CN111548164B - 一种持续自增韧氮化物结合碳化硅耐火材料 - Google Patents

一种持续自增韧氮化物结合碳化硅耐火材料 Download PDF

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CN111548164B
CN111548164B CN202010423824.5A CN202010423824A CN111548164B CN 111548164 B CN111548164 B CN 111548164B CN 202010423824 A CN202010423824 A CN 202010423824A CN 111548164 B CN111548164 B CN 111548164B
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曹会彦
吕春江
黄志刚
李�杰
吴吉光
张新华
黄一飞
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Sinosteel Luoyang Institute of Refractories Research Co Ltd
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Abstract

本发明涉及干熄炉用耐火材料，具体涉及一种持续自增韧氮化物结合碳化硅耐火材料。提出的一种持续自增韧氮化物结合碳化硅耐火材料在氮化物结合碳化硅耐火材料中引入含锆物质；以碳化硅为主晶相，氮化物为结合相，含锆物质弥散分布在氮化物结合相内；所述持续自增韧氮化物结合碳化硅耐火材料中氮化物的含量为10~25%，含锆物质的含量为1~8%，碳化硅的含量为70~82%。本发明充分发挥氮化物结合碳化硅耐火材料常、高温抗折强度高的特性，提高其抗氧化性和抗热震性，改善炉体的整体性，提高炉体的使寿命。

Description

一种持续自增韧氮化物结合碳化硅耐火材料
技术领域
本发明涉及干熄炉用耐火材料，具体涉及一种持续自增韧氮化物结合碳化硅耐火材料，所述持续自增韧氮化物结合碳化硅耐火材料是用于干熄炉斜道区牛腿支柱、横梁等部位的关键耐火材料。
背景技术
干熄焦技术具有用水节约、大气污染物排放少、能源效率高、焦炭质量提高等优势，是国家重点推广的节能环保技术，近年来在我国得到快速发展。随着设计院在结构设计方面水平提升（包括双斜道技术的采用，传热行为模拟研究等），配套设备国产化及相关工业基础的完善，干熄炉终端用户操作经验增多，斜道区碳化硅耐火材料的广泛应用等，长期以来制约干熄炉一代炉役寿命的瓶颈问题逐渐得到解决，特别是以复相氮化物结合碳化硅为代表的工程应用已经达到8年的使用寿命。目前国内干熄炉整体装备的普遍寿命在10年左右，干熄炉斜道区耐火材料的使用寿命仍有进一步提升的空间和市场需求。碳化硅耐火材料和传统红柱石-莫来石相比，最明显的优势就是初始抗折强度高。对斜道区耐火材料的损毁有很多的研究和报道，大部分集中在对斜道区结构设计、受力点、砌筑质量和运行操作的研究上。普遍认为，该部位结构复杂，炉内工况变化大，是影响斜道支柱耐火材料的主要因素：（a）在整体结构设计上，斜道支撑梁必须承受预存段上部直筒部分全部耐火材料的重量，高温荷重必然导致结构强度的逐渐降低；（b）在焦炭自上而下、循环气体自下而上的运动过程中，斜道支柱的耐火材料承受焦炭的冲击、磨损以及气流和粉尘的剧烈冲刷；（c）斜道支撑梁下部的温度约为300℃，上部温度约为1000℃，支撑梁的耐火材料由下到上存在近700℃的温度梯度，致使耐火材料内部应力聚集，产生裂纹、变形；(d)耐火材料热震损伤。材料由于温度剧变，急冷急热的条件下产生热应力，在热冲击循环作用下，材料先出现开裂、剥落，然后碎裂或变质，最终整体损伤。
张善学等认为，斜道牛腿受到上下方向压力作用产生剪切力，温度波动造成耐火砖内部温度应力，同时斜道牛腿拱水平环向产生拉应力共同作用。上下方向压力作用产生剪切力，是剪应力的主要来源，同时，温度应力加重了耐火砖的破损，水平拉应力也起到了牛腿砌筑结构的破坏作用。
专利201410741616.4公布了一种干熄焦炉用高强度碳化硅耐火材料及其制备方法；专利201010209273.9公布了一种用于干熄焦炉的高导热Sialon-SiC复相陶瓷耐火材料及其制备方法；专利201410040255.0公布了一种干熄焦炉用碳化硅砖及其制备方法；专利200910032994.4公布了一种干熄焦用耐火材料。所有这些专利都仅仅局限于原始材料的高强度，而未针对材料服役过程中强度的衰减做任何改进说明。干熄焦斜道区材料损毁的重要原因之一就是在温度300℃~1000℃频繁波动情况下，材料的抗折强度下降，不足以支撑上部预存段耐材而开裂。
论文“锆英石制备非氧化物复合材料新进展”综述了国内外利用锆英石制备氧化锆-碳化硅复合材料、碳化锆-碳化硅复合材料、氮化锆-氮化硅基复合材料、氮化锆-赛隆复合材料和硼化锆-碳化硅基复合材料的研究现状;文中提及的这些材料有的涉及碳热还原制备碳化硅、有的涉及炭黑、稀有金属添加剂、氧化钙等，有的为粉体制备而非制品，主要成分中不涉及本发明专利提及的氮化物，和本发明专利属于不同的应用领域，并且大部分科研成果还停留在实验室阶段，工业化、系统化的生产还有很长的路要走。
发明内容
本发明的目的是提供一种持续自增韧氮化物结合碳化硅耐火材料，使其能提高现有干熄炉斜道区牛腿支柱、横梁等氮化物结合碳化硅耐火材料的抗热震性，最终提高其使用寿命。
本发明为完成上述目的采用如下技术方案：
一种持续自增韧氮化物结合碳化硅耐火材料，持续自增韧氮化物结合碳化硅耐火材料在氮化物结合碳化硅耐火材料中引入含锆物质；以碳化硅为主晶相，氮化物为结合相，含锆物质弥散分布在氮化物结合相内；所述持续自增韧氮化物结合碳化硅耐火材料中氮化物的含量为10~25%，含锆物质的含量为1~8%，碳化硅的含量为70~82%。
作为结合相的氮化物为氮化硅、氧氮化硅、赛隆中的一种或几种。
所述的含锆物质为ZrB2、ZrO2、ZrSiO4、ZrC中的一种或几种。
本发明提出的一种持续自增韧氮化物结合碳化硅耐火材料，首先利用含锆物质在氧化气氛中的优先氧化特性提高氮化物结合碳化硅耐火材料的抗氧化性，其次利用干熄炉斜道区现场工况条件频繁的300℃~1000℃的温度波动，诱发氧化产物二氧化锆发生单斜二氧化锆和四方二氧化锆之间的相变，在材料内部产生微裂纹增韧，同时在现场微量杂质及氧化产物二氧化硅共同作用的液相环境中，微裂纹可以实现自愈合。该方案可以充分发挥氮化物结合碳化硅耐火材料常、高温抗折强度高的特性，提高其抗氧化性和抗热震性，改善干熄炉斜道区牛腿支柱、横梁等部位的整体性，提高炉体的使寿命。
本发明的有益效果是通过将含锆物质引入到氮化物结合碳化硅耐火材料中，充分发挥了氮化物结合碳化硅常、高温抗折强度高的优点，同时又巧妙利用了弥散分布在氮化物结合相内的含锆物质的两种特性。一是在干熄炉内以氮气为主、一氧化碳、二氧化碳等为辅的气氛中，含锆物质会优先于结合相氮化物发生氧化，生成二氧化锆，减少结合相的破坏，提高结合相的抗氧化性；氧化产物二氧化锆借助干熄炉斜道区频繁的300℃~1000℃温度波动（在补充空气的情况下，该部位由于碳粉燃烧，最高温度可以达到1350℃）发生单斜氧化锆和四方氧化锆之间的相变反应，利用在氮化物结合相内弥散、均匀分布的相变增韧产生微裂纹，释放材料内部积聚的热应力和结构应力，提高材料的抗热震性，使材料的损毁机理由热震断裂向热震损伤转移，有助于氮化物结合碳化硅耐火材料长久服役性能的稳定。
下表列出了新研制的持续自增韧氮化物结合碳化硅耐火材料和传统的氮化物结合碳化硅耐火材料的的常规性能及抗热震性能比较结果。
Figure DEST_PATH_IMAGE001
本发明的创新点就是关注了材料的服役动态变化，通过引入的含锆物质的增韧效果维持材料的高抗折强度，进而达到提高材料的服役寿命的目的。
具体实施方式
实施例1：
持续自增韧氮化物结和碳化硅的设计配方为：碳化硅比例82%，氮化硅比例17%，ZrB2 比例1%；制品的显气孔率为11.9%，体积密度为2.75g/cm3，常温强度60Mpa，1200℃高温强度58Mpa，1200℃保温30min，风冷5次残余抗折强度为54.0Mpa，强度保持率为90%。
实施例2：
持续自增韧氮化物结和碳化硅的设计配方为：碳化硅比例74%，氧氮化硅比例20%，ZrSiO4比例6%。制品的显气孔率为14.0%，体积密度为2.70g/cm3，常温强度55.0Mpa，1200℃高温强度54.2Mpa，1200℃保温30min，风冷5次残余抗折强度为57.8Mpa，强度保持率为105%。
实施例3：
持续自增韧氮化物结和碳化硅的设计配方为：碳化硅比例82%，赛隆比例10%，ZrC+ZrSiO4比例8%。制品的显气孔率为15.2%，体积密度为2.64g/cm3，常温强度50.0Mpa，1200℃高温强度48.0Mpa，1200℃保温30min，风冷5次残余抗折强度为52.8Mpa，强度保持率为110%。
实施例4：
持续自增韧氮化物结和碳化硅的设计配方为：碳化硅比例70%，氮化硅比例15%，氧氮化硅比例为10%，ZrO2比例为5%。制品的显气孔率为14.6%，体积密度为2.69g/cm3，常温强度58.0Mpa，1200℃高温强度60.0Mpa，1200℃保温30min，风冷5次残余抗折强度为58.0Mpa，强度保持率为100%。

Claims (3)

1.一种持续自增韧氮化物结合碳化硅耐火材料，其特征在于：持续自增韧氮化物结合碳化硅耐火材料在氮化物结合碳化硅耐火材料中引入含锆物质；以碳化硅为主晶相，氮化物为结合相，含锆物质弥散分布在氮化物结合相内；所述持续自增韧氮化物结合碳化硅耐火材料中氮化物的含量为10~25%，含锆物质的含量为1~8%，碳化硅的含量为70~82%；利用干熄炉斜道区现场工况条件频繁的300℃~1000℃的温度波动，诱发氧化产物二氧化锆发生单斜二氧化锆和四方二氧化锆之间的相变，在材料内部产生微裂纹增韧，同时在现场微量杂质及氧化产物二氧化硅共同作用的液相环境中，微裂纹可以实现自愈合。
2.如权利要求1所述的一种持续自增韧氮化物结合碳化硅耐火材料，其特征在于：作为结合相的氮化物为氮化硅、氧氮化硅、赛隆中的一种或几种。
3.如权利要求1所述的一种持续自增韧氮化物结合碳化硅耐火材料，其特征在于：所述的含锆物质为ZrB2、ZrO2、ZrSiO4、ZrC中的一种或几种。
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