CN114907127B - 一种基体改性的SiC/SiC复合材料及其制备方法 - Google Patents

一种基体改性的SiC/SiC复合材料及其制备方法 Download PDF

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CN114907127B
CN114907127B CN202210501121.9A CN202210501121A CN114907127B CN 114907127 B CN114907127 B CN 114907127B CN 202210501121 A CN202210501121 A CN 202210501121A CN 114907127 B CN114907127 B CN 114907127B
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余煜玺
魏永金
吕璇
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Namite New Materials Technology Chongqing Co ltd
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Abstract

一种基体改性的SiC/SiC复合材料及其制备方法，涉及碳化硅陶瓷基复合材料的制备。包括以下步骤：S1：制备改性NITE‑SiC浆料预制板：将纳米SiC粉体、改性颗粒、聚碳硅烷与有机溶剂混合成浆料后干燥制成浆料预制板；S2：交替堆叠：将SiC纤维布与浆料预制板交替、叠层，加压固定获得SiC/SiC胚体；S3：热压烧结：将胚体在惰性气体气氛下高温下加压烧结，获得基体改性的SiC/SiC复合材料。可降低NITE制备SiC/SiC复合材料的难度，在制备NITE‑SiC浆料时引入改性颗粒，提高SiC/SiC复合材料的性能，扩宽SiC/SiC复合材料的应用领域。

Description

一种基体改性的SiC/SiC复合材料及其制备方法
技术领域
本发明涉及碳化硅陶瓷基复合材料的制备领域，具体是涉及一种基体改性的SiC/SiC复合材料及其制备方法。
背景技术
SiC/SiC复合材料具有高温耐蒸汽腐蚀、耐辐照、耐高温、高强度、高化学稳定性等优异性能，在航空航天和核能等领域具有广阔的应用前景。SiC/SiC复合材料由SiC纤维、SiC基体和连接两者的界面相组成，它的性能是复合材料结构设计、制备工艺等共同协同作用的结果，对制备工艺的改进仍是SiC/SiC复合材料性能优化的一种手段。
现有SiC/SiC复合材料的制备工艺有化学气相沉积法(CVI)、先驱体浸渍裂解法(PIP)、纳米渗透共晶转变法(NITE)、反应熔渗法(RMI)。其中纳米渗透共晶转变法(NITE)是本世纪初才被日本开发的一种SiC/SiC复合材料制备工艺，在热压烧结工艺基础上发展起来的，基本工艺流程为：将SiC粉体和烧结助剂与有机溶剂混合成浆料，然后浸渍纤维编织体，最后热压烧结获得SiC/SiC复合材料。NITE一次烧结即可成型，制备周期短，得到的SiC基体致密度高、结晶度高、热导率高、接近化学计量比、化学稳定性好的特点，具有较高的强度和韧性，但是需要高温高压条件和复杂的模具。
综上，NITE虽然能获得的致密度高、基体结晶度高的SiC/SiC复合材料，但是其制备难度大，适用范围小。因此，如何优化NITE制备SiC/SiC复合材料制备工艺困难的问题和提高SiC/SiC复合材料的性能是目前NITE制备SiC/SiC复合材料亟需解决的问题，为此，本发明提出了一种基体改性的SiC/SiC复合材料及其制备方法，在克服NITE制备工艺困难的基础上，对基体进行改性，提高SiC/SiC复合材料的性能，扩宽SiC/SiC复合材料的应用领域。
发明内容
本发明的目的在于针对现有技术的上述不足，提供可降低NITE制备SiC/SiC复合材料的难度，通过基体改性提高SiC/SiC复合材料性能的一种基体改性的SiC/SiC复合材料及其制备方法。
本发明首先制备含SiC颗粒、改性颗粒和聚碳硅烷的浆料预制板，之后与SiC纤维布交替堆叠，最后进行热等静压烧结获得SiC/SiC复合材料，可提高SiC/SiC复合材料的性能。
一种基体改性的SiC/SiC复合材料的制备方法，包括以下步骤：
1)制备改性NITE-SiC浆料预制板：将纳米SiC粉体、改性颗粒、聚碳硅烷与有机分散剂混合成浆料后干燥制成浆料预制板；
2)交替堆叠：将SiC纤维布与浆料预制板交替、叠层，加压固定获得SiC/SiC胚体；
3)热等静压烧结：将胚体在惰性气氛下高温下加压烧结，获得基体改性的SiC/SiC复合材料。
在步骤1)中，所述改性颗粒可选自不同陶瓷颗粒中任一种或多种的组合颗粒，优选为氧化铝、氧化钇、氧化锆、铝中的任一种或混合物，颗粒直径可为200～400μm；所述改性颗粒︰纳米SiC粉体︰聚碳硅烷＝(5～6)︰(3～4)︰1，在制备浆料前将各粉体共混置于行星式球磨机球磨，浆料中液相︰固相＝(0.5～1)︰4。
在步骤1)中，所述浆料预制板厚度为300～500μm。
在步骤2)中，所述SiC纤维布可以为二维双轴和二维三轴纤维布，纤维布厚度为0.3～0.5μm；所述加压的条件为：施加恒压30～50MPa，保压时间为15～30min。
步骤3)中，所述惰性气氛为氩气，烧结温度为1700～1900℃，升温速率为10～15℃/min，加压压力为20～40MPa，保温温度为2～4h。
本发明提供一种降低NITE制备SiC/SiC复合材料的难度和对SiC/SiC复合材料进行改性的技术思路，通过制备改性NITE-SiC浆料预制板、交替堆叠和热等静压烧结从而得到一种基体改性的SiC/SiC复合材料，本发明至少包含下列优点：
1)本发明在传统NITE-SiC浆料的基础上添加一定比例的聚碳硅烷，聚碳硅烷裂解可以将纳米SiC颗粒和改性颗粒固定在SiC胚体上，保证结构完整性，降低烧结难度。
2)本发明所使用的浆料为干燥后的浆料预制板，避免液相浆料需要真空浸渗或者电泳浸渗工序，减少制备工序，提高制备效率。
3)本发明使用陶瓷颗粒对SiC基体进行改性，在烧结前后，陶瓷的组成和性能没有发生改变，是最终产品的一部分，可以提高SiC/SiC复合材料的性能，同时也可以作为烧结助剂，降低SiC烧结的难度。
附图说明
图1为实施例1制备的复合材料实物图。
图2为实施例2制备的复合材料微观形貌。
图3为实施例2制备的复合材料的XRD图谱。
图4为实施例3制备的复合材料的TG-DSC曲线。
具体实施方式
为更进一步阐述本发明为达成预定发明目的所采取的的技术手段及功效，下面将结合本发明较佳实施例，对本发明提出的一种基体改性的SiC/SiC复合材料及其制备方法的具体实施方式、结构、特征及其功效，详细说明如后。显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。本发明中未限定的材料可采用市售或常用产品。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。此外，一或多个实施例中的特定特征、结构、或特点可由任何合适形式组合。
本发明在原有的NITE-SiC浆料的基础上添加一定比例的改性颗粒和聚碳硅烷，将浆料干燥制成浆料预制板，将SiC纤维布与浆料预制板交替、叠层，加压固定获得SiC/SiC胚体，对胚体在惰性气体气氛下高温下加压烧结，获得基体改性的SiC/SiC复合材料。
实施例1：
(1)制备改性NITE-SiC浆料预制板：将聚碳硅烷10％，碳化硅粉体30％和氧化铝颗粒60％分散在有机分散剂中，液相︰固相＝1︰4，通过球磨法混合均匀，球料比为6︰4，时间为10h，制成NITE-SiC浆料，在100℃烘箱中干燥5h获得改性NITE-SiC浆料预制板，预制板厚度为264μm。
(2)交替堆叠：将SiC纤维布(厚度为250μm)与浆料预制板交替、叠层(6层)，施加30MPa压力进行压制，并保压15min，获得SiC/SiC胚体。
(3)热等静压烧结：将SiC/SiC胚体在氩气气氛保护下，以10℃/min升温至1700℃，气象压力为20MPa，并保温2h，随炉冷却得到SiC/SiC复合材料。
经检测，本实施例得到的基体改性的SiC/SiC复合材料的孔隙率为11％，密度为2.41g/cm3，弯曲强度为257MPa。图1为实施例1制备的复合材料实物图。
实施例2：
(1)制备改性NITE-SiC浆料预制板：将聚碳硅烷10％，碳化硅粉体35％和氧化锆颗粒55％分散在有机分散剂中，液相︰固相＝0.5︰4，通过球磨法混合均匀，球料比为6︰4，时间为10h，制成NITE-SiC浆料，在100℃烘箱中干燥5h获得改性NITE-SiC浆料预制板，预制板厚度为298μm。
(2)交替堆叠：将SiC纤维布(厚度为250μm)与浆料预制板交替、叠层(6层)，施加40MPa压力进行压制，并保压20min，获得SiC/SiC胚体。
(3)热等静压烧结：将SiC/SiC胚体在氩气气氛保护下，以15℃/min升温至1800℃，气象压力为30MPa，并保温4h，随炉冷却得到SiC/SiC复合材料。
经检测，本实施例得到的基体改性的SiC/SiC复合材料的孔隙率为13％，密度为2.53g/cm3，弯曲强度为212MPa。
实施例3：
(1)制备改性NITE-SiC浆料预制板：将聚碳硅烷10％，碳化硅粉体40％和氧化铝颗粒50％分散在有机分散剂中，液相︰固相＝0.5︰4，通过球磨法混合均匀，球料比为6︰4，时间为10h，制成NITE-SiC浆料，在100℃烘箱中干燥5h获得改性NITE-SiC浆料预制板，预制板厚度为395μm。
(2)交替堆叠：将SiC纤维布(厚度为250μm)与浆料预制板交替、叠层(6层)，施加40MPa压力进行压制，并保压20min，获得SiC/SiC胚体。
(3)热等静压烧结：将SiC/SiC胚体在氩气气氛保护下，以15℃/min升温至1900℃，气象压力为40MPa，并保温2h，随炉冷却得到SiC/SiC复合材料。
经检测，本实施例得到的基体改性的SiC/SiC复合材料的孔隙率为9％，密度为2.78g/cm3，弯曲强度为277MPa。
综上所述，本发明立足于NITE能获得的致密度高、基体结晶度高的SiC/SiC复合材料和制备难度大的特点，结合先驱体转化法和颗粒增强复合材料的优势，提出基体改性的SiC/SiC复合材料的新型制备体系，采用干燥后的浆料预制板可以避免液相浆料需要真空浸渗或者电泳浸渗工序，减少制备工序，提高制备效率。
在制备方法上，可以采用不同的SiC先驱体、改性颗粒和SiC粉体共混，经制备的SiC/SiC复合材料孔隙率为9％～13％，密度为241～2.78g/cm3，弯曲强度为212～277MPa。与传统二维SiC/SiC复合材料的性能(孔隙率约20％，弯曲强度150～250MPa)对比，本发明的制备方法制备得到的基体改性的SiC/SiC复合材料具有低孔隙率和良好的力学性能。
另外，采用扫描电子显微镜观测本发明的实施例2制备的SiC/SiC复合材料的微观形貌，如图2所示，可以看到复合材料具有致密的结构，颗粒被SiC基体包覆，因此，本发明提出的基体改性的SiC/SiC复合材料的新型制备体系，即保持二维SiC/SiC复合材料的力学性能，又提高SiC/SiC复合材料的致密度。
采用XRD技术分析了实施例2制备的SiC/SiC复合材料的相组成情况，如图3所示，可以看出复合材料的相组成包括SiC、ZrO2。
采用超高温同步热分析仪分析实施例3制备的SiC/SiC复合材料的热稳定情况，TG-DSC曲线如图4所示，SiC/SiC复合材料具有良好的热稳定性，不会因为基体的改性而发生变化。
需要说明的是，尽管已经示出和描述本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及等同物限定。以上所述仅是本发明的一部分较佳实施例而已，而不是全部的实施例，也并非对本发明作任何形式上的限制。依据本发明的技术实质对以上实施例所作的任何简单修改，等同变化与修饰，没有做出创造性劳动前提下所获得的所有其他实施例，均仍属于本发明技术方案的范围内。

Claims (3)

1.一种基体改性的SiC/SiC复合材料的制备方法，其特征在于包括以下步骤：
1）制备改性NITE-SiC浆料预制板：将纳米SiC粉体、改性颗粒、聚碳硅烷与有机分散剂混合成浆料后干燥制成浆料预制板；所述改性颗粒︰纳米SiC粉体︰聚碳硅烷=（5～6）︰（3～4）︰1，在制备浆料前将各粉体共混置于行星式球磨机球磨，浆料中液相︰固相=（0.5～1）︰4；所述改性颗粒为氧化铝、氧化钇、氧化锆、铝中的任一种或混合物，颗粒直径为200～400μm；
2）交替堆叠：将SiC纤维布与浆料预制板交替、叠层，加压固定获得SiC/SiC胚体；所述SiC纤维布为二维双轴和二维三轴纤维布，纤维布厚度为0.3～0.5μm；所述加压的条件为：施加恒压30～50 MPa，保压时间为15～30 min；
3）热等静压烧结：将胚体在惰性气氛下高温下加压烧结，获得基体改性的SiC/SiC复合材料；所述惰性气氛为氩气，烧结的温度为1700～1900℃，升温速率为10～15℃/min，加压的压力为20～40 MPa，保温时间为2～4h。
2.如权利要求1所述一种基体改性的SiC/SiC复合材料的制备方法，其特征在于在步骤1）中，所述浆料预制板厚度为300～500 μm。
3.如权利要求1～2中任一项所述制备方法制备的基体改性的SiC/SiC复合材料。
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