CN113135740B - 一种陶瓷基复合材料及其制备方法和应用 - Google Patents

一种陶瓷基复合材料及其制备方法和应用 Download PDF

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CN113135740B
CN113135740B CN202110224316.9A CN202110224316A CN113135740B CN 113135740 B CN113135740 B CN 113135740B CN 202110224316 A CN202110224316 A CN 202110224316A CN 113135740 B CN113135740 B CN 113135740B
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ceramic
matrix composite
fiber cloth
ceramic matrix
composite material
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CN113135740A (zh
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张勃兴
李豪
邱文丰
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South China University of Technology SCUT
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Abstract

本发明公开了一种陶瓷基复合材料及其制备方法和应用。本发明的陶瓷基复合材料的制备方法包括以下步骤：将有机粘接剂、无机粘接剂和不同级配的陶瓷粉体配制成陶瓷浆料，再将纤维布涂覆陶瓷浆料后进行层压和预烧，再浸渍陶瓷前驱体溶液后进行原位交联和烧结。本发明中的陶瓷浆料可与多种连续纤维匹配，有效地浸入到纤维束间和纤维束内部，再结合陶瓷前驱体真空‑加压浸渍‑原位交联工艺，可以使氧化物陶瓷基体在低于1200℃的条件下有效烧结，制备得到的陶瓷基复合材料在1100℃空气环境下放置1000h弯曲强度可以保留80％以上。

Description

一种陶瓷基复合材料及其制备方法和应用
技术领域
本发明涉及陶瓷基复合材料技术领域，具体涉及一种陶瓷基复合材料及其制备方法和应用。
背景技术
陶瓷基复合材料具有较低的密度、优异的热稳定性和抗氧化能力，且生产成本比金属材料低，近年来备受关注。连续纤维增强陶瓷基复合材料主要由连续纤维和陶瓷基体组成，常见的连续纤维有碳纤维、氧化物陶瓷纤维、碳化硅纤维、氮化硅纤维等，陶瓷基体根据组成可以分为非氧化物陶瓷基体(例如：碳化硅、碳化锆、硼化锆、硼化铪以及由前几种陶瓷组成的复相陶瓷等)和氧化物陶瓷基体(例如：氧化硅、氧化铝、莫来石、氧化铪、氧化锆等)。
氧化物陶瓷连续纤维增强氧化物陶瓷基复合材料(简写为氧化物/氧化物陶瓷基复合材料)与非氧化物陶瓷连续纤维增强非氧化物陶瓷基复合材料(简写为非氧化物/非氧化物陶瓷基复合材料)相比，其在含有氧气、水汽和二氧化碳的高温环境下具有更好的耐腐蚀性和更长的使用寿命，因而在航空发动机和高温燃气轮机等领域具有广阔的应用前景。
目前，常见的商品化氧化物陶瓷连续纤维为美国3M公司的Nextel-610和Nextel-720，二者的主要成分均为氧化铝，使用温度上限都不超过1200℃，在此温度之上，组成纤维的陶瓷晶粒会迅速增长，导致纤维的力学性能快速衰减。因此，受限于氧化铝纤维的使用温度，氧化物陶瓷基体需要在1200℃以下完成烧结，这对传统的氧化物陶瓷来说是个巨大的挑战。
在早期研究中，国内学者多采用氧化硅溶胶和氧化铝溶胶作为陶瓷基体的原材料，虽然氧化硅溶胶和氧化铝溶胶具有较高的烧结活性，可以在1200℃以下实现烧结，但其高温热稳定性差，在1000℃以上的高温环境下无法长时间使用。在这之后，又有研究人员将纳米陶瓷粉体与陶瓷前驱体结合，用以解决陶瓷基体的烧结问题，但同样无法保证陶瓷基体在高温环境下的热稳定性。
发明内容
本发明的目的之一在于提供一种力学性能优异、可在1000℃以上的含有水汽、氧气和二氧化碳的环境中长期使用的陶瓷基复合材料。
本发明的目的之二在于提供上述陶瓷基复合材料的制备方法。
本发明的目的之三在于提供上述陶瓷基复合材料在制备航空发动机和燃气轮机中的应用。
本发明所采取的技术方案是：
一种陶瓷基复合材料的制备方法包括以下步骤：将有机粘接剂、无机粘接剂和不同级配的陶瓷粉体配制成陶瓷浆料，再将纤维布涂覆陶瓷浆料后进行层压和预烧，再浸渍陶瓷前驱体溶液后进行原位交联和烧结。
优选的，一种陶瓷基复合材料的制备方法包括以下步骤：将有机粘接剂、无机粘接剂和不同级配的陶瓷粉体配制成陶瓷浆料，再将纤维布涂覆陶瓷浆料后进行层压和预烧，再浸渍陶瓷前驱体溶液后进行原位交联和烧结，重复进行浸渍陶瓷前驱体溶液、原位交联和烧结多次。
进一步优选的，一种陶瓷基复合材料的制备方法包括以下步骤：将有机粘接剂、无机粘接剂和不同级配的陶瓷粉体配制成陶瓷浆料，再将纤维布涂覆陶瓷浆料后进行干燥、层压、固化、热解和预烧，再浸渍陶瓷前驱体溶液后进行原位交联、干燥、热解和烧结，重复进行浸渍陶瓷前驱体溶液、原位交联、干燥、热解和烧结多次。
优选的，所述有机粘接剂为聚乙烯醇、聚乙二醇、聚环氧乙烷、聚丙烯酸、羟甲基纤维素、羟乙基纤维素、羟丙基纤维素、聚乙烯吡咯烷酮中的至少一种。
优选的，所述无机粘接剂为硅酸锂、硅酸钠、硅酸钾、硅酸镁锂、硼酸钠、硅溶胶、铝溶胶、钛溶胶、锆溶胶中的至少一种。
优选的，所述陶瓷粉体为氧化硅粉体、氧化铝粉体、氧化钛粉体、氧化锆粉体、氧化钇粉体、氧化镁粉体、氧化钙粉体中的至少一种。
优选的，所述陶瓷粉体的中位粒径(D50)为10nm～10μm。将不同级配的陶瓷粉体搭配(例如：D50分别为20nm、200nm和2μm的陶瓷粉体搭配)使用，可以获得较高的堆积密度和高温环境下的尺寸稳定性。
优选的，所述纤维布为碳纤维布、碳化硅纤维布、氮化硅纤维布、玻璃纤维布、石英纤维布、氧化铝纤维布、氧化硅-氧化铝复合纤维布、氧化铝-氧化锆复合纤维布、氧化硅-氧化铝-氧化锆复合纤维布中的一种。
优选的，所述陶瓷浆料通过单/双面刷涂或浸渍的方式涂覆到纤维布上。
优选的，所述预烧在800℃～1500℃下进行。
优选的，所述陶瓷前驱体溶液为小分子陶瓷前驱体溶液或聚合物陶瓷前驱体溶液。
优选的，所述小分子陶瓷前驱体溶液为含有异丙醇铝、钛酸乙酯、钛酸丙酯、钛酸异丙酯、钛酸丁酯、锆酸乙酯、锆酸丙酯、锆酸异丙酯、锆酸丁酯中的至少一种的溶液。
优选的，所述聚合物陶瓷前驱体溶液为含有聚硅氧烷、聚铝氧烷、聚锆氧烷、聚钛氧烷中的至少一种的溶液。
优选的，所述浸渍陶瓷前驱体溶液的具体操作为：将预烧过的产品放入反应器中，抽真空，再加入陶瓷前驱体溶液，加压并保持。
进一步优选的，所述浸渍陶瓷前驱体溶液的具体操作为：将预烧过的产品放入反应器中，抽真空，再加入陶瓷前驱体溶液，加压至0.5MPa～10MPa并保持。
优选的，所述固化在40℃～300℃下进行。
进一步优选的，所述固化在150℃～250℃下进行。
优选的，所述热解在200℃～1000℃下进行。
进一步优选的，所述热解在300℃～800℃下进行。
优选的，所述烧结在800℃～1500℃下进行。
进一步优选的，所述烧结在1000℃～1200℃下进行。
本发明的有益效果是：本发明中的陶瓷浆料可与多种连续纤维匹配，有效地浸入到纤维束间和纤维束内部，再结合陶瓷前驱体真空-加压浸渍-原位交联工艺，可以使氧化物陶瓷基体在低于1200℃的条件下有效烧结，制备得到的陶瓷基复合材料在1100℃空气环境下放置1000h弯曲强度可以保留80％以上。
具体来说：
1)本发明中的陶瓷浆料的组成设计灵活性高，可以加入多种陶瓷组分，适用于预浸布工艺和三维预制体浸渍工艺，可以满足多种应用需求；
2)本发明通过陶瓷浆料结合陶瓷前驱体真空-高压浸渍-原位交联工艺，可以同时实现高烧结活性和优异热稳性，这是传统工艺无法达到的；
3)本发明中的氧化物陶瓷基体与连续纤维之间由多孔界面控制，无需制备纤维防护涂层，在应对外力破坏过程中，不会发生脆性断裂，可以通过基体与纤维剥离、纤维拔出、纤维断裂等多种机制进行能量耗散，使制备得到的氧化物陶瓷基复合材料具有良好的机械强度和断裂韧性。
附图说明
图1为本发明的陶瓷基复合材料的基体组成与演变过程示意图。
图2为实施例2的陶瓷基复合材料断面的SEM图。
图3为实施例2的陶瓷基复合材料的弯曲应力-应变曲线。
图4为实施例3的陶瓷基复合材料断面的SEM图。
图5为实施例3的陶瓷基复合材料的弯曲应力-应变曲线。
具体实施方式
下面结合具体实施例对本发明作进一步的解释和说明。
实施例1：
一种陶瓷基复合材料，其制备方法包括以下步骤：
1)将10g的聚乙烯醇和5g的硅酸钠加入200mL的水中，搅拌溶解，再依次加入20g的D50为20nm的氧化铝粉体、40g的D50为200nm的氧化铝粉体和40g的D50为2μm的氧化铝粉体，进行球磨，得到陶瓷浆料；
2)将陶瓷浆料刷涂到氧化铝纤维布上，再置于烘箱中60℃干燥2h，得到预浸布，再将预浸布叠放到金属模具中，在压力2MPa、温度100℃的条件下层压处理1h，得到复合材料坯体，再将复合材料坯体置于烘箱中200℃固化1h，再置于马弗炉中500℃热解6h，900℃预烧2h，得到预烧的样品；
3)将预烧的样品置于压力罐中，抽真空0.5h，再注入浓度0.5mol/L的异丙醇铝的甲苯溶液，加压至2MPa并保持0.5h，再升温至150℃保温保压1h，再取出样品置于烘箱中150℃干燥2h，再置于马弗炉中500℃热解6h，900℃预烧2h；
4)重复步骤3)的操作5次，再将样品置于马弗炉中1200℃烧结2h，即得陶瓷基复合材料。
经测试，陶瓷基复合材料的最大弯曲应力约为180MPa，且陶瓷基复合材料在空气气氛中1100℃放置1000h后弯曲强度可以保留80％以上。
实施例2：
一种陶瓷基复合材料，其制备方法包括以下步骤：
1)将10g的羟甲基纤维素和50g质量分数20％的硅溶胶加入200mL的水中，搅拌溶解，再依次加入50g的D50为200nm的氧化铝粉体和50g的D50为1μm的氧化铝粉体，进行球磨，得到陶瓷浆料；
2)将陶瓷浆料刷涂到氧化铝纤维布上，再置于烘箱中60℃干燥2h，得到预浸布，再将预浸布叠放到金属模具中，在压力2MPa、温度100℃的条件下层压处理1h，得到复合材料坯体，再将复合材料坯体置于烘箱中200℃固化1h，再置于马弗炉中500℃热解6h，900℃预烧2h，得到预烧的样品；
3)将预烧的样品置于压力罐中，抽真空0.5h，再注入浓度0.5mol/L的异丙醇铝的甲苯溶液，加压至2MPa并保持0.5h，再升温至150℃保温保压1h，再取出样品置于烘箱中150℃干燥2h，再置于马弗炉中500℃热解6h，900℃预烧2h；
4)重复步骤3)的操作5次，再将样品置于马弗炉中1200℃烧结2h，即得陶瓷基复合材料。
陶瓷基复合材料的基体组成与演变过程示意图如图1所示。
陶瓷基复合材料断面的SEM图如图2所示。
由图2可知：陶瓷基复合材料的断面处有明显的纤维拔出现象，呈现韧性断裂。
陶瓷基复合材料的弯曲应力-应变曲线如图3所示。
由图3可知：陶瓷基复合材料的最大弯曲应力约为200MPa。
此外，经测试陶瓷基复合材料在空气气氛中1100℃放置1000h后弯曲强度可以保留80％以上。
实施例3：
一种陶瓷基复合材料，其制备方法包括以下步骤：
1)将10g的聚乙烯吡咯烷酮和50g质量分数20％的铝溶胶加入200mL的水中，搅拌溶解，再依次加入50g的D50为200nm的氧化铝粉体和50g的D50为1.5μm的氧化铝粉体，进行球磨，得到陶瓷浆料；
2)将陶瓷浆料刷涂到氧化铝纤维布上，再置于烘箱中60℃干燥2h，得到预浸布，再将预浸布叠放到金属模具中，在压力2MPa、温度100℃的条件下层压处理1h，得到复合材料坯体，再将复合材料坯体置于烘箱中200℃固化1h，再置于马弗炉中500℃热解6h，900℃预烧2h，得到预烧的样品；
3)将预烧的样品置于压力罐中，抽真空0.5h，再注入浓度0.5mol/L的聚铝氧烷的异丙醇溶液，加压至6MPa并保持0.5h，再升温至200℃保温保压1h，再取出样品置于烘箱中150℃干燥2h，再置于马弗炉中500℃热解6h，900℃预烧2h；
4)重复步骤3)的操作3次，再将样品置于马弗炉中1200℃烧结2h，即得陶瓷基复合材料。
陶瓷基复合材料断面的SEM图如图4所示。
由图4可知：陶瓷基复合材料的断面处有明显的纤维拔出现象，呈现韧性断裂。
陶瓷基复合材料的弯曲应力-应变曲线如图5所示。
由图5可知：陶瓷基复合材料的最大弯曲应力约为250MPa。
此外，经测试陶瓷基复合材料在空气气氛中1100℃放置1000h后弯曲强度可以保留80％以上。
实施例4：
一种陶瓷基复合材料，其制备方法包括以下步骤：
1)将10g的羟丙基纤维素和50g质量分数10％的锆溶胶加入200mL的水中，搅拌溶解，再依次加入10g的D50为50nm的氧化锆粉体和90g的D50为1μm的氧化锆粉体，进行球磨，得到陶瓷浆料；
2)将陶瓷浆料刷涂到氧化铝纤维布上，再置于烘箱中60℃干燥2h，得到预浸布，再将预浸布叠放到金属模具中，在压力2MPa、温度100℃的条件下层压处理1h，得到复合材料坯体，再将复合材料坯体置于烘箱中200℃固化1h，再置于马弗炉中500℃热解6h，900℃预烧2h，得到预烧的样品；
3)将预烧的样品置于压力罐中，抽真空0.5h，再注入浓度0.5mol/L的聚锆氧烷的异丙醇溶液，加压至3MPa并保持0.5h，再升温至220℃保温保压1h，再取出样品置于烘箱中150℃干燥2h，再置于马弗炉中500℃热解6h，900℃预烧2h；
4)重复步骤3)的操作3次，再将样品置于马弗炉中1200℃烧结2h，即得陶瓷基复合材料。
经测试，陶瓷基复合材料的最大弯曲应力约为180MPa，且陶瓷基复合材料在空气气氛中1100℃放置1000h后弯曲强度可以保留80％以上。
实施例5：
一种陶瓷基复合材料，其制备方法包括以下步骤：
1)将10g的羟丙基纤维素和50g质量分数10％的锆溶胶加入200mL的水中，搅拌溶解，再依次加入20g的D50为50nm的氧化锆粉体和80g的D50为1μm的氧化铝粉体，进行球磨，得到陶瓷浆料；
2)将陶瓷浆料刷涂到氧化铝纤维布上，再置于烘箱中60℃干燥2h，得到预浸布，再将预浸布叠放到金属模具中，在压力2MPa、温度100℃的条件下层压处理1h，得到复合材料坯体，再将复合材料坯体置于烘箱中200℃固化1h，再置于马弗炉中500℃热解6h，900℃预烧2h，得到预烧的样品；
3)将预烧的样品置于压力罐中，抽真空0.5h，再注入浓度0.5mol/L的聚铝氧烷-聚锆氧烷的异丙醇溶液(聚铝氧烷、聚锆氧烷的质量比为5:1)，加压至3MPa并保持0.5h，再升温至220℃保温保压1h，再取出样品置于烘箱中150℃干燥2h，再置于马弗炉中500℃热解6h，900℃预烧2h；
4)重复步骤3)的操作3次，再将样品置于马弗炉中1200℃烧结2h，即得陶瓷基复合材料。
经测试，陶瓷基复合材料的最大弯曲应力约为210MPa，且陶瓷基复合材料在空气气氛中1100℃放置1000h后弯曲强度可以保留80％以上。
实施例6：
一种陶瓷基复合材料，其制备方法包括以下步骤：
1)将10g的聚丙烯酸和50g质量分数20％的铝溶胶加入200mL的水中，搅拌溶解，再依次加入50g的D50为50nm的氧化铝粉体和50g的D50为1μm的氧化铝粉体，进行球磨，得到陶瓷浆料；
2)将陶瓷浆料刷涂到氧化铝纤维布上，再置于烘箱中60℃干燥2h，得到预浸布，再将预浸布叠放到金属模具中，在压力2MPa、温度100℃的条件下层压处理1h，得到复合材料坯体，再将复合材料坯体置于烘箱中200℃固化1h，再置于马弗炉中500℃热解6h，900℃预烧2h，得到预烧的样品；
3)将预烧的样品置于压力罐中，抽真空0.5h，再注入浓度0.5mol/L的聚铝氧烷的异丙醇溶液，加压至3MPa并保持0.5h，再升温至200℃保温保压1h，再取出样品置于烘箱中150℃干燥2h，再置于马弗炉中500℃热解6h，900℃预烧2h；
4)重复步骤3)的操作2次，再将陶瓷前驱体溶液替换成浓度0.5mol/L的聚锆氧烷的异丙醇溶液后重复步骤3)的操作2次，再将样品置于马弗炉中1200℃烧结2h，即得陶瓷基复合材料。
经测试，陶瓷基复合材料的最大弯曲应力约为230MPa，且陶瓷基复合材料在空气气氛中1100℃放置1000h后弯曲强度可以保留80％以上。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (6)

1.一种陶瓷基复合材料的制备方法，其特征在于，包括以下步骤：将有机粘接剂、无机粘接剂和不同级配的陶瓷粉体配制成陶瓷浆料，再将纤维布涂覆陶瓷浆料后进行层压和预烧，再浸渍陶瓷前驱体溶液后进行原位交联和烧结，重复进行浸渍陶瓷前驱体溶液、原位交联和烧结多次；所述陶瓷前驱体溶液为小分子陶瓷前驱体溶液或聚合物陶瓷前驱体溶液；所述小分子陶瓷前驱体溶液为含有异丙醇铝、钛酸乙酯、钛酸丙酯、钛酸异丙酯、钛酸丁酯、锆酸乙酯、锆酸丙酯、锆酸异丙酯、锆酸丁酯中的至少一种的溶液；所述聚合物陶瓷前驱体溶液为含有聚硅氧烷、聚铝氧烷、聚锆氧烷、聚钛氧烷中的至少一种的溶液；所述浸渍陶瓷前驱体溶液的具体操作为：将预烧过的产品放入反应器中，抽真空，再加入陶瓷前驱体溶液，加压至0.5MPa～10MPa并保持；所述陶瓷粉体为氧化硅粉体、氧化铝粉体、氧化钛粉体、氧化锆粉体、氧化钇粉体、氧化镁粉体、氧化钙粉体中的至少一种；所述不同级配的陶瓷粉体包括以下几种情况：1）中位粒径20nm、200nm和2µm的陶瓷粉体搭配；2）中位粒径200nm和1µm的陶瓷粉体搭配；3）中位粒径200nm和1.5µm的陶瓷粉体搭配；4）中位粒径50nm和1µm的陶瓷粉体搭配。
2.根据权利要求1所述的陶瓷基复合材料的制备方法，其特征在于：所述有机粘接剂为聚乙烯醇、聚乙二醇、聚环氧乙烷、聚丙烯酸、羟甲基纤维素、羟乙基纤维素、羟丙基纤维素、聚乙烯吡咯烷酮中的至少一种。
3.根据权利要求1所述的陶瓷基复合材料的制备方法，其特征在于：所述无机粘接剂为硅酸锂、硅酸钠、硅酸钾、硅酸镁锂、硼酸钠、硅溶胶、铝溶胶、钛溶胶、锆溶胶中的至少一种。
4.根据权利要求1所述的陶瓷基复合材料的制备方法，其特征在于：所述纤维布为碳纤维布、碳化硅纤维布、氮化硅纤维布、玻璃纤维布、石英纤维布、氧化铝纤维布、氧化硅-氧化铝复合纤维布、氧化铝-氧化锆复合纤维布、氧化硅-氧化铝-氧化锆复合纤维布中的一种。
5.一种陶瓷基复合材料，其特征在于：由权利要求1～4中任意一项所述的方法制备得到。
6.权利要求5所述的陶瓷基复合材料在制备航空发动机和燃气轮机中的应用。
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