CN113004043A - 重结晶碳化硅制品等静压成型工艺 - Google Patents

重结晶碳化硅制品等静压成型工艺 Download PDF

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CN113004043A
CN113004043A CN201911321859.1A CN201911321859A CN113004043A CN 113004043 A CN113004043 A CN 113004043A CN 201911321859 A CN201911321859 A CN 201911321859A CN 113004043 A CN113004043 A CN 113004043A
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刘骏
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Abstract

本发明属于重结晶碳化硅制品成型领域，尤其涉及重结晶碳化硅制品等静压成型工艺。本发明提供的重结晶碳化硅制品等静压成型工艺，包括以下步骤：将如下重量份的原料混合：碳化硅粒度砂70‑85份，碳化硅微粉15‑30份，粘接剂0.7‑2份；将混合料装袋封口；将混合料等静压成型，压力为175‑240MPa，得到素坯；将素坯保压，保压时间为120‑170s，得到生坯；将生坯分别进行卸压、开盖取出、毛坯加工和烧结，得到重结晶碳化硅制品。本发明制得的碳化硅制品素坯中配入的粒度砂和微粉分布均匀、结合紧密，致密化的素坯，颗粒紧密接触，容易烧结，烧结制品的密度高，重结晶碳化硅制品的性能和附加值高。

Description

重结晶碳化硅制品等静压成型工艺
技术领域
本发明属于重结晶碳化硅制品成型领域，尤其涉及重结晶碳化硅制品等静压成型工艺。
背景技术
碳化硅制品是典型的以共价键为主的材料，具较高的高温强度、良好的抗氧化性、高热导率和低热膨胀系数、抗热震和耐化学腐蚀等优良特性，广泛应用于机械、冶金、化工和航空航天等领域的关键陶瓷部件。碳化硅制品的生坯密度是其一相非常重要的参数，它对烧成后碳化硅制品的密度起着至关重要的作用。碳化硅制品密度对碳化硅制品的使用寿命与其工作寿命有着非常大的影响。碳化硅制品随着使用温度和使用时间的增加，其碳化硅材料的高导热、抗热震、高强度将逐渐失效，最终因变化过大而不能继续使用。主要是因为制品在使用过程中，碳化硅发生氧化导致其化学与物理性能改变，从而降低了其使用寿命和使用温度。为防止它的氧化，尽可能地降低其气孔率、增大制品密度，这样可以大大提高制品的各项性能包括导热率、抗折强度、抗氧化性能和使用温度、使用寿命。由于原料堆积密度直接影响制品的生坯密度和烧成的制品密度，而现有的重结晶碳化硅制品的成型工艺，其原料堆积密度小，导致重结晶碳化硅制品的密度小，结晶碳化硅制品的性能较低。
发明内容
为解决上述技术问题，本发明的目的在于提供重结晶碳化硅制品等静压成型工艺，通过等静压成型，再进行烧结，可以提高重结晶碳化硅制品的密度，提高重结晶碳化硅制品的性能和附加值。
为实现上述目的，本发明采用以下技术方案，包括以下步骤：
将如下重量份的原料混合：碳化硅粒度砂70-85份，碳化硅微粉15-30份，粘接剂0.7-2份，以获得混合料；
将上述混合料装袋封口；
将装袋封口的混合料等静压成型，压力为175-240MPa，得到素坯；
将等静压成型的素坯保压，保压时间为120-170s，得到生坯；
将生坯分别进行卸压、开盖取出、毛坯加工和烧结，得到重结晶碳化硅制品。
优选地，所述碳化硅粒度砂由200um碳化硅粒度砂、100um碳化硅粒度砂和50um碳化硅粒度砂组成，各组分重量份配比为200um碳化硅粒度砂：100um碳化硅粒度砂：50um碳化硅粒度砂＝6:1:3。
优选地，所述碳化硅微粉由5um碳化硅微粉、10um碳化硅微粉和20um碳化硅微粉组成，各组分重量份配比为5um碳化硅微粉：10um碳化硅微粉：20um碳化硅微粉＝1:1:1。
优选地，所述粘接剂为70％的低分子量水溶性纤维素和30％低分子量水溶性聚乙烯醇。
优选地，烧结温度为2000-2400℃。
与现有技术相比，本发明具有以下有益效果：本发明制得的碳化硅制品素坯中配入的粒度砂和微粉分布均匀、结合紧密、坯体密实。粒度砂颗粒和微粉颗粒相互比较紧密地接触、啮合，其中微粉颗粒紧密的附着于粒度砂颗粒周围，并填充在粒度砂颗粒之间的空隙中，等静压成型压力大，压力来自三维方向，压力大且加压均匀，使带粘结剂、具有塑性的微粉颗粒，在大的三维压力下填入粒度砂的空隙中，使粒度砂原料颗粒紧密堆积，原料堆积密度大，因此获得了近于致密的素坯，在静压成型的压力和保压时间作用下粒度砂颗粒发生破碎、变形，提高生坯致密度，由于等静压成型的素坯已经致密化，致密化的素坯，颗粒紧密接触，容易烧结，烧结制品的密度高，重结晶碳化硅制品的性能和附加值高。
具体实施方式
为了使本发明要解决的技术问题、技术方案及有益效果更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
实施例1：
本发明实施例中，重结晶碳化硅制品等静压成型工艺，将如下重量份的原料混合：碳化硅粒度砂70份，碳化硅微粉30份，粘接剂0.7份，以获得混合料；所述碳化硅粒度砂由200um碳化硅粒度砂、100um碳化硅粒度砂和50um碳化硅粒度砂组成，各组分重量份配比为200um碳化硅粒度砂：100um碳化硅粒度砂：50um碳化硅粒度砂＝6:1:3。所述碳化硅微粉由5um碳化硅微粉、10um碳化硅微粉和20um碳化硅微粉组成，各组分重量份配比为5um碳化硅微粉：10um碳化硅微粉：20um碳化硅微粉＝1:1:1。所述粘接剂为70％的低分子量水溶性纤维素和30％低分子量水溶性聚乙烯醇。
将上述混合料装袋封口；
将装袋封口的混合料等静压成型，压力为175MPa，得到素坯；
将等静压成型的素坯保压，保压时间为120s，得到生坯；
将生坯分别进行卸压、开盖取出、毛坯加工和烧结，烧结温度为2000℃。得到重结晶碳化硅制品。
实施例2：
重结晶碳化硅制品等静压成型工艺，将如下重量份的原料混合：碳化硅粒度砂85份，碳化硅微粉15份，粘接剂2份，以获得混合料。静压成型的压力为240MPa，保压时间为170s，烧结温度为2400℃。
其余步骤与实施例1一致。
实施例3：
重结晶碳化硅制品等静压成型工艺，将如下重量份的原料混合：碳化硅粒度砂80份，碳化硅微粉20份，粘接剂2份，以获得混合料。静压成型的压力为210MPa，保压时间为160s，烧结温度为2200℃。
其余步骤与实施例1一致。
上述步骤制得的碳化硅制品素坯中配入的粒度砂和微粉分布均匀、结合紧密、坯体密实。50～200μm左右的粒度砂颗粒和5～20μm的微粉颗粒相互比较紧密地接触、啮合，其中5～20μm的微粉颗粒紧密的附着于大颗粒周围，并填充在大颗粒之间的空隙中，在静压成型的210MPa压力和160s的保压时间作用下大颗粒发生破碎、变形，合适的压力和保压时间，可提高生坯致密度。这主要是由于等静压成型压力大，压力来自三维方向，压力大且加压均匀，使粒度砂原料颗粒紧密堆积，原料堆积密度大；使带粘结剂、具有塑性的微粉颗粒，在大的三维压力下填入粒度砂的空隙中，因此获得了近于致密的素坯，素坯在静压成型的210MPa压力和160s的保压时间作用下完全致密，素坯的空隙不多。由于等静压成型的素坯已经致密化，致密化的素坯，颗粒紧密接触，在2200℃的烧成温度下容易烧结，烧结制品的密度高，重结晶碳化硅制品的性能和附加值高，素坯中配入的粒度砂和微粉完全烧结，大小颗粒完全融为一体，人们可以使用电镜看到一些重结晶后的颗粒边界，但颗粒之间是紧密相结的，颗粒之间只有微小的气孔。
上述步骤使碳化硅微粉和碳化硅粒度砂混合后通过等静压成型，再进行烧结，可以提高重结晶碳化硅制品的密度，提高重结晶碳化硅制品的性能和附加值。
对于本领域技术人员而言，显然本发明不限于上述示范性实施例的细节，而且在不背离本发明的精神或基本特征的情况下，能够以其它的具体形式实现本发明，因此，无论从哪一点来看，均应将实施例看作是示范性的，而且是非限制性的，本发明的范围由所附权利要求而不是上述说明限定，因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。
此外，应当理解，虽然本说明书按照实施方式加以描述，但并非每个实施方式公包含一个独立的技术方案，说明书的这种叙述方式仅仅是为清楚起见，本领域技术人员应当将说明书作为一个整体，各实施例中的技术方案也可以经适当组合，形成本领域技术人员可以理解的其它实施方式。

Claims (5)

1.重结晶碳化硅制品等静压成型工艺，其特征在于，包括以下步骤：
将如下重量份的原料混合：碳化硅粒度砂70-85份，碳化硅微粉15-30份，粘接剂0.7-2份，以获得混合料；
将上述混合料装袋封口；
将装袋封口的混合料等静压成型，压力为175-240MPa，得到素坯；
将等静压成型的素坯保压，保压时间为120-170s，得到生坯；
将生坯分别进行卸压、开盖取出、毛坯加工和烧结，得到重结晶碳化硅制品。
2.根据权利要求1所述的重结晶碳化硅制品等静压成型工艺，其特征在于，
所述碳化硅粒度砂由200um碳化硅粒度砂、100um碳化硅粒度砂和50um碳化硅粒度砂组成，各组分重量份配比为200um碳化硅粒度砂：100um碳化硅粒度砂：50um碳化硅粒度砂＝6:1:3。
3.根据权利要求1或2所述的重结晶碳化硅制品等静压成型工艺，其特征在于，
所述碳化硅微粉由5um碳化硅微粉、10um碳化硅微粉和20um碳化硅微粉组成，各组分重量份配比为5um碳化硅微粉：10um碳化硅微粉：20um碳化硅微粉＝1:1:1。
4.根据权利要求1所述的重结晶碳化硅制品等静压成型工艺，其特征在于，
所述粘接剂为70％的低分子量水溶性纤维素和30％低分子量水溶性聚乙烯醇。
5.根据权利要求1所述的重结晶碳化硅制品等静压成型工艺，其特征在于，烧结温度为2000-2400℃。
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