CN115385706A - 一种提高微纳纤维增强碳化硅材料抗冲击韧性的方法 - Google Patents

一种提高微纳纤维增强碳化硅材料抗冲击韧性的方法 Download PDF

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CN115385706A
CN115385706A CN202211012048.5A CN202211012048A CN115385706A CN 115385706 A CN115385706 A CN 115385706A CN 202211012048 A CN202211012048 A CN 202211012048A CN 115385706 A CN115385706 A CN 115385706A
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silicon carbide
parts
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fiber reinforced
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梁志
罗统斌
陈强
甘乐
陈诚
陈显彬
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Guangxi Sanyuan Huaxin Special Ceramics Co ltd
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Abstract

本发明提供一种提高微纳纤维增强碳化硅材料抗冲击韧性的方法，涉及家居厨房技术领域。该提高微纳纤维增强碳化硅材料抗冲击韧性的方法，包括以下制备步骤：S1、准备包括以下重量份数的原料：碳化硅15‑25份、碳化硅晶须1‑10份、高铝矾2‑12份、蜡石粉3‑9份、氮化硅5‑15份、氮化硅铁1‑6份、碳素材料2‑7份；S2、将一定份数的四氧化三铁和钴粉通过球磨机构进行球磨得到一定直径的微粒，然后将微粒溶于异丙醇和去离子水的混合溶液内，在干燥机构内进行干燥得到固体粉末。通过碳化硅、碳化硅晶须、氮化硅提升微纳纤维增强碳化硅材料的抗高温性能、抗冲击韧性和抗拉伸韧性以及抗腐蚀性能，保证了微纳纤维增强碳化硅材料使用过程中的整体性能。

Description

一种提高微纳纤维增强碳化硅材料抗冲击韧性的方法
技术领域
本发明涉及材料制备技术领域，具体为一种提高微纳纤维增强碳化硅材料抗冲击韧性的方法。
背景技术
微纳纤维增强碳化硅材料因具有高强度、低密度、高温性能好、抗腐蚀及非脆性断裂等优良性能受到越来越多的材料工作者的重视，在国防军工和航空航天领域，碳化硅材料在新型航天飞行器等方面表现出广阔的应用前景，在交通运输和新能源等民用领域，核聚变等离子发电装置及高速列车、高速电梯的刹车片等也对碳化硅材料提出强烈的需求。
目前，现有的微纳纤维增强碳化硅材料在实际的应用过程中由于抗冲击韧性较低，从而导致整个材料的应用范围较为狭隘，并且应用过程中容易被冲击力损坏，并且现有的微纳纤维增强碳化硅材料由于抗高温和抗腐蚀性能较差，从而导致材料的使用寿命缩短，因此需要研发一种提高微纳纤维增强碳化硅材料抗冲击韧性的方法。
发明内容
针对现有技术的不足，本发明提供了一种提高微纳纤维增强碳化硅材料抗冲击韧性的方法，解决了现有的微纳纤维增强碳化硅材料抗冲击韧性低、抗高温和抗腐蚀性能差的问题。
为实现以上目的，本发明通过以下技术方案予以实现：一种提高微纳纤维增强碳化硅材料抗冲击韧性的方法，包括以下制备步骤：
S1、准备包括以下重量份数的原料：碳化硅15-25份、碳化硅晶须1-10份、高铝矾2-12份、蜡石粉3-9份、氮化硅5-15份、氮化硅铁1-6份、碳素材料2-7份、结合剂1-5份、四氧化三铁2-10份、钴粉1-2份、聚碳硅烷10-20份；
S2、将一定份数的四氧化三铁和钴粉通过球磨机构进行球磨得到一定直径的微粒，然后将微粒溶于异丙醇和去离子水的混合溶液内，在干燥机构内进行干燥得到固体粉末；
S3、将一定份数的聚碳硅烷溶于三元混合溶剂中，在特定的温度和容器中进行混合搅拌，得到聚硅烷溶液；
S4、将一定份数的碳化硅、碳化硅晶须、高铝矾、蜡石粉、氮化硅、氮化硅铁、碳素材料投入到聚硅烷溶液中，将溶液置于特定的混合容器内进行加热并搅拌混合得到混合溶液A；
S5、将一定份数的固体粉末和结合剂加入到混合溶液A中，并在一定温度环境下对混合溶液进行搅拌混合，得到混合溶液B；
S6、将混合溶液B在特定温度下萃取一定时间和次数，然后进行冷却干燥，得到第一前驱体；
S7、将第一前驱体在惰性气体的保护下进行辐射交联后，在特定温度和时间内进行退火工艺得到第二前驱体；
S8、在保护气体氛围下，将第二前驱体放入管式炉中，然后在第一升温速率下升温至400℃～800℃，并保温1h～2h，然后在第二升温速率下升温至1200℃～1800℃，并保温1.5h～3.5h，然后在第一降温速率下降至室温，即可得到微纳纤维增强碳化硅材料。
优选的，所述结合剂为聚乙烯醇、硅酸钠、三聚磷酸钠和羧甲基纤维素，所述碳素材料包括焦炭和炭黑。
优选的，所述四氧化三铁和钴粉球磨得到的微粒直径为10nm～25nm。
优选的，所述S3中的三元混合溶剂为碳酸二甲酯－甲醇－氨按一定比例混合后的液体，所述S3的温度为30-70℃，搅拌速度为40-150r/min，持续时长为20-60min。
优选的，所述S4的温度为40-80℃，搅拌速度为50-200r/min，持续时长为30-70min。
优选的，所述S5的温度为40-80℃，搅拌速度为60-250r/min，持续时长为40-80min。
优选的，所述S6中的萃取温度为零下45－零下15℃，萃取时间为65-110min，萃取次数为5-7次。
优选的，所述S7中的惰性气体为氦气，所述退火温度控制在50-110℃，退火时间控制在40-80min。
本发明提供了一种提高微纳纤维增强碳化硅材料抗冲击韧性的方法。具备以下有益效果：
1、本发明在制取微纳纤维增强碳化硅材料时通过加入一定份数的碳化硅、碳化硅晶须、氮化硅、氮化硅铁、碳素材料在原料中，其中碳化硅晶须具有相当好的抗高温性能、很高的抗拉伸强度以及抗腐蚀性能，从而有利于提升微纳纤维增强碳化硅材料的抗高温性能、抗冲击韧性和抗拉伸韧性以及抗腐蚀性能，保证了微纳纤维增强碳化硅材料使用过程中的整体性能，并且氮化硅、氮化硅铁、碳化硅晶须以及碳素材料在特定的温度条件下可以反应生成碳化硅，后面制备出的微纳纤维增强碳化硅材料具有强烈的抗侵蚀性能和抗冲击性能。
2、本发明在制取微纳纤维增强碳化硅材料时加入的高铝矾、蜡石粉、氮化硅等粒径较小的物质可以对制取的微纳纤维增强碳化硅材料中较小的缝隙进行填充，提高了微纳纤维增强碳化硅材料的密度，配合加入的四氧化三铁和钴粉，利用四氧化三铁的磁性可以吸附钴粉，钴粉与材料中的硅反应得到硅化钴，硅化钴是一种具有较强稳定性的结构，从而使得微纳纤维增强碳化硅材料的整体稳定性和强度得到进一步提升。
具体实施方式
下面将结合本发明实施例，对本发明实施例中的技术方案进行清楚、完整地描述，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。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。
实施例一：
本发明实施例提供一种提高微纳纤维增强碳化硅材料抗冲击韧性的方法，包括以下制备步骤：
S1、准备包括以下重量份数的原料：碳化硅15份、碳化硅晶须1份、高铝矾2份、蜡石粉3份、氮化硅5份、氮化硅铁1份、碳素材料2份、结合剂1份、四氧化三铁2份、钴粉1份、聚碳硅烷10份；
S2、将一定份数的四氧化三铁和钴粉通过球磨机构进行球磨得到一定直径的微粒，然后将微粒溶于异丙醇和去离子水的混合溶液内，在干燥机构内进行干燥得到固体粉末；
S3、将一定份数的聚碳硅烷溶于三元混合溶剂中，在特定的温度和容器中进行混合搅拌，得到聚硅烷溶液；
S4、将一定份数的碳化硅、碳化硅晶须、高铝矾、蜡石粉、氮化硅、氮化硅铁、碳素材料投入到聚硅烷溶液中，将溶液置于特定的混合容器内进行加热并搅拌混合得到混合溶液A；
S5、将一定份数的固体粉末和结合剂加入到混合溶液A中，并在一定温度环境下对混合溶液进行搅拌混合，得到混合溶液B；
S6、将混合溶液B在特定温度下萃取一定时间和次数，然后进行冷却干燥，得到第一前驱体；
S7、将第一前驱体在惰性气体的保护下进行辐射交联后，在特定温度和时间内进行退火工艺得到第二前驱体；
S8、在保护气体氛围下，将第二前驱体放入管式炉中，然后在第一升温速率下升温至400℃，并保温1h，然后在第二升温速率下升温至1200℃，并保温1.5h，然后在第一降温速率下降至室温，即可得到微纳纤维增强碳化硅材料。
优选的，结合剂为聚乙烯醇、硅酸钠、三聚磷酸钠和羧甲基纤维素，碳素材料包括焦炭和炭黑。
优选的，四氧化三铁和钴粉球磨得到的微粒直径为10nm。
优选的，S3中的三元混合溶剂为碳酸二甲酯－甲醇－氨按一定比例混合后的液体，S3的温度为30℃，搅拌速度为40r/min，持续时长为20min。
优选的，S4的温度为40℃，搅拌速度为50r/min，持续时长为30min。
优选的，S5的温度为40℃，搅拌速度为60r/min，持续时长为40min。
优选的，S6中的萃取温度为零下45℃，萃取时间为65min，萃取次数为5次。
优选的，S7中的惰性气体为氦气，退火温度控制在50℃，退火时间控制在40min。
实施例二：
本发明实施例提供一种提高微纳纤维增强碳化硅材料抗冲击韧性的方法，包括以下制备步骤：
S1、准备包括以下重量份数的原料：碳化硅25份、碳化硅晶须10份、高铝矾12份、蜡石粉9份、氮化硅15份、氮化硅铁6份、碳素材料7份、结合剂5份、四氧化三铁10份、钴粉2份、聚碳硅烷20份；
S2、将一定份数的四氧化三铁和钴粉通过球磨机构进行球磨得到一定直径的微粒，然后将微粒溶于异丙醇和去离子水的混合溶液内，在干燥机构内进行干燥得到固体粉末；
S3、将一定份数的聚碳硅烷溶于三元混合溶剂中，在特定的温度和容器中进行混合搅拌，得到聚硅烷溶液；
S4、将一定份数的碳化硅、碳化硅晶须、高铝矾、蜡石粉、氮化硅、氮化硅铁、碳素材料投入到聚硅烷溶液中，将溶液置于特定的混合容器内进行加热并搅拌混合得到混合溶液A；
S5、将一定份数的固体粉末和结合剂加入到混合溶液A中，并在一定温度环境下对混合溶液进行搅拌混合，得到混合溶液B；
S6、将混合溶液B在特定温度下萃取一定时间和次数，然后进行冷却干燥，得到第一前驱体；
S7、将第一前驱体在惰性气体的保护下进行辐射交联后，在特定温度和时间内进行退火工艺得到第二前驱体；
S8、在保护气体氛围下，将第二前驱体放入管式炉中，然后在第一升温速率下升温至800℃，并保温2h，然后在第二升温速率下升温至1800℃，并保温3.5h，然后在第一降温速率下降至室温，即可得到微纳纤维增强碳化硅材料。
优选的，结合剂为聚乙烯醇、硅酸钠、三聚磷酸钠和羧甲基纤维素，碳素材料包括焦炭和炭黑。
优选的，四氧化三铁和钴粉球磨得到的微粒直径为25nm。
优选的，S3中的三元混合溶剂为碳酸二甲酯－甲醇－氨按一定比例混合后的液体，S3的温度为70℃，搅拌速度为150r/min，持续时长为60min。
优选的，S4的温度为80℃，搅拌速度为200r/min，持续时长为70min。
优选的，S5的温度为80℃，搅拌速度为250r/min，持续时长为80min。
优选的，S6中的萃取温度为零下15℃，萃取时间为110min，萃取次数为7次。
优选的，S7中的惰性气体为氦气，退火温度控制在110℃，退火时间控制在80min。
尽管已经示出和描述了本发明的实施例，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其等同物限定。

Claims (8)

1.一种提高微纳纤维增强碳化硅材料抗冲击韧性的方法，其特征在于：包括以下制备步骤：
S1、准备包括以下重量份数的原料：碳化硅15-25份、碳化硅晶须1-10份、高铝矾2-12份、蜡石粉3-9份、氮化硅5-15份、氮化硅铁1-6份、碳素材料2-7份、结合剂1-5份、四氧化三铁2-10份、钴粉1-2份、聚碳硅烷10-20份；
S2、将一定份数的四氧化三铁和钴粉通过球磨机构进行球磨得到一定直径的微粒，然后将微粒溶于异丙醇和去离子水的混合溶液内，在干燥机构内进行干燥得到固体粉末；
S3、将一定份数的聚碳硅烷溶于三元混合溶剂中，在特定的温度和容器中进行混合搅拌，得到聚硅烷溶液；
S4、将一定份数的碳化硅、碳化硅晶须、高铝矾、蜡石粉、氮化硅、氮化硅铁、碳素材料投入到聚硅烷溶液中，将溶液置于特定的混合容器内进行加热并搅拌混合得到混合溶液A；
S5、将一定份数的固体粉末和结合剂加入到混合溶液A中，并在一定温度环境下对混合溶液进行搅拌混合，得到混合溶液B；
S6、将混合溶液B在特定温度下萃取一定时间和次数，然后进行冷却干燥，得到第一前驱体；
S7、将第一前驱体在惰性气体的保护下进行辐射交联后，在特定温度和时间内进行退火工艺得到第二前驱体；
S8、在保护气体氛围下，将第二前驱体放入管式炉中，然后在第一升温速率下升温至400℃～800℃，并保温1h～2h，然后在第二升温速率下升温至1200℃～1800℃，并保温1.5h～3.5h，然后在第一降温速率下降至室温，即可得到微纳纤维增强碳化硅材料。
2.根据权利要求1所述的一种提高微纳纤维增强碳化硅材料抗冲击韧性的方法，其特征在于：所述结合剂为聚乙烯醇、硅酸钠、三聚磷酸钠和羧甲基纤维素，所述碳素材料包括焦炭和炭黑。
3.根据权利要求1所述的一种提高微纳纤维增强碳化硅材料抗冲击韧性的方法，其特征在于：所述四氧化三铁和钴粉球磨得到的微粒直径为10nm～25nm。
4.根据权利要求1所述的一种提高微纳纤维增强碳化硅材料抗冲击韧性的方法，其特征在于：所述S3中的三元混合溶剂为碳酸二甲酯－甲醇－氨按一定比例混合后的液体，所述S3的温度为30-70℃，搅拌速度为40-150r/min，持续时长为20-60min。
5.根据权利要求1所述的一种提高微纳纤维增强碳化硅材料抗冲击韧性的方法，其特征在于：所述S4的温度为40-80℃，搅拌速度为50-200r/min，持续时长为30-70min。
6.根据权利要求1所述的一种提高微纳纤维增强碳化硅材料抗冲击韧性的方法，其特征在于：所述S5的温度为40-80℃，搅拌速度为60-250r/min，持续时长为40-80min。
7.根据权利要求1所述的一种提高微纳纤维增强碳化硅材料抗冲击韧性的方法，其特征在于：所述S6中的萃取温度为零下45－零下15℃，萃取时间为65-110min，萃取次数为5-7次。
8.根据权利要求1所述的一种提高微纳纤维增强碳化硅材料抗冲击韧性的方法，其特征在于：所述S7中的惰性气体为氦气，所述退火温度控制在50-110℃，退火时间控制在40-80min。
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Application publication date: 20221125

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