CN107266101A - 一种短切碳纤维增强碳化硼基复合材料的制备方法 - Google Patents
一种短切碳纤维增强碳化硼基复合材料的制备方法 Download PDFInfo
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Abstract
本发明属于碳化硼基复合材料的制备领域,公开了一种短切碳纤维增强碳化硼基复合材料的制备方法。将液态酚醛树脂分散于无水乙醇中;将B4C粉加入所得溶液中,40~60 ℃搅拌均匀;将短切碳纤维加入所得溶液中,60~80 ℃继续搅拌,直至浆料粘稠不能搅拌为止;将浆料烘干,造粒过筛,将所得颗粒粉置于模具中,压制成型,得到坯体;用硅粉、钛粉中的一种或两者的组合物包覆坯体,置于石墨坩埚中,在真空1550~1650 ℃下反应1~3 h,即得到短切碳纤维增强碳化硼基复合材料。本发明具有工艺简单、操作方便等优点,C/B4C同时具有短切碳纤维和碳化硼的优点,并且克服了B4C韧性低等缺陷。
Description
技术领域
本发明属于碳化硼基复合材料的制备领域,具体涉及一种短切碳纤维增强碳化硼基复合材料的制备方法。
背景技术
碳化硼陶瓷具有优良的性能,尤其是其具备极高的硬度,在常温下,硬度仅次于金刚石和立方氮化硼,常温下化学性质稳定,几乎不与酸碱反应,可用作研磨剂、耐磨部件和制造坦克防弹装甲;其密度小,只有2.51~2.52g/cm3;碳化硼化学性质稳定,且中子吸收能力强,成为核工业中理想的防护材料,既可以作为核反应堆的控制棒,又可作为核反应屏蔽材料。
但是纯碳化硼陶瓷致命的弱点是其断裂韧性低,常常以脆性断裂为主,且致密化困难,难以烧结,需要价格昂贵的烧结炉,因此严重地限制了其在防弹材料等方面的应用。为了解决这些问题,如何提高碳化硼陶瓷的断裂韧性已经成为当前的研究热点。目前提高断裂韧性的方法有:采用颗粒和晶须增韧补强以及具有特定晶粒取向结构的排布等。采用颗粒增韧时,硼化物颗粒的应用较广泛,效果较理想;金属颗粒增韧时,由于碳化硼与金属润湿性差,限制了金属的加入量,而且由于金属的抗氧化性、耐腐蚀性差,金属的加入往往会降低碳化硼的化学稳定性,其增韧的机理主要是通过微裂纹增韧、裂纹偏转增韧。晶须增韧主要采用碳化硅晶须,但是其含量需要加以控制,不可过多,否则会使材料的抗弯强度下降,其增韧机理主要是裂纹偏转增韧、桥联增韧、拔出效应等效果来实现。采用具有特定晶粒取向结构的排布主要是指通过对材料的显微结构的调整能显著提高材料的断裂性能,降低材料中的晶体缺陷密度,但是调整需要适度,不然会造成微裂纹的连通和强度下降。
发明内容
本发明的目的在于提供一种短切碳纤维增强碳化硼基复合材料的制备方法,具有工艺简单、操作方便等优点,C/B4C同时具有短切碳纤维和碳化硼的优点,并且克服了B4C韧性低等缺陷。
为实现上述目的,本发明采取的技术方案如下:
一种短切碳纤维增强碳化硼基复合材料的制备方法,步骤如下:
(1)、将液态酚醛树脂分散于无水乙醇中,保证分散液中液态酚醛树脂的含量为5~12wt%;
(2)、按B4C粉与无水乙醇的质量比为(0.5~1.2)︰1计,将B4C粉加入步骤(1)所得溶液中,40~60 ℃搅拌均匀;
(3)、按短切碳纤维与B4C粉的质量比为(0.1~0.2)︰1计,将短切碳纤维加入步骤(2)所得溶液中,60~80 ℃继续搅拌,直至浆料粘稠不能搅拌为止;
(4)、将浆料烘干,造粒过筛,将所得颗粒粉置于模具中,压制成型,得到坯体;
(5)、用硅粉、钛粉中的一种或两者的组合物包覆坯体,置于石墨坩埚中,在真空1550~1650 ℃下反应1~3 h,即得到短切碳纤维增强碳化硼基复合材料。
较好地,所述液态酚醛树脂的固含量≥50 wt%。
较好地,所述B4C粉的平均直径为5 μm。
较好地,所述短切碳纤维的长度为5~20 mm。
较好地,所述烘干的温度为60~80 ℃。
较好地,过60~100目筛。
较好地,压制成型的压力控制在150~250MPa。
较好地,硅粉、钛粉组合时,硅粉︰钛粉的质量比为(1.8~2.5)︰1。
本发明提供一种短切碳纤维增强碳化硼基复合材料的制备方法,工艺简单,操作方便等。用短切碳纤维增强碳化硼,使其同时具有碳纤维和二硼化钛两者优异的性能,高强度,低密度,抗热震稳定性,良好的抗氧化性,碳纤维的加入更是弥补了B4C脆性较大的缺陷,有利于其在喷砂嘴、防弹装甲材料、中子吸收剂材料等方向越来越广泛的应用。同时由于加入碳纤维增强相,降低了工业上对碳化硼原料纯度的要求,从而大幅降低制备成本。因此C/B4C将受到越来越广泛的关注。
具体实施方式
以下结合具体实施例,对本发明做进一步说明。应理解,以下实施例仅用于说明本发明而非用于限制本发明的范围。
实施例1
一种短切碳纤维增强碳化硼基复合材料的制备方法,步骤如下:
(1)、将液态酚醛树脂(固含量为50 wt%)分散于无水乙醇中,保证分散液中液态酚醛树脂的含量为8 wt%;
(2)、按B4C粉(平均直径为5μm)与无水乙醇的质量比为1︰1计,将B4C粉加入步骤(1)所得溶液中,50 ℃加热搅拌均匀;
(3)、按10mm长的短切碳纤维与B4C粉的质量比为0.15︰1计,将短切碳纤维加入步骤(2)所得溶液中,70 ℃继续搅拌,直至浆料粘稠不能搅拌为止;
(4)、将浆料放置于干燥箱中,70 ℃烘干;造粒过60目筛后将粉粒置于模具中,在200MPa下压制成型,得到坯体;
(5)、用硅粉和钛粉的混合粉(Si/Ti的质量比为2.4︰1)包覆坯体,置于石墨坩埚中,在真空1600 ℃下保温2 h增加致密化,自然降温冷却,即得短切碳纤维增强碳化硼基复合材料。
本实施例制得的C/B4C复合材料的抗弯强度为(516MPa),断裂韧性为(9.4MPa·m1 /2)。
实施例2
一种短切碳纤维增强碳化硼基复合材料的制备方法,步骤如下:
(1)、将液态酚醛树脂(固含量为50 wt%)分散于无水乙醇中,保证分散液中液态酚醛树脂的含量为6 wt%;
(2)、按B4C粉(平均直径为5μm)与无水乙醇的质量比为0.5︰1计,将B4C粉加入步骤(1)所得溶液中,40 ℃加热搅拌均匀;
(3)、按5mm长的短切碳纤维与B4C粉的质量比为0.1︰1计,将短切碳纤维加入步骤(2)所得溶液中,60 ℃继续搅拌,直至浆料粘稠不能搅拌为止;
(4)、将浆料放置于干燥箱中,60 ℃烘干;造粒过80目筛后将粉粒置于模具中,在250MPa下压制成型,得到坯体;
(5)、用硅粉和钛粉的混合粉(Si/Ti的质量比为2︰1)包覆坯体,置于石墨坩埚中,在真空1550 ℃下保温3 h增加致密化,自然降温冷却,即得短切碳纤维增强碳化硼基复合材料。
本实施例制得的C/B4C复合材料的抗弯强度为(425MPa),断裂韧性为(7.1MPa·m1 /2)。
实施例3
一种短切碳纤维增强碳化硼基复合材料的制备方法,步骤如下:
(1)、将液态酚醛树脂(固含量为50 wt%)分散于无水乙醇中,保证分散液中液态酚醛树脂的含量为10 wt%;
(2)、按B4C粉(平均直径为5μm)与无水乙醇的质量比为1.2︰1计,将B4C粉加入步骤(1)所得溶液中,60 ℃加热搅拌均匀;
(3)、按15mm长的短切碳纤维与B4C粉的质量比为0.2︰1计,将短切碳纤维加入步骤(2)所得溶液中,80 ℃继续搅拌,直至浆料粘稠不能搅拌为止;
(4)、将浆料放置于干燥箱中,80 ℃烘干;造粒过100目筛后将粉粒置于模具中,在150MPa下压制成型,得到坯体;
(5)、用硅粉和钛粉的混合粉(Si/Ti的质量比为1.8︰1)包覆坯体,置于石墨坩埚中,在真空1650 ℃下保温1 h增加致密化,自然降温冷却,即得短切碳纤维增强碳化硼基复合材料。
本实施例制得的C/B4C复合材料的抗弯强度为(467MPa),断裂韧性为(7.9MPa·m1 /2)。
Claims (8)
1.一种短切碳纤维增强碳化硼基复合材料的制备方法,其特征在于:步骤如下:
(1)、将液态酚醛树脂分散于无水乙醇中,保证分散液中液态酚醛树脂的含量为5~12wt%;
(2)、按B4C粉与无水乙醇的质量比为(0.5~1.2)︰1计,将B4C粉加入步骤(1)所得溶液中,40~60 ℃搅拌均匀;
(3)、按短切碳纤维与B4C粉的质量比为(0.1~0.2)︰1计,将短切碳纤维加入步骤(2)所得溶液中,60~80 ℃继续搅拌,直至浆料粘稠不能搅拌为止;
(4)、将浆料烘干,造粒过筛,将所得颗粒粉置于模具中,压制成型,得到坯体;
(5)、用硅粉、钛粉中的一种或两者的组合物包覆坯体,置于石墨坩埚中,在真空1550~1650 ℃下反应1~3 h,即得到短切碳纤维增强碳化硼基复合材料。
2.如权利要求1所述的制备方法,其特征在于:所述液态酚醛树脂的固含量≥50 wt%。
3.如权利要求1所述的制备方法,其特征在于:所述B4C粉的平均直径为5 μm。
4.如权利要求1所述的制备方法,其特征在于:所述短切碳纤维的长度为5~20 mm。
5.如权利要求1所述的制备方法,其特征在于:所述烘干的温度为60~80 ℃。
6.如权利要求1所述的制备方法,其特征在于:过60~100目筛。
7.如权利要求1所述的制备方法,其特征在于:压制成型的压力控制在150~250MPa。
8.如权利要求1所述的制备方法,其特征在于:硅粉、钛粉组合时,硅粉︰钛粉的质量比为(1.8~2.5)︰1。
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CN113277863A (zh) * | 2021-06-18 | 2021-08-20 | 衡阳凯新特种材料科技有限公司 | 陶瓷复合材料及其制备方法、防弹板及装甲防护装备 |
CN115504800A (zh) * | 2022-11-21 | 2022-12-23 | 湖南大学 | 一种层状结构纤维增强碳化硼复合材料的制备方法、应用 |
CN115745642A (zh) * | 2022-11-21 | 2023-03-07 | 湖南大学 | 一种短切纤维增强碳化硼陶瓷片材及其制备方法、应用 |
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CN108911773A (zh) * | 2018-06-20 | 2018-11-30 | 浙江立泰复合材料股份有限公司 | 一种碳化硅纤维增强碳化硼陶瓷材料的制备方法 |
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