CN112321318A - 一种基于3d打印技术的聚合物先驱体制多孔磁性陶瓷系统及其制备方法 - Google Patents
一种基于3d打印技术的聚合物先驱体制多孔磁性陶瓷系统及其制备方法 Download PDFInfo
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Abstract
本发明涉及陶瓷材料制备技术领域,具体为一种基于3D打印技术的聚合物先驱体制多孔磁性陶瓷系统,所述系统包括:浆料配置单元、3D打印机和煅烧锅炉;所述浆料配置单元包括:预处理罐和超声搅拌釜;所述预处理罐用于制备改性造孔剂,所述超声搅拌釜用于将改性造孔剂、磁性纳米颗粒、惰性填料与聚合物先驱体加入有机溶剂中进行搅拌混合,并通过超声波处理挥发有机溶剂,得到打印浆料;所述3D打印机利用打印浆料打印得到素胚;所述煅烧锅炉煅烧素胚得到多孔磁性陶瓷。本发明的制备方法,用于制备所述的多孔磁性陶瓷,包括A:浆料配置;B:素胚制备;C:气氛烧结。该发明制备工艺简单、生产成本低,且制备产物经济价值高。
Description
技术领域
本发明涉及陶瓷材料制备技术领域,具体为一种基于3D打印技术的聚合物先驱体制多孔磁性陶瓷系统及其制备方法。
背景技术
聚合物先驱体转化陶瓷将陶瓷前驱体经交联固化处理转化为热固性聚合物,再经高温裂解而制得陶瓷产物。聚合物先驱体转化陶瓷具有特殊的无定形结构,且含有自由碳,具有良好的介电性能,与此同时,还具有陶瓷材料本身具有的抗氧化、耐高温、硬度高等优异性能,因此在雷达及无线电发射设备的吸波领域得到广泛关注,可以防止电磁辐射,减轻电磁污染,保障人体健康和操作安全。
目前,传统性陶瓷的成型方式只能制备于简单形状的陶瓷材料。而随着现代电磁器件趋向于高性能、定制化的方向发展,传统工艺已不能满足多孔陶瓷材料个性化的需求,且生产成本昂贵,产物的经济价值较低。
申请号为CN201910096993.X的中国专利公开了一种3D打印磁性陶瓷的方法及其制备的磁性陶瓷,使用价格便宜的前驱体颗粒粉末为原料,通过将前驱体粉末进行球磨的方式使颗粒更为均匀,并首次使用球磨后前驱体粉末进行3D打印磁性陶瓷。该方法使用粘接剂,使这种3D打印技术存在一定的技术挑战,且只能制备磁性基体的陶瓷如氧化铁陶瓷、碳酸钡陶瓷、碳酸锶陶瓷或碳酸铅陶瓷。
申请号为CN201910961461.8的中国专利公开了一种利用粉煤灰制备球形磁性陶瓷复合微波吸收材料的方法,首先对粉煤灰进行球磨、筛分处理,得到粉煤灰粉,通过缓慢喷入粘结剂和金属盐离子溶液造粒形成粉煤灰基复合微球,接着将复合微球经干燥、还原处理获得负载系列磁性组分的复合微波吸收材料。该方法使用粘接剂,制备的陶瓷可能存在裂纹较多,且无法制备形状复杂的多孔陶瓷。
鉴于此,我们提出一种基于3D打印技术的聚合物先驱体制多孔磁性陶瓷系统及其制备方法。
发明内容
本发明的目的在于提供一种基于3D打印技术的聚合物先驱体制多孔磁性陶瓷系统及其制备方法,以解决上述背景技术中提出的问题。
为实现上述目的,本发明提供如下技术方案:
一种基于3D打印技术的聚合物先驱体制多孔磁性陶瓷系统,所述系统包括:浆料配置单元、3D打印机和煅烧锅炉;
所述浆料配置单元包括:预处理罐和超声搅拌釜;
所述预处理罐用于制备改性造孔剂,
所述超声搅拌釜用于将改性造孔剂、磁性纳米颗粒、惰性填料与聚合物先驱体加入有机溶剂中进行搅拌混合,并通过超声波处理挥发有机溶剂,得到打印浆料;
所述3D打印机利用打印浆料打印得到素胚;
所述煅烧锅炉煅烧素胚得到多孔磁性陶瓷。
本发明还提供一种制备方法,用于制备所述的多孔磁性陶瓷,包括以下步骤:
A:浆料配置
将有机造孔剂倒入预处理罐中,并添加改性剂进行改性,处理得到改性造孔剂;
将改性造孔剂、磁性纳米颗粒、惰性填料与聚合物先驱体加入超声搅拌釜中,并添加有机溶剂进行高速搅拌混合,并通过超声波处理挥发有机溶剂,得到打印浆料;
其中:造孔剂∶纳米磁性颗粒∶惰性填料∶陶瓷先驱体质量比为:5-50∶1-20∶1-20∶50-150,打印浆料在1s-1剪切速率下的粘性为200Pa·s-1500Pa·s;
B:素胚制备
将步骤A中得到的打印浆料置于3D打印机中,并通过墨水直写3D打印得到素胚;
C:气氛烧结
将步骤B得到的素胚置于煅烧锅炉中在30-50℃条件下干燥5-15小时,再在氩气气氛下经500-1200℃恒温烧结0.5-5小时后,随炉冷却至室温得到多孔磁性陶瓷。
优选的,步骤A中,所述有机造孔剂为:淀粉、天然纤维、纳米晶纤维素中的一种或多种混合;
所述改性剂为硅烷偶联剂、琥珀酸酐、氢氧化钠溶液中的一种。
优选的,步骤A中,所述磁性纳米颗粒为:铁、钴、镍的单质或其化合物中的一种或多种混合,磁性纳米颗粒外包裹有聚合物层或二氧化硅层。
优选的,步骤A中,所述惰性填料为:碳化硅粉末、氮化硅粉末、二氧化硅粉末、氧化锆粉末、氧化铝粉末中的一种或多种混合,且所述惰性填料通过表面处理,粒径小于1μm。
优选的,步骤A中,所述聚合物先驱体为:聚碳硅烷、聚硅氧烷、聚硅烷、聚硅氮烷中的一种或多种混合。
优选的,步骤A中,所述有机溶剂为:正己烷、环己烷、异丙醇、二甲苯、四氢呋喃、甲苯中的一种或多种混合。
与现有技术相比,本发明的有益效果是:
(1)通过3D打印直写成型技术可以制备形状结构复杂的多孔磁性陶瓷;
(2)采用聚合物转化陶瓷前驱体具有分子可设计性,转化成陶瓷的温度低的特点,可以通过设计聚合物分子和热解工艺过程来调整所得陶瓷的成分和结构,而且工艺所需温度低,降低制备成本;
(3)通过添加惰性填料调节打印浆料的粘度,实现浆料的可3D打印;
(4)本发明制备的磁性多孔陶瓷不仅具有陶瓷所具备的热稳定性高、抗氧化性强等优势,还具有良好的电磁吸波性能,具有较为广阔的应用前景。
附图说明
图1为本发明实施例1的整体结构框图;
图2为本发明实施例2的工艺流程图。
图中:100、浆料配置单元;101、预处理罐;102、超声搅拌釜;200、3D打印机;300、煅烧锅炉。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
在本专利的描述中,需要说明的是,除非另有明确的规定和限定,术语“安装”、“相连”、“连接”、“设置”应做广义理解,例如,可以是固定相连、设置,也可以是可拆卸连接、设置,或一体地连接、设置。对于本领域的普通技术人员而言,可以根据具体情况理解上述术语在本专利中的具体含义。
实施例1
如图1所示,一种基于3D打印技术的聚合物先驱体制多孔磁性陶瓷系统,系统包括:浆料配置单元100、3D打印机200和煅烧锅炉300;
浆料配置单元100包括:预处理罐101和超声搅拌釜102;
预处理罐101用于制备改性造孔剂,
超声搅拌釜102用于将改性造孔剂、磁性纳米颗粒、惰性填料与聚合物先驱体加入有机溶剂中进行搅拌混合,并通过超声波处理挥发有机溶剂,得到打印浆料;
3D打印机200利用打印浆料打印得到素胚;
煅烧锅炉300煅烧素胚得到多孔磁性陶瓷。
该制备系统结构简单,且工艺流程简易,能充分利用原料的特性制备多孔磁性陶瓷,降低了制备系统的生产成本,便于使用。
实施例2
如图2所示,本发明还提供一种制备方法,用于制备所述的多孔磁性陶瓷,包括以下步骤:
A:浆料配置
将有机造孔剂倒入预处理罐中,并添加改性剂进行改性,处理得到改性造孔剂;
将改性造孔剂、磁性纳米颗粒、惰性填料与聚合物先驱体加入超声搅拌釜中,并添加有机溶剂进行高速搅拌混合,并通过超声波处理挥发有机溶剂,得到打印浆料;
其中:造孔剂∶纳米磁性颗粒∶惰性填料∶陶瓷先驱体质量比为:5-50∶1-20∶1-20∶50-150,打印浆料在1s-1剪切速率下的粘性为200Pa·s-1500Pa·s;
B:素胚制备
将步骤A中得到的打印浆料置于3D打印机中,并通过墨水直写3D打印得到素胚;
C:气氛烧结
将步骤B得到的素胚置于煅烧锅炉中在30-50℃条件下干燥5-15小时,再在氩气气氛下经500-1200℃恒温烧结0.5-5小时后,随炉冷却至室温得到多孔磁性陶瓷。
本实施例中,步骤A中,有机造孔剂为:淀粉、天然纤维、纳米晶纤维素中的一种或多种混合;
改性剂为硅烷偶联剂、琥珀酸酐、氢氧化钠溶液中的一种。
值得说明的是,步骤A中,磁性纳米颗粒为:铁、钴、镍的单质或其化合物中的一种或多种混合,磁性纳米颗粒外包裹有聚合物层或二氧化硅层。
具体的,步骤A中,惰性填料为:碳化硅粉末、氮化硅粉末、二氧化硅粉末、氧化锆粉末、氧化铝粉末中的一种或多种混合,且惰性填料通过表面处理,粒径小于1μm。
除此之外,步骤A中,聚合物先驱体为:聚碳硅烷、聚硅氧烷、聚硅烷、聚硅氮烷中的一种或多种混合。
具体的,步骤A中,有机溶剂为正己烷、环己烷、异丙醇、二甲苯、四氢呋喃、甲苯中的一种或多种混合。
实施例3
制备所述的多孔磁性陶瓷,包括以下步骤:
A:浆料配置
用硅烷偶联剂KH570对纳米晶纤维素进行预处理得到改性纳米晶纤维素;
将改性纳米晶纤维素、表面包覆有硅烷的三氧化四铁纳米颗粒、碳化硅粉末与聚碳硅烷加入正己烷中高速搅拌混合,再超声处理,挥发部分有机溶剂得到打印浆料;
其中:改性纳米晶纤维素、表面包覆有硅烷的三氧化四铁纳米颗粒、碳化硅粉末与聚碳硅烷质量比为:20∶6∶12:120,打印浆料在1s-1剪切速率下的粘性为656Pa·s;
B:素胚制备:将打印浆料置于3D打印机中通过墨水直写3D打印得到素胚;
C:气氛烧结:将素胚置于烘箱中在35℃条件下干燥10小时,再在氩气气氛下经1100℃下烧结3小时后随炉冷却至室温得到多孔磁性陶瓷。
得到的多孔磁性陶瓷性能测试结果见表1
实施例4
制备所述的多孔磁性陶瓷,包括以下步骤:
A:浆料配置:
用琥珀酸酐对淀粉进行预处理得到改性淀粉;
将改性淀粉、表面包覆有二氧化硅的氧化钴纳米颗粒、氮化硅粉末与聚硅氮烷加入异丙醇中高速搅拌混合,再超声处理,挥发部分有机溶剂得到打印浆料;
其中:改性淀粉、表面包覆有二氧化硅的氧化钴纳米颗粒、氮化硅粉末与聚硅氮烷质量比为:6∶9∶15:100,打印浆料在1s-1剪切速率下的粘性为882Pa·s;
B:素胚制备:将打印浆料置于3D打印机中通过墨水直写3D打印得到素胚;
C:气氛烧结:将素胚置于烘箱中在35℃条件下干燥13小时,再在氩气气氛下经1150℃下烧结5小时后随炉冷却至室温。
得到的多孔磁性陶瓷性能测试结果见表1
实施例5
制备所述的多孔磁性陶瓷,包括以下步骤:
A:浆料配置:用氢氧化钠溶液对聚甲基丙烯酸甲酯(PMMA)微球进行预处理得到改性PMMA微球;
将改性淀粉、表面包覆有二氧化硅的氧化钴纳米颗粒、氮化硅粉末与聚硅氮烷加入环己烷中高速搅拌混合,再超声处理,挥发部分有机溶剂得到打印浆料;
其中:改性PMMA微球、表面包覆聚苯乙烯的镍纳米颗粒、二氧化硅粉末与聚硅氧烷质量比为:20∶7∶12:150,打印浆料在1s-1剪切速率下的粘性为1137Pa·s;
B:素胚制备:将打印浆料置于3D打印机中通过墨水直写3D打印得到素胚;
C:气氛烧结:将素胚置于烘箱中在46℃条件下干燥6小时,再在氩气气氛下经1200℃下烧结2小时后随炉冷却至室温。
得到的多孔磁性陶瓷性能测试结果见表1
表1
通过上述内容不难看出,本发明的基于3D打印技术的聚合物先驱体制多孔磁性陶瓷系统及其制备方法:
(1)通过3D打印直写成型技术可以制备形状结构复杂的多孔磁性陶瓷;
(2)采用聚合物转化陶瓷前驱体具有分子可设计性,转化成陶瓷的温度低的特点,可以通过设计聚合物分子和热解工艺过程来调整所得陶瓷的成分和结构,而且工艺所需温度低;
(3)通过添加惰性填料调节打印浆料的粘度,实现浆料的可3D打印;
(4)本发明制备的磁性多孔陶瓷不仅具有陶瓷所具备的热稳定性高、抗氧化性强等优势,还具有良好的电磁吸波性能,具有较为广阔的应用前景。
以上显示和描述了本发明的基本原理、主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的仅为本发明的优选例,并不用来限制本发明,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (7)
1.一种基于3D打印技术的聚合物先驱体制多孔磁性陶瓷系统,其特征在于,所述系统包括:浆料配置单元、3D打印机和煅烧锅炉;
所述浆料配置单元包括:预处理罐和超声搅拌釜;
所述预处理罐用于制备改性造孔剂,
所述超声搅拌釜用于将改性造孔剂、磁性纳米颗粒、惰性填料与聚合物先驱体加入有机溶剂中进行搅拌混合,并通过超声波处理挥发有机溶剂,得到打印浆料;
所述3D打印机利用打印浆料打印得到素胚;
所述煅烧锅炉煅烧素胚得到多孔磁性陶瓷。
2.一种制备方法,用于制备权利要求1所述的多孔磁性陶瓷,其特征在于,包括以下步骤:
A:浆料配置
将有机造孔剂倒入预处理罐中,并添加改性剂进行改性,处理得到改性造孔剂;
将改性造孔剂、磁性纳米颗粒、惰性填料与聚合物先驱体加入超声搅拌釜中,并添加有机溶剂进行高速搅拌混合,并通过超声波处理挥发有机溶剂,得到打印浆料;
其中:造孔剂∶纳米磁性颗粒∶惰性填料∶陶瓷先驱体质量比为:5-50∶1-20∶1-20∶50-150,打印浆料在1s-1剪切速率下的粘性为200Pa·s-1500Pa·s;
B:素胚制备
将步骤A中得到的打印浆料置于3D打印机中,并通过墨水直写3D打印得到素胚;
C:气氛烧结
将步骤B得到的素胚置于煅烧锅炉中在30-50℃条件下干燥5-15小时,再在氩气气氛下经500-1200℃恒温烧结0.5-5小时后,随炉冷却至室温得到多孔磁性陶瓷。
3.根据权利要求2所述的制备方法,其特征在于:步骤A中,所述有机造孔剂为:淀粉、天然纤维、纳米晶纤维素中的一种或多种混合;
所述改性剂为硅烷偶联剂、琥珀酸酐、氢氧化钠溶液中的一种。
4.根据权利要求2所述的制备方法,其特征在于:步骤A中,所述磁性纳米颗粒为:铁、钴、镍的单质或其化合物中的一种或多种混合,磁性纳米颗粒外包裹有聚合物层或二氧化硅层。
5.根据权利要求2所述的制备方法,其特征在于:步骤A中,所述惰性填料为:碳化硅粉末、氮化硅粉末、二氧化硅粉末、氧化锆粉末、氧化铝粉末中的一种或多种混合,且所述惰性填料通过表面处理,粒径小于1μm。
6.根据权利要求2所述的制备方法,其特征在于:步骤A中,所述聚合物先驱体为:聚碳硅烷、聚硅氧烷、聚硅烷、聚硅氮烷中的一种或多种混合。
7.根据权利要求2所述的制备方法,其特征在于:步骤A中,所述有机溶剂为:正己烷、环己烷、异丙醇、二甲苯、四氢呋喃、甲苯中的一种或多种混合。
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