CN109020549A - 一种直写型3D打印机用SiC墨水及其制备方法和应用 - Google Patents
一种直写型3D打印机用SiC墨水及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及一种直写型3D打印机用SiC墨水及其制备方法和应用,所述SiC墨水包括50~67wt%的SiC陶瓷粉体、20~25wt%的碳粉、3~7wt%的粘结剂和10~19wt%的溶剂。本发明的配比所得到的墨水,在直写型3D打印机上,具有成型率高、挤出的丝体的表面光滑、可以较好的达到预期效果。
Description
技术领域
本发明涉及一种直写型3D打印机上所使用的SiC墨水及其制备方法和应用,属于3D打印技术领域。
背景技术
自20世纪90年代,陶瓷素坯加工工艺被提出,这是一种“自上而下”的工艺,利用数控加工技术对陶瓷块状素坯进行三维加工,直接或间接获得各种形状的陶瓷制品,如凝胶注模成型、干压成型和注浆成型等。然而碳化硅陶瓷具有高强度、高硬度、耐腐蚀性等优良的力学、热学、电学性能和化学稳定性,因而在SiC陶瓷成型及加工时,带来很大难度,比如需要借助于复杂的模具来实现,而复杂模具具有很高的技术难度,不但加长了碳化硅陶瓷生产周期,也大大提高制作成本。
发明内容
针对上述问题,本发明旨在提供一种可用于直写型3D打印机的SiC墨水及其制备方法和应用。
一方面,本发明提供了一种直写型3D打印机用SiC墨水,所述SiC墨水包括50~67wt%的SiC陶瓷粉体、20~25wt%的碳粉、3~7wt%的粘结剂和10~19wt%的溶剂。
本发明通过配置粘结剂、碳粉和SiC粉体以及溶剂的比例,混合均匀后,其具有较大固含量,能使其具有剪切变稀的流变特征的胶状物质(当施力挤出时,墨水可流动并挤出,并在挤出后瞬间可固化,从而可以用于直写型3D打印技术)。碳粉的加入,有利于反应烧结制备碳化硅陶瓷。
较佳地,所述SiC墨水包括63~67wt%的SiC陶瓷粉体、20~25wt%的碳粉、3~6wt%的粘结剂和10~15wt%的溶剂。较佳地,所述SiC陶瓷粉体的粒径为300nm~0.8μm。
较佳地,所述碳粉的粒径为200nm~0.3μm。
较佳地,所述溶剂为水或丙醇。
较佳地,所述粘结剂为普罗沙姆、聚乙烯醇、聚乙烯醇缩丁醛和聚乙二醇中的至少一种。
较佳地,所述SiC墨水的屈服应力为800~1100Pa。
另一方面,本发明还提供了一种上述SiC墨水的制备方法,包括:
将粘结剂加入到溶剂中制得粘结剂溶液;
将SiC粉体、碳粉加至所述粘结剂溶液中,在800~2000rpm下离心2~5分钟制得所述SiC墨水。
另一方面,本发明还提供了上述SiC墨水的应用,即、一种3D打印SiC陶瓷的方法,包括:
将所述SiC墨水置于直写型3D打印机中的,用于挤出SiC墨水的针筒中;
将所述针筒于在1000~2000rpm下离心2~5分钟,并进行排泡;
通过施加压力控制SiC墨水的打印速度,再利用3D打印设备中三维立体结构模型,3D打印制备得到陶瓷坯体;
将所得陶瓷坯体干燥后,经反应渗硅得到SiC陶瓷。
本发明利用计算机辅助设计软件可构造出SiC陶瓷素坯的结构,并进行烧结,最终达到产品要求。采用直写型3D打印机,并可根据需求,通过计算机辅助设计制备不同结构的SiC陶瓷,该方法无需模具,具有降低成本、对产品复杂程度敏感度低等优点。
较佳地,所述压力为15~30MPa,打印速度为6~10mm/s。所述在直写型3D打印时,其压力为20MPa,打印速度为8mm/min。
本发明的有益效果:
以此配方中配比得到的墨水,在直写型3D打印机上,具有成型率高、挤出的丝体的表面光滑、可以较好的达到预期效果。
附图说明
图1为本发明实施例1经计算机辅助设计获得的复杂形状的SiC陶瓷素坯的实物照片;
图2为本发明实施例1烧结后获得的最终复杂形状的SiC陶瓷的实物照片。
具体实施方式
以下通过下述实施方式进一步说明本发明,应理解,下述实施方式仅用于说明本发明,而非限制本发明。
本发明通过配置粘结剂和SiC粉体以及水的比例,并在离心机下混合均匀能使其具有剪切变稀的流变特征的胶状物质。所述SiC墨水在其屈服应力处于800-1100Pa之间,墨水的屈服应力为贮能剪切模量和损耗剪切模量的交点所对应的应力大小。
本发明所制备的SiC墨水,所述SiC墨水包括50~67wt%的SiC陶瓷粉体、20~25wt%的碳粉、3~7wt%的粘结剂和10~19wt%的溶剂,所述碳粉和SiC陶瓷粉体的质量比可为1:2~1:4。优选包括63~67wt%的SiC陶瓷粉体、20~25wt%的碳粉(有利于反应烧结制备碳化硅陶瓷)、3~6wt%的粘结剂和10~15wt%的溶剂。所述溶剂可为水或/和丙醇。所述粘结剂可为普罗沙姆、聚乙烯醇、聚乙烯醇缩丁醛和聚乙二醇中的至少一种,优选为普罗沙姆,聚乙烯醇缩丁醛PVB、聚乙烯醇或聚乙二醇PEG600。所述碳粉的粒径可为200nm~0.3μm。所述SiC陶瓷粉体的粒径可为300nm~0.8μm。
以下示例性地说明本发明提供的SiC墨水的制备方法。
将粘结剂与溶剂按比例在一定条件下混合均匀,然后加入SiC粉体和碳粉,并使其均匀混合制成SiC墨水,其固含量可为81~90wt%,当施力挤出时,墨水可流动并挤出,并在挤出后瞬间可固化,从而可以用于直写型3D打印技术。若其总固含量超过90wt%时,挤出墨水容易发生断裂;固含量低于81wt%,打印出的结构容易发生坍塌,不能成型。所述粘结剂在水中混合比例可为15~25wt%,粘结剂在水中混合比例优选可为25wt%。所述部分粘结剂还可在在冰浴条件(具体温度为-5~0℃)下与水混合。本发明中,SiC墨水的混合方法包括但不仅限于离心法、机械搅拌法等。
作为一个示例,将SiC粉体、碳粉、粘结剂与水混合,并在离心机作用(800~2000rpm,例如2000rpm)下离心2~5分钟,使其均匀混合。
本发明制备的SiC墨水,在施加压力时,可以流动并挤出,并且挤出后瞬间固化,逐层打印,最后形成一个碳化硅素坯。碳化硅素坯形状可有计算机辅助设计软件设计,并实现其最终结构。本发明利用计算机辅助设计软件可构造出SiC陶瓷素坯的结构,并进行烧结,最终达到产品要求。
具体来说,将上述SiC墨水置于直写型3D打印机中的用于挤出SiC墨水的针筒中,连着针筒一起在放入离心机进行离心处理(1000~2000rpm,2~5分钟)、并进行排泡。通过施加压力控制SiC墨水的打印速度,再利用3D打印设备中三维立体结构模型,制备得到陶瓷坯体。所述在直写型3D打印时,其压力为15~30MPa,打印速度为6~10mm/s。
将所得陶瓷坯体干燥后,经1350~1700℃反应渗硅2~3小时,得到所述SiC陶瓷。在其反应渗硅过程中加入碳粉可与Si进行反应生成SiC,有利于反应烧结制备碳化硅陶瓷。所述干燥的温度可为20~60℃,时间为24小时。
总的来说,本发明采用碳化硅材料无模成型技术(SFF),该技术是一种“自下而上的生长型”的成型方法,通过计算机程序设计,进行逐层打印,所以也称增材制造、快速成形等等,是近年来全球先进制造领域兴起的一项集机械、计算机、数控和材料于一体的、全新的数字化成形制造技术,它将传统的面向制造工艺的零部件设计变为面向性能的全新设计,被称为当今制造业的一张革命。如此,大大的减少的在加工及模具上的成本。本发明中所得具有较大固含量的浆料可用于直写型3D打印机,并打出SiC素坯。
下面进一步例举实施例以详细说明本发明。同样应理解,以下实施例只用于对本发明进行进一步说明,不能理解为对本发明保护范围的限制,本领域的技术人员根据本发明的上述内容作出的一些非本质的改进和调整均属于本发明的保护范围。下述示例具体的工艺参数等也仅是合适范围中的一个示例,即本领域技术人员可以通过本文的说明做合适的范围内选择,而并非要限定于下文示例的具体数值。若为特殊说明,下述实施例中所用SiC陶瓷粉体的粒径一般为300nm~0.8μm,所述碳粉的粒径一般为200nm~0.3μm。
实施例1
将72gSiC粉体与28g碳粉经球磨均匀混合后,加入到20g粘结剂水溶液(其中,粘结剂为普罗沙姆,其质量分数为20wt%),然后离心机作用下以2000rpm的转速运转5分钟,将制得的墨水放入针管内,再次进行离心混合,进行排泡(以2000rpm的转速运转2分钟),所述SiC墨水的屈服应力为956Pa;
上述墨水,根据计算机辅助设计软件构造SiC陶瓷素坯的结构模型,并在20MPa的气压下,以8mm/min的速度逐层打印形成如图1所示的SiC素坯;
该素坯在1700℃,通过反应渗硅,真空气氛下烧结1h,最后随炉冷却至室温。最终得到具有复杂形状的SiC陶瓷如图2所示。
实施例2
将54gSiC粉体与21g碳粉经球磨均匀混合后,加入到25g粘结剂水溶液(其中,粘结剂为普罗沙姆,其质量分数为23wt%及聚乙烯醇,其质量分数为2wt%),然后离心机作用下以2000rpm的转速运转5分钟,将制得的墨水放入针管内,再次进行离心混合,进行排泡(以2000rpm的转速运转3分钟),所述SiC墨水的屈服应力为1000Pa;
上述墨水,根据计算机辅助设计软件构造SiC陶瓷素坯的结构模型,并在30MPa的气压下,以10mm/min的速度逐层打印形成SiC素坯;
该素坯在1700℃,通过反应渗硅,真空气氛下烧结1h,最后随炉冷却至室温。
实施例3
将75gSiC粉体与25g碳粉经球磨均匀混合后,加入到20g粘结剂水溶液(其中,粘结剂为普罗沙姆,其质量分数为25wt%),然后离心机作用下以2000rpm的转速运转5分钟,将制得的墨水放入针管内,再次进行离心混合,进行排泡(以2000rpm的转速运转2分钟),所述SiC墨水的屈服应力为1050Pa;
上述墨水,根据计算机辅助设计软件构造SiC陶瓷素坯的结构模型,并在30MPa的气压下,以10mm/min的速度逐层打印形成SiC素坯;
该素坯在1700℃,通过反应渗硅,真空气氛下烧结1h,最后随炉冷却至室温。
实施例4
将61.2gSiC粉体与23.8g碳粉经球磨均匀混合后,加入到15g粘结剂水溶液(其中,粘结剂为普罗沙姆,其质量分数为25wt%),然后离心机作用下以2000rpm的转速运转5分钟,将制得的墨水放入针管内,再次进行离心混合,进行排泡(以2000rpm的转速运转2分钟),所述SiC墨水的屈服应力为1000Pa;
上述墨水,根据计算机辅助设计软件构造SiC陶瓷素坯的结构模型,并在30MPa的气压下,以8mm/min的速度逐层打印形成SiC素坯。该素坯在1700℃,通过反应渗硅,真空气氛下烧结1h,最后随炉冷却至室温。
实施例5
将57.6gSiC粉体与22.4g碳粉经球磨均匀混合后,加入到20g粘结剂水溶液(其中,粘结剂为普罗沙姆,质量分数为20wt%),然后离心机作用下以2000rpm的转速运转5分钟,将制得的墨水放入针管内,再次进行离心混合,进行排泡(以2000rpm的转速运转2分钟),所述SiC墨水的屈服应力为900Pa;
上述墨水,根据计算机辅助设计软件构造SiC陶瓷素坯的结构模型,并在30MPa的气压下,以8mm/min的速度逐层打印形成SiC素坯。该素坯在1700℃,通过反应渗硅,真空气氛下烧结1h,最后随炉冷却至室温。
Claims (9)
1.一种直写型3D打印机用SiC墨水,其特征在于,所述SiC墨水包括50~67wt%的SiC陶瓷粉体、20~25wt%的碳粉、3~7wt%的粘结剂和10~19wt%的溶剂。
2.根据权利要求1所述的SiC墨水,所述SiC陶瓷粉体的粒径为300~800nm。
3.根据权利要求1或2所述的SiC墨水,其特征在于,所述碳粉的粒径为200~300 nm。
4.根据权利要求1-3中任一项所述的SiC墨水,其特征在于,所述溶剂为水或丙醇。
5.根据权利要求1-4中任一项所述的SiC墨水,其特征在于,所述粘结剂为普罗沙姆、聚乙烯醇、聚乙烯醇缩丁醛和聚乙二醇中的至少一种。
6.根据权利要求1-5中任一项所述的SiC墨水,其特征在于,所述SiC墨水的屈服应力为800~1100Pa。
7.一种根据权利要求1-6中任一项所述的SiC墨水的制备方法,包括:
将粘结剂加入到溶剂中制得粘结剂溶液;
将SiC粉体、碳粉加至所述粘结剂溶液中,在800~2000rpm下离心2~5分钟制得所述SiC墨水。
8.一种根据权利要求1-6中任一项所述的SiC墨水的应用,其特征在于,包括:
将所述SiC墨水置于直写型3D打印机中的用于挤出SiC墨水的针筒中;
将所述针筒于在1000~2000rpm下离心2~5分钟,并进行排泡;
通过施加压力控制SiC墨水的打印速度,再利用3D打印设备中三维立体结构模型,3D打印制备得到陶瓷坯体;
将所得陶瓷坯体干燥后,经反应渗硅得到SiC陶瓷。
9.根据权利要求8所述的应用,其特征在于,所述压力为15~30MPa,打印速度为6~10mm/s。
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