CN106830969A - 一种刚性短切碳纤维预制体的制备方法 - Google Patents
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Abstract
本发明公开一种刚性短切碳纤维预制体的制备方法。将短切碳纤维、热塑性酚醛树脂粉、多糖类高分子和分散剂加入到水中,研磨均匀,制成料浆;将所得料浆加热至40~80℃,搅拌形成溶胶;将所得溶胶倒入模具内,待其形成凝胶之后,在100~120℃常压干燥60~120min,再自然冷却至室温,制得短切碳纤维预制体生坯;对短切碳纤维预制体生坯进行高温碳化处理,制得刚性短切碳纤维预制体。本发明以多糖类高分子作为短切碳纤维的粘接剂,采用溶胶‑凝胶、常压干燥、高温碳化的方法制备出了刚性短切碳纤维预制体,克服了现有技术制备碳纤维预制体时材料易分层、性能各向异性明显、工艺耗时的缺陷。
Description
技术领域
本发明属于烧蚀体材料领域,具体涉及一种刚性短切碳纤维预制体的制备方法。
背景技术
热防护系统(Thermal protection system, TPS) 是保护飞行器在高超声速穿越星球大气层时免遭严酷气动加热环境的损伤,安全进入星球的飞行器子系统。通常可将热防护材料分为可重复使用热防护材料和烧蚀热防护材料两类。酚醛浸渍碳烧蚀体材料(Phenolic impregnated carbon ablator, PICA)是众多烧蚀型热防护材料的一种。公开资料表明,PICA是由酚醛树脂溶液浸渍短切碳纤维预制体制备出具有纤维增强的酚醛气凝胶结构材料。根据PICA的制备工艺流程,可将其分为刚性短切碳纤维预制体的制备和酚醛树脂碳气凝胶结构的制备。对于PICA刚性短切碳纤维预制体的制备,目前主要采用真空抽滤成型和压力抽滤成型。真空抽滤成型,(1)工艺耗时,需要使用价格较贵的模具造型设备;(2)材料性能呈现各向异性(碳纤维沿xy面择优取向,在z向纤维含量较少);(3)碳纤维层层抽滤叠加,易分层。压力抽滤成型,工艺相对简单,解决了碳纤维叠加易分层的缺陷,但是仍无法解决材料性能各向异性的问题。
发明内容
本发明的目的旨在提供一种刚性短切碳纤维预制体的制备方法,从而克服现有技术中短切碳纤维预制体制备过程中材料易分层、性能各向异性、工艺耗时的缺陷。
为实现上述目的,本发明采用的技术方案如下:
一种刚性短切碳纤维预制体的制备方法,包括以下步骤:
(1)将短切碳纤维、热塑性酚醛树脂粉、多糖类高分子和分散剂加入到水中,研磨均匀,制成料浆;其中,短切碳纤维占短切碳纤维和水总质量的40~60wt%,分散剂占水质量的0.5~1.0wt%,热塑性酚醛树脂粉占短切碳纤维质量的5~10wt%,多糖类高分子占短切碳纤维质量的1~8wt%;
(2)将步骤(1)所得料浆加热至40~80℃,搅拌形成溶胶;
(3)将步骤(2)所得溶胶倒入模具内,待其形成凝胶之后,在100~120℃常压干燥60~120min,再自然冷却至室温,制得短切碳纤维预制体生坯;
(4)对步骤(3)所得短切碳纤维预制体生坯进行高温碳化处理,制得刚性短切碳纤维预制体。
较好地,所述短切碳纤维的长度为100μm~1mm。
较好地,所述热塑性酚醛树脂粉的粒径为80~300目。
较好地,所述多糖类高分子为琼脂、琼脂糖、明胶或果胶。
较好地,所述分散剂为聚丙烯酰胺、聚丙烯酸钠、羟乙基纤维素、羧甲基纤维素、十二烷基苯磺酸钠、聚丙烯酸或聚丙烯酸铵。
较好地,步骤(4)具体为:将步骤(3)所得短切碳纤维预制体生坯放置于炭化炉中,以100~120℃/h的升温速率升温至300~500℃,保温60~90min;再以25~50℃/h的升温速率升温至600~800℃,保温60~90min;再以10~25℃/h的升温速率升温至900~1000℃,保温60~90min;降至室温,制得刚性短切碳纤维预制体。
本发明提供了一种刚性短切碳纤维预制体的制备方法,以短切碳纤维作为增强体,以多糖类高分子作为短切碳纤维的粘接剂,以热塑性酚醛树脂作为后续碳气凝胶的前驱体,采用溶胶-凝胶、常压干燥、高温碳化的方法制备出了刚性短切碳纤维预制体,克服了现有技术制备碳纤维预制体时材料易分层、性能各向异性明显、工艺耗时的缺陷。由于是将短切碳纤维、热塑性酚醛树脂、多糖类高分子与水混合制备成料浆,然后将该料浆倒入模具中,经常压干燥、高温碳化获得刚性短切碳纤维预制体,可根据最终零部件结构的不同,可将具有低粘度、高短切碳纤维含量的料浆浇注进不同形状及尺寸的模具中,具有结构的可调节性。根据本发明制备出的刚性短切碳纤维预制体,可用于生产酚醛浸渍碳烧蚀体材料,该种材料具有良好的隔热性,可用于高超声速飞行器的热防护系统。
具体实施方式
以下结合具体实施例,对本发明做进一步的说明。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
一种刚性短切碳纤维预制体的制备方法,包括以下步骤:
(1)将短切碳纤维粉分散到分散剂含量0.5wt%的水溶液中,制成料浆,其中分散剂为聚丙烯酸,短切碳纤维的长度为100μm,短切碳纤维占短切碳纤维和水总质量的40wt%;
(2)将5wt%(以所用短切碳纤维粉的质量为基准,酚醛树脂的质量为短切碳纤维粉质量的5wt%)的热塑性酚醛树脂粉(粒径80目)加入到步骤(1)所得料浆中;
(3)将1wt%(以所用短切碳纤维粉的质量为基准,琼脂糖的质量为短切碳纤维粉质量的1wt%)的琼脂糖粉加入到步骤(2)所得料浆中;
(4)将步骤(3)所得料浆放入球磨机中,混合均匀;
(5)将步骤(4)中混合均匀的料浆加热至40℃,搅拌至形成溶胶;
(6)将步骤(5)所得溶胶倒入模具内,待其形成凝胶之后,放入100℃烘箱内常压干燥120min,再自然冷却至室温,制得短切碳纤维预制体生坯;
(7)将步骤(6)所得短切碳纤维预制体生坯放置于炭化炉中,以120℃/h的升温速率升温至300℃,保温60min;再以50℃/h的升温速率升温至600℃,保温60min;再以25℃/h的升温速率升温至900℃,保温60min;断电随炉自然降至室温,获得刚性短切碳纤维预制体。
对制得的刚性短切碳纤维预制体的性能进行测试:材料密度为0.27g/cm3,xy向压缩强度为0.22MPa,z向压缩强度为0.35MPa,xy向热导率为0.27W/m·K(室温),z向热导率为0.33W/m·K(室温)。
实施例2
一种刚性短切碳纤维预制体的制备方法,包括以下步骤:
(1)将短切碳纤维粉分散到分散剂含量0.5wt%的水溶液中,制成料浆,其中分散剂为聚丙烯酸铵,短切碳纤维的长度为500μm,短切碳纤维占短切碳纤维和水总质量的50wt%;
(2)将5wt%(以所用短切碳纤维粉的质量为基准,酚醛树脂的质量为短切碳纤维粉质量的5wt%)的热塑性酚醛树脂粉(粒径100目)加入到步骤(1)所得料浆中;
(3)将5wt%(以所用短切碳纤维粉的质量为基准,明胶粉的质量为短切碳纤维粉质量的5wt%)的明胶粉加入到步骤(2)所得料浆中;
(4)将步骤(3)所得料浆放入球磨机中,混合均匀;
(5)将步骤(4)中混合均匀的料浆加热至60℃,搅拌至形成溶胶;
(6)将步骤(5)所得溶胶倒入模具内,待其形成凝胶之后,放入110℃烘箱内常压干燥90min,再自然冷却至室温,制得短切碳纤维预制体生坯;
(7)将步骤(6)所得短切碳纤维预制体生坯放置于炭化炉中,以110℃/h的升温速率升温至400℃,保温90min;再以30℃/h的升温速率升温至700℃,保温90min;再以15℃/h的升温速率升温至950℃,保温90min;断电随炉自然降至室温,获得刚性短切碳纤维预制体。
对制得的刚性短切碳纤维预制体的性能进行测试:材料密度为0.20g/cm3,xy向压缩强度为0.29MPa,z向压缩强度为0.28MPa,xy向热导率为0.19W/m·K(室温),z向热导率为0.22W/m·K(室温)。
对照例2′
与实施例2的不同之处在于:省略步骤(3),即没有加入明胶粉。其它均同实施例2。
对制得的刚性短切碳纤维预制体的性能进行测试:材料密度为0.23g/cm3,xy向压缩强度为0.31MPa,z向压缩强度为0.17MPa,xy向热导率为0.25W/m·K(室温),z向热导率为0.19W/m·K(室温)。
实施例3
一种刚性短切碳纤维预制体的制备方法,包括以下步骤:
(1)将短切碳纤维粉分散到分散剂含量1.0wt%的水溶液中,制成料浆,其中分散剂为聚丙烯酰胺,短切碳纤维的长度为1mm,短切碳纤维占短切碳纤维和水总质量的60wt%;
(2)将10wt%(以所用短切碳纤维粉的质量为基准,酚醛树脂的质量为短切碳纤维粉质量的10wt%)的热塑性酚醛树脂粉(300目)加入到步骤(1)所得料浆中,混合制得料浆;
(3)将7.5wt%(以所用短切碳纤维粉的质量为基准,果胶粉的质量为短切碳纤维粉质量的7.5wt%)的果胶粉加入到步骤(2)所得料浆中;
(4)将步骤(3)所得料浆放入球磨机中,混合均匀;
(5)将步骤(4)中混合均匀的料浆加热至80℃,搅拌至形成溶胶;
(6)将步骤(5)所得溶胶倒入模具内,待其形成凝胶之后,放入120℃烘箱内常压干燥60min,再自然冷却至室温,制得短切碳纤维预制体生坯;
(7)将步骤(6)所得短切碳纤维预制体生坯放置于炭化炉中,以100℃/h的升温速率升温至500℃,保温90min;再以25℃/h的升温速率升温至800℃,保温90min;再以10℃/h的升温速率升温至1000℃,保温90min;断电随炉自然降至室温,获得刚性短切碳纤维预制体。
对制得的刚性短切碳纤维预制体的性能进行测试:材料密度为0.23g/cm3,xy向压缩强度为0.31MPa,z向压缩强度为0.34MPa,xy向热导率为0.38W/m·K(室温),z向热导率为0.36W/m·K(室温)。
结论:
1、根据发明人的研究,当所述短切碳纤维占短切碳纤维和水总质量的40~60wt%时,均可以制得本发明的刚性短切碳纤维预制体。当短切炭纤维的含量超过60wt%时,短切碳纤维不易均匀分散;而当短切炭纤维的含量低于40wt%时,纤维之间不易搭接,不能形成性能良好的三维网状结构;
2、通过上述实施例1~3可知,根据本发明所提供的方法制备的刚性短切碳纤维预制体的密度、压缩强度和热导率均满足作为酚醛树脂浸渍碳烧蚀体的要求。在上述三个实施例中,特别是当短切碳纤维占短切碳纤维和水总质量的50wt%、酚醛树脂粉的含量为5wt%、明胶粉的质量为5wt%时,制备出的刚性短切碳纤维预制体的性能最优;
3、通过实施例2与对照例2′可知:在其他条件完全相同的条件下,加入多糖类高分子可以克服制备碳纤维预制体时性能各向异性明显的缺陷。
以上所述实施例,仅为本发明的较佳实施例,并非用以限定本发明的范围,本发明的上述实施例还可以做出各种变化。即凡是依据本发明申请的权利要求书及说明书内容所作的简单、等效变化与修饰,皆落入本发明专利的权利要求保护范围。本发明未详尽描述的均为常规技术内容。
Claims (6)
1.一种刚性短切碳纤维预制体的制备方法,其特征在于,包括以下步骤:
(1)将短切碳纤维、热塑性酚醛树脂粉、多糖类高分子和分散剂加入水中,研磨均匀,制成料浆;其中,短切碳纤维占短切碳纤维和水总质量的40~60wt%,分散剂占水质量的0.5~1.0wt%,热塑性酚醛树脂粉占短切碳纤维质量的5~10wt%,多糖类高分子占短切碳纤维质量的1~8wt%;
(2)将步骤(1)所得料浆加热至40~80℃,搅拌形成溶胶;
(3)将步骤(2)所得溶胶倒入模具内,待其形成凝胶之后,在100~120℃常压干燥60~120min,再自然冷却至室温,制得短切碳纤维预制体生坯;
(4)对步骤(3)所得短切碳纤维预制体生坯进行高温碳化处理,制得刚性短切碳纤维预制体。
2.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100μm~1mm。
3.如权利要求1所述的制备方法,其特征在于:所述热塑性酚醛树脂粉的粒径为80~300目。
4.如权利要求1所述的制备方法,其特征在于:所述多糖类高分子为琼脂、琼脂糖、明胶或果胶。
5.如权利要求1所述的制备方法,其特征在于:所述分散剂为聚丙烯酰胺、聚丙烯酸钠、羟乙基纤维素、羧甲基纤维素、十二烷基苯磺酸钠、聚丙烯酸或聚丙烯酸铵。
6.如权利要求1所述的制备方法,其特征在于,步骤(4)具体为:将步骤(3)所得短切碳纤维预制体生坯放置于炭化炉中,以100~120℃/h的升温速率升温至300~500℃,保温60~90min;再以25~50℃/h的升温速率升温至600~800℃,保温60~90min;再以10~25℃/h的升温速率升温至900~1000℃,保温60~90min;降至室温,制得刚性短切碳纤维预制体。
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