CN111807843B - 一种轻质高强碳化硅泡沫陶瓷及其制备方法 - Google Patents
一种轻质高强碳化硅泡沫陶瓷及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种轻质高强碳化硅泡沫陶瓷及其制备方法,属于泡沫陶瓷制备技术领域。本发明以聚氨酯泡沫为模板,将高残碳树脂与无水乙醇混合均匀,制成具有不同粘度的浆料。通过挂浆、干燥及热解碳化的步骤得到孔筋结构和强度可控的泡沫碳前驱体,然后通过原位气固碳热还原反应烧结制得轻质高强碳化硅泡沫陶瓷。与传统的模板法比较,本发明通过控制挂浆量调控碳化后泡沫碳骨架的残碳量,从而实现碳化硅泡沫陶瓷制品孔筋结构、孔隙率和强度的控制。该法制备的碳化硅泡沫陶瓷为三维开孔互联网状骨架结构,具有孔筋芯部中空、孔筋壁光滑致密等结构特点,制品具有轻质、高强的特性。
Description
技术领域
本发明属于泡沫陶瓷制备技术领域,具体涉及一种轻质高强碳化硅泡沫陶瓷及其制备方法。
背景技术
碳化硅(SiC)泡沫陶瓷具有高气孔率(70%-95%)、低密度、高比表面积、高渗透性、耐高温、耐腐蚀以及抗氧化性等优异性能,可作为催化剂载体、熔融金属过滤器、复合材料增强相以及人造关节等器/部件使用,广泛应用于过滤催化、保温隔热、生物医疗、电子器件、航空航天和能源化工等领域。
传统有机模板浸渍法制备SiC泡沫陶瓷的实验流程为混料、挂浆、干燥、热解炭化以及烧结,具体浆料组成主要分为两大类。第一类为水系SiC浆料加烧结助剂混料,经烧结制得SiC泡沫陶瓷。如中国专利《一种低温液相烧结碳化硅泡沫陶瓷的制备方法》(申请号201310145115.5,申请公布号CN103253980A,申请公布日2013.8.21)采用碳化硅粉、氧化铝、氧化镁为主要原料,以氧化铝及氧化镁等为烧结助剂,通过液相烧结制得SiC泡沫陶瓷。这种方法在SiC陶瓷中引入烧结助剂虽然可降低烧结温度,但不利于其在生物医疗领域应用,因此极大程度上限制了SiC泡沫陶瓷的应用领域。第二类主要采用反应烧结方法制备SiC泡沫陶瓷并引入烧结助剂提高制品强度。此法可采用聚碳硅烷(PCS)为前驱体进行热解反应获得SiC泡沫陶瓷,或以Si粉和高残碳树脂为原料高温反应烧结制备SiC泡沫陶瓷。然而,以PCS为前驱体制备SiC泡沫陶瓷的原料成本高且制品易收缩开裂;而以Si粉和高残碳树脂为原料进行反应烧结时,由于硅碳反应产生体积收缩,会在SiC泡沫陶瓷孔筋上形成孔洞,导致SiC泡沫陶瓷强度极低。如中国专利《一种高强度碳化硅泡沫陶瓷及其一次挂浆炭化烧结制备方法》(申请号CN201810885523.7,申请公布号CN109133933A,申请公布日2019.1.4)以硅粉和高残碳树脂为主要原料,通过硅粉与高残碳树脂热解碳化后的无定形碳反应烧结制备SiC泡沫陶瓷。此方法主要是依靠反应烧结剩余的残余硅作为粘结剂以及添加烧结助剂来提升SiC泡沫陶瓷的强度,制备工艺较为繁琐,实验成本高且产物易发生成分不均匀的现象。除此以外,烧结助剂的引入也极大程度上限制了SiC泡沫陶瓷的应用领域。
发明内容
为了克服上述现有技术的缺点,本发明的目的在于提供一种轻质高强碳化硅泡沫陶瓷及其制备方法,该方法无须添加烧结助剂,操作简单,实验成本低,易实现工业化生产和应用,而且此法制得的SiC泡沫陶瓷为三维开孔互联网状骨架结构,具有孔筋芯部中空、孔筋壁光滑致密的形貌和结构特征,制品具有轻质高强等特性。
为了达到上述目的,本发明采用以下技术方案予以实现:
本发明公开了一种轻质高强碳化硅泡沫陶瓷的制备方法,包括以下步骤:
1)浆料制备:以高残碳树脂为碳源,无水乙醇为溶剂,将高残碳树脂和无水乙醇以1:(0.3~1)的摩尔比充分混合均匀,制备成粘度为60~350mPa·s的浆料;
2)挂浆:采用聚氨酯泡沫作为模板,将聚氨酯泡沫浸渍于配制好的浆料中,使其充分挂浆,然后排除多余浆料后干燥,制得聚氨酯泡沫前驱体;
3)热解碳化:将聚氨酯泡沫前驱体在惰性气体气氛中,于1000℃热解碳化,得到具有表面致密光滑、芯部中空的三角形孔筋的泡沫碳骨架;
4)烧结:在烧结炉中的坩埚底部铺一层SiO粉,将步骤3)制得的泡沫碳骨架置于坩埚中部,在惰性气体气氛中于1650℃~1850℃保温处理2~6h,使SiO蒸汽与泡沫碳骨架进行原位气固碳热还原反应形成轻质高强碳化硅泡沫陶瓷。
优选地,所述高残碳树脂为环氧树脂、酚醛树脂、氨酚醛树脂、钡酚醛树脂、糠醛树脂、酚糠醛树脂和甲基酚醛树脂中的一种或几种。
优选地,采用的聚氨酯泡沫的规格为20-65PPI。
优选地,步骤2)中,在浸渍过程中充分揉搓聚氨酯泡沫使其充分挂浆,然后通过辊压法排除多余浆料,在室温下自然阴干。
优选地,步骤3)中,热解碳化是在氩气气氛下,自室温起,以1℃/min升温至1000℃,保温2~4h完成的。
优选地,步骤4)中,SiO粉与泡沫碳骨架的质量比为(6~12):1。
优选地,步骤4)中,惰性气体采用氩气,氩气压力为0.2~0.6MPa。
优选地,步骤4)中,烧结是以5℃/min的升温速率从室温升温至1650℃~1850℃。
本发明还公开了采用上述的轻质高强碳化硅泡沫陶瓷的制备方法制得的轻质高强碳化硅泡沫陶瓷,所述轻质高强碳化硅泡沫陶瓷为三维开孔互联网状骨架结构,具有三角形中空孔筋及光滑致密的孔筋壁;且该轻质高强碳化硅泡沫陶瓷的孔径分布均匀且无堵孔,孔径直径为200~350μm,孔筋直径为50~75μm,孔筋壁厚为3~8μm。
优选地,该轻质高强碳化硅泡沫陶瓷的抗压强度为60~80kPa,密度为0.05~0.08g/cm3,气孔率为97.5%~98.5%
与现有技术相比,本发明具有以下有益效果:
本发明公开的轻质高强SiC泡沫陶瓷的原位碳热还原反应制备方法,以聚氨酯泡沫为模板,将高残碳树脂与无水乙醇混合均匀,制成具有不同粘度的浆料,不同粘度的浆料可控制挂浆量。把聚氨酯泡沫模板浸渍在制备好的浆料中充分揉搓浸渍,使浆料均匀涂覆于聚氨酯泡沫模板孔筋表面,排除多余浆料后将泡沫前驱体干燥,然后将泡沫前驱体在氩气气氛下热解碳化,得到具有表面光滑致密、芯部中空的三角形孔筋结构的泡沫碳骨架。最后将泡沫碳骨架置于底部铺放SiO粉的坩埚中,通过原位气固碳热还原反应制得轻质高强SiC泡沫陶瓷。与传统的模板法比较,泡沫碳骨架与SiO蒸气通过原位气固碳热反应生成的SiC泡沫陶瓷为三维开孔互联网状骨架结构,具有孔筋芯部中空、孔筋壁光滑致密等结构特点,因此采用此法制备的SiC泡沫陶瓷具有轻质高强的特性。
进一步地,通过将高残碳树脂与无水乙醇以不同比例均匀混合以调控浆料的粘度,实现挂浆量的调控,进而控制碳化后泡沫碳骨架的残碳量,从而实现SiC泡沫陶瓷制品孔筋结构和强度的控制。除此以外,样品孔径均匀无堵孔、强度高且无烧结助剂、固化剂等添加剂,有利于SiC泡沫陶瓷在生物医疗领域发挥巨大的应用潜力。此法操作简单、实验成本低,可实现工业化大规模应用。
附图说明
图1为坩埚结构示意图。包括:1-炉体;2-坩埚盖;3-坩埚;4-泡沫碳骨架;5-镂空石墨纸支架;6-SiO粉末。
图2为实施例1制备的SiC泡沫陶瓷的宏观形貌照片。
图3为实施例1制备的SiC泡沫陶瓷的XRD。
图4为实施例1制备的SiC泡沫陶瓷的微观形貌照片。
图5为实施例1制备的SiC泡沫陶瓷孔筋断口SEM照片。
具体实施方式
为了使本技术领域的人员更好地理解本发明方案,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的实施例,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,都应当属于本发明保护的范围。
需要说明的是,本发明的说明书和权利要求书及上述附图中的术语“第一”、“第二”等是用于区别类似的对象,而不必用于描述特定的顺序或先后次序。应该理解这样使用的数据在适当情况下可以互换,以便这里描述的本发明的实施例能够以除了在这里图示或描述的那些以外的顺序实施。此外,术语“包括”和“具有”以及他们的任何变形,意图在于覆盖不排他的包含,例如,包含了一系列步骤或单元的过程、方法、系统、产品或设备不必限于清楚地列出的那些步骤或单元,而是可包括没有清楚地列出的或对于这些过程、方法、产品或设备固有的其它步骤或单元。
下面结合附图对本发明做进一步详细描述:
实施例1
按照无水乙醇与酚醛树脂摩尔比1:0.3配制浆料,将50PPI聚氨酯泡沫模板放置在混合均匀的浆料中充分揉搓浸渍,通过辊压法排出多余浆料后把挂好浆的聚氨酯泡沫于室温下阴干24h。将制备好的泡沫前驱体放置在管式炉中,充入氩气,以1℃/min的升温速率升温至1000℃保温2h。把热解碳化好的泡沫碳骨架放置在坩埚中层,在坩埚底部铺一层SiO粉,SiO粉的质量为泡沫碳骨架质量的6倍,然后将坩埚放置在炉体中后通入0.2MPa的氩气气氛压力,以5℃/min的升温速率升温至1750℃,保温4h。
制得的SiC泡沫陶瓷的宏观形貌如图2所示。从图2可看出样品呈灰绿色的多孔形貌,且孔径均匀无堵孔。利用X射线衍射仪(XRD)和扫描电子显微镜对所得产物进行表征。图3是所得SiC泡沫陶瓷的XRD图谱,所有谱峰指标化为β-SiC相,没有出现任何杂质相的谱峰。图4是所得SiC泡沫陶瓷的SEM照片,可见制得的SiC泡沫陶瓷为孔径均匀的三维开孔互联网状骨架结构,孔筋壁上有少量纳米碳化硅晶须生成。图5是所得SiC泡沫陶瓷孔筋断口SEM照片,结果显示SiC泡沫陶瓷的孔筋具有三角形中空结构且孔筋壁光滑致密。因此,本发明可实现一种轻质高强SiC泡沫陶瓷的制备,通过对SiC泡沫陶瓷制品孔筋结构的控制可实现对其孔隙率和强度的调控,有效拓宽了SiC泡沫陶瓷的制备技术及应用领域。
实施例2
按照无水乙醇与酚醛树脂摩尔比1:1配制浆料,将65PPI的聚氨酯泡沫模板放置在混合均匀的浆料中充分揉搓浸渍,通过辊压法排出多余浆料后把挂好浆的聚氨酯泡沫于室温下阴干24h。将制备好的泡沫前驱体放置在管式炉中,充入氩气,以1℃/min的升温速率升温至1000℃保温2h。把热解碳化好的泡沫碳骨架放置在坩埚中层,在坩埚底部铺一层SiO粉,SiO粉的质量为泡沫碳骨架质量的10倍,然后将坩埚放置在炉体中后通入0.6MPa的氩气气氛压力,烧结炉以5℃/min的升温速率升温至1800℃,保温4h。
实施例3
按照无水乙醇与酚醛树脂摩尔比1:0.5配制浆料,将20PPI聚氨酯泡沫模板放置在混合均匀的浆料中充分揉搓浸渍,通过辊压法排出多余浆料后把挂好浆的聚氨酯泡沫于室温下阴干24h。将制备好的泡沫前驱体放置在管式炉中,充入氩气,以1℃/min的升温速率升温至1000℃保温4h。把热解碳化好的泡沫碳骨架放置在坩埚中层,在坩埚底部铺一层SiO粉,SiO粉的质量为泡沫碳骨架质量的8倍,然后将坩埚放置在炉体中后通入0.4MPa的氩气气氛压力,以5℃/min的升温速率升温至1650℃,保温6h。
实施例4
按照无水乙醇与酚醛树脂摩尔比1:0.5配制浆料,将50PPI聚氨酯泡沫模板放置在混合均匀的浆料中充分揉搓浸渍,通过辊压法排出多余浆料后把挂好浆的聚氨酯泡沫于室温下阴干24h。将制备好的泡沫前驱体放置在管式炉中,充入氩气,以1℃/min的升温速率升温至1000℃保温2h。把热解碳化好的泡沫碳骨架放置在坩埚中层,在坩埚底部铺一层SiO粉,SiO粉的质量为泡沫碳骨架质量的10倍,然后将坩埚放置在炉体中后通入0.2MPa的氩气气氛压力,以5℃/min的升温速率升温至1700℃,保温2h。
实施例5
按照无水乙醇与酚醛树脂摩尔比1:0.5配制浆料,将60PPI聚氨酯泡沫模板放置在混合均匀的浆料中充分揉搓浸渍,通过辊压法排出多余浆料后把挂好浆的聚氨酯泡沫于室温下阴干24h。将制备好的泡沫前驱体放置在管式炉中,充入氩气,以1℃/min的升温速率升温至1000℃保温4h。把热解碳化好的泡沫碳骨架放置在坩埚中层,在坩埚底部铺一层SiO粉,SiO粉的质量为泡沫碳骨架质量的12倍,然后将坩埚放置在炉体中后通入0.3MPa的氩气气氛压力,以5℃/min的升温速率升温至1850℃,保温2h。
实施例6
按照无水乙醇与酚醛树脂摩尔比1:0.8配制浆料,将40PPI聚氨酯泡沫模板放置在混合均匀的浆料中充分揉搓浸渍,通过辊压法排出多余浆料后把挂好浆的聚氨酯泡沫于室温下阴干24h。将制备好的泡沫前驱体放置在管式炉中,充入氩气,以1℃/min的升温速率升温至1000℃保温2h。把热解碳化好的泡沫碳骨架放置在坩埚中层,在坩埚底部铺一层SiO粉,SiO粉的质量为泡沫碳骨架质量的8倍,然后将坩埚放置在炉体中后通入0.5MPa的氩气气氛压力,以5℃/min的升温速率升温至1800℃,保温4h。
综上所述,本发明以聚氨酯泡沫为模板,将高残碳树脂与无水乙醇混合均匀,制成具有不同粘度的浆料。通过挂浆、干燥及热解碳化的步骤得到孔筋结构和强度可控的泡沫碳前驱体,然后通过原位气固碳热还原反应烧结制得轻质高强碳化硅泡沫陶瓷。与传统的模板法比较,本发明通过控制挂浆量调控碳化后泡沫碳骨架的残碳量,从而实现碳化硅泡沫陶瓷制品孔筋结构、孔隙率和强度的控制。该法制备的碳化硅泡沫陶瓷为三维开孔互联网状骨架结构,具有孔筋芯部中空、孔筋壁光滑致密等结构特点,制品具有轻质、高强的特性。
本发明上述实施例采用如图1所示的烧结炉坩埚,包括:1-炉体;2-坩埚盖;3-坩埚;4-泡沫碳骨架;5-镂空石墨纸支架;6-SiO粉末。烧结时,在烧结炉中的坩埚底部铺一层SiO粉,将制得的泡沫碳骨架置于坩埚中部,在惰性气体气氛中保温处理,使SiO蒸汽与泡沫碳骨架进行原位气固碳热还原反应形成轻质高强碳化硅泡沫陶瓷。
以上内容仅为说明本发明的技术思想,不能以此限定本发明的保护范围,凡是按照本发明提出的技术思想,在技术方案基础上所做的任何改动,均落入本发明权利要求书的保护范围之内。
Claims (7)
1.一种轻质高强碳化硅泡沫陶瓷的制备方法,其特征在于,包括以下步骤:
1)浆料制备:以高残碳树脂为碳源,无水乙醇为溶剂,将高残碳树脂和无水乙醇以1:(0.3~1)的摩尔比充分混合均匀,制备成粘度为60~350 mPa•s的浆料;高残碳树脂为环氧树脂、酚醛树脂、氨酚醛树脂、钡酚醛树脂、糠醛树脂、酚糠醛树脂和甲基酚醛树脂中的一种或几种;
2)挂浆:采用聚氨酯泡沫作为模板,将聚氨酯泡沫浸渍于配制好的浆料中,充分揉搓聚氨酯泡沫使其充分挂浆,通过辊压法排除多余浆料,在室温下自然阴干,制得聚氨酯泡沫前驱体;
3)热解碳化:将聚氨酯泡沫前驱体在惰性气体气氛中,于1000℃热解碳化,得到具有表面致密光滑、芯部中空的三角形孔筋的泡沫碳骨架;
4)烧结:在烧结炉中的坩埚底部铺一层SiO粉,将步骤3)制得的泡沫碳骨架置于坩埚中部,在惰性气体气氛中于1650℃~1850℃保温处理2~6h,使SiO蒸汽与泡沫碳骨架进行原位气固碳热还原反应形成轻质高强碳化硅泡沫陶瓷。
2.根据权利要求1所述的轻质高强碳化硅泡沫陶瓷的制备方法,其特征在于,采用的聚氨酯泡沫的规格为20-65 PPI。
3.根据权利要求1所述的轻质高强碳化硅泡沫陶瓷的制备方法,其特征在于,步骤3)中,热解碳化是在氩气气氛下,自室温起,以1℃/min升温至1000℃,保温2~4h完成的。
4.根据权利要求1所述的轻质高强碳化硅泡沫陶瓷的制备方法,其特征在于,步骤4)中,SiO粉与泡沫碳骨架的质量比为(6~12):1。
5.根据权利要求1所述的轻质高强碳化硅泡沫陶瓷的制备方法,其特征在于,步骤4)中,惰性气体采用氩气,氩气压力为0.2~0.6 MPa。
6.根据权利要求1所述的轻质高强碳化硅泡沫陶瓷的制备方法,其特征在于,步骤4)中,烧结是以5℃/min的升温速率从室温升温至1650℃~1850℃。
7.采用权利要求1~6中任意一项所述的轻质高强碳化硅泡沫陶瓷的制备方法制得的轻质高强碳化硅泡沫陶瓷,其特征在于,所述轻质高强碳化硅泡沫陶瓷为三维开孔互联网状骨架结构,具有三角形中空孔筋及光滑致密的孔筋壁;且该轻质高强碳化硅泡沫陶瓷的孔径分布均匀且无堵孔,孔径直径为200~350μm,孔筋直径为50~75μm,孔筋壁厚为3~8μm;该轻质高强碳化硅泡沫陶瓷的抗压强度为60~80kPa,密度为0.05~0.08g/cm3,气孔率为97.5%~98.5%。
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