CN110256091B - 多晶莫来石纤维增强磷酸盐复合陶瓷天线罩高效成型方法 - Google Patents

多晶莫来石纤维增强磷酸盐复合陶瓷天线罩高效成型方法 Download PDF

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CN110256091B
CN110256091B CN201910550330.0A CN201910550330A CN110256091B CN 110256091 B CN110256091 B CN 110256091B CN 201910550330 A CN201910550330 A CN 201910550330A CN 110256091 B CN110256091 B CN 110256091B
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glue solution
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polycrystalline mullite
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吴广力
佘平江
刘俊君
刘义华
王芬
陈海昆
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Hubei Sanjiang Space Jiangbei Mechanical Engineering Co Ltd
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Abstract

本发明公开了一种多晶莫来石纤维增强磷酸盐复合陶瓷天线罩高效成型方法，步骤如下：1、对石英纤维进行表面预处理，并制作成两种尺寸规格的短切纤维。2、将磷酸二氢铝胶液和微米氧化铝固化剂，按照比例混合制备磷酸盐胶液；3、将短切纤维浸渍磷酸盐胶液，取出后的短切纤维铺在天线罩芯模上，达到所需厚度，并用针刺针法向随机针刺。晾置后，采用真空袋加压。4、保持真空压力状态下预固化，去掉真空袋升高温度进行终固化，脱模。5、将天线罩坯料在磷酸盐胶液中进行浸渍，加热固化，提高材料均匀性和纤维结合性。根据要求将天线罩坯料加工至设计尺寸。本方法制备工艺效率高、成本低，耐高温，抗烧蚀、法向强度高，均匀性好。

Description

多晶莫来石纤维增强磷酸盐复合陶瓷天线罩高效成型方法
技术领域
本发明涉及陶瓷基透波复合材料技术领域，具体地指一种多晶莫来石纤维增强磷酸盐复合陶瓷天线罩高效成型方法。
技术背景
天线罩是弹头结构重要组成部分，是透波、承载、防热和抗蚀功能与结构一体化产品。随着导弹等航天飞行器向高马赫长航时精确制导方向发展，要求天线罩具有更高的耐温性、抗烧蚀性、高强度以及高透波率，在特种情况下，目前最为成熟的石英增强石英复合陶瓷天线罩耐温度和抗烧蚀性能不能更好的满足航天产品要求，迫切需要开发新型透波复合材料。并且在军民融合的大市场环境下，军工武器成本控制要求越来越高，透波天线罩也向着低成本化方向发展，对成型效率和成本提出较高要求。
纤维增强磷酸盐复合陶瓷材料，具有低密度、低介电、低膨胀、耐高温、抗老化、高强度的优异性能，且结构可设计性强，工艺制备温度低，工艺成本低，是各种火箭、导弹等航天飞行器透波天线罩理想的材料选择。
发明内容
针对上述技术问题，本发明提出了一种多晶莫来石纤维增强磷酸盐复合陶瓷天线罩高效成型方法，该方法制备的透波天线罩成型速度快，工艺成本低，耐高温性能和机械性能优异。
为实现此目的，本发明所设计的多晶莫来石纤维增强磷酸盐复合陶瓷天线罩高效成型方法，其特征在于，它包括如下步骤：
步骤1：采用铝溶胶对多晶莫来石纤维进行表面预处理，提高纤维表面活性，表面预处理后的纤维短切成30～50mm和3～5mm的两种规格，并将30～50mm和3～5mm的两种规格的纤维按照5：1～10：1的比例混合，形成混合后短切纤维；该规格尺寸的纤维工艺性好，过长或过段均易结团，分散不均匀，且长短两种规格的纤维搭配使用对能够较好的兼顾强度和均匀性。采用铝溶胶对纤维表面进行预处理利于提高界面结合强度。采用多晶莫来石纤维相对普通莫来石纤维材料介电损耗低，利于天线罩产品透波；
步骤2：制备磷酸盐胶液；
步骤3：将混合后短切纤维，放入配制好的磷酸盐胶液中浸渍，将浸渍后的混合后短切纤维随机分布的铺在天线罩锥形芯模上，达到复合陶瓷天线罩的设计厚度，采用针刺方法法向刺纤维，晾置后，套上真空袋，抽真空加压；法向刺纤维能够有效增强法相作用力；
步骤4：保持真空压力状态下，对套有真空袋的天线罩锥形芯模加热预固化，加热预固化后，去掉真空袋，对天线罩锥形芯模升温进行终固化，脱模，形成天线罩坯料；采用真空袋加压状态下固化，一方面利于坯料内部微观气泡的排出，提高均匀性和界面结合性，另一方面真空压力条件下预固化利于结合强度和产品定型；
步骤5：天线罩坯料在低固含量磷酸盐胶液中进行浸渍，室温晾置12小时，然后放置在鼓风干燥箱中进行固化，将固化后的天线罩坯料加工至设计尺寸，即形成天线罩。
上述技术方案的步骤1中，多晶莫来石纤维不加捻度，多晶莫来石纤维放入氧化铝固含量5～10％铝溶胶中搅拌后静置15～30min，取出室温晾干，预处理后的纤维短切成30～50mm和3～5mm两种规格，按照5：1～10：1的比例混合。长规格纤维比例越高，复合材料强度越高，短规格比例越高，复合材料均匀性相对越好透波性能好，可根据产品强度和透波性需要调整比例。采用铝溶胶对多晶莫来石纤维表面处理，形成表面活性层，能够大大提高纤维与基体之间界面作用力。
上述技术方案的步骤2中，将磷酸二氢铝胶液和微米级氧化铝固化剂，按照1比0.8比例混合搅拌均匀，形成磷酸盐胶液。上述技术方案的步骤2中，磷酸二氢铝胶液中磷酸二氢铝固含量为30～40％，磷酸二氢铝胶液的溶剂为水和乙醇的混合物，水和乙醇质量比为10：1，加入的乙醇溶剂降低粘度，提高胶液的流动性，微米级氧化铝固化剂中氧化铝的粒径为50～300微米，材料的结合强度最优。
上述技术方案的步骤3中，采用针刺方法法向刺纤维，晾置要求在室温条件下进行，晾置时间12～24h至纤维表面表干不粘手。
上述技术方案中，所述抽真空压力要求为≤-0.95kPa，加压后如存在厚度不均，可打开真空袋，补铺浸胶后的纤维，至坯料平整，重新抽真空加压，该工步可重复进行。
上述技术方案的步骤4中，加热预固化制度为以3～6℃/h的升温速率，升温至100℃，保温2～3h，预固化过程中要求保持真空压力0.9～-0.99kPa，终固化制定为以10～15℃/h的升温速率，升温至200℃，保温2～3h，固化后脱模形成天线罩坯料。缓慢的升温速率利于溶剂挥发排出，能够提高固化效果。
上述技术方案的步骤5中，磷酸盐胶液由磷酸二氢铝胶液和纳米级氧化铝固化剂，按照1比0.8比例混合搅拌均匀，磷酸盐胶液中磷酸二氢铝固含量15～20％，浸渍后天线罩坯料室温晾置，放置鼓风干燥箱中，以10～15℃/h的升温速率，升温至200℃，保温2h～3h，进行固化，可升温至300～400℃保温2～3h进行后固化，然后加工至设计尺寸。采用纳米级固化剂进行浸渍能够有效增加磷酸盐胶液的渗透效果。300～400℃后固化能够降低材料介电损耗，提高材料透波性能。
本发明具有如下优点：
1、本发明中提出的多晶莫来石纤维增强磷酸盐复合陶瓷天线罩高效成型方法，相比石英增强石英复合天线罩的材料成本低且利用率高，成型效率高，工艺成本低。
2、本发明中制备的多晶莫来石纤维增强磷酸盐复合陶瓷材料，具有更高的耐高温性能(1600℃较长时间使用)、抗烧蚀性能、机械强度(弯曲强度100MPa以上)。
3、本发明中制备的复合材料采用混合短切纤维且各项无序分布，提高了纤维体积含量(40％以上)，增加材料强度，铺层后法向刺纤维，有效提高了法向层间强度(层间剪切强度10MPa以上)。
具体实施方式
以下结合实施例对本发明作进一步的详细说明：
实施例，某磷酸盐复合陶瓷天线罩成型方法，步骤如下：
步骤1：采用无捻多晶莫来石纤维，放入固含量5％纳米铝溶胶中搅拌后静置30min，取出室温晾干。预处理后的纤维短切成30～50mm和3～5mm两种规格，按照8：1的比例混合。
步骤2：将固含量为30～40％磷酸二氢铝胶液(溶剂为水和乙醇的混合物，质量比为10：1)和氧化铝固化剂(粒径100～200微米)，按照比例混合搅拌均匀，制备磷酸盐胶液；
步骤3：将混合后短切纤维，放入配制好的磷酸盐胶液中浸渍，晾置12h，取出后随机分布的铺在天线罩锥形芯模上，等厚度8mm，采用针刺针法向刺纤维。晾置后表面不粘手，套上真空袋，抽真空压力至≤-0.99kPa，针对不平整部位进行二次补铺浸胶后的纤维，至坯料平整，重新抽真空加压。
步骤4：保持真空压力状态下加热预固化，以4℃/h的升温速率，升温至100℃，保温3h；去掉真空袋升温进行终固化，以10℃/h的升温速率，升温至200℃，保温2h～3h，脱模，形成天线罩坯料。
步骤5：将天线罩坯料在20％磷酸盐胶液中进行浸渍，室温晾置至表面不粘手后，放置鼓风干燥箱中，以10℃/h的升温速率，升温至200℃，保温2h～3h，进行固化，然后在350℃条件下后固化2h，根据要求将天线罩坯料加工至设计尺寸，即形成天线罩。
本说明书未作详细描述的内容属于本领域专业技术人员公知的现有技术。

Claims (6)

1.一种多晶莫来石纤维增强磷酸盐复合陶瓷天线罩高效成型方法，其特征在于，它包括如下步骤：
步骤1：采用铝溶胶对多晶莫来石纤维进行表面预处理，表面预处理后的纤维短切成30～50mm和3～5mm的两种规格，并将30～50mm和3～5mm的两种规格的纤维按照5：1～10：1的比例混合，形成混合后短切纤维；
步骤2：制备磷酸盐胶液；
步骤3：将混合后短切纤维，放入配制好的磷酸盐胶液中浸渍，将浸渍后的混合后短切纤维随机分布的铺在天线罩锥形芯模上，达到复合陶瓷天线罩的设计厚度，采用针刺方法法向刺纤维，晾置后，套上真空袋，抽真空加压；
步骤4：保持真空压力状态下，对套有真空袋的天线罩锥形芯模加热预固化，加热预固化后，去掉真空袋，对天线罩锥形芯模升温进行终固化，脱模，形成天线罩坯料；
步骤5：天线罩坯料在磷酸盐胶液中进行浸渍，室温晾置，然后放置在鼓风干燥箱中进行固化，将固化后的天线罩坯料加工至设计尺寸，即形成天线罩；
所述步骤1中，多晶莫来石纤维不加捻度，多晶莫来石纤维放入氧化铝固含量5～10％铝溶胶中搅拌后静置15～30min，取出室温晾干，预处理后的纤维短切成30～50mm和3～5mm两种规格，按照5：1～10：1的比例混合。
2.根据权利要求1所述的多晶莫来石纤维增强磷酸盐复合陶瓷天线罩高效成型方法，其特征在于：所述步骤2中，将磷酸二氢铝胶液和微米级氧化铝固化剂，按照1比0.8比例混合搅拌均匀，形成磷酸盐胶液。
3.根据权利要求2所述的多晶莫来石纤维增强磷酸盐复合陶瓷天线罩高效成型方法，其特征在于：所述步骤2中，磷酸二氢铝胶液中磷酸二氢铝固含量为30～40％，磷酸二氢铝胶液的溶剂为水和乙醇的混合物，水和乙醇质量比为10：1，微米级氧化铝固化剂中氧化铝的粒径为50～300微米。
4.根据权利要求1所述的多晶莫来石纤维增强磷酸盐复合陶瓷天线罩高效成型方法，其特征在于：所述步骤3中，采用针刺方法法向刺纤维，晾置要求在室温条件下进行，晾置时间12～24h。
5.根据权利要求4所述的多晶莫来石纤维增强磷酸盐复合陶瓷天线罩高效成型方法，其特征在于：所述抽真空压力要求为≤-0.95kPa。
6.根据权利要求1所述的多晶莫来石纤维增强磷酸盐复合陶瓷天线罩高效成型方法，其特征在于：所述步骤5中，磷酸盐胶液由磷酸二氢铝胶液和纳米级氧化铝固化剂，按照1比0.8比例混合搅拌均匀，磷酸盐胶液中磷酸二氢铝固含量15～20％，浸渍后天线罩坯料室温晾置，放置鼓风干燥箱中，以10～15℃/h的升温速率，升温至200℃，保温2h～3h，进行固化，然后在350℃条件下后固化2h，然后加工至设计尺寸。
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