CN113307625A - 一种ZrO2-C纤维复合材料及其制备方法 - Google Patents
一种ZrO2-C纤维复合材料及其制备方法 Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 239000000835 fiber Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 83
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 25
- 239000010439 graphite Substances 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 20
- 229910052580 B4C Inorganic materials 0.000 claims abstract description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 12
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 12
- 239000011230 binding agent Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims description 29
- 239000002245 particle Substances 0.000 claims description 20
- 210000001170 unmyelinated nerve fiber Anatomy 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 13
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- 238000001816 cooling Methods 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 238000010907 mechanical stirring Methods 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical group [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 3
- 239000005011 phenolic resin Substances 0.000 claims description 3
- 229920001568 phenolic resin Polymers 0.000 claims description 3
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 2
- 229910002077 partially stabilized zirconia Inorganic materials 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 238000005245 sintering Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims 1
- 229910052726 zirconium Inorganic materials 0.000 claims 1
- 230000035939 shock Effects 0.000 abstract description 22
- 239000000463 material Substances 0.000 abstract description 18
- PUAQLLVFLMYYJJ-UHFFFAOYSA-N 2-aminopropiophenone Chemical compound CC(N)C(=O)C1=CC=CC=C1 PUAQLLVFLMYYJJ-UHFFFAOYSA-N 0.000 abstract description 7
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- 230000006872 improvement Effects 0.000 abstract description 2
- 238000009749 continuous casting Methods 0.000 description 13
- 238000010438 heat treatment Methods 0.000 description 13
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 11
- 239000002893 slag Substances 0.000 description 9
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Abstract
本发明公开了一种ZrO2‑C纤维复合材料及其制备方法，包括以下质量百分比的组分：石墨为12‑18％，金属硅粉为3‑5％，氧化锆纤维为0.3‑1.2％，结合剂加入量为5‑8％，碳化硼0.1‑1％，氧化锆细粉为22‑28％，余量为氧化锆粗颗粒。本发明在ZrO2‑C材料中加入ZrO2纤维，在不增加碳的情况下显著的提高了ZrO2‑C材料的抗热震性能，极大的提升了浸入式水口的常温力学性能以及高温性能，进而延长了浸入式水口的使用寿命。
Description
技术领域
本发明涉及含碳耐火材料领域，尤其是涉及一种ZrO2-C纤维复合材料及其制备方法。
背景技术
连铸机是钢铁连铸生产过程的核心装备，是钢铁能够实现连铸生产的关键。连铸结晶器被认为是整个连铸机的“心脏”，而如何维持连铸结晶器的高效运行是实现连铸高效高质生产的关键。为了维持连铸结晶器的正常运转，需要在结晶器内使用浸入式水口和连铸保护渣作为关键的辅助材料，而浸入式水口的渣线部位又是水口中的重中之重，浸入式水口渣线部位材料性能的好坏决定着浸入式水口使用寿命。
浸入式水口其主要作用是防止钢夜二次氧化，控制钢夜流动速度和流动状态，防止结晶器内的保护渣进入到钢夜当中，浸入式水口需要具备良好的抗侵蚀性和抗热震性，若浸入式水口抗侵蚀性能不好，会导致水口断裂和穿孔，失去对钢水的控流作用，导致连铸坯表面产生质量问题，若浸入式水口的抗热震性能不好，会使水口发生炸裂，严重时还会导致连铸漏钢警告。如何提高浸入式水口渣线部位ZrO2-C材料的抗热震性能和抗侵蚀性一直是有待解决的问题。
延长浸入式水口渣线部位的使用寿命，不仅可以提高连铸生产的效率，还可以节约资源，降低连铸生产的成本，在实际浸入式水口的生产和应用中，通常来调节浸入式水口渣线部位的氧化锆和石墨的含量来调节浸入式水口的抗侵蚀性能和抗热震性。一般来讲，增加渣线部位氧化锆的含量，减少石墨的含量可以提高浸入式水口的抗侵蚀性能，但是降低了水口的抗热震性能，而增加渣线部位的石墨含量降低氧化锆的含量，可以增加水口的抗热震性能，但是损失了水口的抗侵蚀性能。
发明内容
有鉴于此，本发明的目的是针对现有技术的不足，提供一种热震性能更好、力学性能更优的浸入式水口渣线的ZrO2-C纤维复合材料及其制备方法。
为达到上述目的，本发明采用以下技术方案：
一种ZrO2-C纤维复合材料，其特征在于：包括以下质量百分比的组分：石墨为12-18％，金属硅粉为3-5％，氧化锆纤维为0.3-1.2％，结合剂加入量为5-8％，碳化硼0.1-1％，氧化锆细粉为22-28％，余量为氧化锆粗颗粒。
优选的，所述氧化锆为部分稳定氧化锆，氧化锆粗颗粒的粒径小于425um，氧化锆细粉的粒径小于150um。
优选的，所述石墨为鳞片石墨，粒径小于75um。
优选的，所述金属硅粉粒径小于75um，所述碳化硼粒径小于75um。
优选的，所述氧化锆纤维的长度为3-0.1mm，直径小于3-5um。
优选的，所述所采用的结合剂为酚醛树脂。
一种ZrO2-C纤维复合材料的制备方法，其特征在于：包括如下步骤：
(1)先将粉料放入超速混炼机中进行混合，其中粉料包括氧化锆细粉、石墨、金属硅粉、碳化硼，然后在将氧化锆纤维放入混合料中，进行机械搅拌分散；
(2)将氧化锆粗颗粒与一半结合剂混合均匀后，在与步骤(1)中的一半预混料进行混合；
(3)将步骤(2)制得的混合料与步骤(1)中剩余的预混料用剩余的一半结合剂进行混练；
(4)将原料混合后，困料12-16h后压制成型，将成形后的制品放入干燥箱中进行干燥；
(5)将步骤(4)压制成型干燥后的制品，放入匣钵中，并在匣钵中埋入石墨，盖过试样，并放入由碳化硅加热的高温窑炉中在1000℃-1200℃下进行烧结，随炉冷却得到所述的ZrO2-C纤维复合材料。
优选的，所述步骤(1)的机械搅拌分散，搅拌速度为1200-2000r/min，分散时长为5-10min。
优选的，所述步骤(4)干燥的温度和时间为80℃保温6h，120℃保温12h，200℃保温3h。
本发明的有益效果是：
本发明采用干法混合、半干压制成型和高温热处理工艺制备ZrO2-C材料，添加ZrO2纤维的ZrO2-C材料的显气孔率与不添加ZrO2纤维的ZrO2-C材料的显气孔率相差甚微，其常温耐压强度提升至30-34Mpa，常温抗折强度提升至16-20Mpa，热震后抗折强度提升至12-14Mpa，残余强度保持率由60％提升至70-80％，本发明在ZrO2-C材料中加入ZrO2纤维，在不增加碳的情况下显著的提高了ZrO2-C材料的抗热震性能，极大的提升了浸入式水口的常温力学性能以及高温性能，进而延长了浸入式水口的使用寿命。
本发明在碳含量保持在12％-18％的前提下，不增加碳含量，通过加入ZrO2纤维，提高了浸入式水口的抗热震性能。
本发明采用ZrO2纤维复合ZrO2-C材料，用该种方法制备的ZrO2-C质复合材料抗热震性能更好，力学性能更佳。其制备工艺简单，纤维分散的效果较好，节约了实际的生产成本。
本发明的其他优点、目标和特征在某种程度上将在随后的说明书中进行阐述，并且在某种程度上，基于对下文的考察研究对本领域技术人员而言将是显而易见的，或者可以从本发明的实践中得到教导。本发明的目标和其他优点可以通过下面的说明书中所特别指出的结构来实现和获得。
具体实施方式
下面结合实施例对本发明作进一步描述，但不局限于下列实施例。
实施例1：
本实施例的一种ZrO2-C纤维复合材料包括如下组分：二氧化锆粗颗粒45％，二氧化锆细粉22％，鳞片石墨17.7％，金属硅粉4％，碳化硼0.3％，氧化锆纤维1％，长度为3mm。
其中，所采用的氧化锆为CaO部分稳定的氧化锆，粗颗粒氧化锆的粒径小于425um，粉状氧化锆的粒径小于150um。所采用的石墨为鳞片石墨，粒径小于75um。所采用的金属硅粉粒径小于75um。所采用的碳化硼粒径小于75um。所采用的ZrO2纤维长度为3-0.1mm，直径小于3-5um。所采用的结合剂为酚醛树脂。
本实施例的一种ZrO2-C纤维复合材料的制备方法，包括如下步骤：
(1)按照上述质量百分比进行称料，先将粉料包括氧化锆细粉、片状石墨、金属硅粉、碳化硼，放入高速混炼机中进行混合，转速为1000r/min，分撒时间为5-10min，制备混合料；
(2)将粗颗粒氧化锆与一半结合剂进行混合，混合之后再与步骤(1)中的一半混合料进行混料，再倒入剩下结合剂与剩下的一半混合料进行混炼；
(3)将步骤(2)制备好的原料进行困料12-16h；
(4)将步骤(3)中困好的原料，放入压机进行压制成型，成型压力为120Mpa；
(5)将步骤(4)中成型制品放入烘箱中进行干燥，烘干温度和时间如下：80℃保温6h；120℃保温12h；200℃保温3h；
(6)将步骤(5)中烘干的制品放入匣钵中，在匣钵内埋入适量的石墨，盖过样品，放入高温炉中进行烧制，温度制度如下：(a)从室温升至1000℃，升温速率为5℃/min；(b)从1000℃升至1200℃，升温速率为3℃/min，在1200℃时保温5min；(c)随炉降温至室温。
本实施例所制备的ZrO2-C纤维复合材料的气孔率为14％，体积密度为3.38g/cm3，耐压强度为31.5Mpa，抗折强度为16.6Mpa，经1100℃热震三次后抗折强度为12.3Mpa，热震强度保持率高达74.09％。
实施例2：
本实施例提供的一种ZrO2-C纤维复合材料，包括如下组分：二氧化锆粗颗粒45％，二氧化锆细粉22％，鳞片石墨17.4％，金属硅粉4％，碳化硼1％，ZrO2纤维0.6％，长度为0.3mm。
本实施例的ZrO2-C纤维复合材料的制备方法，包括如下步骤：
(1)按照质量百分比进行称料，先将粉料包括氧化锆细粉、片状石墨、金属硅粉、碳化硼，放入高速混炼机中进行混合，转速为1000r/min，分撒时间为5-10min，制备混合料；
(2)将粗颗粒氧化锆与一半结合剂进行混合，混合之后在与步骤(1)中的一半混合料进行混料，再倒入剩下结合剂与剩下的一半混合料进行混炼；
(3)将步骤(2)制备好的原料进行困料12-16h；
(4)将步骤(3)中困好的原料，放入压机进行压制成型，成型压力为120Mpa；
(5)将步骤(4)中成型制品放入烘箱中进行干燥，烘干温度和时间如下：80℃保温6h；120℃保温12h；200℃保温3h；
(6)将步骤(5)中烘干的制品放入匣钵中，在匣钵内埋入适量的石墨，盖过样品，放入高温炉中进行烧制，温度制度如下：(a)从室温升至1000℃，升温速率为5℃/min；(b)从1000℃升至1200℃，升温速率为3℃/min，在1200℃时保温5min；(c)随炉降温至室温。
本实施例所制备的ZrO2-C纤维复合材料的气孔率为13.8％，体积密度为3.40g/cm3，耐压强度为34Mpa，抗折强度为17.7Mpa，经1100℃热震三次后抗折强度为14.2Mpa，热震强度保持率高达80.22％。
实施例3：
本实施例的一种ZrO2-C纤维复合材料，包括如下组分：二氧化锆粗颗粒45％，二氧化锆细粉22％，鳞片石墨17.1％，金属硅粉0.9％，碳化硼1％，ZrO2纤维1％，长度为3mm。
本实施例提供一种提高浸入式水口的力学性能和抗热震性能的ZrO2-C纤维复合材料制备方法，包括如下步骤：
(1)按照质量百分比进行称料，先将粉料包括氧化锆细粉、片状石墨、金属硅粉、碳化硼，放入高速混炼机中进行混合，转速为1000r/min，分撒时间为5-10min，制备混合料；
(2)将粗颗粒氧化锆与一半结合剂进行混合，混合之后在与步骤(1)中的一半混合料进行混料，再倒入剩下结合剂与剩下的一半混合料进行混炼；
(3)将步骤(2)制备好的原料进行困料12-16h；
(4)将步骤(3)中困好的原料，放入压机进行压制成型，成型压力为120Mpa；
(5)将步骤(4)中成型制品放入烘箱中进行干燥，烘干温度和时间如下：80℃保温6h；120℃保温12h；200℃保温3h；
(6)将步骤(5)中烘干的制品放入匣钵中，在匣钵内埋入适量的石墨，盖过样品，放入高温炉中进行烧制，温度制度如下：(a)从室温升至1000℃，升温速率为5℃/min；(b)从1000℃升至1200℃，升温速率为3℃/min，在1200℃时保温5min；(c)随炉降温至室温。
本实施例所制备的ZrO2-C纤维复合材料的气孔率为13.9％，体积密度为3.38g/cm3，耐压强度为30.9Mpa，抗折强度为18.0Mpa，经1100℃热震三次后抗折强度为13.2Mpa，热震强度保持率高达73.33％。
对比例1：
对比例1与实施例1、2、3不同的是对比例1中没有加入ZrO2纤维，对比例1与实施例1、2、3的原料重量份数以及原料配比均相同，所用混合设备、压制设备、烘干设备、烧制设备均相同，在相同的条件下进行测试，ZrO2-C材料的气孔率为13.22％，体积密度为3.37g/cm3，耐压强度为30.4Mpa，抗折强度为15.5Mpa，经1100℃水冷三次后热震残余强度为9.8Mpa，残余强度保持率达到63.23％。
实施例1、2、3与对比例1相比显气孔率与体积密度相差甚微，抗折与耐压强度均有一定程度的提高，抗折强度提高了10％以上，热震后的抗折强度提高了40％左右，残余强度保持率由63％提高至73-80％。由此可见，加入ZrO2纤维后，ZrO2-C材料的抗热震性能有大幅度提高。
以上实施仅用于说明本发明的技术方案而非限制，本领域普通技术人员对本发明的技术方案所做的其他修改或者等同替换，只要不脱离本发明的技术方案的实质和精神的基础上，均应涵盖在本发明的权利要求的保护范围内。
Claims (9)
1.一种ZrO2-C纤维复合材料，其特征在于：包括以下质量百分比的组分：石墨为12-18％，金属硅粉为3-5％，氧化锆纤维为0.3-1.2％，结合剂加入量为5-8％，碳化硼0.1-1％，氧化锆细粉为22-28％，余量为氧化锆粗颗粒。
2.根据权利要求1所述的一种ZrO2-C纤维复合材料，其特征在于：所述氧化锆为部分稳定氧化锆，氧化锆粗颗粒的粒径小于425um，氧化锆细粉的粒径小于150um。
3.根据权利要求1所述的一种ZrO2-C纤维复合材料，其特征在于：所述石墨为鳞片石墨，粒径小于75um。
4.根据权利要求1所述的一种ZrO2-C纤维复合材料，其特征在于：所述金属硅粉粒径小于75um，所述碳化硼粒径小于75um。
5.根据权利要求1所述的一种ZrO2-C纤维复合材料，其特征在于：所述氧化锆纤维的长度为3-0.1mm，直径小于3-5um。
6.根据权利要求1所述的一种ZrO2-C纤维复合材料，其特征在于：所述所采用的结合剂为酚醛树脂。
7.根据权利要求1-6中任一项所述的一种ZrO2-C纤维复合材料的制备方法，其特征在于：包括如下步骤：
(1)先将粉料放入超速混炼机中进行混合，其中粉料包括氧化锆细粉、石墨、金属硅粉、碳化硼，然后在将氧化锆纤维放入混合料中，进行机械搅拌分散；
(2)将氧化锆粗颗粒与一半结合剂混合均匀后，在与步骤(1)中的一半预混料进行混合；
(3)将步骤(2)制得的混合料与步骤(1)中剩余的预混料用剩余的一半结合剂进行混练；
(4)将原料混合后，困料12-16h后压制成型，将成形后的制品放入干燥箱中进行干燥；
(5)将步骤(4)压制成型干燥后的制品，放入匣钵中，并在匣钵中埋入石墨，盖过试样，并放入由碳化硅加热的高温窑炉中在1000℃-1200℃下进行烧结，随炉冷却得到所述的ZrO2-C纤维复合材料。
8.根据权利要求7的一种ZrO2-C纤维复合材料的制备方法，其特征在于：所述步骤(1)的机械搅拌分散，搅拌速度为1200-2000r/min，分散时长为5-10min。
9.根据权利要求7或8的一种ZrO2-C纤维复合材料的制备方法，其特征在于：所述步骤(4)干燥的温度和时间为80℃保温6h，120℃保温12h，200℃保温3h。
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Application publication date: 20210827 |