CN116768642A - 一种长螺旋纤维增韧陶瓷基复合材料的制备方法 - Google Patents
一种长螺旋纤维增韧陶瓷基复合材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种长螺旋纤维增韧陶瓷基复合材料的制备方法，具体涉及增材制造技术领域，包括以下步骤：1）制备长螺旋纤维的酚醛树脂复合材料；2）对目标结构进行建模并拆分，根据需求将长螺旋纤维的酚醛树脂复合材料加工制得结构规整的模块；3）将模块使用酚醛树脂进行组装粘接，得到酚醛树脂材料；4）将制得酚醛树脂材料进行碳化处理，得到含碳预制体；5）在真空环境中，将液态硅渗入含碳预制体内反应，制备得到连续致密的长螺旋纤维增韧陶瓷基复合材料。本发明的目的在于提供一种全新的且行之有效的，可以突破具有复杂结构的长螺旋纤维增强陶瓷难以成型的问题，从而满足飞速发展的航空航天技术对高性能陶瓷基复合材料及部件的迫切需求。
Description
技术领域
本发明涉及增材制造技术领域，具体是指一种长螺旋纤维增韧陶瓷基复合材料的制备方法。
背景技术
随着航空航天领域飞行器向着更高速度的发展，热防护器件对材料的性能提出了更高的挑战。陶瓷基复合材料由于其相较合金具有更低的密度和更高的耐热温度，使其成为未来航空航天领域极具应用前景的热结构材料。然而，单一的陶瓷材料脆性大，往往不能被直接应用，通常需要引入碳化硅纤维或碳纤维等高性能纤维作为增强相以提升陶瓷材料的韧性。纤维增强陶瓷复合材料的成型过程基本上均是先采用连续纤维预先编织成所需的形貌结构，之后在模具工装的辅助下，经过反应渗透或前驱体预浸-裂解等方法最终获得纤维增强的陶瓷复合材料。除了传统的编制结构外，近年来受自然界启发而引入复合材料领域的长螺旋纤维不仅可以提升复合材料的拉伸强度，同时也可以大幅改善材料的冲击韧性，使其受到越来越多的关注。然而，长螺旋纤维增强复合材料的制备过程中，不仅作为增强相的长螺旋纤维制备复杂，纤维在复合过程中往往也需要依赖特殊的模具作为固定装置，目前仅适合制备结构比较简单的聚合物基复合材料，在纤维增强陶瓷基复合材料领域几乎未见报道。因此，开发一种将长螺旋纤维作为一种新的增强相引入到陶瓷复合材料中，同时也能制备复杂构件的新方法，将具有十分重要的研究意义和应用价值。
通过文献调研（Ceramics International 48 (2022) 19542–19556; J Am CeramSoc. 2019;102:3244–3255），我们发现近年发展起来的陶瓷增材制造技术虽然解决了复杂陶瓷构件成型困难的问题，但打印陶瓷中通常只能采用短切纤维或晶须等微纳米填料作为增强相，至今仍难以实现较长纤维尤其是长螺旋纤维增强碳化硅陶瓷的制备。
发明内容
本发明的目的在于提供一种全新的且行之有效的，可以突破具有复杂结构的长螺旋纤维增强陶瓷难以成型的问题，从而满足飞速发展的航空航天技术对高性能陶瓷基复合材料及部件的迫切需求的基于模块化设计的长螺旋纤维增韧陶瓷基复合材料的制备方法。
本发明通过下述技术方案实现：一种长螺旋纤维增韧陶瓷基复合材料的制备方法，其特征在于，包括以下步骤：
步骤S1：制备长螺旋纤维的酚醛树脂复合材料；
步骤S2：将需制备得到的目标结构进行建模并拆分为不同结构单元，根据不同结构的需求，将步骤S1制备得到的长螺旋纤维的酚醛树脂复合材料通过加工制得结构规整的模块；
步骤S3：将步骤S2制得的结构规整的模块进行组装，并使用酚醛树脂作为粘接剂对相邻模块进行粘接，从而得到与目标结构相近的酚醛树脂材料；
步骤S4：将步骤S3制得酚醛树脂材料进行碳化处理，从而得到与目标结构相近的含碳预制体；
步骤S5：在真空环境中，将液态硅渗入步骤S4中得到的含碳预制体内反应，从而制备得到连续致密的长螺旋纤维增韧陶瓷基复合材料。
本技术方案工作原理为，由于长螺旋纤维引入的裂纹偏转和多重联锁结构，裂纹倾向于沿着纤维的螺旋界面传递，而这些纤维在陶瓷内有序且螺旋排列，阻碍了裂纹在基体內部的快速传播，从而使碳化硅陶瓷的韧性大幅提升，通过类似砌墙的方式实现碳化硅陶瓷的制备，从而可以在引入长螺旋纤维增强的基础上实现复杂结构的制备。
为了更好地实现本发明的方法，进一步地，所述步骤S1中制备长螺旋纤维的酚醛树脂复合材料的具体包括以下步骤：
步骤S11：将纤维通过牵线转子均匀且紧密地缠绕在钢丝上，并将纤维的两端固定；
步骤S12：在纤维表面涂刷酚醛树脂溶液，通过加热固化使纤维的长螺旋结构得到固定；
步骤S13：将长螺旋结构的纤维固定在模具中，并均匀地浇筑酚醛树脂，经过热固化步骤处理从而制备得到长螺旋纤维的酚醛树脂复合材料。
为了更好地实现本发明的方法，进一步地，所述步骤S11中使用的钢丝直径为50µm-500µm。
为了更好地实现本发明的方法，进一步地，所述步骤S11中所用的纤维为碳化硅织物、碳纤维、氮化硼纤维和氮化硅纤维织物中一种。
为了更好地实现本发明的方法，进一步地，所述步骤S11中所用的纤维为单丝纤维或束丝纤维。
为了更好地实现本发明的方法，进一步地，所述步骤S11中所用的纤维为单丝数量为1K-24K的束丝纤维。
为了更好地实现本发明的方法，进一步地，所述步骤S11中所用的纤维通过化学气相沉积或浸渍裂解在表面引入了热解碳界面、氮化硼界面、氮化硅界面或者碳化硅界面中的一种。
为了更好地实现本发明的方法，进一步地，所述步骤S12中，所用的酚醛树脂溶液为能溶解于甲醇和乙醇等有机溶剂中热塑性树脂配置而成，所述酚醛树脂溶液的固含量为50wt%。
为了更好地实现本发明的方法，进一步地，步骤S12中，所用的酚醛树脂溶液中还添加有微纳米填料或功能性填料。
为了更好地实现本发明的方法，进一步地，所述步骤S3中，模块组装的方式为交错堆砌。
本发明与现有技术相比，具有以下优点及有益效果：
（1）本发明通过长螺旋纤维引入的裂纹偏转和多重联锁结构，裂纹倾向于沿着纤维的螺旋界面传递，而这些纤维在陶瓷内有序且螺旋排列，阻碍了裂纹在基体內部的快速传播，从而使碳化硅陶瓷的韧性大幅提升；
（2）本发明通过模块化的设计思路，以类似砌墙的方式实现碳化硅陶瓷的制备，从而可以在引入长螺旋纤维增强的基础上实现复杂结构的制备，不仅可以将长纤维尤其是长螺旋纤维引入到陶瓷基复合材料中，同时可以实现具有复杂结构部件的制备；
（3）本发明的制备方法可以结合有限元等模拟手段，针对不同构件不同部位的性能需求定制模块，从而在克服“短板效应”的同时有效减少整体用料成本，相较传统的减材制造不仅可以节省大量的原料和工装模具，同时也能减少后续的加工步骤；
（4）本发明通过模块化设计，可以在构件的不同部位引入具有不同强度和不同功能的模块，从而实现传统陶瓷材料的结构与功能一体化设计与制造，适宜广泛推广应用。
附图说明
通过阅读参照以下附图对非限制性实施例所作的详细描述，本发明的其他特征、目的和优点将会变得更为明显：
图1为本发明中螺旋纤维的制备模型示意图；
图2为本发明中四种不同复合长螺旋纤维的酚醛树脂模块示意图，具体包括（a）第一种构型，（b）第二种构型，（c）第三种构型，（d）第四种构型；
图3为本发明中四种具有不同体积分数长螺旋纤维的模块示意图；具体包括（a）第一种构型，（b）第二种构型，（c）第三种构型，（d）第四种构型；
图4为本发明中模块的组装的横截面图；
图5为本发明中模块的组装结构示意图。
具体实施方式
下面详细描述本发明的实施例，所述实施例的示例在附图中示出，其中自始至终相同或类似的标号表示相同或类似的元件或具有相同或类似功能的元件。下面通过参考附图描述的实施例是示例性的，仅用于解释本发明，而不能理解为对本发明的限制。
为使本发明的目的、工艺条件及优点作用更加清楚明白，结合以下实施实例，对本发明作进一步详细说明，但本发明的实施方式不限于此，在不脱离本发明上述技术思想情况下，根据本领域普通技术知识和惯用手段，做出各种替换和变更，均应包括在本发明的范围内，此处所描述的具体实施实例仅用以解释本发明，并不用于限定本发明。
实施例1：
本实施例提供一种长螺旋纤维增韧陶瓷基复合材料的制备方法，其具体制备过程包括以下步骤：
（1）通过螺旋纤维成型装置将具有氮化硼界面层的碳化硅纤维制备成直径为300µm的长螺旋纤维，接着将螺旋纤维的固定在预定的模具中（横截面每平方厘米平行铺设12根长螺旋纤维），并均匀地浇筑复合1wt%碳化硅晶须的酚醛树脂，经过热固化处理从而制备得到复合长螺旋纤维的酚醛树脂复合材料。
（2）根据不同目标结构的使用需求，将上述制备得到的复合材料通过加工分别制得相应种类的模块，如图2所示，给出了（a）、（b）、（c）、（d）四种加工成型的模块，本实施例优选制得长度为20mm，宽度为10mm，高度为5mm的模块，即图2中所示的第一种模块。
（3）将得到的模块进行组装，如图5所示，并以复合3wt%碳化硅晶须的酚醛树脂做粘接剂，从而得到与目标结构相近的酚醛树脂材料，组装方式的横截面，如图4所示；其中，根据目标结构的使用工况，可在结构的薄弱处独立制备强度更高的模块，如图3所示，给出了（a）、（b）、（c）、（d）四种具有不同体积分数长螺旋纤维的模块，从而使目标结构服役能力大幅提升，同时尽可能控制了整体的用料成本。
（4）将得到的酚醛树脂材料进行碳化处理，碳化工艺为：
a.室温（30℃或50℃）→180℃，升温时间2h，升温速率约1.25℃/min；
b.180℃，保温2h；
c.180℃→500℃，升温时间4h，升温速率约80℃/h（1.33℃/min）；
d.500℃，保温2h；
e.500℃→850℃，升温时间14h，升温速率约25℃/h（0.42℃/min）；
f.850℃，保温2h；
g.自然冷却降温至室温取出从而得到与目标结构相近的含碳预制体。
（5）在真空环境中，将液态硅渗入得到的预制体内反应，渗硅工艺为：将预制体置于石墨坩埚中，并且加入两倍质量的硅粉，在真空环境下升温至1500℃，保温20min后降温并移除多余硅粉，从而制备碳化硅陶瓷从而制备得到连续致密的长螺旋纤维增韧陶瓷基复合材料。
实施例2：
本实施例根据上述实施例制备的长螺旋纤维增韧陶瓷基复合材料，对其进行机械性能测试，并将其与单一碳化硅、短切纤维/碳化硅、编织连续纤维/碳化硅、长纤维/碳化硅进行机械性能对比，结果如表一所示，
表1 不同材料的机械机械性能
根据表一可知，相较短切纤维增强碳化硅陶瓷以及长直纤维增强碳化硅陶瓷具有明显的提升，接近编织连续纤维增强碳化硅陶瓷的水平。
实施例3：
本实施例在上述实施例的基础上，进一步限定制备长螺旋纤维的酚醛树脂复合材料的制备模型如图1所示，具体制备过程如下：
（1.1）将纤维通过牵线转子均匀且紧密地缠绕在钢丝上，并将纤维的两端固定；其中，使用的钢丝直径为50µm-500µm，所用的纤维为碳化硅织物、碳纤维、氮化硼纤维和氮化硅纤维织物中一种；所用的纤维为单丝数量为1K-24K的束丝纤维；所用的纤维通过化学气相沉积或浸渍裂解在表面引入了热解碳界面、氮化硼界面、氮化硅界面或者碳化硅界面中的一种；
（1.2）在纤维表面涂刷酚醛树脂溶液，通过加热固化使纤维的长螺旋结构得到固定；所用的酚醛树脂溶液为能溶解于甲醇和乙醇等有机溶剂中热塑性树脂配置而成，所述酚醛树脂溶液的固含量为50wt%；所用的酚醛树脂溶液中还添加有微纳米填料或功能性填料；
（1.3）将长螺旋结构的纤维固定在模具中，并均匀地浇筑酚醛树脂，经过热固化处理从而制备得到长螺旋纤维的酚醛树脂复合材料。
尽管已经示出和描述了本发明的实施例，本领域的普通技术人员可以理解：在不脱离本发明的原理和宗旨下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由权利要求及其等同物限定。
Claims (10)
1.一种长螺旋纤维增韧陶瓷基复合材料的制备方法，其特征在于，包括以下步骤：
步骤S1：制备长螺旋纤维的酚醛树脂复合材料；
步骤S2：将需制备得到的目标结构进行建模并拆分为不同结构单元，根据不同结构的需求，将步骤S1制备得到的长螺旋纤维的酚醛树脂复合材料通过加工制得结构规整的模块；
步骤S3：将步骤S2制得的结构规整的模块进行组装，并使用酚醛树脂作为粘接剂对相邻模块进行粘接，从而得到与目标结构相近的酚醛树脂材料；
步骤S4：将步骤S3制得酚醛树脂材料进行碳化处理，从而得到与目标结构相近的含碳预制体；
步骤S5：在真空环境中，将液态硅渗入步骤S4中得到的含碳预制体内反应，从而制备得到连续致密的长螺旋纤维增韧陶瓷基复合材料。
2.根据权利要求1所述的一种长螺旋纤维增韧陶瓷基复合材料的制备方法，其特征在于，所述步骤S1中制备长螺旋纤维的酚醛树脂复合材料的具体包括以下步骤：
步骤S11：将纤维通过牵线转子均匀且紧密地缠绕在钢丝上，并将纤维的两端固定；
步骤S12：在纤维表面涂刷酚醛树脂溶液，通过加热固化使纤维的长螺旋结构得到固定；
步骤S13：将长螺旋结构的纤维固定在模具中，并均匀地浇筑酚醛树脂，经过热固化步骤处理从而制备得到长螺旋纤维的酚醛树脂复合材料。
3.根据权利要求2所述的一种长螺旋纤维增韧陶瓷基复合材料的制备方法，其特征在于，所述步骤S11中使用的钢丝直径为50µm-500µm。
4.根据权利要求3所述的一种长螺旋纤维增韧陶瓷基复合材料的制备方法，其特征在于，所述步骤S11中所用的纤维为碳化硅织物、碳纤维、氮化硼纤维和氮化硅纤维织物中的一种。
5.根据权利要求3所述的一种长螺旋纤维增韧陶瓷基复合材料的制备方法，其特征在于，所述步骤S11中所用的纤维为单丝纤维或束丝纤维。
6.根据权利要求5所述的一种长螺旋纤维增韧陶瓷基复合材料的制备方法，其特征在于，所述步骤S11中所用的纤维为单丝数量为1K-24K的束丝纤维。
7.根据权利要求3所述的一种长螺旋纤维增韧陶瓷基复合材料的制备方法，其特征在于，所述步骤S11中所用的纤维通过化学气相沉积或浸渍裂解在表面引入了热解碳界面、氮化硼界面、氮化硅界面或者碳化硅界面中的一种。
8.根据权利要求3所述的一种长螺旋纤维增韧陶瓷基复合材料的制备方法，其特征在于，所述步骤S12中，所用的酚醛树脂溶液为能溶解于甲醇或乙醇的热塑性树脂配置而成，所述酚醛树脂溶液的固含量为50wt%。
9.根据权利要求1或2所述的一种长螺旋纤维增韧陶瓷基复合材料的制备方法，其特征在于，步骤S12中，所用的酚醛树脂溶液中还添加有微纳米填料或功能性填料。
10.根据权利要求1或2所述的一种长螺旋纤维增韧陶瓷基复合材料的制备方法，其特征在于，所述步骤S3中，模块组装的方式为交错堆砌。
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