CN116199518B - 一种高厚度、低线膨胀系数的透波隔热瓦及其制备方法 - Google Patents
一种高厚度、低线膨胀系数的透波隔热瓦及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种高厚度、低线膨胀系数的透波隔热瓦及其制备方法;按照重量份数计,包括陶瓷纤维、烧结助剂、分散剂、消泡剂和淀粉,其中,烧结助剂添加量为陶瓷纤维总质量的2‑8%,分散剂添加量为陶瓷纤维总质量的0.1‑1.0%,消泡剂添加量为陶瓷纤维总质量的0.005‑0.1%,淀粉添加量为陶瓷纤维总质量的5‑15%;本发明的目的在于提供一种高厚度、低线膨胀系数透波隔热瓦及其制备方法,通过高厚度、低线膨胀系数透波隔热瓦的设计以解决现有技术中存在的传统的透波隔热瓦材料线性膨胀系数过大,将会导致隔热瓦与透波罩脱粘、开裂,从而导致隔热瓦隔热功能失灵,影响飞行器的正常通讯的技术问题。
Description
技术领域
本发明涉及透波瓦制备技术领域,尤其是涉及一种高厚度、低线膨胀系数的透波隔热瓦及其制备方法。
背景技术
透波隔热瓦材料以其低密度、低导热系数以及优异的介电性能而广泛应用于航空、航天的热防护和透波材料领域。目前,传统的透波隔瓦主要应用于透波窗口,对材料线膨胀系数要求不高,线膨胀系数较大。然而,随着航空航天技术的发展,越来越多的透波隔热瓦材料开始应用于飞行器天线罩罩体中,装配于透波罩内外表面。传统的透波隔热瓦材料线性膨胀系数过大,将会导致隔热瓦与透波罩脱粘、开裂,从而导致隔热瓦隔热功能失灵,影响飞行器的正常通讯。
因此,针对上述问题本发明急需提供一种高厚度、低线膨胀系数透波隔热瓦及其制备方法。
发明内容
本发明的目的在于提供一种高厚度、低线膨胀系数透波隔热瓦及其制备方法,通过高厚度、低线膨胀系数透波隔热瓦的设计以解决现有技术中存在的传统的透波隔热瓦材料线性膨胀系数过大,将会导致隔热瓦与透波罩脱粘、开裂,从而导致隔热瓦隔热功能失灵,影响飞行器的正常通讯的技术问题。
本发明提供的一种高厚度、低线膨胀系数的透波隔热瓦,包括陶瓷纤维、烧结助剂、分散剂、消泡剂和淀粉,其中,烧结助剂添加量为陶瓷纤维总质量的2-8%,分散剂添加量为陶瓷纤维总质量的0.1-1.0%,消泡剂添加量为陶瓷纤维总质量的0.005-0.1%,淀粉添加量为陶瓷纤维总质量的5-15%。
优选地,分散剂为聚丙烯酸铵或聚丙烯酰胺中的至少一种。
优选地,当分散剂为聚丙烯酸铵和聚丙烯酰胺,聚丙烯酸铵与聚丙烯酰胺质量比为(1-2):1。
优选地,陶瓷纤维为石英纤维、石英纤维棉或氧化铝纤维(莫来石纤维)中的至少两种。
优选地,石英纤维的长度为1mm-5mm,氧化铝纤维(莫来石纤维)的长度为1-5mm;石英纤维棉直径为1-7μm。
优选地,消泡剂为有机硅类消泡剂。
优选地,烧结剂为氮化硼或碳化硼中的至少一种.
优选地,当烧结剂为氮化硼和碳化硼,氮化硼质量和碳化硼质量质量比为(1-2):1。
本发明还提供了一种基于如上述中任一项所述的高厚度、低线膨胀系数的透波隔热瓦的制备方法,
按照比例将烧结助剂和淀粉加入到无水乙醇中,搅拌均匀后,再将分散剂和消泡剂加入到无水乙醇中,继续搅拌,获得混合液;
按照比例,将混合液和陶瓷纤维依次加入到去离子水中,搅拌均匀后,获得浆料;
将浆料倒入到模具中,抽滤压制,同时通过限位块控制湿坯高度,获得陶瓷隔热瓦湿坯;
将陶瓷隔热瓦湿坯在模具内干燥,脱模后再烘干,得到陶瓷隔热瓦干坯;
将陶瓷隔热瓦干坯分别在200-400℃烧结1-3小时、400-600℃烧结1-3小时、700-900℃烧结1-3小时,1100-1300℃高温烧结2-4h,得到低线膨胀系数透波隔热瓦。
优选地,去离子水与陶瓷纤维的质量比为(5-60):1;
依次将混合液、石英纤维棉、石英纤维、氧化铝纤维(莫来石纤维)依次加入到去离子水中进行搅拌,搅拌速度为1000-4000r/min;
陶瓷隔热瓦湿坯在模具进行干燥的温度为80-150℃,烘干12-48h;脱模后,在80-150℃烘干12-48h。
本发明提供的高厚度、低线膨胀系数的透波隔热瓦及其制备方法,与现有技术相比具有以下进步:
1、本发明提供的高厚度、低线膨胀系数的透波隔热瓦制备方法,由于合理的添加了分散剂和消泡剂,可以减小密度梯度,使得透波隔热瓦不会在烧结过程中开裂,获得的低线膨胀系数透波隔热瓦的密度为0.2-0.8g/cm3,可以获得厚度超过30mm的产品,同时产品的线膨胀系数<2×10-6/℃,进而可以获得具有高厚度、低线膨胀系数的透波隔热瓦。
2、本发明提供的高厚度、低线膨胀系数的透波隔热瓦,由于添加了氧化铝系纤维或者莫来石纤维,提高了隔热瓦的耐热性能,以石英纤维为主要成分,克服了纯氧化铝系纤维或者莫来石纤维的抗热震性差的缺点。
3、本发明在湿坯成型过程中,采用边搅拌、边放料的防腐,可以使得浆料各组分分散均匀,减少隔热瓦坯料出现孔洞的情况,力学性能更高。
4、湿坯在干燥过程中,先带模具烘干,可以使得隔热瓦湿坯体积保持稳定,最后,脱模烘干,可以使得隔热瓦湿坯烘干更充分。
5、在烧结过程中采用梯度烧结,在各个梯度设置保温时间,有效的避免烧结不充分以及烧结开裂的问题。
具体实施方式
下面将对本发明的技术方案进行清楚、完整地描述,显然,所描述的实施例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。
本发明提供的一种高厚度、低线膨胀系数的透波隔热瓦,包括陶瓷纤维、烧结助剂、分散剂、消泡剂和淀粉,其中,烧结助剂添加量为陶瓷纤维总质量的2-8%,分散剂添加量为陶瓷纤维总质量的0.1-1.0%,消泡剂添加量为陶瓷纤维总质量的0.005-0.1%,淀粉添加量为陶瓷纤维总质量的5-15%。
具体地,分散剂为聚丙烯酸铵或聚丙烯酰胺中的至少一种。
具体地,当分散剂为聚丙烯酸铵和聚丙烯酰胺,聚丙烯酸铵与聚丙烯酰胺质量比为(1-2):1。
具体地,陶瓷纤维为石英纤维、石英纤维棉或氧化铝纤维(莫来石纤维)中的至少两种。
具体地,石英纤维的长度为1mm-5mm,氧化铝纤维(莫来石纤维)的长度为1-5mm;石英纤维棉直径为1-7μm。
具体地,消泡剂为有机硅类消泡剂。
具体地,烧结剂为氮化硼或碳化硼中的至少一种.
具体地,当烧结剂为氮化硼和碳化硼,氮化硼质量和碳化硼质量质量比为(1-2):1。
本发明还提供了一种基于如上述中任一项所述的高厚度、低线膨胀系数的透波隔热瓦的制备方法,
按照比例将烧结助剂和淀粉加入到无水乙醇中,搅拌均匀后,再将分散剂和消泡剂加入到无水乙醇中,继续搅拌,获得混合液;
按照比例,将混合液和陶瓷纤维依次加入到去离子水中,搅拌均匀后,获得浆料;
将浆料倒入到模具中,抽滤压制,同时通过限位块控制湿坯高度,获得陶瓷隔热瓦湿坯;
将陶瓷隔热瓦湿坯在模具内干燥,脱模后再烘干,得到陶瓷隔热瓦干坯;
将陶瓷隔热瓦干坯分别在200-400℃烧结1-3小时、400-600℃烧结1-3小时、700-900℃烧结1-3小时,1100-1300℃高温烧结2-4h,得到低线膨胀系数透波隔热瓦。
具体地,去离子水与陶瓷纤维的质量比为(5-60):1;
依次将混合液、石英纤维棉、石英纤维、氧化铝纤维(莫来石纤维)依次加入到去离子水中进行搅拌,搅拌速度为1000-4000r/min;
陶瓷隔热瓦湿坯在模具进行干燥的温度为80-150℃,烘干12-48h;脱模后,在80-150℃烘干12-48h。
本发明在隔热瓦中以石英纤维为主要成分,有效的克服了纯氧化铝纤维或莫来石纤维的抗热震性差的缺点。
本发明采用硼系烧结助剂,高温下预陶瓷纤维反应充分,结构稳定,提高了热稳定性以及抗高温收缩性,线膨胀系数降低。
本发明在湿坯成型过程中,采用边搅拌,边放料的方法,可以使得浆料各组分分散均匀,减少隔热瓦坯料出现孔洞的情况,力学性能更高。
本发明在湿坯干燥过程中,先带模具烘干,可使得隔热瓦湿坯体积保持稳定,最后,脱模烘干,可以使得隔热瓦湿坯烘干更加充分。
本发明在烧结过程中采用梯度烧结的方法,在各个梯度设置保温时间,避免烧结不充分以及烧结开裂的问题。
本发明由于合理的添加了分散剂和消泡剂,可以减小密度梯度,使得透波隔热瓦不会在烧结过程中开裂,获得的低线膨胀系数透波隔热瓦的密度为0.2-0.8g/cm3,可以获得厚度超过30mm的产品,同时产品的线膨胀系数<2×10-6/℃,进而可以获得具有高厚度、低线膨胀系数的透波隔热瓦。
实施例一
高厚度、低线膨胀系数的透波隔热瓦的制备:
101)将99.25g的氮化硼和99.25g的碳化硼混合后,在加入317.6g的淀粉,混合均匀后,加入到5000ml无水乙醇中,继续搅拌均匀,再加入19.85g的分散剂和0.8g消泡剂,搅拌均匀后获得混合液;
102)将依次将混合液、540g的石英纤维棉、3430g石英纤维依次加入到100L去离子水中进行搅拌,搅拌速度为3000r/min,搅拌均匀后,获得浆料,在搅拌过程中,边搅拌边放入纤维;
103)将浆料倒入到模具中,抽滤压制,同时通过限位块控制湿坯高度,获得陶瓷隔热瓦湿坯;
104)将陶瓷隔热瓦湿坯在模具内干燥,干燥的温度为100℃,干燥35h,脱模后再烘干,烘干温度为100℃,烘干35h,得到陶瓷隔热瓦干坯;
105)将陶瓷隔热瓦干坯分别在300℃烧结2小时、500℃烧结2小时、800℃烧结2小时,1200℃高温烧结3h,得到低线膨胀系数透波隔热瓦。
其中,石英纤维的长度为3mm,石英纤维棉直径为5μm。
其中,分散剂为聚丙烯酸铵;
消泡剂为有机硅类消泡剂;
低线膨胀系数透波隔热瓦的密度为0.33g/cm3,可以获得厚度超过250mm低线膨胀系数透波隔热瓦。同时,室温导热率0.055W/m·K;平面拉伸强度0.6MPa;压缩强度1.75MPa。
再有获得的低线膨胀系数透波隔热瓦的线膨胀系数0.5×10-6/℃,700℃比热容1.1J(g·K),具有良好的隔热性、热稳定性和力学性能。
实施例二
高厚度、低线膨胀系数的透波隔热瓦的制备:
201)将92.56g的氮化硼和46.28g的碳化硼混合后,在加入231.4g的淀粉,混合均匀后,加入到4000ml无水乙醇中,继续搅拌均匀,再加入6.94g的分散剂和0.4g消泡剂,搅拌均匀后获得混合液;
202)将依次将混合液、317g的石英纤维棉、1461g石英纤维、536g莫来石纤维纤维依次加入到60L去离子水中进行搅拌,搅拌速度为3000r/min,搅拌均匀后,获得浆料;
203)将浆料倒入到模具中,抽滤压制,同时通过限位块控制湿坯高度,获得陶瓷隔热瓦湿坯;
204)将陶瓷隔热瓦湿坯在模具内干燥,干燥的温度为150℃,干燥48h,脱模后再烘干,烘干温度为150℃,烘干48h,得到陶瓷隔热瓦干坯;
205)将陶瓷隔热瓦干坯分别在400℃烧结1-3小时、600℃烧结3小时、900℃烧结3小时,1300℃高温烧结3h,得到低线膨胀系数透波隔热瓦。
其中,石英纤维的长度为5mm,莫来石纤维的长度为5mm;石英纤维棉直径为5μm。
其中,分散剂为聚丙烯酸铵和聚丙烯酰胺,聚丙烯酸铵和聚丙烯酰胺的质量比为1:1;
消泡剂为有机硅类消泡剂;
低线膨胀系数透波隔热瓦的密度为0.33g/cm3,可以获得厚度超过100mm低线膨胀系数透波隔热瓦。同时,室温导热率0.06W/m·K;平面拉伸强度0.65Mpa;压缩强度1.84Mpa。
再有获得的低线膨胀系数透波隔热瓦的线膨胀系数0.78×10-6/℃,700℃比热容1.1J(g·K),具有良好的隔热性、热稳定性和力学性能。
实施例三
高厚度、低线膨胀系数的透波隔热瓦的制备:
301)向22.48g的氮化硼中加入42.15g的淀粉,混合均匀后,加入到500ml无水乙醇中,继续搅拌均匀,再加入2.81g的分散剂和0.281g消泡剂,搅拌均匀后获得混合液;
302)将依次将混合液、36g的石英纤维棉、245g氧化铝系纤维依次加入到15L去离子水中进行搅拌,搅拌速度为4000r/min,搅拌均匀后,获得浆料;
303)将浆料倒入到模具中,抽滤压制,同时通过限位块控制湿坯高度,获得陶瓷隔热瓦湿坯;
304)将陶瓷隔热瓦湿坯在模具内干燥,干燥的温度为80℃,干燥12h,脱模后再烘干,烘干温度为80℃,烘干12h,得到陶瓷隔热瓦干坯;
305)将陶瓷隔热瓦干坯分别在200℃烧结1-3小时、400℃烧结1小时、700℃烧结1小时,1100℃高温烧结2h,得到低线膨胀系数透波隔热瓦。
其中,石英纤维的长度为3mm,氧化铝纤维的长度为5mm;石英纤维棉直径为5μm。
其中,分散剂为聚丙烯酸铵;
消泡剂为有机硅类消泡剂;
低线膨胀系数透波隔热瓦的密度为0.33g/cm3,可以获得厚度超过30mm低线膨胀系数透波隔热瓦。同时,室温导热率0.06W/m·K;平面拉伸强度0.7MPa;压缩强度>1.95MPa。
再有获得的低线膨胀系数透波隔热瓦的线膨胀系数1.2×10-6/℃,700℃比热容1.1J(g·K),具有良好的隔热性、热稳定性和力学性能。
实施例四
高厚度、低线膨胀系数的透波隔热瓦的制备:
401)将39.7g的氮化硼和39.7g的碳化硼混合后,在加入397的淀粉,混合均匀后,加入到5000ml无水乙醇中,继续搅拌均匀,再加入15.8g的分散剂和0.4g消泡剂,搅拌均匀后获得混合液;
402)将依次将混合液、540g的石英纤维棉、3430g石英纤维依次加入到100L去离子水中进行搅拌,搅拌速度为3000r/min,搅拌均匀后,获得浆料,在搅拌过程中,边搅拌边放入纤维;403)将浆料倒入到模具中,抽滤压制,同时通过限位块控制湿坯高度,获得陶瓷隔热瓦湿坯;
404)将陶瓷隔热瓦湿坯在模具内干燥,干燥的温度为100℃,干燥35h,脱模后再烘干,烘干温度为100℃,烘干35h,得到陶瓷隔热瓦干坯;
405)将陶瓷隔热瓦干坯分别在300℃烧结2小时、500℃烧结2小时、800℃烧结2小时,1200℃高温烧结3h,得到低线膨胀系数透波隔热瓦。
其中,石英纤维的长度为3mm,石英纤维棉直径为5μm。
其中,分散剂为聚丙烯酸铵与聚丙烯酰胺,聚丙烯酸铵与聚丙烯酰胺质量比为2:1;
消泡剂为有机硅类消泡剂;
低线膨胀系数透波隔热瓦的密度为0.33g/cm3,可以获得厚度超过250mm低线膨胀系数透波隔热瓦。同时,室温导热率0.056W/m·K;平面拉伸强度0.64MPa;压缩强度1.72MPa。
再有获得的低线膨胀系数透波隔热瓦的线膨胀系数0.53×10-6/℃,700℃比热容1.08J(g·K),具有良好的隔热性、热稳定性和力学性能。
实施例五
高厚度、低线膨胀系数的透波隔热瓦的制备:
501)将79.4g的氮化硼和198.5g的淀粉,混合均匀后,加入到8000ml无水乙醇中,继续搅拌均匀,再加入3.97g的分散剂和0.2g消泡剂,搅拌均匀后获得混合液;
502)将依次将混合液、540g的石英纤维棉、3430g石英纤维依次加入到100L去离子水中进行搅拌,搅拌速度为3000r/min,搅拌均匀后,获得浆料,在搅拌过程中,边搅拌边放入纤维;
503)将浆料倒入到模具中,抽滤压制,同时通过限位块控制湿坯高度,获得陶瓷隔热瓦湿坯;
504)将陶瓷隔热瓦湿坯在模具内干燥,干燥的温度为100℃,干燥35h,脱模后再烘干,烘干温度为100℃,烘干35h,得到陶瓷隔热瓦干坯;
505)将陶瓷隔热瓦干坯分别在300℃烧结2小时、500℃烧结2小时、800℃烧结2小时,1200℃高温烧结3h,得到低线膨胀系数透波隔热瓦。
其中,石英纤维的长度为3mm,石英纤维棉直径为5μm。
其中,分散剂为聚丙烯酸铵;
消泡剂为有机硅类消泡剂;
低线膨胀系数透波隔热瓦的密度为0.33g/cm3,可以获得厚度超过250mm低线膨胀系数透波隔热瓦。同时,室温导热率0.058W/m·K;平面拉伸强度0.62MPa;压缩强度1.85MPa。
再有获得的低线膨胀系数透波隔热瓦的线膨胀系数0.56×10-6/℃,700℃比热容1.05J(g·K),具有良好的隔热性、热稳定性和力学性能。
对比例
以实施例一为基准,区别在于不添加分散剂和消泡剂,获得透波隔热瓦的的密度为0.33g/cm3,室温热导率0.067W/m·K,平面拉伸强度0.45MPa,压缩强度1.45MPa,再有获得的低线膨胀系数透波隔热瓦的线膨胀系数0.7×10-6/℃,700℃比热容0.98J(g·K)。
实施例一的线膨胀系数低于对比例,由此,分散剂和消泡剂的加入可以减小密度梯度,使得透波隔热瓦不会在烧结过程中开裂。
最后应说明的是:以上各实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述各实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分或者全部技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。
Claims (5)
1.一种高厚度、低线膨胀系数的透波隔热瓦,其特征在于:包括陶瓷纤维、烧结助剂、分散剂、消泡剂和淀粉,其中,烧结助剂添加量为陶瓷纤维总质量的2-8%,分散剂添加量为陶瓷纤维总质量的0.1-1.0%,消泡剂添加量为陶瓷纤维总质量的0.005-0.1%,淀粉添加量为陶瓷纤维总质量的5-15%;分散剂为聚丙烯酸铵或聚丙烯酰胺中的至少一种;
陶瓷纤维为石英纤维、石英纤维棉或氧化铝纤维中的至少两种;石英纤维的长度为1mm-5mm,氧化铝纤维的长度为1-5mm;石英纤维棉直径为1-7μm;
消泡剂为有机硅类消泡剂;
高厚度、低线膨胀系数的透波隔热瓦的制备方法包括
按照比例将烧结助剂和淀粉加入到无水乙醇中,搅拌均匀后,再将分散剂和消泡剂加入到无水乙醇中,继续搅拌,获得混合液;
按照比例,将混合液和陶瓷纤维依次加入到去离子水中,搅拌均匀后,获得浆料;
将浆料倒入到模具中,抽滤压制,同时通过限位块控制湿坯高度,获得陶瓷隔热瓦湿坯;
将陶瓷隔热瓦湿坯在模具内干燥,脱模后再烘干,得到陶瓷隔热瓦干坯;
将陶瓷隔热瓦干坯分别在200-400℃烧结1-3小时、400-600℃烧结1-3小时、700-900℃烧结1-3小时,1100-1300℃高温烧结2-4h,得到低线膨胀系数透波隔热瓦。
2.根据权利要求1所述的高厚度、低线膨胀系数的透波隔热瓦,其特征在于:当分散剂为聚丙烯酸铵和聚丙烯酰胺,聚丙烯酸铵与聚丙烯酰胺质量比为(1-2):1。
3.根据权利要求1所述的高厚度、低线膨胀系数的透波隔热瓦,其特征在于:烧结助剂为氮化硼或碳化硼中的至少一种。
4.根据权利要求3所述的高厚度、低线膨胀系数的透波隔热瓦,其特征在于:当烧结助剂为氮化硼和碳化硼,氮化硼和碳化硼质量比为(1-2):1。
5.根据权利要求4所述的高厚度、低线膨胀系数的透波隔热瓦,其特征在于:去离子水与陶瓷纤维的质量比为(5-60):1;
依次将混合液、石英纤维棉、石英纤维、氧化铝纤维依次加入到去离子水中进行搅拌,搅拌速度为1000-4000r/min;
陶瓷隔热瓦湿坯在模具进行干燥的温度为80-150℃,烘干12-48h;脱模后,在80-150℃烘干12-48h。
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