CN112707738A - 整体有序-局部无序多孔陶瓷及其制备方法 - Google Patents
整体有序-局部无序多孔陶瓷及其制备方法 Download PDFInfo
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Abstract
本申请涉及多孔材料领域,涉及一种整体有序‑局部无序多孔陶瓷及其制备方法。该方法包括以粘接有有机粘接材料的陶瓷粉末为原料,按照预设的路径进行打印构筑,得到包含多个有序孔的多孔材料;然后,将打印得到的多孔材料中的有机粘接材料去除,并在多孔材料中留下无序孔,得到多孔陶瓷材料;将多孔陶瓷材料进行烧结。按照预设的路径进行打印构筑,使得整个多孔陶瓷内部的孔按照预设的有序路径进行排列,从而实现整体有序的效果。然后将多孔材料中的有机粘接材料去除后,原来的有机粘接材料所在的位置成为新的孔。由于有机粘接材料在多孔材料中的位置是无序的,因此能够使得多孔陶瓷中的局部出现无序孔,进而获得整体有序‑局部无序的多孔陶瓷。
Description
技术领域
本申请涉及多孔材料领域,具体而言,涉及一种整体有序-局部无序多孔陶瓷及其制备方法。
背景技术
目前公开报道了多种制备多孔陶瓷的方法,包括泡沫模板法、模具成型法、造孔剂法、光固化3D打印法。
泡沫模板法,主要步骤为将含有粉末的陶瓷浆料涂覆在具有多孔结构的有机泡沫模板上,干燥后烧掉有机泡沫模板获得多孔陶瓷;
模具成型法,主要步骤为将陶瓷粉末、烧结助剂等造粒,然后将造粒料填入模具中,采用压力成型工艺得到成型坯件,放入气氛炉中,在气氛下烧结,获得多孔陶瓷;
造孔剂法,主要步骤为将陶瓷粉末与造孔剂混合在一起,而后将造孔剂通过烧结或溶解的方法去处,得到多孔陶瓷。
光固化3D打印法,主要步骤为以陶瓷粉末和光敏树脂为主要起始原料,通过激光选择固化制造多孔陶瓷。
然而,上述的泡沫模板法、模具成型法和造孔剂法制备的多孔陶瓷都是无序结构,孔结构均为随机分布,无法设计。而上述的光固化3D打印法制备的多孔陶瓷无法实现整体有序,局部无序结构的多孔陶瓷。
发明内容
本申请实施例的目的在于提供一种整体有序-局部无序多孔陶瓷及其制备方法。
第一方面,本申请提供一种整体有序-局部无序多孔陶瓷的制备方法,包括:
以粘接有有机粘接材料的陶瓷粉末为原料,按照预设的路径进行打印构筑,得到包含多个有序孔的多孔材料;
然后,将打印得到的多孔材料中的有机粘接材料去除,并在多孔材料中留下无序孔,得到多孔陶瓷材料;
将多孔陶瓷材料进行烧结。
本申请的方法,能够按照预设的路径进行打印构筑,能够得到包含多个有序孔的多孔材料,使得整个多孔陶瓷内部的孔按照预设的有序路径进行排列,从而实现整体有序的效果。然后将包含多个有序孔的多孔材料中的有机粘接材料去除后,原来的有机粘接材料所在的位置成为新的孔。由于有机粘接材料在多孔材料中的位置是无序的,因此能够使得多孔陶瓷中的局部出现无序孔,进而获得整体有序-局部无序的多孔陶瓷。
在本申请的其他实施例中,上述预设的路径是采用三维建模软件进行多孔材料结构设计得到;
可选地,多孔材料的整体形状包括:立方体、正十二面体、正四面体或者圆柱体中的任意一种;
可选地,有序孔的形状选择方形孔。
在本申请的其他实施例中,上述有序孔的孔径尺度在10μm~10mm范围内。
在本申请的其他实施例中,上述打印构筑是在加热的条件下,使原料中的有机粘接材料熔化,得到陶瓷浆料,采用陶瓷浆料进行打印。
在本申请的其他实施例中,上述加热的温度在120-300℃。
在本申请的其他实施例中,上述原料按照以下步骤制得:
将陶瓷粉末和有机粘接材料在加热条件下混合均匀,使有机粘接材料与陶瓷粉末粘接在一起,然后进行破碎;
可选地,原料的粒径破碎在0.1-5mm范围内;
可选地,加热温度120-300℃。
在本申请的其他实施例中,上述陶瓷粉末的粒度范围为50nm~10μm。
在本申请的其他实施例中,上述按照体积比计,原料中陶瓷粉末35%~70%且有机粘接材料30%~65%;
可选地,陶瓷粉末包括:氧化锆、氧化铝、碳化硅、氮化硅、硼化锆或者钛铝碳中的至少一种;
可选地,按照体积比计,有机粘接材料包括:1%~3%表面活性剂,34%~65%高分子大骨架材料,3%~8%增塑剂,25%~55%润滑剂;
可选地,表面活性剂选择硬脂酸;
可选地,高分子大骨架材料包括聚乙烯和聚丙烯中的一种或者两种;可选地,当高分子大骨架材料同时包括聚乙烯和聚丙烯时,聚乙烯占有机粘接材料的体积比为15%~35%,聚丙烯占有机粘接材料的体积比为15%~30%;
可选地,增塑剂选择聚乙二醇;
可选地,润滑剂选择石蜡。
在本申请的其他实施例中,上述将打印得到的多孔材料中的有机粘接材料去除的步骤,包括:
将多孔材料进行微波加热处理。
第二方面,本申请提供一种整体有序-局部无序多孔陶瓷,该多孔陶瓷内部包含多个有序孔和多个无序孔;
可选地,有序孔尺度范围为10μm~10mm;无序孔尺度范围为50nm~300nm;
可选地,多孔陶瓷的孔隙率在20%~90%范围内。
该多孔陶瓷具有整体有序-局部无序的结构,孔隙率分布范围广,可设计范围广。
附图说明
为了更清楚地说明本申请实施例的技术方案,下面将对实施例中所需要使用的附图作简单地介绍,应当理解,以下附图仅示出了本申请的某些实施例,因此不应被看作是对范围的限定,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他相关的附图。
图1为本申请实施例1提供的整体有序-局部无序多孔陶瓷的宏观图片;
图2为本申请实施例1提供的整体有序-局部无序多孔陶瓷的局部无序孔的扫描电镜图。
具体实施方式
为使本申请实施例的目的、技术方案和优点更加清楚,下面将对本申请实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本申请一部分实施例,而不是全部的实施例。
此外,术语“第一”、“第二”等仅用于区分描述,而不能理解为指示或暗示相对重要性。
本申请实施方式提供了一种整体有序-局部无序多孔陶瓷的制备方法,包括以下步骤:
步骤S1、以粘接有有机粘接材料的陶瓷粉末为原料,按照预设的路径进行打印构筑,得到包含多个有序孔的多孔材料。
进一步地,在本申请一些实施方式中,上述的原料是按照以下步骤制得的:
将陶瓷粉末和有机粘接材料在加热条件下混合搅拌至均匀,使得有机粘接材料与陶瓷粉末粘接在一起。然后将粘接在一起的较大粒径的物料破碎为粒径在0.1-5mm范围内的颗粒状原料。
进一步地,原料的粒径在0.1-5mm。
进一步可选地,原料的粒径在0.2-4.9mm。
进一步可选地,原料的粒径在0.5-4.0mm。
示例性地,上述原料的粒径为0.8mm、1.0mm、1.5mm、2.0mm、2.5mm、3.0mm或者3.5mm。
进一步可选地,上述将陶瓷粉末和有机粘接材料在加热条件下混合的加热温度是120~300℃范围内。
进一步可选地,上述将陶瓷粉末和有机粘接材料在加热条件下混合的加热温度是130~290℃范围内。
进一步可选地,上述将陶瓷粉末和有机粘接材料在加热条件下混合的加热温度是140~280℃范围内。
示例性地,上述将陶瓷粉末和有机粘接材料在加热条件下混合的加热温度为150℃、160℃、170℃、180℃、190℃、200℃、220℃或者250℃。
进一步地,上述的陶瓷粉末包括:氧化锆、氧化铝、碳化硅、氮化硅、硼化锆或者钛铝碳中的至少一种。
示例性地,在本申请一些实施方式中,上述的陶瓷粉末为氧化锆、氧化铝、碳化硅、氮化硅、硼化锆或者钛铝碳中的一个。
示例性地,在本申请一些实施方式中,上述的陶瓷粉末为氧化锆和氧化铝。
示例性地,在本申请一些实施方式中,上述的陶瓷粉末为氧化锆、氧化铝、碳化硅、氮化硅、硼化锆以及钛铝碳。
进一步地,上述的陶瓷粉末的粒度范围为50nm~10μm。
进一步可选地,上述的陶瓷粉末的粒度范围为60nm~9μm。
进一步可选地,上述的陶瓷粉末的粒度范围为70nm~8μm。
示例性地,上述的陶瓷粉末的粒度为70nm、100nm、1μm、2μm、3μm、4μm、5μm或者6μm。
进一步地,按照体积比计,原料中陶瓷粉末35%~70%;有机粘接材料30%~65%。
进一步可选地,按照体积比计,原料中陶瓷粉末36%~69%;有机粘接材料31%~64%。
进一步可选地,按照体积比计,原料中陶瓷粉末36%~69%;有机粘接材料32%~63%。
示例性地,按照体积比计,原料中陶瓷粉末40%;有机粘接材料60%。或者,按照体积比计,原料中陶瓷粉末45%;有机粘接材料55%。或者,按照体积比计,原料中陶瓷粉末50%;有机粘接材料50%。或者,按照体积比计,原料中陶瓷粉末60%;有机粘接材料40%。
进一步地,按照体积比计,有机粘接材料包括:1%~3%表面活性剂,34%~65%高分子大骨架材料,3%~8%增塑剂,25%~55%润滑剂。
进一步可选地,按照体积比计,有机粘接材料包括:1.1%~2.9%表面活性剂,35%~64%高分子大骨架材料,3.1%~7.9%增塑剂,26%~54%润滑剂。
进一步可选地,按照体积比计,有机粘接材料包括:1.2%~2.8%表面活性剂,40%~55%高分子大骨架材料,3.2%~7.8%增塑剂,28%~53%润滑剂。
进一步可选地,在本申请一些实施方式中,上述的表面活性剂选择硬脂酸。
进一步可选地,在本申请一些实施方式中,上述的高分子大骨架材料包括聚乙烯和聚丙烯中的一种或者两种;可选地,当高分子大骨架材料同时包括聚乙烯和聚丙烯时,聚乙烯占有机粘接材料的体积比为15%~35%,聚丙烯占有机粘接材料的体积比为15%~30%。
进一步可选地,当高分子大骨架材料同时包括聚乙烯和聚丙烯时,聚乙烯占有机粘接材料的体积比为16%~34%,聚丙烯占有机粘接材料的体积比为16%~31%。通过将上述的高分子大骨架材料选择同时包括聚乙烯和聚丙烯,由于二者的分子量一个较大,一个较小,因此,同时存在时能够起到协同增效的作用,从而提高粘接效果,进而提高陶瓷粉末与有机粘接材料的成型均匀性。
进一步可选地,在本申请一些实施方式中,上述的增塑剂选择聚乙二醇。
进一步可选地,在本申请一些实施方式中,上述的润滑剂选择石蜡。
进一步地,在本申请一些实施方式中,上述按照预设的路径进行打印构筑的步骤包括:
采用三维建模软件进行多孔材料结构设计得到预设的路径。
进一步地,采用三维建模软件进行多孔材料结构设计时可以选择将整个多孔陶瓷的整体形状设计为规则形状,示例性地,立方体、正十二面体、正四面体或者圆柱体等。
进一步地,采用三维建模软件进行多孔材料结构设计时可以选择将规则形状的多孔陶瓷内部的有序孔的形状设计为方形孔等。
进一步地,有序孔的孔径尺度设计在10μm~10mm范围内。
进一步可选地,有序孔的孔径尺度设计在11μm~9mm范围内。
进一步可选地,有序孔的孔径尺度设计在12μm~8mm范围内。
示例性地,有序孔的孔径尺度设计50μm、100μm、500μm、1mm、2mm、3mm、4mm、5mm、6mm或者7mm等。
进一步地,按照预设的路径进行打印构筑的步骤包括:
在加热的条件下,使原料中的有机粘接材料熔化,得到陶瓷浆料,采用陶瓷浆料进行打印。
进一步可选地,上述加热的条件的加热温度在120-300℃范围内。
进一步可选地,上述加热的条件的加热温度在150-280℃范围内。
进一步可选地,上述加热的条件的加热温度在180-250℃范围内。
示例性地,上述加热的条件的加热温度为190℃、200℃、210℃、220℃、230℃、240℃或者250℃。
在本申请一些实施方式中,按照预设的路径进行打印构筑是将前述制得的颗粒状原料导入设备(例如3D打印设备)料仓内,而后通过设备的送料系统将颗粒状原料运输至样品构筑机构(例如3D打印设备的喷嘴等),随后对构筑机构进行加热,温度为120-300℃,使得原料熔化,从构筑机构流出,然后按照前述预设的路径的进行打印构筑,得到包含多个有序孔的多孔材料。
步骤S2、然后,将打印得到的多孔材料中的有机粘接材料去除,使多孔材料局部形成多个无序孔,得到多孔陶瓷材料。
进一步地,将打印得到的多孔材料中的有机粘接材料去除的步骤,包括:
将多孔材料进行微波加热处理,去除有机粘接材料。
通过对上述的多孔材料进行微波加热处理,能够将制得的多孔材料中的有机材料去除,并在多孔材料中留下无序孔,从而使得多孔材料的局部出现无序孔。
进一步地,在本申请其他可选的实施方式中,也可以采用其他的加热方式去除有机粘接材料。
进一步地,在本申请一些实施方式中,上述的微波处理的时间为10~30分钟。
进一步可选地,在本申请一些实施方式中,上述的微波处理的时间为15~25分钟。
示例性地,在本申请一些实施方式中,上述的微波处理的时间为16分钟、17分钟、18分钟、19分钟、20分钟、21分钟、22分钟、23分钟、24分钟或者25分钟。
步骤S3、将多孔陶瓷材料进行烧结。
烧结按照陶瓷材料需要的烧结温度进行烧结即可。烧结工艺可采用本领域对应的陶瓷材料常规烧结工艺。
通过将上述的多孔陶瓷材料进行烧结,能够得到整体有序-局部无序多孔陶瓷。
采用该方法制备的整体有序-局部无序多孔陶瓷其孔隙率在20%~90%范围内。
本申请一些实施方式还提供一种整体有序-局部无序多孔陶瓷,该整体有序-局部无序多孔陶瓷能够采用前述实施方式提供的整体有序-局部无序多孔陶瓷的制备方法制得。
进一步地,该多孔陶瓷内部包含多个有序孔和多个无序孔。
进一步地,该多孔陶瓷的有序孔尺度范围为10μm~10mm;无序孔尺度范围为50nm~300nm。
进一步地,该多孔陶瓷的孔隙率在20%~90%范围内。
进一步可选地,该多孔陶瓷的孔隙率在21%~89%范围内。
进一步可选地,该多孔陶瓷的孔隙率在22%~88%范围内。
示例性地,该多孔陶瓷的孔隙率为25%、30%、35%、40%、45%、50%、55%、60%、65%、70%、75%、80%或者85%。
以下结合实施例对本申请的特征和性能作进一步的详细描述:
实施例1
提供一种整体有序-局部无序多孔陶瓷,按照以下步骤制备:
粒度为3μm的氧化锆80g,石蜡8g、聚乙烯6g、聚丙烯3.5g、聚乙二醇2g、硬脂酸0.5g,在160℃加热混合搅拌至均匀,然后进行破碎,得到粒径为2mm的颗粒状原料。采用三维建模软件进行多孔材料结构设计,有序孔的孔径为2mm,多孔材料的形状为立方体结构。然后将制备的氧化锆颗粒状原料导入打印设备的料仓内,而后通过送料系统将颗粒料运输至样品构筑机构,随后将构筑机构加热至160℃,喂入氧化锆颗粒状原料并熔化,从构筑机构流出,按设计的模型进行打印构筑得到孔结构有序的多孔陶瓷构筑体。对多孔陶瓷构筑体进行微波处理20分钟,将有机粘接剂去除,并对陶瓷构筑体进行烧结,得到整体有序-局部无序多孔陶瓷。
制得的整体有序-局部无序多孔陶瓷的宏观图片如说明书附图1所示;对该整体有序-局部无序多孔陶瓷的局部无序孔采用扫面电镜进行观察,结果如说明书附图2所示。
从图1可以看出,制得的多孔陶瓷整体成立方体结构,其内部具有多个有序的方形孔。从图2可以看出,制得的多孔陶瓷的微观结构中存在多个无序孔,由此说明制得的多孔陶瓷具有整体有序、局部无序的多孔结构。
实施例2
提供一种整体有序-局部无序多孔陶瓷,其与实施例1制备步骤相同,所不同之处在于原料组成以及多孔结构设计,具体如下:
粒度为5μm的氧化铝78.2g,石蜡9.5g、聚乙烯5.5g、聚丙烯4.5g、聚乙二醇1.8g、硬脂酸0.5g,在160℃加热混合搅拌至均匀,然后进行破碎,得到粒径为1mm的颗粒状原料。采用三维建模软件进行多孔材料结构设计,有序孔的孔径为1mm,多孔材料的形状为正十二面体结构。
实施例3
提供一种整体有序-局部无序多孔陶瓷,其与实施例1制备步骤相同,所不同之处在于原料组成以及多孔结构设计,具体如下:
粒度为5μm的氮化硅75.5g,石蜡10g、聚乙烯7.5g、聚丙烯4g、聚乙二醇2g、硬脂酸1g,在160℃加热混合搅拌至均匀,然后进行破碎,得到粒径为2mm的颗粒状原料。采用三维建模软件进行多孔材料结构设计,有序孔的孔径为3mm,多孔材料的形状为正四面体结构。
实施例2和3制得的多孔陶瓷也具有与实施例1类似的整体有序、局部无序的结构。
以上所述仅为本申请的优选实施例而已,并不用于限制本申请,对于本领域的技术人员来说,本申请可以有各种更改和变化。凡在本申请的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本申请的保护范围之内。
Claims (10)
1.一种整体有序-局部无序多孔陶瓷的制备方法,其特征在于,包括:
以粘接有有机粘接材料的陶瓷粉末为原料,按照预设的路径进行打印构筑,得到包含多个有序孔的多孔材料;
然后,将打印得到的所述多孔材料中的所述有机粘接材料去除,并在多孔材料中留下无序孔,得到多孔陶瓷材料;
将所述多孔陶瓷材料进行烧结。
2.根据权利要求1所述的整体有序-局部无序多孔陶瓷的制备方法,其特征在于,
所述预设的路径是采用三维建模软件进行所述多孔材料结构设计得到;
可选地,所述多孔材料的整体形状包括:立方体、正十二面体、正四面体或者圆柱体中的任意一种;
可选地,所述有序孔的形状选择方形孔。
3.根据权利要求2所述的整体有序-局部无序多孔陶瓷的制备方法,其特征在于,
所述有序孔的孔径尺度在10μm~10mm范围内。
4.根据权利要求1所述的整体有序-局部无序多孔陶瓷的制备方法,其特征在于,
所述打印构筑是在加热的条件下,使所述原料中的所述有机粘接材料熔化,得到陶瓷浆料,采用所述陶瓷浆料进行打印。
5.根据权利要求4所述的整体有序-局部无序多孔陶瓷的制备方法,其特征在于,
所述加热的温度在120-300℃。
6.根据权利要求1所述的整体有序-局部无序多孔陶瓷的制备方法,其特征在于,
所述原料按照以下步骤制得:
将所述陶瓷粉末和所述有机粘接材料在加热条件下混合均匀,使所述有机粘接材料与所述陶瓷粉末粘接在一起,然后进行破碎;
可选地,所述原料的粒径破碎在0.1-5mm范围内;
可选地,加热温度120-300℃。
7.根据权利要求6所述的整体有序-局部无序多孔陶瓷的制备方法,其特征在于,
所述陶瓷粉末的粒度范围为50nm~10μm。
8.根据权利要求6所述的整体有序-局部无序多孔陶瓷的制备方法,其特征在于,
按照体积比计,所述原料中陶瓷粉末35%~70%且所述有机粘接材料30%~65%;
可选地,所述陶瓷粉末包括:氧化锆、氧化铝、碳化硅、氮化硅、硼化锆或者钛铝碳中的至少一种;
可选地,按照体积比计,所述有机粘接材料包括:1%~3%表面活性剂,34%~65%高分子大骨架材料,3%~8%增塑剂,25%~55%润滑剂;
可选地,所述表面活性剂选择硬脂酸;
可选地,所述高分子大骨架材料包括聚乙烯和聚丙烯中的一种或者两种;可选地,当所述高分子大骨架材料同时包括所述聚乙烯和所述聚丙烯时,所述聚乙烯占所述有机粘接材料的体积比为15%~35%,所述聚丙烯占所述有机粘接材料的体积比为15%~30%;
可选地,所述增塑剂选择聚乙二醇;
可选地,所述润滑剂选择石蜡。
9.根据权利要求1-8任一项所述的整体有序-局部无序多孔陶瓷的制备方法,其特征在于,
所述将打印得到的所述多孔材料中的所述有机粘接材料去除的步骤,包括:
将所述多孔材料进行微波加热处理。
10.一种整体有序-局部无序多孔陶瓷,其特征在于,所述多孔陶瓷内部包含多个有序孔和多个无序孔;
可选地,所述有序孔尺度范围为10μm~10mm;所述无序孔尺度范围为50nm~300nm;
可选地,所述多孔陶瓷的孔隙率在20%~90%范围内。
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