CN113213936B - 一种陶瓷粉掺杂改性自烧结石墨复合材料的制备方法 - Google Patents
一种陶瓷粉掺杂改性自烧结石墨复合材料的制备方法 Download PDFInfo
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Abstract
一种陶瓷粉掺杂改性自烧结石墨复合材料的制备方法,属于特种石墨复合材料制备技术领域,解决陶瓷颗粒在原料压粉中分散困难、效率低下、基体相与陶瓷相界面结合强度差的问题,本发明通过原位包覆法将陶瓷粉引入到制备石墨的原料中,不仅有效改善了陶瓷颗粒分布不均的现象,又能对陶瓷颗粒形成有效碳包覆,使材料的微观界面得到改善。材料制备过程中,首先将陶瓷粉加入到改制沥青中,其作为形核剂促进改制沥青的液相半炭化,制成生焦包覆的复合陶瓷粉;其表面生焦所具有的自烧结性,能够使材料在后续的热处理过程中陶瓷组份与炭组份同步收缩致密化,最终制备出陶瓷颗粒分布均与、界面结合强度良好、综合性能优异的陶瓷掺杂改性自烧结石墨复合材料。
Description
技术领域
本发明属于特种石墨复合材料制备技术领域,具体涉及一种陶瓷粉掺杂改性自烧结石墨复合材料的制备方法。
背景技术
利用陶瓷所具有的高硬度、耐摩擦或高温抗氧化等特性改善石墨基体相应的性能缺陷是制备陶瓷掺杂石墨复合材料的初衷。例如,引入碳化硅能够改善石墨材料的硬度和耐磨性,使材料的磨损量有效降低;对于低石墨化度的石墨材料,引入氮化硼或碳化硅能够在材料磨损面上形成润滑磨料层,降低摩擦系数,改善摩擦环境;引入含硼化合物能够使石墨材料在600~900℃的有氧环境下形成隔氧薄膜,有效提高材料的抗氧化性;所以引入不同陶瓷使石墨的特定属性得到了改善,有力的促进了石墨材料在摩擦、密封或高温环境下的应用。
传统方法制备陶瓷掺杂石墨复合材料主要采用以下步骤:首先将陶瓷粉、骨料焦与粘结剂沥青进行混捏操作,然后将混捏料破碎到规定粒度制成压粉,将压粉利用等静压或模压工艺压制成生坯,再经过炭化、浸渍、二次炭化以及石墨化等过程,完成复合材料的制备。在上述制备过程中只是将陶瓷粉与其他原料经过简单的混合,很难达到陶瓷粉均匀分布的目的,碳基体在后续的热处理过程中由于发生炭化石墨化而收缩,与此同时陶瓷晶体结构或形态基本不发生变化,使得陶瓷相与基体相发生明显脱节,界面粗糙化,明显不利于复合材料综合性能的提升。近些年来,自烧结石墨以其广泛的原料、简单的制备工艺、优异的性能逐步发展为耐磨、密封领域重要的石墨应用种类。这种方法主要采用具有自烧结性的生焦或MCMB为原料,经过成型、炭化以及石墨化过程,最终完成自烧结石墨材料的制备。这种石墨制备方法与陶瓷掺杂工艺结合起来,将原料破碎与陶瓷混合结合起来,在亚微米级程度上实现了陶瓷粉与原料的均匀混合,但在后续热处理过程中由于碳基体发生收缩,同样存在相与界脱节的现象,不利于材料的微观结构均匀化、精细化。
发明内容
为了克服现有陶瓷掺杂石墨制备技术的不足,一方面解决陶瓷颗粒在原料压粉中分散困难、效率低下的问题,另一方面解决基体相与陶瓷相界面结合强度差的问题,本发明提供一种陶瓷掺杂改性自烧结石墨复合材料的制备方法。
本发明的设计构思为:本发明通过原位包覆法将陶瓷粉引入到制备石墨的原料中,不仅有效改善了陶瓷颗粒分布不均的现象,又能对陶瓷颗粒形成有效碳包覆,使材料的微观界面得到改善。材料制备过程中,首先将陶瓷粉加入到改制沥青中,其作为形核剂促进改制沥青的液相半炭化,制成生焦包覆的复合陶瓷粉;其表面生焦所具有的自烧结性,能够使材料在后续的热处理过程中陶瓷组份与炭组份同步收缩致密化,最终制备出陶瓷颗粒分布均与、界面结合强度良好、综合性能优异的陶瓷掺杂改性自烧结石墨复合材料。
本发明将自烧结石墨原料制备、自烧结石墨制备以及陶瓷掺杂工艺有机的结合起来,将陶瓷粉在自烧结原料半焦化前的液体状态时引入,一方面由于表面活性能使其在液体原料中均与分布,另一方面其作为液相形核剂促进了原料的半焦化,在后续的热处理过程中陶瓷颗粒作为碳质成份的核心,一同发生位移,有效的改善了相界脱节的现象,使最终制备的陶瓷掺杂改性自烧结石墨复合材料微观结构致密、界面结合强度高、宏观性能优良。
本发明通过以下技术方案予以实现。
一种陶瓷粉掺杂改性自烧结石墨复合材料的制备方法,以改制沥青和增强陶瓷粉为原料,经过原料混合、半炭化处理、物料破碎、压制成型、炭化(浸渍、二次炭化)以及石墨化等工序,最终制备出陶瓷颗粒均匀分布、界面结合良好、综合性能优异的陶瓷掺杂改性自烧结石墨复合材料,包括以下步骤:
S1、将将陶瓷粉与改制沥青粉按质量比(2~3):(7~8)加入混料机进行密封混合操作,混合转速为30r/min,混合时间为24h,制得混合料;
S2、首先,将步骤S1制得的混合料放入高压釜,采用氮气置换出高压釜内的空气;然后,高压釜密闭升温,控制釜内压力为0-3MPa,升温速率为50℃/h,釜心终温为400-420℃,终温保温时间为8-12h;最后,待高压釜自然降温后完成半炭化过程,制成生焦包覆的复合陶瓷粉;
S3、将步骤S2制成的生焦包覆的复合陶瓷粉通过机械或气流粉碎,然后进行压制成型,制得生坯;
S4、将步骤S3制得的生坯放入炭化炉中,在氮气氛围下以10℃/h升温到1000℃并保温1h,制得炭制品;
S5、将步骤S4制得的炭制品放入石墨化炉中,在氩气氛围下以100℃/h升温到1800~2400℃,并保温1h,制得陶瓷粉掺杂改性自烧结石墨复合材料。
进一步地,在所述步骤S1中,陶瓷粉为氮化物陶瓷粉、碳化物陶瓷粉、硼化物陶瓷粉或氧化物陶瓷粉中的一种或多种的混合物,陶瓷粉的粒径为1-5μm。
进一步地,在所述步骤S1中,改制沥青粉的软化点≥95℃,残炭值≥40%,甲苯可溶喹啉不溶物≥28%,灰分≤0.1%,粒度D50≤150μm。
进一步地,在所述步骤S2中,高压釜置换气体后初压为常压,然后随着反应的进行通过气体缓慢外排的方式降低反应釜内压力。
进一步地,在所述步骤S3中,机械或气流粉碎后生焦包覆的复合陶瓷粉的粒径D50为2-10μm,D90≤15μm。
进一步地,在所述步骤S3中,所述压制成型为等静压压制成型或者模压成型,等静压成型压力为80-160MPa,模压成型压力为100-150MPa。
进一步地,等静压压制成型或者模压成型后生坯的密度ρ≥1.25g/cm3。
进一步地,在所述步骤S5中,根据掺杂陶瓷粉的种类及石墨复合材料最终性能要求确定石墨化的终温温度。
进一步地,在所述步骤S1中,所述混料机为四维混料机。
与现有技术相比本发明的有益效果为:
本发明通过原位制备生焦包覆陶瓷颗粒,使陶瓷颗粒在材料基体中均与分布,并使碳质基体与陶瓷颗粒紧密结合,改善材料内部界面结合情况,最终制备出组分均与分布、界面结合紧密、综合性能优良的陶瓷掺杂改性自烧结石墨复合材料。本发明原料来源广泛,工序短,制备工艺稳定可控,是制备高性能动摩擦密封材料或高温抗氧化石墨复合材料的有效备选方法。
具体实施方式
为了进一步说明本发明,下面结合实例对本发明进行详细地描述,但不用来限制本发明的范围。若未特别指明,实施例均按照常规实验条件。另外,对于本领域技术人员而言,在不偏离本发明的实质和范围的前提下,对这些实施方案中的物料成分和用量进行的各种修改或改进,均属于本发明要求保护的范围。
实施例1
一种陶瓷粉掺杂改性自烧结石墨复合材料的制备方法,包括以下步骤:
S1、将粒径为1-3μm的氮化硼粉末与粒径为100目改制沥青粉按质量比2:8的比例加入四维混料机进行密封混合操作,混合转速为30r/min,混合时间为24h,制得混合料;
S2、首先,将步骤S1制得的混合料放入高压釜,采用氮气置换出高压釜内的空气;然后,高压釜密闭升温,控制釜内压力为0-3MPa,升温速率为50℃/h,釜心终温为420℃,终温保温时间为12h;最后,待高压釜自然降温后完成半炭化过程,制成生焦包覆的复合陶瓷粉;
S3、将步骤S2制成的生焦包覆的复合陶瓷粉通过气流粉碎,粉碎粒度D50为3-6μm,然后进行等静压成型操作,成型压力为150MPa,保压30min,制得生坯;
S4、将步骤S3制得的生坯放入炭化炉中,在氮气氛围下以10℃/h升温到1000℃并保温1h,制得炭制品;
S5、将步骤S4制得的炭制品放入石墨化炉中,在氩气氛围下以100℃/h升温到1850℃,并保温1h,制得陶瓷粉掺杂改性自烧结石墨复合材料,其性能如下。
实施例2
一种陶瓷粉掺杂改性自烧结石墨复合材料的制备方法,包括以下步骤:
S1、将粒径为1-3μm的炭化硼粉末与粒径为100目改制沥青粉按质量比3:7的比例加入四维混料机进行密封混合操作,混合转速为30r/min,混合时间为24h,制得混合料;
S2、首先,将步骤S1制得的混合料放入高压釜,采用氮气置换出高压釜内的空气;然后,高压釜密闭升温,控制釜内压力为0-3MPa,升温速率为50℃/h,釜心终温为410℃,终温保温时间为8h;最后,待高压釜自然降温后完成半炭化过程,制成生焦包覆的复合陶瓷粉;
S3、将步骤S2制成的生焦包覆的复合陶瓷粉通过机械粉碎,粉碎粒度D50为4-6μm,然后进行模压成型操作,成型压力为170MPa,保压30min,制得生坯;
S4、将步骤S3制得的生坯放入炭化炉中,在氮气氛围下以10℃/h升温到1000℃并保温1h,制得炭制品;
S5、将步骤S4制得的炭制品放入石墨化炉中,在氩气氛围下以100℃/h升温到2000℃,并保温1h,制得陶瓷粉掺杂改性自烧结石墨复合材料,其性能如下。
实施例3
一种陶瓷粉掺杂改性自烧结石墨复合材料的制备方法,包括以下步骤:
S1、将粒径为1-3μm的氮化硼与氮化硅粉末混合物(硅硼摩尔比为1:6)以及粒径为100目改制沥青粉按质量比2.5:7.5的比例加入四维混料机进行密封混合操作,混合转速为30r/min,混合时间为24h,制得混合料;
S2、首先,将步骤S1制得的混合料放入高压釜,采用氮气置换出高压釜内的空气;然后,高压釜密闭升温,控制釜内压力为0-3MPa,升温速率为50℃/h,釜心终温为400℃,终温保温时间为12h;最后,待高压釜自然降温后完成半炭化过程,制成生焦包覆的复合陶瓷粉;
S3、将步骤S2制成的生焦包覆的复合陶瓷粉通过机械粉碎,粉碎粒度D50为4-6μm,然后进行等静压成型操作,成型压力为150MPa,保压30min,制得生坯;
S4、将步骤S3制得的生坯放入炭化炉中,在氮气氛围下以10℃/h升温到1000℃并保温1h,制得炭制品;
S5、将步骤S4制得的炭制品放入石墨化炉中,在氩气氛围下以100℃/h升温到1850℃,并保温1h,制得陶瓷粉掺杂改性自烧结石墨复合材料,其性能如下。
实施例4
一种陶瓷粉掺杂改性自烧结石墨复合材料的制备方法,包括以下步骤:
S1、将粒径为1-3μm的氮化硼与氮化硅粉末混合物(硅硼摩尔比为1:2)以及粒径为100目改制沥青粉按质量比2:8的比例加入四维混料机进行密封混合操作,混合转速为30r/min,混合时间为24h,制得混合料;
S2、首先,将步骤S1制得的混合料放入高压釜,采用氮气置换出高压釜内的空气;然后,高压釜密闭升温,控制釜内压力为0-3MPa,升温速率为50℃/h,釜心终温为400℃,终温保温时间为12h;最后,待高压釜自然降温后完成半炭化过程,制成生焦包覆的复合陶瓷粉;
S3、将步骤S2制成的生焦包覆的复合陶瓷粉通过机械粉碎,粉碎粒度D50为4-6μm,然后进行等静压成型操作,成型压力为150MPa,保压30min,制得生坯;
S4、将步骤S3制得的生坯放入炭化炉中,在氮气氛围下以10℃/h升温到1000℃并保温1h,制得炭制品;
S5、将步骤S4制得的炭制品放入石墨化炉中,在氩气氛围下以100℃/h升温到1850℃,并保温1h,制得陶瓷粉掺杂改性自烧结石墨复合材料,其性能如下:
以上所述,仅为本发明的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉技术领域的技术人员在本发明揭露的技术范围内,可轻易想到的变化或替换,都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应以所述权利要求的保护范围为准。
Claims (2)
1.一种陶瓷粉掺杂改性自烧结石墨复合材料的制备方法,其特征在于包括以下步骤:
S1、将陶瓷粉与改制沥青粉按质量比(2~3):(7~8)加入混料机进行密封混合操作,混合转速为30r/min,混合时间为24h,制得混合料;
所述陶瓷粉为氮化物陶瓷粉、碳化物陶瓷粉、硼化物陶瓷粉或氧化物陶瓷粉中的一种或多种的混合物,陶瓷粉的粒径为1-5μm;
所述改制沥青粉的软化点≥95℃,残炭值≥40%,甲苯可溶喹啉不溶物≥28%,灰分≤0.1%,粒度D50≤150μm;
S2、首先,将步骤S1制得的混合料放入高压釜,采用氮气置换出高压釜内的空气,高压釜置换气体后初压为常压,然后随着反应的进行通过气体缓慢外排的方式降低反应釜内压力;然后,高压釜密闭升温,控制釜内压力为0-3MPa,升温速率为50℃/h,釜心终温为400-420℃,终温保温时间为8-12h;最后,待高压釜自然降温后完成半炭化过程,制成生焦包覆的复合陶瓷粉;
S3、将步骤S2制成的生焦包覆的复合陶瓷粉通过机械或气流粉碎,机械或气流粉碎后生焦包覆的复合陶瓷粉的粒径D50为2-10μm,D90≤15μm;然后进行压制成型,制得生坯;
所述压制成型为等静压压制成型或者模压成型,等静压成型压力为80-160MPa,模压成型压力为100-150MPa;
等静压压制成型或者模压成型后生坯的密度ρ≥1.25g/cm3;
S4、将步骤S3制得的生坯放入炭化炉中,在氮气氛围下以10℃/h升温到1000℃并保温1h,制得炭制品;
S5、将步骤S4制得的炭制品放入石墨化炉中,在氩气氛围下以100℃/h升温到1800~2400℃,并保温1h,根据掺杂陶瓷粉的种类及石墨复合材料最终性能要求确定石墨化的终温温度,制得陶瓷粉掺杂改性自烧结石墨复合材料。
2.根据权利要求1所述的一种陶瓷粉掺杂改性自烧结石墨复合材料的制备方法,其特征在于:在所述步骤S1中,所述混料机为四维混料机。
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