CN113045297B - 一种3d直写打印复合陶瓷浆料、制备方法及得到的陶瓷 - Google Patents
一种3d直写打印复合陶瓷浆料、制备方法及得到的陶瓷 Download PDFInfo
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Abstract
本发明公开了一种3D直写打印复合陶瓷浆料,包括微纳米主体材料、添加物粉体材料、分散剂和粘结剂,所述的微纳米主体材料与添加物粉体材料的重量比为1:20~1:45;所述的分散剂添加量为浆料总重量的0.1~1%;所述的粘结剂的添加量为浆料总重量的0.2~0.5%。本发明还公开了上述陶瓷浆料的制备方法以及通过3D直写打印成坯、热处理后烧制得到的具有仿生结构高强高韧复合陶瓷。本发明采用的原料无毒无害,环保经济,得到的陶瓷浆料固含量高,复合陶瓷采用3D直写打印可以实现复合陶瓷的个性化、精细化和复杂化制备,摆脱模具形状的制约,可应用于航空航天、电气、生物工程、陶瓷燃料电池、压电材料等诸多领域。
Description
技术领域
本发明涉及仿生复合材料领域,具体涉及一种3D直写打印复合陶瓷浆料、制备方法及得到的具有仿生结构高强高韧复合陶瓷。
背景技术
工业发展和社会进步对陶瓷材料的力学性能不断提出越来越高的要求,同时在复杂化、个性化、环保等方面对其发展提出诸多限制。对陶瓷材料进行优化设计与制备,以增加其综合力学性能,且满足陶瓷产品当前的发展趋势,对于促进陶瓷材料更好地满足实际应用需求具有重要意义。
自然界中的天然生物材料具有无与伦比的优异性能,如贝壳、珍珠、牙齿、骨骼等,这与其微观精巧复杂的组织结构息息相关。从微观尺度出发自下而上体外模拟生物质基质的组装,进而构筑仿生多级精细结构,有助于制备性能优异的合成材料,并推动材料科学的发展。
陶瓷产品的传统成型方式包括压制成型法、可塑成型法、浆料成型法等。这类成型方法需要依赖模具,步骤繁琐,生产周期较长,难以制造个性化和复杂化的陶瓷部件。3D直写打印作为一种高度技术集成的陶瓷制造方法,可以实现设计制造一体化,以三维数字模型文件为基础,利用压力挤出等方法将金属、非金属、高分子等材料逐层累加黏结,在脱离模具的情况下,可快速成型个性化的零部件。此外,3D直写打印技术具有精密化的特点,其自下而上的原料成型过程和生物材料的形成过程具有相似性,可实现复杂结构陶瓷材料的制造。通过电脑辅助设计,3D直写打印可以为仿生材料制造提供平台,将两者有机结合在一起可更好地发挥协同作用,为制备优异力学性能的复杂陶瓷材料提供有效方法。
公开号为CN109336613A的中国专利文献中公开了一种高强度仿生陶瓷及其制备方法,其采用氮化硅、松木碎屑、玉米秸秆等作为主要原料,高压高温的条件下制得该复合材料,松木碎屑的加入可以提高陶瓷材料强度和断裂韧性,但此发明的原料复杂,操作步骤较为繁琐,能耗大。
公开号为CN109336613A的中国专利文献中公开了一种高强高韧陶瓷复合材料及其在制造刀具中的应用,其采用氧化锆、氧化铝、氧化铈、氧化镧等为主要原料,经球磨过筛煅烧热压等一系列操作制备高强高韧陶瓷复合材料,该复合材料具有很高的硬度和耐磨性,适合用于制备陶瓷刀具,但此方法制备得到的材料形式单一,不能满足实现个性化、精细化和复杂化陶瓷器件的制备,无法摆脱热压制品形状的制约。
发明内容
针对本领域存在的不足之处,为克服传统陶瓷材料制备的局限性,本发明提供了一种3D直写打印复合陶瓷浆料及其制备方法,并结合3D直写打印和热处理技术制备得到具有仿生结构高强高韧复合陶瓷,具有原料环保经济,制备工艺简单,制备条件温和,且可以成型复杂精细几何结构的特点。
具体采用的技术方案如下:
一种3D直写打印复合陶瓷浆料,包括以下原料:
微纳米主体材料:氧化铝、氧化锆、氧化钛、碳化硅、氮化硅中的至少一种;
添加物粉体材料:氧化硅、氧化钇、氧化铈中的至少一种;
分散剂:聚乙二醇、硬脂酰胺、六偏磷酸钠中的至少一种;
粘结剂:海藻酸钠、黄原胶、羟甲基纤维素钠、聚乙烯吡咯烷酮中的至少一种;
所述的微纳米主体材料与添加物粉体材料的重量比为1:20~1:45;
所述的分散剂添加量为浆料总重量的0.1~1%;
所述的粘结剂添加量为浆料总重量的0.2~0.5%。
所述的微纳米主体材料粒径分布为2~10μm;
所述的添加物粉体材料粒径分布为80~2000nm,根据仿生结构设计,进一步优选为500~2000nm。
优选地,所述的微纳米主体材料为氧化铝或碳化硅;
优选地,所述的添加物粉体材料为氧化硅、氧化钇、氧化铈中的一种或两种。
分散剂、粘结剂分别溶于水或有机溶剂形成溶液后加入,最后形成的3D直写打印复合陶瓷浆料的固含量为65~90wt%,根据其挤出特性,进一步优选为68~75wt%。
优选地,所述的分散剂为六偏磷酸钠和聚乙二醇6000的混合物,六偏磷酸钠和聚乙二醇6000的重量比为1:10~1:100,为保持浆料的含水量,进一步优选为1:20~1:50,采用聚乙二醇6000溶液的质量浓度为15~25%,六偏磷酸钠溶液为的质量浓度为0.1~1%,其中,六偏磷酸钠对陶瓷颗粒起到主要的润湿分散作用,聚乙二醇可防止陶瓷颗粒间的团聚,同时起到润滑打印浆料和管壁的作用和保湿的作用。
优选地,所述的粘结剂为海藻酸钠和聚乙烯吡咯烷酮(PVPK30)的混合物,海藻酸钠和聚乙烯吡咯烷酮的重量比为1:0.1~1:10,进一步优选为1:0.5~1:5。海藻酸钠溶液的质量浓度为5~10%,PVPK30溶液的质量浓度为5~20%,其中,海藻酸钠主要起到粘结剂和稳定剂的作用,聚乙烯吡咯烷酮一方面起到粘结的作用,另一方面起到分散的作用。
优选地,所述的3D直写打印复合陶瓷浆料在1s-1剪切速率下的粘度为300~4000Pa·S,进一步优选为600~2000Pa·S。
本发明还公开了一种3D直写打印复合陶瓷浆料的制备方法,包括以下步骤:
(1)将微纳米主体材料和添加物粉体材料干燥,研磨过筛,取出添加物粉体材料加入分散剂溶液中,超声预分散,得到悬浊液;
(2)将粘结剂加入悬浊液中,以600~1000r/min的转速搅拌30~60min,再加入干燥后的微纳米主体材料粉末,逐渐提升转速至1200~2000r/min,搅拌2~3h,将混匀的浆料放入真空箱进行去除气泡1~2h,获得3D直写打印复合陶瓷浆料。
步骤(1)中,将添加物粉体材料进行预分散,既可防止搅拌过程中粒子之间严重团聚包覆,又能避免打印过程中发生喷头堵塞,引入缺陷。优选地,步骤(1)中所述的过筛的筛网目数为大于2000目;
步骤(1)中所述的干燥方式为常压干燥,干燥温度为110~120℃,干燥时间为12~24h;
优选地,所述的超声预分散在细胞粉碎机中进行,功率在500W以上,超声时间为10~20min。
本发明还公开了所述的3D直写打印复合陶瓷浆料制备得到的具有仿生结构高强高韧复合陶瓷,该具有仿生结构高强高韧复合陶瓷的制备方法,包括:
1)利用3D直写打印技术将所述的3D直写打印复合陶瓷浆料打印成复合陶瓷生坯;
2)复合陶瓷生坯在室温下干燥,再放入温度大于80℃的鼓风干燥烘箱中保温12h以上,最后放入设定好升温程序的马弗炉中烧制得到具有仿生结构高强高韧复合陶瓷。。
步骤1)中所述的3D直写打印步骤为:采用三维软件建模,利用切片软件对图形进行逐层切片,对每片进行线条路径G-code生成,主机控制三维移动平台根据路径进行陶瓷浆料的挤出和堆积,得到复合陶瓷生坯。
步骤1)中3D直写打印技术参数为:喷嘴直径为1~3mm,打印层厚为1.2~3.6mm,打印速度为200~300mm/min;
步骤2)中所述的升温程序为以5~10℃/min的升温速率由室温升温至500℃,保温去除有机粘结剂后,在500~1600℃以3~5℃/min升温,空气气氛下烧结2~3h。
与现有技术相比,本发明具有如下优点:
(1)本发明所用的陶瓷微纳米主体材料、添加物粉体材料、分散剂、粘结剂及溶剂均为无毒无害,环保经济。
(2)本发明采用的陶瓷浆料固含量高,复合陶瓷材料的制备工艺简单,制备条件温和,可有效改善陶瓷材料成型条件苛刻的问题。同时,对于高固含量陶瓷浆料难以打印的技术瓶颈,本发明改善了打印喷头堵塞,挤出困难的问题。
(3)本发明利用复合陶瓷浆料中微纳米主体材料的片状结构和添加物粉体材料的球状结构在3D直写打印挤出过程中的拖曳力的相互作用,及3D直写打印技术层层堆叠的特性,自下而上体外模拟生物质基质的组装,构筑得到微观砖墙型结构的具有仿生结构的高强高韧复合陶瓷,抗弯强度为50~55Mpa,断裂韧性为3~6Mpa·m0.5。
(4)本发明通过3D直写打印技术可以实现复合陶瓷的个性化、精细化和复杂化制备,摆脱模具形状的制约,可应用于航空航天、电气、生物工程、陶瓷燃料电池、压电材料等诸多领域。
附图说明
图1为本发明实施例1中使用的氧化铝(4μm)和两种不同尺度氧化硅(500nm、2μm)粉末的SEM图。
图2为实施例1制备得到的氧化铝复合陶瓷的微观砖墙型结构的SEM图。
图3为图2的放大图。
图4为实施例2中75wt%固含量的3D直写打印复合氧化铝陶瓷浆料制备得到的氧化铝复合陶瓷的微观砖墙型结构的SEM图。
图5为图4的放大图。
图6为本发明实施例2中由不同固含量的3D直写打印复合氧化铝陶瓷浆料制备的复合陶瓷三维圆柱形打印样件图片。
具体实施方式
实施例1
采用氧化铝为微纳米主体材料,氧化硅为添加物粉体材料,海藻酸钠、聚乙烯吡咯烷酮为粘结剂,六偏磷酸钠和聚乙二醇6000为分散剂,去离子水为溶剂,制备复合陶瓷浆料。
优选陶瓷浆料固含量为68wt%,取230g,粒径4μm氧化铝和10g不同粒径(粒径为500nm、2μm)氧化硅陶瓷粉体放于烘箱常压干燥,氧化铝和两种不同尺度氧化硅粉末的扫描电镜图如图1所示。干燥温度设置为110~120℃,干燥时间为12~24h。干燥完全后,用2000目的筛网研磨过筛,取出的氧化硅粉末在分散剂溶液中超声预分散10min,超声设备为细胞粉碎机,功率在500W以上。
分散剂溶液为0.3g六偏磷酸钠和15g聚乙二醇6000溶解于75mL去离子水制得。
将5.1g海藻酸钠和7.5g聚乙烯吡咯烷酮作为粘结剂加入到分散好的混合有氧化硅和分散剂的悬浊液中均匀混合,在机械搅拌器中以600r/min的转速搅拌30min,再加入烘干的氧化铝粉末,逐渐提升转速至1200r/min,搅拌2h,放入真空箱去除气泡2h,获得高固含量的3D直写打印陶瓷浆料。
将配置好的浆料装入到料筒内,同时将1mm打印喷头、输料管、活塞连接,整体安装在螺杆推进器上,并且设置好1.2mm打印层厚、200~300mm/s打印速度等相关工艺参数。然后操作主机的预挤功能,向打印料筒中施加压力,进行预挤出处理,以排出在输料管内和料筒内残余的空气。待打印喷头能够出丝连续之后,进行断丝处理。
随后,借助主机辅助设计的三维图形,自动控制活塞后的螺杆推进器调控挤出速率,使浆料流出,并沉积在按照步进电机移动的X~Y轴成型平台上,从而获得圆柱形三维结构生坯,再将生坯进行热处理,首先在室温下干燥2h,其次放入80℃的鼓风干燥烘箱中保温12h以上。最后,放入1600℃的马弗炉中,在空气气氛下烧结2h即可得到致密氧化铝复合陶瓷。升温制度为室温~500℃以5℃/min的升温速率进行,500℃保温0.5h以去除有机粘结剂,500~1600℃以3℃/min进行,在1600℃保温2h,得到具有仿生结构高强高韧复合陶瓷。图2为该氧化铝复合陶瓷材料的扫描电镜图,氧化铝主体材料和氧化硅粉体材料在3D直写打印挤出过程中由于拖曳力的作用形成平整的片层结构,再经由3D直写打印技术层层堆叠,形成了微观砖墙型结构,此外,该氧化铝复合陶瓷的抗弯强度为55Mpa,断裂韧性为5Mpa·m0.5。
对比例1
采用氧化铝为微纳米主体材料,海藻酸钠、聚乙烯吡咯烷酮为粘结剂,六偏磷酸钠和聚乙二醇6000为分散剂,去离子水为溶剂,制备复合陶瓷浆料。
取230g氧化铝陶瓷粉体放于烘箱常压干燥,温度设置为110~120℃,干燥时间为12~24h。干燥完全后,用2000目的筛网研磨过筛。分散剂溶液为0.3g六偏磷酸钠和15g聚乙二醇6000溶解于75mL去离子水制得。
将5.1g海藻酸钠和7.5g聚乙烯吡咯烷酮作为粘结剂加入到分散好的混合有分散剂的悬浊液中均匀混合,在机械搅拌器中以600r/min的转速搅拌30min,再加入烘干的氧化铝粉末,并且逐渐提升转速至1200r/min,搅拌2h,放入真空箱去除气泡2h,获得高固含量的3D直写打印陶瓷浆料。
将配置好的浆料装入到料筒内,同时将1mm打印喷头、输料管、活塞连接,整体安装在螺杆推进器上,并且设置好1.2mm打印层厚、200~300mm/s打印速度等相关工艺参数。然后操作主机的预挤功能,向打印料筒中施加压力,进行预挤出处理,以排出在输料管内和料筒内残余的空气。待打印喷头能够出丝连续之后,进行断丝处理。
随后,借助主机辅助设计的三维图形,自动控制活塞后的螺杆推进器调控挤出速率,使浆料流出,并沉积在按照步进电机移动的X~Y轴成型平台上,从而获得圆柱形三维结构生坯,再将生坯进行热处理,首先在室温下干燥2h,其次放入80℃的鼓风干燥烘箱中保温12h以上。最后,放入1600℃的马弗炉中,在空气气氛下烧结2h即可得到致密氧化铝陶瓷。升温制度为室温~500℃以5℃/min的升温速率进行,500℃保温0.5h以去除有机粘结剂,500~1600℃以3℃/min进行,在1600℃保温2h。未加氧化硅的陶瓷浆料的表观粘度较大,达到3100Pa·S,会对打印会造成堵塞。
实施例2
采用氧化铝为微纳米主体材料,氧化硅为添加物粉体材料,海藻酸钠、聚乙烯吡咯烷酮为粘结剂,六偏磷酸钠和聚乙二醇6000为分散剂,去离子水为溶剂,制备复合陶瓷浆料。
设置陶瓷浆料的固含量为68wt%、70wt%、75wt%、80wt%,取10g氧化硅和对应不同固含量(230g、254g、330g、442g)的氧化铝粉末放于烘箱常压干燥,温度设置为110~120℃,干燥时间为12~24h。干燥完全后,用2000目的筛网研磨过筛,取出的氧化硅粉末在分散剂溶液中进行超声预分散10min,超声设备为细胞粉碎机,功率在500W以上。分散剂溶液为0.3g六偏磷酸钠和15g聚乙二醇6000溶解于75mL去离子水制得。
将5.1g海藻酸钠和7.5g聚乙烯吡咯烷酮作为粘结剂加入到分散好的混合有氧化硅和分散剂的悬浊液中均匀混合,在机械搅拌器中以600r/min的转速搅拌30min,再加入烘干的氧化铝粉末,并逐渐提升转速至1200r/min,搅拌2h,放入真空箱去除气泡2h,获得高固含量的3D直写打印陶瓷浆料。
将配置好的浆料装入到料筒内,同时将1mm打印喷头、输料管、活塞连接,整体安装在螺杆推进器上,并且设置好1.2mm打印层厚、200~300mm/s打印速度等相关工艺参数。然后操作主机的预挤功能,向打印料筒中施加压力,进行预挤出处理,以排出在输料管内和料筒内残余的空气。待打印喷头能够出丝连续之后,进行断丝处理。
随后,借助主机辅助设计的三维构图形,自动控制活塞后的螺杆推进器调控挤出速率,使浆料流出,并沉积在按照步进电机移动的X~Y轴成型平台上,从而获得圆柱形三维结构生坯,再将生坯进行热处理,首先在室温下干燥2h,其次放入80℃的鼓风干燥烘箱中保温12h以上。最后,放入1600℃的马弗炉中,在空气气氛下烧结2h即可得到致密氧化铝复合陶瓷。升温制度为室温~500℃以5℃/min的升温速率进行,500℃保温0.5h以去除有机粘结剂,500~1600℃以3℃/min进行,在1600℃保温2h制备得到具有仿生结构高强高韧复合陶瓷。图3为75wt%固含量的3D直写打印陶瓷浆料制备得到的氧化铝复合陶瓷的SEM图。图4为不同固含量3D直写打印陶瓷浆料制备得到的氧化铝复合陶瓷打印样件,其中,75wt%固含量的3D直写打印陶瓷浆料的成型性能最好,打印纹理清晰,层层均匀。
实施例3
采用碳化硅粉末为为微纳米主体材料,以氧化钇、氧化铈为添加物粉体材料,海藻酸钠、聚乙烯吡咯烷酮为粘结剂,六偏磷酸钠和聚乙二醇6000为分散剂,去离子水为溶剂,制备复合陶瓷浆料。
取10g氧化钇、2g氧化铈和330g碳化硅粉末放于烘箱常压干燥,温度设置为110~120℃,干燥时间为12~24h。干燥完全后,用2000目的筛网研磨过筛,随后取出的氧化钇、氧化铈粉末需在分散剂溶液中进行超声预分散10min,超声设备为细胞粉碎机,功率在500W以上。
分散剂溶液为0.3g六偏磷酸钠和15g聚乙二醇6000溶解于75mL去离子水制得。
将5.1g海藻酸钠和7.5g聚乙烯吡咯烷酮作为粘结剂加入分散好的混合有添加物和分散剂的悬浊液中均匀混合,在机械搅拌器中以600r/min的转速搅拌30min,再加入烘干的碳化硅粉末,并且逐渐提升转速至1200r/min,搅拌2h,放入真空箱去除气泡2h,获得高固含量的3D直写打印陶瓷浆料。
将配置好的浆料装入到料筒内,同时将1mm打印喷头、输料管、活塞连接,整体安装在螺杆推进器上,并且设置好1.2mm打印层厚、200~300mm/s打印速度等相关工艺参数。然后操作主机的预挤功能,向打印料筒中施加压力,进行预挤出处理,以排出在输料管内和料筒内残余的空气。待打印喷头能够出丝连续之后,进行断丝处理。
接着,借助主机辅助设计的三维构图形,自动控制活塞后的螺杆推进器调控挤出速率,使浆料流出,并沉积在按照步进电机移动的X~Y轴成型平台上,从而获得圆柱形三维结构生坯,再将生坯进行热处理,首先在室温下干燥2h,其次放入80℃的鼓风干燥烘箱中保温12h以上。最后,放入1600℃的马弗炉中,在空气气氛下烧结2h即可得到致密碳化硅复合陶瓷。升温制度为室温~500℃以5℃/min的升温速率进行,500℃保温0.5h以去除有机粘结剂,500~1600℃以3℃/min进行,在1400℃保温2h。该碳化硅复合陶瓷的抗弯强度为53Mpa,断裂韧性为6Mpa·m0.5。
Claims (7)
1.一种3D直写打印复合陶瓷浆料,其特征在于,包括以下原料:
微纳米主体材料:氧化铝或碳化硅;
添加物粉体材料:氧化硅、氧化钇、氧化铈中的一种或两种;
分散剂:聚乙二醇、硬脂酰胺、六偏磷酸钠中的至少一种;
粘结剂:海藻酸钠、黄原胶、羟甲基纤维素钠、聚乙烯吡咯烷酮中的至少一种;
所述的微纳米主体材料与添加物粉体材料的重量比为20:1~45:1;
所述的分散剂添加量为浆料总重量的0.1~1%;
所述的粘结剂的添加量为浆料总重量的0.2~0.5%;
所述的微纳米主体材料粒径分布为2~10μm,添加物粉体材料粒径分布为80~2000nm;
所述的3D直写打印复合陶瓷浆料的制备方法,包括以下步骤:
(1)将微纳米主体材料和添加物粉体材料干燥,研磨过筛,取出添加物粉体材料加入分散剂溶液中预分散,得到悬浊液;
(2)将粘结剂加入悬浊液中,以600~1000r/min的转速搅拌30~60min搅拌,再加入干燥后的微纳米主体材料粉末,逐渐提升转速至1200~2000r/min,搅拌2~3h,将混匀的浆料放入真空箱进行去除气泡,获得3D直写打印复合陶瓷浆料;
所述的3D直写打印复合陶瓷浆料在1s-1剪切速率下的粘度优选为600~2000Pa·S。
2.根据权利要求1所述的3D直写打印复合陶瓷浆料,其特征在于,所述的分散剂为六偏磷酸钠和聚乙二醇6000的混合物,六偏磷酸钠和聚乙二醇6000的重量比为1:10~1:100。
3.根据权利要求1所述的3D直写打印复合陶瓷浆料,其特征在于,所述的粘结剂为海藻酸钠和聚乙烯吡咯烷酮的混合物,海藻酸钠与聚乙烯吡咯烷酮的重量比为1:0.1~1:10。
4.根据权利要求1-3任一权利所述的3D直写打印复合陶瓷浆料制备得到的具有仿生结构高强高韧复合陶瓷。
5.根据权利要求4所述的具有仿生结构高强高韧复合陶瓷的制备方法,其特征在于,包括:
(1)利用3D直写打印技术将所述的3D直写打印复合陶瓷浆料打印成复合陶瓷生坯;
(2)复合陶瓷生坯在室温下干燥,再放入温度大于80℃的鼓风干燥烘箱中保温12h以上,最后放入设定好升温程序的马弗炉中烧制得到具有仿生结构高强高韧复合陶瓷。
6.根据权利要求5所述的具有仿生结构高强高韧复合陶瓷的制备方法,其特征在于,步骤(1)中的3D直写打印技术参数为:喷嘴直径为1~3mm,打印层厚为1.2~3.6mm,打印速度为200~300mm/min。
7.根据权利要求5所述的具有仿生结构高强高韧复合陶瓷的制备方法,其特征在于,步骤(2)中的升温程序为以5~10℃/min的升温速率,由室温升温至500℃,保温去除有机粘结剂后,在500~1600℃以3~5℃/min升温,空气气氛下烧结2~3h。
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