CN111848136A - 一种高韧性、高硬度氧化铝基耐磨陶瓷的制备方法 - Google Patents

一种高韧性、高硬度氧化铝基耐磨陶瓷的制备方法 Download PDF

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CN111848136A
CN111848136A CN201910356115.7A CN201910356115A CN111848136A CN 111848136 A CN111848136 A CN 111848136A CN 201910356115 A CN201910356115 A CN 201910356115A CN 111848136 A CN111848136 A CN 111848136A
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alumina
biscuit
silicon carbide
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徐正平
史彦民
龙成勇
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North Yangzhou Sanshan Industrial Ceramics Co ltd
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Abstract

本发明涉及一种高韧性、高硬度氧化铝基耐磨陶瓷的制备方法。该方法包括步骤一：原料研磨，步骤二：喷雾造粒，步骤三：素坯压制，步骤四：素坯烧结，步骤五：喷砂处理，步骤六：附着耐磨涂层，步骤七：包装入库。由于氧化铝为基体，碳化硅、氧化锆作为增强相，碳酸镁为烧结助剂，碳化硅与氧化锆可以与氧化铝形成晶内/晶间混合型结构，裂纹从晶间到晶内再到晶间的路径扩展，消耗了更多的断裂能，形成了沿晶/穿晶混合的断裂模式，从而大大提高复合材料的综合力学性能；碳酸镁作为烧结助剂，可以降低烧结温度，防止晶粒的长大，该方法科学严谨，烧结过程中能够形成耐磨坯体，化学沉积过程中形成碳化硅与碳化锆混合层，有效增强耐磨陶瓷的耐磨性。

Description

一种高韧性、高硬度氧化铝基耐磨陶瓷的制备方法
技术领域
本发明涉及耐磨陶瓷制造技术领域，尤其涉及一种高韧性、高硬度氧化铝基耐磨陶瓷的制备方法。
背景技术
氧化铝陶瓷是一种常见的结构陶瓷材料，其机械强度好、硬度高、耐磨性强，广泛的应用于石油、化工、矿山等行业之中。尤其在矿山破碎和输送机械设备中耐磨陶瓷对设备的运行至关重要。随着经济的不断发展，矿山设备的产量不断提高，对设备的运转效率提出了更高的要求。目前矿山设备用的氧化铝耐磨陶瓷存在以下几个问题：一是氧化铝耐磨陶瓷运行寿命短，一般在2-3个月，导致设备需要经常停机检修，更换陶瓷内衬；二是对于整条生产而言，不同部位对耐磨陶瓷的性能要求不一，如破碎部位就要求陶瓷要有极高的韧性来抵御矿石的冲击，而遛道、弯管等部位则需要陶瓷有高的硬度来抵御矿石颗粒的磨蚀。当前矿山机械设备中常用的传统氧化铝耐磨陶瓷抗弯强度420MPa、硬度在1320-1400MPa、韧性3.0-3.5MPa·m1/2，其性能指标较低，难以满足当前及未来的工作要求。
发明内容
本发明的目的是针对现有技术存在的不足，即耐磨性欠佳，致密度较低，提供一种高韧性、高硬度氧化铝基耐磨陶瓷的制备方法。
为了实现上述目的，本发明一种高韧性、高硬度氧化铝基耐磨陶瓷的制备方法所采取的技术方案：
一种高韧性、高硬度氧化铝基耐磨陶瓷的制备方法，包括下列步骤：
步骤一：原料研磨，将75-85重量份的氧化铝、5-20重量份的钇稳定氧化锆溶胶、0-1重量份的高岭土、0.5-1重量份的轻质碳酸镁、10-15重量份的纳米碳化硅、60-90重量份的去离子水以及2-8重量份的有机助剂加入到搅拌磨中粗磨，粗磨24小时后得粗磨浆料，每隔5小时测量粗磨浆料的粒度，直至粗磨浆料的平均粒径小于1.5um时停止粗磨，将粗磨浆料加入到砂磨机中进行精磨处理，精磨3小时后得精磨浆料，每隔1小时测量精磨浆料的粒度，直至精磨浆料的平均粒径小于0.6um时停止研磨，出浆；
步骤二：喷雾造粒，将步骤一中的精磨浆料直接喷入喷雾造粒机中，喷雾造粒机入料口温度为300-350℃，出料口温度为90-110℃，喷雾造粒机转速为15000-30000r/min，精磨浆料进料速度为30-50kg/h，得到造粒粉，留以待用；
步骤三：素坯压制，将步骤二中的造粒粉放入在真空环境下的模具内，使用6-8MPa压力进行干压成型，得到预压成型素坯，真空环境为0.6MPa大气压，使用等静压机以180-230MPa压力，对预压成型素坯进行二次成型，得到成型素坯，确保成型素坯密度为2.6±0.05g/cm3，留以待用；
步骤四：素坯烧结，将步骤三中的成型素坯投放至真空烧结炉内进行烧结，烧结时真空度小于0.1MPa，烧结时以3-5℃/min升温至1520-1680℃，并保温3h，然后将温度降至1500-1650℃保温9h，使部分氧化锆与成型素坯中残留碳反应生成碳化锆，在无氧环境下自然冷却得到坯体；
步骤五：喷砂处理，使用喷砂机对步骤四中的坯体进行喷砂，降低坯体表面的残余应力，修理坯体表面，留以待用；
步骤六：附着耐磨涂层，将步骤五中的坯体置于真空的沉积反应室内，真空度为1-3KPa，沉积反应室内温度为900-1400℃，沉积反应室内通入三氯甲基硅烷、四氯化锆、氩气和氢气，保温10-25小时，在坯体表面形成碳化硅与碳化锆混合层，在无氧环境下自然冷却得到耐磨陶瓷，留以待用；
步骤七：包装入库，将步骤六中耐磨陶瓷进行密封包装入库。
与现有技术相比，本发明的有益效果为：由于氧化铝为基体，碳化硅、氧化锆作为增韧助剂，碳酸镁为烧结助剂的存在，碳化硅、氧化锆颗粒粒径小，分散性好，能够均匀的分散于氧化铝陶瓷基体之中，在烧结过程中一部分纳米增韧助剂能够因氧化铝晶粒生长，而被包覆于氧化铝晶粒内部，形成大量“晶内”结构，产生大量次晶界；另一部分增韧助剂会处于氧化铝晶界处，产生钉扎作用，抑制氧化铝晶粒的生长，起到细化氧化铝晶粒的作用。次晶界、细化的晶粒以及氧化锆相变作用共同提升氧化铝基陶瓷的韧性，同时碳化硅与氧化锆可以与氧化铝形成晶内/晶间混合型结构，裂纹从晶间到晶内再到晶间的路径扩展，消耗了更多的断裂能，形成了沿晶/穿晶混合的断裂模式，从而大大提高复合材料的综合力学性能；，碳酸镁作为烧结助剂，可以降低烧结温度，防止晶粒的长大，该方法科学严谨，烧结过程中能够形成耐磨坯体，化学沉积过程中形成碳化硅与碳化锆混合层，有效增强耐磨陶瓷的耐磨性，在真空烧结过程中，有机粘结剂碳化形成微量的残留炭，在整个体系中，只有氧化锆还原碳化反应的吉布斯自由能ΔG<0，因此，残留碳会与氧化锆反应在氧化锆颗粒表面生成少量高硬度相-碳化锆，与碳化硅一起提升陶瓷的硬度。
所述有机助剂为氨基醇分散剂、聚氧乙烯制剂以及水溶性酚醛树脂的混合液，混合液起到分散、增塑以及粘结的作用。
所述纳米碳化硅为球形氧化铝包覆碳化硅，球形氧化铝包覆碳化硅粒径为18-20nm。
具体实施方式
一种高韧性、高硬度氧化铝基耐磨陶瓷的制备方法，包括下列步骤：
步骤一：原料研磨，将75-85重量份的氧化铝、5-20重量份的钇稳定氧化锆溶胶、0-1重量份的高岭土、0.5-1重量份的轻质碳酸镁、10-15重量份的纳米碳化硅、60-90重量份的去离子水以及2-8重量份的有机助剂加入到搅拌磨中粗磨，所述纳米碳化硅为球形氧化铝包覆碳化硅，球形氧化铝包覆碳化硅粒径为18-20nm，所述有机助剂为氨基醇分散剂、聚氧乙烯制剂以及水溶性酚醛树脂的混合液，混合液起到分散、增塑以及粘结的作用，粗磨24小时后得粗磨浆料，每隔5小时测量粗磨浆料的粒度，直至粗磨浆料的平均粒径小于1.5um时停止粗磨，将粗磨浆料加入到砂磨机中进行精磨处理，精磨3小时后得精磨浆料，每隔1小时测量精磨浆料的粒度，直至精磨浆料的平均粒径小于0.6um时停止研磨，出浆；
步骤二：喷雾造粒，将步骤一中的精磨浆料直接喷入喷雾造粒机中，喷雾造粒机入料口温度为300-350℃，出料口温度为90-110℃，喷雾造粒机转速为15000-30000r/min，精磨浆料进料速度为30-50kg/h，得到造粒粉，留以待用；
步骤三：素坯压制，将步骤二中的造粒粉放入在真空环境下的模具内，使用6-8MPa压力进行干压成型，得到预压成型素坯，真空环境为0.6MPa大气压，使用等静压机以180-230MPa压力，对预压成型素坯进行二次成型，得到成型素坯，确保成型素坯密度为2.6±0.05g/cm3，留以待用；
步骤四：素坯烧结，将步骤三中的成型素坯投放至真空烧结炉内进行烧结，烧结时真空度小于0.1MPa，烧结时以3-5℃/min升温至1520-1680℃，并保温3h，然后将温度降至1500-1650℃保温9h，使部分氧化锆与成型素坯中残留碳反应生成碳化锆，在无氧环境下自然冷却得到坯体；
步骤五：喷砂处理，使用喷砂机对步骤四中的坯体进行喷砂，降低坯体表面的残余应力，修理坯体表面，留以待用；
步骤六：附着耐磨涂层，将步骤五中的坯体置于真空的沉积反应室内，真空度为1-3KPa，沉积反应室内温度为900-1400℃，沉积反应室内通入三氯甲基硅烷、四氯化锆、氩气和氢气，保温10-25小时，在坯体表面形成碳化硅与碳化锆混合层，在无氧环境下自然冷却得到耐磨陶瓷，留以待用；
步骤七：包装入库，将步骤六中耐磨陶瓷进行密封包装入库。
本发明并不局限于上述实施例，在本发明公开的技术方案的基础上，本领域的技术人员根据所公开的技术内容，不需要创造性的劳动就可以对其中的一些技术特征作出一些替换和变形，这些替换和变形均在本发明的保护范围内。

Claims (3)

1.一种高韧性、高硬度氧化铝基耐磨陶瓷的制备方法，其特征在于，包括下列步骤：
步骤一：原料研磨，将75-85重量份的氧化铝、5-20重量份的钇稳定氧化锆溶胶、0-1重量份的高岭土、0.5-1重量份的轻质碳酸镁、10-15重量份的纳米碳化硅、60-90重量份的去离子水以及2-8重量份的有机助剂加入到搅拌磨中粗磨，粗磨24小时后得粗磨浆料，每隔5小时测量粗磨浆料的粒度，直至粗磨浆料的平均粒径小于1.5um时停止粗磨，将粗磨浆料加入到砂磨机中进行精磨处理，精磨3小时后得精磨浆料，每隔1小时测量精磨浆料的粒度，直至精磨浆料的平均粒径小于0.6um时停止研磨，出浆；
步骤二：喷雾造粒，将步骤一中的精磨浆料直接喷入喷雾造粒机中，喷雾造粒机入料口温度为300-350℃，出料口温度为90-110℃，喷雾造粒机转速为15000-30000r/min，精磨浆料进料速度为30-50kg/h，得到造粒粉，留以待用；
步骤三：素坯压制，将步骤二中的造粒粉放入在真空环境下的模具内，使用6-8MPa压力进行干压成型，得到预压成型素坯，真空环境为0.6MPa大气压，使用等静压机以180-230MPa压力，对预压成型素坯进行二次成型，得到成型素坯，确保成型素坯密度为2.6±0.05g/cm3，留以待用；
步骤四：素坯烧结，将步骤三中的成型素坯投放至真空烧结炉内进行烧结，烧结时真空度小于0.1MPa，烧结时以3-5℃/min升温至1520-1680℃，并保温3h，然后将温度降至1500-1650℃保温9h，使部分氧化锆与成型素坯中残留碳反应生成碳化锆，在无氧环境下自然冷却得到坯体；
步骤五：喷砂处理，使用喷砂机对步骤四中的坯体进行喷砂，降低坯体表面的残余应力，修理坯体表面，留以待用；
步骤六：附着耐磨涂层，将步骤五中的坯体置于真空的沉积反应室内，真空度为1-3KPa，沉积反应室内温度为900-1400℃，沉积反应室内通入三氯甲基硅烷、四氯化锆、氩气和氢气，保温10-25小时，在坯体表面形成碳化硅与碳化锆混合层，在无氧环境下自然冷却得到耐磨陶瓷，留以待用；
步骤七：包装入库，将步骤六中耐磨陶瓷进行密封包装入库。
2.根据权利要求1所述的一种高韧性、高硬度氧化铝基耐磨陶瓷的制备方法，其特征在于：所述有机助剂为氨基醇分散剂、聚氧乙烯制剂以及水溶性酚醛树脂的混合液，混合液起到分散、增塑以及粘结的作用。
3.根据权利要求2所述的一种高韧性、高硬度氧化铝基耐磨陶瓷的制备方法，其特征在于：所述纳米碳化硅为球形氧化铝包覆碳化硅，球形氧化铝包覆碳化硅粒径为18-20nm。
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