pol. (4,6 x 104 N/m) Espessura ~ 0,007 pol.
[0045] A formulação de resina foi misturada, revestida sobre o pano do mesmo modo que no Exemplo 1. Após secagem, a camada de casca seca tinha um teor de resina de aproximadamente 28% em peso e uma espessura de aproximadamente 195 pm. a camada de casca rica em resina foi então testada do mesmo modo que no Exemplo 1. Resultado similar foi visto - uma camada fina de aproximadamente 3-10 pm de resina de camada de casca foi deixada no topo do prepreg após a camada de casca rica em resina ser removida, porém nenhuma fibra quebrada do pano permanece.
[0046] Uma camada de casca rica em resina foi preparada por impregnar um pano de poliéster com a formulação de resina revelada no Exemplo 6. O pano de poliéster tinha as seguintes propriedades: Pano Tecedura lisa, torcido, fibras de poliéster Peso 110 g/m2 Densidade de massa linear urdidura 126 denier; enchimento 126 denier Resistência à tração urdidura 105 Ibf/pol.(1,8 x 104 N/m); enchimento 105 Ibf/pol. (1,8 x 104 N/m) Espessura ~ 0,0045 pol.
[0047] A formulação de resina foi misturada, revestida sobre o pano, seca e testada do mesmo modo que no Exemplo 1. Resultado similar foi visto - uma camada fina de aproximadamente 3-10 pm de resina de camada de casca foi deixada no topo do prepreg após a camada de casca rica em resina ser removida, porém nenhuma fibra quebrada do pano permanece.
[0048] Prepregs de CYCOM 970 (da Cytec Industries Inc.) foram ligados entre si utilizando um adesivo comercialmente disponível FM 318M.05 psf (da Cytec Industries Inc.). Três a quatro amostras de prepreg ligado foram testadas em cada temperatura de teste. Antes da ligação, a superfície de ligação dos prepregs foi preparada utilizando a camada de casca rica em resina como discutido no Exemplo 1. A Tabela 2 mostra os dados médios de cisalhamento em temperaturas de teste de 23°C, -55°C e 72°C com base em Teste de cisalhamento de sobreposição dupla (ASTM D3528). Como visto na Tabela 2, a camada de casca promove falha coesiva nas várias temperaturas de teste. TABELA 2
[0049] Amostras de prepreg ligadas foram formadas utilizando vários materiais de prepreg comercialmente disponíveis e um adesivo comercialmente disponível FM 309-l(da Cytec Industries Inc.). antes da ligação, a superfície de ligação dos prepregs foi preparada utilizando a camada de casca rica em resina como discutido no Exemplo 1. Teste de viga cantilever dupla (ASTM D5528) foi realizado a 23°C e -55°C para medir a tenacidade de fratura inter laminar (Gic) dos prepregs ligados e os resultados são mostrados na figura 6.
[0050] Prepregs CYCOM 5317-6 (da Cytec Industries Inc.) foram ligados em conjunto utilizando adesivo estrutural FM 309-1 M.05 psf. Antes da coligação, uma camada de casca rica em resina formada com o pano de vidro mostrado na figura 4 foi utilizada para preparar a superfície de ligação em um dos prepregs. As figuras 7A e 7B mostram a condição de falha coesiva após teste de Gic dos prepregs ligados em conjunto.
[0051] Os termos “primeiro”, “segundo” e similares, não indicam aqui qualquer ordem, quantidade ou importância, porém em vez disso são utilizados para distinguir um elemento do outro, e os termos “um” e “uma” aqui não indicam uma limitação de quantidade, porém em vez disso indicam a presença de pelo menos um do item referenciado. O modificador “aproximadamente” ou “cerca de” utilizado com relação a uma quantidade é inclusivo do valor mencionado e tem o significado determinado pelo contexto, (por Exemplo, inclui o grau de erro associado à medição da quantidade específica). O sufixo “(s)” como utilizado aqui pretende incluir tanto o singular como o plural do termo que modifica, desse modo incluindo um ou mais daquele termo (por Exemplo, o(s) metal(is) inclui(em) um ou mais metais). Faixas reveladas aqui são inclusivas e independentemente combináveis (por Exemplo, faixas de “aproximadamente 25% em peso, ou mais especificamente, aproximadamente 5% em peso até aproximadamente 20% em peso”, são inclusivas dos pontos finais e todos os valores intermediários das faixas de “aproximadamente 5% em peso a aproximadamente 25% em peso”, etc.).
[0052] Embora várias modalidades sejam descritas aqui, será reconhecido a partir do relatório descritivo que várias combinações de elementos, variações ou aperfeiçoamentos nas mesmas podem ser feitas por aqueles versados na técnica, e estão compreendidas no escopo da invenção. Além disso, muitas modificações podem ser feitas para adaptar uma situação ou material específico aos ensinamentos da invenção sem se afastar do escopo essencial da mesma. Portanto, pretende-se que a invenção não seja limitada à modalidade específica revelada como o melhor modo considerado para realizar a presente invenção, porém que a invenção inclua todas as modalidades compreendidas no escopo das reivindicações apensas.
Claims (15)
1. Sistema de camada de casca para preparação de superfície de vários substratos de compósito, o dito sistema caracterizadopelo fato de que compreende (a) um substrato de compósito (10) compreendendo fibras de reforço impregnadas com uma primeira matriz de resina, curada; e (b) uma camada de casca rica em resina (11), removível aderida a uma superfície do substrato de compósito (10), a dita camada de casca compreendendo um pano tecido (11a) impregnado com uma segunda matriz de resina (11b), curada diferente da primeira matriz de resina, pelo que, após remoção manual da camada de casca da superfície do substrato de compósito, um filme fino da segunda matriz de resina (12) permanece na superfície do substrato de compósito para fornecer uma superfície ligável capaz de ligação em conjunto e ligação secundária com outro substrato de compósito, em que a segunda matriz de resina (11b) é formada de uma composição de resina compreendendo: pelo menos uma resina de novolac epoxidada tendo funcionalidade de epóxi de pelo menos 2; resina de epóxi difuncional selecionada de éteres de diglicidil de fenóis poliídricos; resina de epóxi trifuncional selecionada de éteres de triglicidil de amino fenóis; um agente de cura; e partículas de enchimento inorgânicas; em que a camada de casca (11) tem um teor de resina de pelo menos 20% em peso com base no peso total da camada de casca, e em que o dito pano tecido (11a) compreende uma pluralidade de fios tecidos em um padrão de tecelagem, os ditos fios tendo resistência à tração de urdidura de > 70 Ibf/pol. (1,23 x 104 N/m), resistência a tração de enchimento de > 40 Ibf/pol. (7,00 x 103 N/m), densidade de massa linear de urdidura dentro da faixa de 50-250 deniers, e densidade de massa linear de enchimento dentro da faixa de 50-250 deniers.
2. Sistema, de acordo com a reivindicação 1, caracterizado pelo fato de que os ditos fios têm resistência à tração de urdidura de > 80 Ibf/pol. (1,40 x 104 N/m), resistência a tração de enchimento de > 50 Ibf/pol. (8,76 x 103 N/m), densidade de massa linear de urdidura dentro da faixa de 70-230 deniers, e densidade de massa linear de enchimento dentro da faixa de 70-230 deniers.
3. Sistema, de acordo com a reivindicação 1 ou 2, caracterizado pelo fato de que o filme fino restante da segunda matriz de resina (12) tem uma espessura de 2% a 15% da espessura original da camada de casca (11) antes da remoção.
4. Sistema, de acordo com qualquer uma das reivindicações 1-3, caracterizado pelo fato de que a composição de resina compreende pelo menos uma resina de novolac epoxidada selecionada de resinas de novolac de epóxi fenol e resinas de novolac de epóxi cresol representadas pela seguinte estrutura: em que n é um número inteiro de 0 a 8, R = H ou CH3.
6. Sistema, de acordo com qualquer uma das reivindicações 1-5, caracterizado pelo fato de que o pano tecido (11a) tem um peso de pano dentro da faixa de 50 a 250 gsm ou 70 a 220 gsm.
7. Sistema, de acordo com qualquer uma das reivindicações 1-6, caracterizado pelo fato de que o pano tecido (11a) tem uma espessura de pano dentro da faixa de 50 a 250 pm ou 100 a 200 pm.
8. Sistema, de acordo com qualquer uma das reivindicações 1-7, caracterizado pelo fato de que os fios do pano tecido (11a) são feitos de materiais selecionados do grupo que consiste em: poliésteres, polietileno, polipropileno, náilon, materiais elastoméricos, poliaramidas, poli-imidas, polietileno imina (PEI), polioxazol, polibenzimidazol (PBI), poliéter éter cetona (PEEK) e vidro.
9. Sistema, de acordo com qualquer uma das reivindicações 1-8, caracterizado pelo fato de que a dita camada de casca tem um teor de resina dentro da faixa de 20% a 50% em peso com base no peso total da camada de casca.
10. Sistema, de acordo com qualquer uma das reivindicações 1-9, caracterizado pelo fato de que a dita camada de casca tem uma temperatura de transição vítrea (Tg) dentro da faixa de 140°C a 200°C.
11. Sistema, de acordo com qualquer uma das reivindicações 1-10, caracterizado pelo fato de que o agente de cura é selecionado do grupo que consiste em BF3, BCI3 e complexos dos mesmos.
12. Sistema, de acordo com qualquer uma das reivindicações 1-11, caracterizadopelo fato de que a dita segunda matriz de resina (11b) é formada de uma composição de resina compreendendo: resina novolac de epóxi fenol tendo funcionalidade de epóxi de pelo menos 2; resina novolac de epóxi contendo diciclopentadieno tendo funcionalidade de epóxi de pelo menos 2; éter de diglicidil de bisfenol A; éter de triglicidil de aminofenol; um agente de cura selecionado do grupo que consiste em BF3, BCI3 e complexos dos mesmos; e sílica defumada.
13. Sistema, de acordo com qualquer uma das reivindicações 1-12, caracterizadopelo fato de que as resinas novolac compõem pelo menos 20% em peso com base no peso total da composição.
14. Método para preparação de superfície de vários substratos de compósito que utiliza o sistema como definido na reivindicação 1, caracterizadopelo fato de que compreende: (a) fornecer um substrato de compósito (10) compreendendo fibras de reforço impregnadas com uma primeira matriz de resina; (b) colocar uma camada de casca rica em resina (11) em contato com uma superfície do substrato de compósito (10), a dita camada de casca sendo formada por impregnar um pano tecido (11a) com uma composição de resina curável (11b) diferente da matriz de resina do substrato de compósito e compreendendo: pelo menos uma resina novolac epoxidada tendo funcionalidade de epóxi de pelo menos 2; resina epóxi difuncional selecionada de éteres de diglicidil de fenóis poli-ídricos; resina de epóxi trifuncional selecionada de éteres de triglicidil de aminofenois; um agente de cura; e partículas de enchimento inorgânicas, em que o pano tecido (11a) compreende uma pluralidade de fios tecidos em um padrão de tecelagem, os fios tendo uma resistência à tração de urdidura > 70 Ibf/pol. (1,23 x 104 N/m), resistência à tração de enchimento de > 40 Ibf/pol. (7,00 x 103 N/m), densidade de massa linear de urdidura dentro da faixa de 50-250 deniers, e densidade de massa linear de enchimento dentro da faixa de 50-250 deniers e dita camada de casca (11) tem um teor de resina de pelo menos 20% em peso com base no peso total da camada de casca; (c) curar em conjunto a camada de casca e o substrato de compósito (10); e (d) remover a camada de casca da superfície do substrato de compósito (10) de tal modo que um filme fino de resina a partir da camada de casca permaneça na superfície do substrato de compósito para fornecer uma superfície ligável capaz de ligação em conjunto e ligação secundária com outro substrato de compósito; em que dita cura em conjunto é realizada em uma temperatura maior do que 230°F (110°C) ou 250°F a 375°F (121°C a 190°C).
15. Método de formar uma estrutura de compósito ligada, caracterizadopelo fato de que compreende o método para preparação de superfície de vários substratos de compósito como definido na reivindicação 14 em que a cura em conjunto na etapa (c) é a uma temperatura maior do que 230°F (110°C); e em que após remoção da camada de casca na etapa (d) nenhum material fibroso do pano tecido (11a) permanece na mesma superfície; e compreende ainda as etapas de: (e) fornecer um segundo substrato de compósito compreendendo fibras de reforço impregnadas com uma segunda matriz de resina; (f) aplicar um filme de adesivo na superfície ligável do primeiro substrato ou uma superfície do segundo substrato; (g) colocar a superfície ligável do primeiro substrato de compósito (10) em contato com uma superfície do segundo substrato de compósito com o filme adesivo entre as mesmas; e (h) curar para ligar o primeiro e o segundo substratos.
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