CN116396064B - 一种喷雾热解沉积制备氧化铝基复合材料复杂形状磨粒的方法 - Google Patents

一种喷雾热解沉积制备氧化铝基复合材料复杂形状磨粒的方法 Download PDF

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CN116396064B
CN116396064B CN202310329076.8A CN202310329076A CN116396064B CN 116396064 B CN116396064 B CN 116396064B CN 202310329076 A CN202310329076 A CN 202310329076A CN 116396064 B CN116396064 B CN 116396064B
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鲍瑞
王鹏
刘亮
王荣生
易健宏
冷成
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Jiangsu Fengmang Compound Material Science&tech Group Co ltd
Kunming University of Science and Technology
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Abstract

一种喷雾热解沉积制备氧化铝基复合材料复杂形状磨粒的方法，包括前驱体溶液的制备、喷雾热解沉积、加压烧结，其中前驱体溶液的制备是将铝盐等配置成混合物；喷雾热解沉积将前驱体溶液在高温下分解沉积到复杂形状模具中，获得复杂形状的氧化铝压坯；将已经获得的复杂形状氧化铝压坯进行高温纯化和压力烧结，最终得到接近全致密的纳米或者超细氧化铝基复合材料复杂形状磨料；本发明方法可以实现复杂氧化铝磨料颗粒的大批量、低成本、高稳定和高质量制备。

Description

一种喷雾热解沉积制备氧化铝基复合材料复杂形状磨粒的 方法
技术领域
本发明涉及一种喷雾热解沉积制备氧化铝基复合材料复杂形状磨粒的方法，属于粉末冶金和材料制备领域。
背景技术
喷雾热解沉积(SPHD)是一种制造金属和陶瓷纳米粉末的技术。它通过喷射热解剂，在高温下进行热分解，使得粉末形成沉积在衬底上。喷雾热解沉积是一种高效的制造纳米粉末的方法，如氧化铝磨料颗粒。广泛应用于制造金属和陶瓷纳米粉末，如制造电子、医疗和航空设备。它具有生产高纯度、高精度、高表面积的粉末的优势，同时该技术还具有生产效率高、生产成本低和制备出材质纯度高的优点。
粉末冶金技术可以用于制备各种材料的粉末，例如陶瓷、硬质合金、非金属等。这种技术可以生产出高纯度、高精度、高表面积的粉末，广泛应用于各种领域，例如电子、航空、医疗、汽车等。粉末冶金技术也可以用于制备氧化铝陶瓷，即通过将铝的氧化物或者氮化物和其他物质(如稀土氧化物、碳纳米增强体等)经过混料、压制、烧结等步骤制备成陶瓷复合材料，通过粉末冶金工艺制备的陶瓷粉末具有高纯度、高精度、高表面积等特点，可用于制备各种陶瓷制品，例如陶瓷衬底、陶瓷隔热材料等。
氧化铝磨料是一种常用于磨削加工的高硬度材料。它具有高硬度、高热稳定性和耐磨性等优秀性能，因此广泛用于磨削表面、抛光和清洁等领域。氧化铝磨料的粒径范围较广，从微米级到纳米级都有生产。在磨削加工中，磨料的粒径大小和形貌等因素将直接影响加工精度和表面质量。除了常规的磨削加工外，氧化铝磨料还可以用于纳米抛光、清洁和镀膜等技术。在这些技术中，氧化铝磨料能够提供高效、环保和长期稳定的加工效果。但同时也比较脆，容易在加工过程中断裂。此外由于氧化铝磨粒具有较高的硬度和密度，因此生产和加工成本较高。
氧化铝复杂形状磨粒是指具有不同于常见的圆形氧化铝磨粒的氧化铝颗粒，复杂形状氧化铝磨粒具有更大的接触面积和更高的表面比，因此具有更好的分散性和更高的粘附力。复杂形状氧化铝磨粒可用于磨削、抛光和抛磨等工艺，以获得更优秀的磨削效果。但是通过粉末冶金中的成形工艺难以制备形状复杂的氧化铝磨料，或者制备的磨料成本会大幅增加，不利于磨料的推广和使用。
发明内容
针对现有技术存在的问题，本发明结合喷雾热解沉积和粉末冶金成形的优点，提供一种既简单又容易实现的氧化铝基复合材料复杂形状磨粒的制备方法，步骤包括前驱体溶液的制备、喷雾热解沉积、加压烧结，该方法不仅可以批量化制备氧化铝基复合材料复杂形状磨粒，而且还可以大幅节约成本，提高磨料的综合性能。
本本发明技术方案如下：
一种喷雾热解沉积制备氧化铝基复合材料复杂形状磨粒的方法，具体步骤如下：
(1)将铝盐加溶剂配置成前驱体溶液；
(2)将前驱体溶液进行喷雾热解，喷雾得到的粉体沉积到模具中；
(3)将喷雾热解产物进行高温纯化，再进行加压烧结，最后得到氧化铝基复合材料复杂形状磨粒。
步骤(1)铝盐可以是可溶性的有无机盐或有机盐，如硝酸铝、氯化铝、乙酸铝、碳酸铝、氟化铝等。
步骤(1)前驱体溶液中还加入增强体前驱体和/或助剂；增强体前驱体可以是含有稀土元素的盐(如钇盐、镧盐等)，也可以是能够分解生成六元环碳结构的有机物(如芳香族化合物如苯、萘、蒽等；全氢化合物如环己烷、环庚烷等；咪唑、嘧啶等杂环化合物；二苯基甲烷及其衍生物；芳香醛、芳香酮等含有羰基的化合物；多糖、淀粉等生物大分子等)或者纳米增强体，纳米增强体具体包括碳纳米管、石墨烯、碳量子点、富勒烯、纳米金刚石、纳米氮化硅、纳米氮化硼、纳米碳化硅、纳米碳化钛等；助剂为镁盐、锆盐、钛盐、硅盐等；所述增强体前驱体与铝盐的质量比为1:1.001-1000；助剂添加量为铝盐中质量的0.1-10.0％。
步骤(1)前驱体溶液可以是混合溶液、悬浮液或者乳浊液，若为悬浮液和乳浊液时加入前驱体溶液质量0.5-5.5％的分散剂，分散剂为十二烷基苯磺酸钠等无机表面活性剂，或者聚乙二醇、聚乙烯吡咯烷酮等有机高分子材料。
步骤(2)喷雾热解温度可以是低温喷雾或高温喷雾，低温喷雾的喷雾温度为220-450℃；高温喷雾的喷雾温度为450-1100℃；根据所喷雾的材料选择合适的温度。
步骤(2)喷雾得到的粉体沉积到模具中，模具是高复杂程度的多腔体蜂窝状基底磨具，其中所谓的高复杂程度是指沉积后获得的磨料的几何形状可以是任意可设计的，如正四面体、三棱锥、三棱柱、多齿形等，这些几何体可以是空心或者实心；蜂窝状腔体基底磨具的基底可以是陶瓷材料、金属材料，也可以是高分子材料。
步骤(3)高温纯化的温度不低于250℃，时间不低于5分钟，压力不高于标准大气压。
步骤(3)加压烧结的温度不低于1100℃，压力不小于0.2MPa；加压气氛可以是惰性气体，也可以是空气或者氧气；烧结升温速率不小于10℃/每分钟，烧结时间不超过10小时。本发明的有益效果：
本发明充分结合了喷雾热解沉积和粉末冶金成形的优点，一步制备形状复杂的氧化铝基复合材料，不仅可以批量化生产，大幅节约生产制备成本，而且有利于细化氧化铝晶粒、均分分散增强体，提高氧化铝基复杂形状磨料的综合性能。
附图说明
图1磨具钢制备的多腔体基底磨具即沉积基底的示意图；
图2设计的单个氧化铝基磨料颗粒的尺寸示意图；
图3制备的氧化铝基磨料的实物图照片。
具体实施方式
下面结合具体实施例对本发明做进一步说明。
实施例1
将1000g硫酸铝铵溶解到10升加热至60℃的去离子水中，然后加入20g硝酸镁和8.0g硝酸镧，充分搅拌得到混合溶液，将得到的混合溶液置于喷雾热解设备进行雾化，喷雾温度为250℃，喷雾得到的复合粉体沉积到磨具钢制成的模具中，模具为多腔体基底磨具，内腔基底为实心正四棱锥形的蜂窝结构，其形状如图1，内部预计得到的单个氧化铝基磨料颗粒如图2所示，喷雾完成后，将得到的粉末坯料和模具一同在420℃，保温30分钟，真空度为10Pa；将得到的样品送入加压烧结炉，烧结炉的温度为1350℃，采用纯氩气进行加压烧结，压力为0.8MPa，烧结升温速率为20℃/min，烧结时间为2小时，冷却后得到最终边长为1.5mm的正四棱锥形的氧化铝磨料，如图3所示，其相对致密度达到了99.1％，硬度达到了10.2GPa。
实施例2
将500g硝酸铝溶解到15升加热至80℃的去离子水中，然后加入10.0g氯化锆和8.0g氯化镧，充分搅拌得到混合溶液，将得到的混合溶液置于喷雾热解设备进行雾化，喷雾温度为850℃，喷雾得到的复合粉体沉积到刚玉陶瓷模具中，模具为多腔体基底磨具，模具内腔基底的几何形状为实心正四棱锥形状的蜂窝结构，喷雾完成后，将得到的粉末坯料和模具一同在250℃，保温10分钟，真空度为20Pa；将得到的样品送入加压烧结炉，烧结炉的温度为1300℃，采用纯氮气气氛保护下进行加压烧结，压力为3.0MPa，烧结升温速率为10℃/min，烧结时间为2小时，冷却后得到最终边长为3.0mm的正四棱锥的氧化铝磨料，其相对致密度达到了98.5％；硬度达到了9.88GPa。
实施例3
将1000g氯化铝铵溶解到20升加热至75℃的去离子水中，然后加入30g碳酸氢镁和15.0g碳纳米管分散液(质量分数为10％)，同时加入10g十二烷基苯磺酸钠(SDBS)，充分搅拌得到悬浮液，将得到的悬浮液置于喷雾热解设备进行雾化，喷雾温度为220℃，喷雾得到的复合粉体沉积到聚四氟乙烯的模具中，模具为多腔体基底磨具，模具内腔基底的几何形状为实心正三棱柱的蜂窝结构，喷雾完成后，将得到的粉末坯料和模具一同在260℃，保温10分钟，真空度为10Pa；将得到的样品送入低压烧结炉，烧结炉的温度为1400℃，采用纯氩气进行加压，压力为5.5MPa，烧结升温速率为12℃/min，烧结时间为1.0小时，冷却后得到最终边长为3.0mm的正三棱柱的氧化铝基磨料，其相对致密度达到了98.7％；硬度达到了9.46GPa。
实施例4
将400g氯化铝和20g氯化锆加入到500mL乙醇+去离子水(体积比1:1)中，充分搅拌得到混合溶液，将得到的混合溶液放入喷热热解炉中，喷雾得到的复合粉体沉积到硬质合金模具中，模具为多腔体基底磨具，模具内腔基底的几何形状为实心多齿状的蜂窝结构，将温度设定为560℃，直到溶液完全喷雾热解沉积到模具中，喷雾完成后，将得到的粉末坯料和模具一同在420℃，保温30分钟，真空度为10Pa；将得到的样品送入高温烧结炉中，在氧气气氛下进行加压烧结，压力为5.5MPa，烧结升温速率为10℃/min，烧结温度为1250℃，烧结时间为2.5小时，冷却后得到最终晶粒度在50-100μm之间的齿状氧化铝陶瓷颗粒，其相对致密度达到了99.5％；硬度达到了9.61GPa。
实施例5
将2.0kg碳酸铝加入到6.0L去离子水中，充分搅拌后加入0.5Kg纳米氮化硼，加入50g聚乙二醇作为分散剂，将得到的混合溶液放入喷热热解炉中，喷雾得到的复合粉体沉积到陶瓷模具中，模具内腔基底的几何形状为实心六棱柱的蜂窝结构，将温度设定为850℃，直到溶液完全喷雾热解沉积到模具中，喷雾完成后，将得到的粉末坯料和模具一同在240℃，保温15分钟，真空度为20Pa；将得到的样品送入高温烧结炉中，在氩气气氛下进行加压烧结，压力为3.5MPa，烧结升温速率为12℃/min，烧结温度为1400℃，烧结时间为1.0小时，冷却后得到最终晶粒度在50-80μm之间的六棱柱氧化铝陶瓷颗粒，其相对致密度达到了97.8％；硬度达到了10.68GPa。
实施例6
将320g硝酸铝和18g硝酸镧加入到100mL丙酮+1000mL去离子水的混合溶剂中，充分搅拌得到混合溶液，将得到的混合溶液置于喷雾热解设备进行雾化，喷雾温度为800℃，喷雾得到的复合粉体沉积到刚玉陶瓷模具中，模具为多腔体基底磨具，模具内腔基底的几何形状为中空正三棱柱形状的蜂窝结构，喷雾完成后，将得到的粉末坯料和模具一同在280℃，保温30分钟，真空度为10Pa；将得到的样品送入加压烧结炉，烧结炉的温度为1520℃，采用纯氮气气氛保护下进行加压烧结，压力为6.0MPa，烧结升温速率为20℃/min，烧结时间为6小时，冷却后得到最终边长为3.0mm的中空正三棱柱的氧化铝磨料，其相对致密度达到了99.5％；硬度达到了11.33GPa。
对比例1
将1000g硫酸铝铵溶解到10升加热至60℃的去离子水中，然后加入20g硝酸镁和8.0g硝酸镧，充分搅拌得到混合溶液，将得到的溶液置于喷雾热解设备进行雾化，喷雾温度为320℃，喷雾得到的复合粉体沉积到常规的不锈钢模具中，内腔为常规空腔，喷雾完成后，模具继续真空炉中，在320℃，保温30分钟，真空度为10Pa；将得到的样品进行热处理后送入真空烧结炉，烧结炉的温度为1350℃，烧结升温速率为20℃/min，烧结时间为2小时，冷却后得到氧化铝磨料，其相对致密度达到了91.12％；硬度达到了5.20GPa。
对比例2
将500g硝酸铝溶解到15升加热至80℃的去离子水中，然后加入10.0g氯化锆和8.0g氯化镧，充分搅拌得到混合溶液，将得到的溶液置于喷雾热解设备进行雾化，喷雾温度为180℃，喷雾得到的复合粉体沉积到刚玉陶瓷模具中，模具为多腔体基底磨具，模具内腔基底的几何形状为正四棱锥形状的蜂窝结构，将得到的样品送入加压烧结炉，烧结炉的温度为1300℃，采用纯氮气气氛保护下进行加压，压力为3.0MPa；烧结升温速率为10℃/min，烧结时间为2小时，冷却后得到最终边长为3.0mm的正四棱锥的氧化铝磨料，其相对致密度达到了90.27％；硬度达到了3.08GPa。
对比例3
将1000g氯化铝铵溶解到20升加热至75℃的去离子水中，然后加入30g氯化镁和15.0g碳纳米管分散液(质量分数为10％)，同时加入氯化铝铵和碳纳米管总质量0.5％的十二烷基苯磺酸钠(SDBS)，充分搅拌得到悬浮液，将得到的悬浮液置于喷雾热解设备进行雾化，喷雾温度为220℃，喷雾得到的复合粉体沉积到聚四氟乙烯的模具中，模具的内腔为常规空腔；将得到的样品送入真空烧结炉，烧结炉的温度为1050℃，采用纯氩气进行加压，压力为5.5MPa；烧结升温速率为12℃/min，烧结时间为1.0小时，冷却后得到氧化铝基磨料，其相对致密度达到了88.11％；硬度达到了1.24GPa。

Claims (4)

1.一种喷雾热解沉积制备氧化铝基复合材料复杂形状磨粒的方法，其特征在于，具体步骤如下：
（1）将铝盐加溶剂配置成前驱体溶液；
（2）将前驱体溶液进行喷雾热解，喷雾得到的粉体沉积到模具中；
（3）将喷雾热解产物进行高温纯化，再进行加压烧结，得到氧化铝基复合材料复杂形状磨粒；
步骤（2）喷雾热解温度为220-1100℃；
步骤（2）模具是多腔体蜂窝状基底磨具，所述多腔体蜂窝状基底模具的基底的几何形状为正四面体、三棱锥、三棱柱或多齿形；多腔体蜂窝状基底的基底材料为陶瓷材料、金属材料或高分子材料；
步骤（3）高温纯化的温度不低于250℃，时间不低于5分钟，压力不高于标准大气压；
步骤（3）加压烧结的温度不低于1100℃，压力不小于0.2MPa，加压气氛为惰性气体、空气或氧气；烧结升温速率不小于10℃/分钟，烧结时间不超过10小时。
2.根据权利要求1所述喷雾热解沉积制备氧化铝基复合材料复杂形状磨粒的方法，其特征在于，步骤（1）铝盐为是可溶性盐，溶剂是水或者有机溶剂。
3.根据权利要求1所述喷雾热解沉积制备氧化铝基复合材料复杂形状磨粒的方法，其特征在于，步骤（1）前驱体溶液中还加入增强体前驱体和/或助剂；增强体前驱体为含有稀土元素的盐、能够分解生成六元环碳结构的有机物或纳米增强体，纳米增强体包括碳纳米管、石墨烯、碳量子点、富勒烯、纳米金刚石、纳米氮化硅、纳米氮化硼、纳米碳化硅、纳米碳化钛；助剂为镁盐、锆盐、钛盐或硅盐；增强体前驱体与铝盐的质量比为1:1.001-1000；助剂添加量为铝盐总质量的0.1-10.0%。
4.根据权利要求3所述喷雾热解沉积制备氧化铝基复合材料复杂形状磨粒的方法，其特征在于，步骤（1）前驱体溶液为混合溶液、悬浮液或者乳浊液，若为悬浮液或乳浊液时加入前驱体溶液质量0.5-5.5%的分散剂，分散剂为十二烷基苯磺酸钠、聚乙二醇或聚乙烯吡咯烷酮。
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