CN113773094B - 一种熔融渗硅用硅粉的处理方法 - Google Patents
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Abstract
本发明是一种熔融渗硅用硅粉的处理方法,可用于制备反应烧结碳化硅、碳纤维增强碳化硅基复合材料及碳化硅纤维增强碳化硅基复合材料。传统的反应渗硅多采用硅粉作为渗硅的原料,渗硅过程中容易出现堵孔或者熔渗不均匀等问题。本发明通过对硅粉进行预处理,使其表面形成薄壳,利用其熔化及加热过程体积变化效应,使得硅能够破壳并迅速进入多孔体中,避免反应堵孔等问题,并且有利于提高熔渗效率。
Description
技术领域
本发明是一种熔融渗硅用硅粉的处理方法,属于无机材料领域。
背景技术
反应熔融渗硅是在高温下,将硅熔化,渗入多孔体中,从而形成致密材料的一种方法,该方法由于具有周期短、成本低等优势,被广泛用于反应烧结碳化硅、碳纤维增强碳化硅复合材料、碳化硅纤维增强碳化硅复合材料,在民用及军用领域均有广泛应用。
传统的反应渗硅是将多孔体置于硅粉或者硅颗粒中进行包埋,加热至硅熔点(1410℃)以上时,硅发生熔化,液体硅由于毛细效应进入到多孔体中,形成致密化材料。由于硅粉在熔化过程中,通常外围的温度较高,先发生熔化,在升温过程中,因此会有部分先渗入到多孔体外围周边处,并与多孔体中的碳发生反应,反应形成的碳化硅致使孔径减小,降低了多孔体的透气性,造成部分区域出现渗透不均匀或者“黑芯”的问题。
发明内容
本发明正是针对上述现有技术中存在的问题而设计提供了一种熔融渗硅用硅粉的处理方法,其目的是通过对硅粉进行预处理,使其表面形成薄壳,利用其熔化及加热过程体积变化效应,使得硅能够破壳并迅速进入多孔体中,避免反应堵孔等问题,并且有利于提高熔渗效率。
为实现上述目的,本发明的技术解决方案是:
该种熔融渗硅用硅粉的处理方法是将硅粉与作为反应活性物质的碳或者氮在1200℃~1500℃的高温下进行反应,使硅粉表面形成一层薄壳;
当反应活性物质为碳时,硅粉表面形成碳化硅壳层,当反应活性物质为氮时,硅粉表面形成氮化硅壳层。该技术措施的设计特点是将带有壳层的硅粉,在高于硅的熔点以上进行熔渗,由于硅熔化过程及加热过程体积发生变化,当达到一定温度时,壳层破裂,从而使液体硅在短时间内浸润多孔体并实现致密化。
在实施时,当所述的反应活性物质为碳时,其来源为酚醛树脂、呋喃树脂、裂解碳及沥青中的一种或几种的混合物。
在实施时,当反应活性物质为氮时,其来源为氮气或者其它可以与硅发生反应形成氮化硅的氮源。
在实施时,当反应活性物质为碳时,采用先包裹碳再高温反应的方法实现形壳。
进一步,当碳来源于树脂时,所述包裹碳是首先将树脂与硅粉进行均匀混合,使硅粉周围均匀地包裹一层树脂,进而在800℃~1100℃之间高温裂解成碳。
进一步,当碳来源于裂解碳时,所述包裹碳是将硅粉置于沉积炉中,采用化学气相沉积在硅粉表面沉积碳,化学气相沉积的气源可以为丙烯、丙烷、甲烷、乙炔等,沉积温度在850℃~1000℃之间。
实施时,所述高温下进行反应所需的时间为5~20min。
实施时,所述的硅粉提前进行批量化处理或在熔渗过程中原位反应处理。
所述的硅粉用尺寸较大的硅粒替代,或所述的硅粉选用Si-Zr硅合金粉。
本发明技术方案中,带薄壳的硅颗粒在升温过程中,硅不会渗入到多孔体内部,避免了局部熔化及渗入问题。当升至更高温度时,由于硅颗粒形状及壳层厚度局部的差异性,使得内部的硅颗粒于外周的硅颗粒破壳的同步性趋于相近,从而减弱了硅的熔化的不同步性,并且由于此时温度高,硅的流动性及渗入性显著增加,使硅在短时间内从壳层逸出,从而实现快速致密化,避免了反应堵孔的现象。
本发明技术方案的有益的技术效果是:
1、本发明不同于传统的熔渗时采用硅粉进行包埋,而是通过硅与碳或者氮发生反应,在表层形成碳化硅或氮化硅薄壳。当加热至硅熔点以上时,薄壳内的硅发生熔化,由于薄壳的包裹作用,使得硅不能从薄壳中逸出,避免了较低温度下硅与多孔体中的碳发生反应,形成碳化硅而发生的堵孔现象。当温度进一步升高时,由于液体硅的体积发生胀大及硅熔化时产生的体积效应,致使壳层受到应力,当应力大于壳层强度时,壳层破裂,致使硅逸出,从而实现在较高温度、较低粘度的状态下进入多孔体,避免了反应堵孔现象,从而使得熔渗后的材料均匀性好并且避免“黑芯”现象。
2、本发明工艺较简单,可以将硅粉处理与渗硅过程一次完成,也可以对硅粉单独进行预处理,可以有效提高产品质量与降低生产成本。
具体实施方式
以下结合具体实例说明一种熔融渗硅用硅粉的处理方法。
实施例1
采用本发明技术方案处理熔融渗硅用硅粉的步骤如下:
步骤一、将500克10微米的硅粉置于沉积炉工装内,采用丙烯作为碳源,在硅粉表面沉积一薄层裂解碳,沉积温度为950℃,沉积时间为30min;
步骤二、将上述制备的包裹有碳的硅粉置于高温炉中进行形壳处理,温度为1400℃,时间10min,制备出含有碳化硅壳层的硅粉。该硅粉可以在1600℃时发生破裂,实现多孔体的快速致密化。
实施例2
采用本发明技术方案处理熔融渗硅用硅粉的步骤如下:
将500克10微米的硅粉置于高温炉中,通入氮气进行高温氮化处理,温度为1420℃,处理时间10min,使硅粉表面形成一层氮化硅壳层,该硅粉可以在1550℃时发生破裂,实现多孔体的快速致密化。
实施例3
采用本发明技术方案处理熔融渗硅用硅粉的步骤如下:
步骤一、将20克酚醛树脂溶于300克乙醇中,再将500克10微米的硅粉加入上述溶液中,并球磨5小时。将上述混合物置于离型纸上进行干燥5小时,干燥温度为80℃;
步骤二、将烘干后的混合物置于高温炉中进行裂解,裂解温度为1000℃,时间为60min,再继续升高温度至1400℃进行形壳处理,时间10min,制备出含有碳化硅壳层的硅粉。该硅粉可以在1600℃时发生破裂,实现多孔体的快速致密化。
采用实施例2处理的硅粉制备反应烧结碳化硅,多孔体为树脂裂解形成的多孔碳,熔渗温度为1550℃,熔渗时长30min,制备出的反应烧结碳化硅密度为3.07g/cm3,孔隙率0.83%,内部无黑芯或局部熔渗不均匀现象;未处理过的硅粉,制备出的反应烧结碳化硅密度为2.95g/cm3,孔隙率2.62%,并且试块中间存在局部黑芯问题。
Claims (1)
1.一种熔融渗硅用硅粉的处理方法,其特征在于:将硅粉与作为反应活性物质的碳在1200℃~1500℃的高温下进行反应,反应所需的时间为5~20min,使硅粉表面形成一层薄壳;
所述硅粉选用粒径10微米的硅粒或Si-Zr硅合金粉,并提前进行批量化处理或在熔渗过程中原位反应处理;
作为反应活性物质的碳,其来源为酚醛树脂、呋喃树脂、裂解碳中的一种或几种的混合物,采用先包裹碳再高温反应的方法在硅粉表面形成碳化硅壳层;
当碳来源于酚醛树脂、呋喃树脂时,所述包裹碳是首先将树脂与硅粉进行均匀混合,使硅粉周围均匀地包裹一层树脂,进而在800℃~1100℃之间高温裂解成碳;
当碳来源于裂解碳时,所述包裹碳是将硅粉置于沉积炉中,采用化学气相沉积在硅粉表面沉积碳,化学气相沉积的气源为丙烯、丙烷、甲烷、乙炔,沉积温度在850℃~1000℃之间;
通过硅与碳发生反应,在表层形成碳化硅薄壳;当加热至硅熔点以上时,薄壳内的硅发生熔化,由于薄壳的包裹作用,使得硅不能从薄壳中逸出,避免了较低温度下硅与多孔体中的碳发生反应,形成碳化硅而发生的堵孔现象;当温度进一步升高时,由于液体硅的体积发生胀大及硅熔化时产生的体积效应,致使壳层受到应力,当应力大于壳层强度时,壳层破裂,致使硅逸出,从而实现在较高温度、较低粘度的状态下进入多孔体,避免了反应堵孔现象。
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