CN112592188A - 一种石墨烯复合碳化硅陶瓷材料的制备方法 - Google Patents
一种石墨烯复合碳化硅陶瓷材料的制备方法 Download PDFInfo
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Abstract
本发明提供一种石墨烯复合碳化硅陶瓷材料的制备方法,通过在有机分散剂中将石墨烯进行分散,确保形成均匀稳定的单层石墨烯结构,将石墨烯纳米片同粉体混合成型,并在表面附着高纯硅微粉,在复合陶瓷的烧结阶段,液态硅通过毛管压力将多孔的SiC/C预成型体浸润。炭黑与液态硅反应形成二次β‑SiC,它与初始的α‑SiC颗粒强力结合,形成陶瓷的三维骨架,达到增强、增韧的目的,显著提升了碳化硅材料的力学性能。
Description
技术领域
本发明涉及石墨烯复合陶瓷材料领域,具体地说是一种石墨烯复合碳化硅陶瓷材料的制备方法。
背景技术
碳化硅陶瓷具有高强度、高硬度、高导热系数、低热膨胀系数和优异的化学稳定性的特点,是一种具有优异性能结构陶瓷,可作为热交换器、热辐射管、电偶保护管、柱塞等广泛应用于冶金、电力、机械等工业领域,但较低的韧性导致碳化硅陶瓷的应用范围受限。目前的研究大多是采用第二相增强方法来提高碳化硅陶瓷的力学性能,增韧效果不明显,不易工业化推广应用。
石墨烯是一种由单层碳原子紧密堆积成二维蜂窝状晶格结构的新材料,以六边形周期排列形成的二维蜂窝状晶格结构的无机纳米片层材料,其独特的晶体结构特性使其拥有优异的机械性能、电学性能和热学性能。
若能通过一定的工艺方法,使片状的石墨烯均匀分布到陶瓷材料基体中,可增强裂纹在三维方向上的扩展,出现裂纹桥接、裂纹拔出和强化分层等增韧机制,使复合陶瓷的力学性能增强。
在已有的公开报道的研究进展中,石墨烯复合碳化硅陶瓷材料的制备方式主要有两种:一种是将石墨烯与陶瓷材料粉体直接进行混合,此种工艺易造成石墨烯分散不均,导致石墨烯团聚,从而导致复合材料整体性能降低;一种是将石墨烯材料制成悬浊液,将陶瓷生胚放入其中加压浸渍,此种工艺过程复杂,且浸渍会形成浓度梯度,从而导致复合材料整体性能降低。
专利号CN109704777A公开了一种石墨烯陶瓷材料的制备方法,其采用浸渍的方式将石墨烯与碳化物陶瓷生胚复合,优于专利号CN201710680354.9中直接将石墨烯与陶瓷粉体复合,但是无法解决石墨烯在陶瓷基体中分布不均的问题,且浸渍会形成浓度梯度,导致复合陶瓷材料与基体材料性能相比,提升程度不大。
由上述方式成型的复合陶瓷还存在部分气孔,在复合陶瓷的烧结阶段,可以引入液态硅通过毛管压力将多孔的SiC/C预成型体浸润。炭黑与液态硅反应形成二次β-SiC,它与初始的α-SiC颗粒强力结合,形成陶瓷的三维骨架,达到进一步增强复合陶瓷的目的。
发明内容
本发明为克服现有技术的不足,设计一种石墨烯复合碳化硅陶瓷材料的制备方法,确保形成稳定的网状分散结构,且经过高温烧结,石墨烯纳米片能均匀分散于陶瓷基体材料中,达到增强、增韧的目的,显著提升了碳化硅材料的力学性能。
为实现上述目的,设计一种石墨烯复合碳化硅陶瓷材料的制备方法,以解决上述背景技术中提出的问题,需要以下步骤:步骤(1):将石墨烯纳米片置于有机分散剂中,超声分散成单层的石墨烯纳米片;
步骤(2):将超声分散后的石墨烯纳米片与碳化硅、炭黑和粘结剂在行星式球磨机中混合球磨;
步骤(3):将球磨后的浆料干燥,粉碎后过200目筛网,得到混合均匀的复合粉体;
步骤(4):将复合粉体装入模具中,使用压片机双向压实,使复合粉体胚体干压成型;
步骤(5):将复合粉体胚体置于高温烧结炉烧结,待自然降温后,将胚体取出;
步骤(6):将由步骤(5)得到的复合胚体表面添加高纯硅微粉,并使用压片机单向压实辅助成型;
步骤(7):将复合粉体胚体放入烧结炉,使用真空氛围反应烧结制备石墨烯碳化硅复合陶瓷;
步骤(8):打磨复合陶瓷添加了硅微粉的表面,得到石墨烯碳化硅复合陶瓷材料。
优选的,所述步骤(1)中, 有机分散剂为N-甲基吡咯烷酮,超声时间30~60 min。
优选的,所述步骤(2)中,以100重量份计算,超声分散后的石墨烯纳米片:1~5份,碳化硅:90~94份,炭黑:1~5份;粘结剂:羧甲基纤维素:1份。
优选的,所述步骤(4)中,采用双向压实的压力值大小为15~20MPa。
优选的,所述步骤(5)中,复合粉体胚体使用高温烧结炉时,升温速率为4℃/min,升温至800~1000℃,待自然降温后,将胚体取出。
优选的,所述步骤(6)中,以100重量份计算,称取高纯硅微粉为5~10份,纯度为99.99%;使用单向压实的方式将硅微粉复合在烧结后的复合粉体胚体表面,单向压实的压力值大小为0.1MPa。
优选的,所述步骤(7)中,采用真空氛围反应烧结:复合粉体胚体放入烧结炉中,升温速率为5℃/min,升温至1700~1900℃,保温2~3h,自然降温后得到复合陶瓷材料。
本发明具有如下有益效果:
本发明同现有技术相比,采用的超声有机分散和辅助球磨可以很好的解决石墨烯片由于范德华力产生的团聚作用,使石墨烯能均匀分散于碳化硅陶瓷材料中。在复合陶瓷的烧结阶段,液态硅通过毛管压力将多孔的SiC/C预成型体浸润。炭黑与液态硅反应形成二次β-SiC,它与初始的α-SiC颗粒强力结合,形成陶瓷的三维骨架。最后,本发明通过调整材料组成和工艺参数,利用残余硅填充残孔,减少了复合陶瓷的气孔,制成无孔陶瓷。
本发明工艺制得石墨烯复合碳化硅陶瓷材料抗弯曲强度为350MPa~480MPa,断裂韧性为3.6MPa m1/2~4.9MPa m1/2。与碳化硅陶瓷基体材料相比,抗弯曲强度提升150%~200%,导电性随着石墨烯浓度的递增正向增长,与其他方式成型的石墨烯复合碳化硅陶瓷材料相比,弯曲强度提升28%~55%,断裂韧性提升20%~30%。
附图
图1为实施例2的SEM图;
图2为各实施例样品抗弯曲强度柱形图;
图3为各实施例样品断裂韧性柱形图。
具体实施方式
下面结合具体实例对本发明做进一步的说明,但不应以此限制本发明的保护范围。
实施例1:
以100重量份计算,称取1份改性石墨烯纳米片,将石墨烯纳米片置于N-甲基吡咯烷酮中超声分散30min。称取94份碳化硅、5份炭黑与混合,另称取1份羧甲基纤维素(CMC)作为粘结剂,在行星式球磨机中混合球磨24小时,粉体干燥粉碎后过200目筛。使用压片机15Mpa双向压力,将粉体制成直径为50mm圆盘。将陶瓷胚体置于高温烧结炉,升温至800℃进行排胶处理,升温速率为4℃/min。自然冷却后,将胚体置于模具中,另称取5份高纯硅粉,使用压片机0.1MPa压力单向压实成型。将复合胚体放进反应烧结炉,在真空氛围进行烧结,温度为1700℃,升温速率4℃/min,保温2小时,待自然降温后取出,打磨掉表面多余硅粉,得到复合陶瓷。
对得到的复合陶瓷进行测试结果显示,本实施例制得石墨烯复合碳化硅陶瓷材料抗弯曲强度为407MPa,断裂韧性为4.09MPa m1/2。
实施例2:
以100重量份计算,称取3份改性石墨烯纳米片,将石墨烯纳米片置于N-甲基吡咯烷酮中超声分散60min。称取95份碳化硅、2份炭黑混合,另称取1份羧甲基纤维素(CMC)作为粘结剂,在行星式球磨机中混合球磨24小时,粉体干燥粉碎后过200目筛。使用压片机20Mpa双向压力,将粉体制成直径为50mm圆盘。将陶瓷胚体置于高温烧结炉,升温至900℃进行排胶处理,升温速率为4℃/min。自然冷却后,将胚体置于模具中,另称取7份高纯硅粉,使用0.1MPa压力单向压实成型。将复合胚体放进反应烧结炉,在真空氛围进行烧结,温度为1800℃,升温速率4℃/min,保温2小时,待自然降温后取出,打磨掉表面多余硅粉,得到复合陶瓷。
对得到的复合陶瓷进行测试结果显示,本实施例制得石墨烯复合碳化硅陶瓷材料抗弯曲强度为478MPa,断裂韧性为4.46MPa m1/2。
实施例3:
以100重量份计算,称取5份改性石墨烯纳米片,将石墨烯纳米片置于N-甲基吡咯烷酮中超声分散45min。称取与90份碳化硅、5份炭黑混合,另称取1份羧甲基纤维素(CMC)作为粘结剂,在行星式球磨机中混合球磨24小时,粉体干燥粉碎后过200目筛。使用压片机18Mpa双向压力,将粉体制成直径为50mm圆盘。将陶瓷胚体置于高温烧结炉,升温至800℃进行排胶处理,升温速率为4℃/min。自然冷却后,将胚体置于模具中,称取10份高纯硅粉,使用压片机0.1MPa压力单向压实成型。将复合胚体放进反应烧结炉,在真空氛围进行烧结,温度为1800℃,升温速率4℃/min,保温2小时,待自然降温后取出,打磨掉表面多余硅粉,得到复合陶瓷。
对得到的复合陶瓷进行测试结果显示,本实施例制得石墨烯复合碳化硅陶瓷材料抗弯曲强度为387MPa,断裂韧性为4.03MPa m1/2。
实施例4:
以100重量份计算,称取3份石墨烯纳米片与95份碳化硅、2份炭黑混合,另称取1份羧甲基纤维素(CMC)作为粘结剂,在行星式球磨机中混合球磨24小时,粉体干燥粉碎后过200目筛。使用压片机20Mpa轴向压力,将粉体制成直径为50mm圆盘。将陶瓷胚体置于高温烧结炉,升温至900℃进行排胶处理,升温速率为4℃/min。自然冷却后,将复合胚体放进反应烧结炉,在真空氛围进行烧结,温度为1800℃,升温速率4℃/min,保温2小时,待自然降温后取出,打磨掉表面多余硅粉,得到复合陶瓷。
对得到的复合陶瓷进行测试结果显示,本实施例制得石墨烯复合碳化硅陶瓷材料抗弯曲强度为286MPa,断裂韧性为3.7MPa m1/2,与实施例2相比,我们通过对比可以看出,材料的抗弯曲强度与断裂韧性都远低于使用本发明方法制备得到的复合陶瓷,同实施例2相比较,实施例4没有对石墨烯进行分散,没有添加硅微粉同复合粉体胚体进行复合,材料的抗弯曲强度降低了67%,断裂韧性降低了20.5%。
以上对本发明及其实施方式进行了描述,这种描述没有限制性,附图中所示的也只是本发明的实施方式之一,实际的结构并不局限于此。总而言之如果本领域的普通技术人员受其启示,在不脱离本发明创造宗旨的情况下,不经创造性的设计出与该技术方案相似的结构方式及实施例,均应属于本发明的保护范围。
Claims (7)
1.一种石墨烯复合碳化硅陶瓷材料的制备方法,其特征在于,包括如下步骤:
步骤(1):将石墨烯纳米片置于有机分散剂中,超声分散成单层的石墨烯纳米片;
步骤(2):将超声分散后的石墨烯纳米片与碳化硅、炭黑和粘结剂在行星式球磨机中混合球磨;
步骤(3):将球磨后的浆料干燥,粉碎后过200目筛网,得到混合均匀的复合粉体;
步骤(4):将复合粉体装入模具中,双向压实,使复合粉体胚体干压成型;
步骤(5):将复合粉体胚体置于高温烧结炉烧结,待自然降温后,将胚体取出;
步骤(6):将由步骤(5)得到的复合胚体表面添加高纯硅微粉,并单向压实辅助成型;
步骤(7):将复合粉体胚体放入烧结炉,使用真空氛围反应烧结制备石墨烯碳化硅复合陶瓷;
步骤(8):打磨复合陶瓷添加了硅微粉的表面,得到石墨烯碳化硅复合陶瓷材料。
2.根据权利要求1所述的一种石墨烯复合碳化硅陶瓷材料的制备方法,其特征在于,所述步骤(1)中, 有机分散剂为N-甲基吡咯烷酮,超声时间30~60 min。
3.根据权利要求1所述的一种石墨烯复合碳化硅陶瓷材料的制备方法,其特征在于,所述步骤(2)中,以100重量份计算,超声分散后的石墨烯纳米片:1~5份,碳化硅:90~94份,炭黑:1~5份;粘结剂:羧甲基纤维素:1份。
4.根据权利要求1所述的一种石墨烯复合碳化硅陶瓷材料的制备方法,其特征在于,所述步骤(4)中,采用双向压实的压力值大小为15~20MPa。
5.根据权利要求1所述的一种石墨烯复合碳化硅陶瓷材料的制备方法,其特征在于,所述步骤(5)中,复合粉体胚体使用高温烧结炉时,升温速率为4℃/min,升温至800~1000℃,待自然降温后,将胚体取出。
6.根据权利要求1所述的一种石墨烯复合碳化硅陶瓷材料的制备方法,其特征在于,所述步骤(6)中,以100重量份计算,称取高纯硅微粉为5~10份,纯度为99.99%;使用单向压实的方式将硅微粉复合在烧结后的复合粉体胚体表面,单向压实的压力值大小为0.1MPa。
7.根据权利要求1所述的一种石墨烯复合碳化硅陶瓷材料的制备方法,其特征在于,所述步骤(7)中,采用真空氛围反应烧结:复合粉体胚体放入烧结炉中,升温速率为5℃/min,升温至1700~1900℃,保温2~3h,自然降温后得到复合陶瓷材料。
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