CN107686353A - 一种高强导电碳化硅‑铁复合多孔陶瓷的制备方法 - Google Patents

一种高强导电碳化硅‑铁复合多孔陶瓷的制备方法 Download PDF

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CN107686353A
CN107686353A CN201710725462.3A CN201710725462A CN107686353A CN 107686353 A CN107686353 A CN 107686353A CN 201710725462 A CN201710725462 A CN 201710725462A CN 107686353 A CN107686353 A CN 107686353A
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马北越
张亚然
苏畅
张博文
任鑫明
李世明
于景坤
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Northeastern University China
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Abstract

一种高强导电碳化硅‑铁复合多孔陶瓷的制备方法，属于金属‑陶瓷材料及多孔陶瓷制备技术领域。具体制备方法为：首先，根据氧化铁的含量配置还原剂碳粉，按照设定配比，将原料工业碳化硅粉、氧化铁粉、碳粉湿法球磨，充分干燥后，再添加结合剂酚醛树脂，并充分混匀；然后，施加50～200MPa的压强，制得素坯；最后，将试样置于高温炉中烧结，得到碳化硅‑铁复合多孔陶瓷。该方法解决了汽车尾气催化剂载体冷启动起燃慢的问题，减少了冷启动开始几分钟内有害物质的排放量，保护了大气环境。该制备过程操作简单，原料廉价易得，降低了成本，提高了社会效益和环保效益。

Description

一种高强导电碳化硅-铁复合多孔陶瓷的制备方法
技术领域
本发明属于金属陶瓷复合材料制备技术领域，涉及一种应用于汽车尾气催化剂载体的高强导电多孔陶瓷的制备方法。
背景技术
随着汽车行业的不断发展，汽车尾气排放已成为是大气污染的主要来源。由于多孔陶瓷具有比表面积高、热稳定好、耐热、无毒等特点，可作为汽车尾气催化剂载体使用。在其表面涂覆一层活性氧化铝和贵金属催化剂后，可使汽油燃烧过程中排出的CO、NOx和CxHy等有害气体转化为无毒的CO2、N2和H2O。
目前普遍应用的堇青石蜂窝陶瓷不导电，只能依靠发动机排气和反应放热来催化，造成冷启动前60s燃料燃烧不充分，释放大量的CxHy和CO。因此，减少汽车冷启动后1～3min的尾气排放污染物是降低汽车排放污染的关键。
SiC多孔陶瓷呈三维连通网状结构，具有优异的耐腐蚀性与抗热震性，其抗热震性优于堇青石蜂窝陶瓷，特别适用于温度急剧变化的场合。而金属具有较高的导电性。通过在SiC多孔陶瓷的制备中，添加导电性良好的金属成分，从而得到的高强导电的复合多孔陶瓷。使得催化剂在较短时间内就达到催化剂的起燃温度，能够有效减少冷启动开始几分钟内有害物质的排放量。
发明内容
为了解决汽车尾气催化剂载体冷启动起燃慢的问题，本发明提出了一种高强导电碳化硅-铁复合多孔陶瓷的制备方法。该方法根据氧化铁的含量配置适量的还原剂碳粉，按照设配比，将工业碳化硅粉、氧化铁粉、碳粉湿法球磨，干燥12h后，再添加结合剂酚醛树脂，混匀，成型，置于高温炉中烧结，得到碳化硅-铁复合多孔陶瓷。
一种高强导电碳化硅-铁复合多孔陶瓷的制备方法，按以下步骤进行：
步骤1：球磨混料
(1)根据氧化铁的含量配置还原剂碳粉；所述的还原剂碳粉应将氧化铁全部还原为铁单质；
(2)按照设计配比，将原料工业碳化硅粉、氧化铁粉、碳粉湿法进行球磨；
(3)球磨后的原料在干燥箱中干燥，再添加结合剂酚醛树脂，充分混匀。所述的结合剂添加量为3％～5％；
步骤2：成型与干燥
施加50～200MPa的压强，制得素坯；并充分干燥。
步骤3：高温烧结
将素坯置于高温炉中烧结，得到碳化硅-铁复合多孔陶瓷。烧结温度为1400℃～1700℃，烧结时间为2～10h。
所述的步骤1(1)中，所述的碳粉优选为活性炭、石墨、炭黑、焦炭或煤粉；
所述的适量还原剂碳粉的同时，可添加适量的铁纤维增强碳化硅-铁多孔陶瓷的强度。
所述的步骤1(2)中，所述的湿法球磨中，优选添加无水乙醇、去离子水；
所述球磨设备为行星式球磨机，以200～400r·min-1转速单向运行5～8h；
所述的步骤1(3)中，所述的干燥时间为10～20h。
所述的步骤2中，所述的成型方式为模压成型、等静压成型。
所述的步骤3中，所用保护气为高纯度的Ar气。
所述的步骤3中，高温炉为可通气氛的箱式电阻炉、管式电阻炉和隧道窑。
本发明的有益效果是：本发明解决了汽车尾气催化剂载体冷启动起燃慢的问题，减少了冷启动开始几分钟内有害物质的排放量，保护了大气环境。工艺简化，能耗低，易于实现工业化生产。本发明采用工业碳化硅粉、氧化铁粉为主要原料，制备过程操作简单，原料廉价易得，降低了成本，提高了效益，且适合多种碳化硅-金属复合多孔陶瓷的生产。
附图说明
图1是本发明的工艺流程图。
具体实施方式
下面结合实施例对本发明作进一步的详细说明，但本发明并不局限于以下实施例，所述只是适用本发明的部分实例。
以下实施例中，除特别说明，原料均来自市购。
以下实施例中，一种高强导电碳化硅-铁复合多孔陶瓷的制备方法工艺流程图见图1。
实施例1
一种高强导电碳化硅-铁复合多孔陶瓷的制备方法，按以下步骤进行：
步骤1：球磨混料
(1)根据氧化铁的含量配置还原剂活性炭，其中，活性炭的质量为氧化铁粉质量的30％；
(2)按照实验配比，将原料工业碳化硅粉、氧化铁粉、活性炭湿法球磨；
(3)球磨后的原料在干燥箱中于120℃下干燥12h，再添加质量分数为5％的结合剂酚醛树脂，于研钵中手磨混匀。
步骤2：成型与干燥
施加50～200MPa的压强，得到Φ15×15的柱状试样，并在120℃下干燥12h；
步骤3：高温烧结
将Φ15×15的柱状试样置于高温炉中于1550℃下烧结4h，得到碳化硅-铁复合多孔陶瓷。
经检测，所得的碳化硅-铁复合多孔陶瓷的物相组成为β-SiC、Fe3Si，气孔率为48.01％，常温抗压强度为2.30MPa。物相组成中存在的Fe3Si是电的良导体，提高了碳化硅(β-SiC)多孔陶瓷的电导率。
实施例2
一种高强导电碳化硅-铁复合多孔陶瓷的制备方法，同实施例1，不同之处在于，所需的还原剂碳粉为石墨，其中，石墨含量为氧化铁粉质量的30％。
经检测，所得的碳化硅-铁复合多孔陶瓷的物相组成为β-SiC和Fe3Si，气孔率为54.08％，常温抗压强度为1.85MPa。物相组成Fe3Si是电的良导体，提高了碳化硅(β-SiC)多孔陶瓷的电导率。
实施例3
一种高强导电碳化硅-铁复合多孔陶瓷的制备方法，同实施例1，不同之处在于：
(1)所需的还原剂碳粉为石墨，其中，石墨含量为氧化铁质量的百分比为40％。
(2)步骤3中，烧结温度为1500℃。
经检测，所得的碳化硅-铁复合多孔陶瓷的物相组成为β-SiC、Fe3C，气孔率为58.24％，常温抗压强度为1.66MPa，制品中存在电的良导体Fe3C与少量未反应的石墨C，提高了碳化硅(β-SiC)多孔陶瓷的电导率。

Claims (10)

1.一种高强导电碳化硅-铁复合多孔陶瓷的制备方法，其特征在于，按以下步骤进行：
步骤1：球磨混料
(1)根据氧化铁的含量配置还原剂碳粉，所述的还原剂碳粉应将氧化铁全部还原为铁单质；
(2)按照设定配比，将原料工业碳化硅粉、氧化铁粉、碳粉湿法球磨；
(3)球磨后的原料干燥，再添加结合剂酚醛树脂，充分混匀；结合剂添加量为3％～5％；
步骤2：干压成型与干燥
施加50～200MPa的压强，制得素坯；并充分干燥；
步骤3：高温烧结
将素坯置于高温炉中烧结，得到碳化硅-铁复合多孔陶瓷；烧结温度为1400℃～1 700℃，烧结时间为2～10h。
2.如权利要求1所述的方法，其特征在于，所述的步骤1中，所述的碳粉为活性炭、石墨、炭黑、焦炭或煤粉。
3.如权利要求1或2所述的方法，其特征在于，使用还原剂碳粉的同时，添加适量的铁纤维增强碳化硅-铁多孔陶瓷。
4.如权利要求1或2所述的方法，其特征在于，所述的湿法球磨中，添加无水乙醇或去离子水。
5.如权利要求3所述的方法，其特征在于，所述的湿法球磨中，添加无水乙醇或去离子水。
6.如权利要求1或2或5所述的方法，其特征在于，所述的步骤1(2)中，所述球磨设备为行星式球磨机，以200～400r·min-1转速单向运行5～8h。
7.如权利要求3所述的方法，其特征在于，所述的步骤1(2)中，所述球磨设备为行星式球磨机，以200～400r·min-1转速单向运行5～8h。
8.如权利要求4所述的方法，其特征在于，所述的步骤1(2)中，所述球磨设备为行星式球磨机，以200～400r·min-1转速单向运行5～8h。
9.如权利要求1或2或5或7或8所述的方法，其特征在于，所述的保护气为Ar气。
10.如权利要求9所述的方法，其特征在于，所述的高温炉为可通气氛的箱式电阻炉、管式电阻炉、隧道窑中的一种。
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Cited By (5)

* Cited by examiner, † Cited by third party
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CN109160814A (zh) * 2018-09-20 2019-01-08 东北大学 一种原位碳化硅-铁硅复合材料及其制备方法
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CN109160814A (zh) * 2018-09-20 2019-01-08 东北大学 一种原位碳化硅-铁硅复合材料及其制备方法
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CN109465441A (zh) * 2018-12-27 2019-03-15 马鞍山中科冶金材料科技有限公司 硅钛铬钒合金及其制备方法
CN109482871A (zh) * 2018-12-27 2019-03-19 马鞍山中科冶金材料科技有限公司 硅铬钛合金及其制备方法
CN109628822A (zh) * 2018-12-27 2019-04-16 马鞍山中科冶金材料科技有限公司 硅钛钒合金及其制备方法
CN109628823A (zh) * 2018-12-27 2019-04-16 马鞍山中科冶金材料科技有限公司 硅铬钒合金及其制备方法

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