CN114920577A - 一种碳石墨材料及其制备方法 - Google Patents

一种碳石墨材料及其制备方法 Download PDF

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CN114920577A
CN114920577A CN202210616634.4A CN202210616634A CN114920577A CN 114920577 A CN114920577 A CN 114920577A CN 202210616634 A CN202210616634 A CN 202210616634A CN 114920577 A CN114920577 A CN 114920577A
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李冰
常先恩
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Abstract

本发明提供一种碳石墨材料及其制备方法,涉及碳石墨材料技术领域。该碳石墨材料,材料以石墨粉、碳化硅粉末、硅粉、沥青焦以及炭黑为主要材料,以改性酚醛树脂引发剂,以微型空心碳球为造孔剂,以上材料经过混合、浸药以及干燥后,进行梯度焙烧而成。该材料将造孔剂设置为微型空心碳球,微型空心碳球的内部设置有空气,微型空心碳球在1000℃加热三个小时后,使得微型空心碳球的内部碳与内部气体中的氧气反应,从而使得微型空心碳球内的内孔定型,从而在碳石墨内部形成圆形内孔,微型空心碳球与碳石墨的材料相同,不会因为引入杂质导致碳石墨材料发生改变。

Description

一种碳石墨材料及其制备方法
技术领域
本发明涉及汽车配件技术领域,具体为一种碳石墨材料及其制备方法。
背景技术
碳石墨材料是由碳元素为主要化学成分组成的一类非金属复合材料。碳石墨材料因其具有质轻、高强、耐蚀、抗热震、导电和自润滑等一系列独特性能,被认为是航空航天和原子能等国家安全领域的战略材料。但由于碳石墨材料在制备过程中各组分之间非均质、不匹配且有机组分会发生热分解、热缩聚等一系列的反应,会导致其内部不可避免的产生随机微裂纹和孔隙。这些缺陷的存在使得碳石墨材料具有较低韧性,很容易发生脆性断裂,致使碳石墨材料的应用受到了限制,并且在服役过程中会存在安全隐患。因此,调控碳石墨材料的微观结构,实现基体中各组分之间的相互匹配,是研究的重点和难点之一。
调控碳石墨材料的微观结构的研究主要有正反两个方向,目前研究多聚焦于正向抑制基体内部先天缺陷,提高其结构完整性,使得材料的力热学性能同步提升,并显著提升材料的使用寿命。而通过先天造孔、后天补强的反向结构调控思路研究相对较少。传统的造孔思路是通过在碳石墨材料制备过程中加入造孔剂,在高温条件下造孔剂会发生热解,并在材料内部留下孔道。但是该孔道相对与圆状的内孔之间的结构差距较大。
发明内容
(一)解决的技术问题
针对现有技术的不足,本发明提供了一种碳石墨材料及其制备方法,解决了传统造孔剂产生孔道的问题。
(二)技术方案
为实现以上目的,本发明通过以下技术方案予以实现:一种碳石墨材料,以石墨粉、碳化硅粉末、硅粉、沥青焦以及炭黑为主要材料,以改性酚醛树脂引发剂,以微型空心碳球为造孔剂,其特征在于原料、结合剂按以下重量百分比组成:石墨粉30到40份,碳化硅粉末10到20份,沥青焦70到80份,炭黑为5到10份,改性酚醛树脂8到10份,微型空心碳球为5到8份;以上材料经过混合、浸药以及干燥后,进行梯度焙烧而成。
优选的,所述微型空心碳球的直径设置为200微米。
优选的,所述浸药采用的药剂设置为磷酸氢二铵。
作为一个总的发明构思,本发明还提供一种如上述的碳石墨材料的制备方法,包括以下步骤:
(1)、将石墨粉、碳化硅粉末、硅粉、沥青焦以及炭黑混捏机中先进行干混再热混,然后加入熔融状改性酚醛树脂进行湿混;
(2)、将步骤(1)湿混后的糊料烘干、破碎、筛分后,加入磷酸氢二铵药剂,将浸药后的物料晾干;
(3)、将晾晒后的物料与微型空心碳球均匀混合,随后进行成型、焙烧,得到具有碳石墨材料。
上述的制备方法,优选的,步骤(1)中,干混的时间为1-2h;热混的温度为80℃-140℃,热混的时间为1-2h;湿混的温度为120-160℃,湿混时间为2-4h。
上述的制备方法,优选的,步骤(2)中,浸药的物料通入150℃烘干炉中或自然晾晒,磷酸氢二铵药剂的浓度设置为6%。
上述的制备方法,优选的,步骤(3)中,焙烧的温度呈梯度焙烧:先用1-4h将炉内温度从室温均匀升温至50-100℃,并且使得炉内的中充满氮气以及水蒸气;再用5-9h将温度均匀升温至100-400℃,并且使得炉内的中充满氮气以及水蒸气,最后将10-12h将温度均匀升温至2400℃,并且使得炉内的中充满氩气。
(三)有益效果
本发明提供了一种碳石墨材料及其制备方法。具备以下有益效果:
1、该装置将造孔剂设置为微型空心碳球,微型空心碳球的内部设置有空气,微型空心碳球在1000℃加热三个小时后,使得微型空心碳球的内部碳与内部气体中的氧气反应,从而使得微型空心碳球内的内孔定型,从而在碳石墨内部形成圆形内孔,微型空心碳球与碳石墨的材料相同,不会因为引入杂质导致碳石墨材料发生改变。
2、将混合筛分后的物料进行药浸处理,药浸材料设置为磷酸氢二铵药剂,充当活化阻燃剂,具有高效的活化性能,能在物料表面形成纳米级的微孔,提高其吸附能力,从而提高各组分之间的连强度,提高碳纤维的结构强度。
具体实施方式
下面将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。
本发明实施例提供一种碳石墨材料,以石墨粉、碳化硅粉末、硅粉、沥青焦以及炭黑为主要材料,以改性酚醛树脂引发剂,以微型空心碳球为造孔剂,其特征在于原料、结合剂按以下重量百分比组成:石墨粉30到40份,碳化硅粉末10到20份,沥青焦70到80份,炭黑为5到10份,改性酚醛树脂8到10份,微型空心碳球为5到8份;以上材料经过混合、浸药以及干燥后,进行梯度焙烧而成,所述微型空心碳球的直径设置为200微米,所述浸药采用的药剂设置为磷酸氢二铵,磷酸氢二铵为活化阻燃剂,浓度为6%,具有高效的活化性能,能子在物料表面形成纳米级的微孔,提高其吸附能力。
本实施例的碳石墨材料的制备方法,包括以下步骤:
(1)、将石墨粉、碳化硅粉末、硅粉、沥青焦以及炭黑混捏机中先进行干混再热混,然后加入熔融状改性酚醛树脂进行湿混,干混的时间为1-2h;热混的温度为80℃-140℃,热混的时间为1-2h;湿混的温度为120-160℃,湿混时间为2-4h。
(2)、将步骤(1)湿混后的糊料烘干、破碎、筛分后,加入磷酸氢二铵药剂,将浸药后的物料晾干,浸药的物料通入150℃烘干炉中或自然晾晒,磷酸氢二铵药剂的浓度设置为6%。
(3)、将晾晒后的物料与微型空心碳球均匀混合,随后进行成型、焙烧,得到具有碳石墨材料,焙烧的温度呈梯度焙烧:先用1-4h将炉内温度从室温均匀升温至50-100℃,并且使得炉内的中充满氮气以及水蒸气;再用5-9h将温度均匀升温至100-400℃,并且使得炉内的中充满氮气以及水蒸气,最后将10-12h将温度均匀升温至2400℃,并且使得炉内的中充满氩气。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。

Claims (7)

1.一种碳石墨材料,以石墨粉、碳化硅粉末、硅粉、沥青焦以及炭黑为主要材料,以改性酚醛树脂引发剂,以微型空心碳球为造孔剂,其特征在于原料、结合剂按以下重量百分比组成:石墨粉30到40份,碳化硅粉末10到20份,沥青焦70到80份,炭黑为5到10份,改性酚醛树脂8到10份,微型空心碳球为5到8份;以上材料经过混合、浸药以及干燥后,进行梯度焙烧而成。
2.根据权利要求1所述的一种碳石墨材料及其制备方法,其特征在于:所述微型空心碳球的直径设置为200微米。
3.根据权利要求1所述的一种碳石墨材料及其制备方法,其特征在于:所述浸药采用的药剂设置为磷酸氢二铵。
4.一种如权利要求1-3任一项所述的碳石墨材料的制备方法,其特征在于,包括以下步骤:(1)、将石墨粉、碳化硅粉末、硅粉、沥青焦以及炭黑混捏机中先进行干混再热混,然后加入熔融状改性酚醛树脂进行湿混;
(2)、将步骤(1)湿混后的糊料烘干、破碎、筛分后,加入磷酸氢二铵药剂,将浸药后的物料晾干;
(3)、将晾晒后的物料与微型空心碳球均匀混合,随后进行成型、焙烧,得到具有碳石墨材料。
5.如权利要求4所述的制备方法,其特征在于,步骤(1)中,干混的时间为1-2h;热混的温度为80℃-140℃,热混的时间为1-2h;湿混的温度为120-160℃,湿混时间为2-4h。
6.如权利要求4所述的制备方法,其特征在于,步骤(2)中,浸药的物料通入150℃烘干炉中或自然晾晒,磷酸氢二铵药剂的浓度设置为6%。
7.如权利要求4所述的制备方法,其特征在于,步骤(3)中,焙烧的温度呈梯度焙烧:先用1-4h将炉内温度从室温均匀升温至50-100℃,并且使得炉内的中充满氮气以及水蒸气;再用5-9h将温度均匀升温至100-400℃,并且使得炉内的中充满氮气以及水蒸气,接着再用10-12h温度提升至1000℃,最后将10-12h将温度均匀升温至2400℃,并且使得炉内的中充满氩气。
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