CN116514620A - 一种基于碳纤维陶瓷化的烟幕干扰材料及其制备方法 - Google Patents
一种基于碳纤维陶瓷化的烟幕干扰材料及其制备方法 Download PDFInfo
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 73
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 73
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 239000000463 material Substances 0.000 title claims abstract description 31
- 239000000779 smoke Substances 0.000 title claims abstract description 22
- 238000002468 ceramisation Methods 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000203 mixture Substances 0.000 claims abstract description 30
- 238000001035 drying Methods 0.000 claims abstract description 18
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 17
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 13
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 20
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 9
- 229920002401 polyacrylamide Polymers 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 230000002452 interceptive effect Effects 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 description 12
- 239000010410 layer Substances 0.000 description 11
- 230000009286 beneficial effect Effects 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 239000000835 fiber Substances 0.000 description 4
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- 229910002027 silica gel Inorganic materials 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
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- 230000007062 hydrolysis Effects 0.000 description 2
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
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- 230000005674 electromagnetic induction Effects 0.000 description 1
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- 238000004880 explosion Methods 0.000 description 1
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- 238000007667 floating Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
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- C06D—MEANS FOR GENERATING SMOKE OR MIST; GAS-ATTACK COMPOSITIONS; GENERATION OF GAS FOR BLASTING OR PROPULSION (CHEMICAL PART)
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Abstract
本发明公开了一种基于碳纤维陶瓷化的烟幕干扰材料及其制备方法,制备方法包括以下步骤:对碳纤维进行预处理,得到第一混合物;向第一混合物加入正硅酸乙酯、氨水、乙醇,得到第二混合物;对第二混合物进行烘干处理,得到SiO2包覆碳纤维的烟幕干扰材料。
Description
技术领域
本发明属于烟幕干扰材料技术领域,具体地说涉及一种基于碳纤维陶瓷化的烟幕干扰材料及其制备方法。
背景技术
碳纤维(carbon fiber,CF)是由有机纤维经碳化及石墨化处理得到的微晶石墨材料。作为一种新兴的无源干扰烟幕材料,短切碳纤维具有密度小、导电性好的特点,还具有良好的漂浮性能,能有效衰减电磁波信号强度,同时对红外和毫米波产生干扰作用。
然而短切碳纤维由于其本身具有高导电性、尺寸小,长径比大的特点,易发生断裂且纤维间具有较大的团聚粘附力,从而易导致装填均一性差、难分散、对电子元器件具有电击穿等问题。
发明内容
针对上述问题,本发明设计了一种基于碳纤维陶瓷化的烟幕干扰材料制备方法,包括以下步骤:
对碳纤维进行预处理,得到第一混合物;
向第一混合物加入正硅酸乙酯、氨水、乙醇,得到第二混合物;
对第二混合物进行烘干处理,得到SiO2包覆碳纤维的烟幕干扰材料。
与现有技术相比,本发明的有益效果为:本发明以正硅酸乙脂为前驱物,正硅酸乙酯水解后会在碳纤维表面形成硅胶Si(OH)4产物,经加热后Si(OH)4会形成均匀包覆在碳纤维表面的SiO2陶瓷层,不仅能够提高纤维的分散均匀性,使其具有良好的空中悬浮性,还可以提高碳纤维的绝缘性,同时保证烟幕干扰材料具有良好的电磁感应能力、兼容红外及毫米波段,大量使用时不会造成附近电器损伤,能够充分发挥材料自身优异的电磁衰减性能,有利于提高武器装备的生存能力以及作战机动效能。
本发明对陶瓷化后的单丝碳纤维电阻率进行测试,发现其电阻率不小于105欧米,因此解决了碳纤维导电的问题,有利于防止播散在空气中的碳纤维引起电力设备短路甚至爆炸。
优选的,所述正硅酸乙酯、氨水、乙醇的质量比为(22-26):(5-7):(60-100)。
优选的,将氨水和乙醇混合,得到溶液A;
将正硅酸乙酯和乙醇混合,得到溶液B;
将溶液A和溶液B滴加至第一混合物中,得到第二混合物。
本优选方案的有益效果为:分步滴加正硅酸乙酯和氨水,可以使碳纤维表面的SiO2陶瓷层薄且均匀,本发明碳纤维表面陶瓷层的厚度为0.6-1μm,满足使用需求。
优选的,所述溶液A中氨水与乙醇的质量比为:(5-7):(30-48);
所述溶液B中正硅酸乙酯与乙醇的质量比为:(11-13):(15-24)。
本优选方案的有益效果为:采用低浓度的溶液B,能够控制正硅酸乙酯的水解产物在碳纤维表面的成核与生长,得到最优的陶瓷化包覆处理工艺。
优选的,所述烘干处理的加热温度为60-80℃,加热时间为2-4h,转速为500r。
本优选方案的有益效果为:在烘干处理阶段,有利于促进正硅酸乙酯水解,在碳纤维表面形成硅胶Si(OH)4产物。
优选的,对加热后的第二混合物进行抽滤、洗涤、烘干处理,得到SiO2包覆碳纤维的烟幕干扰材料;所述烘干温度为80-100℃。
本优选方案的有益效果为:硅胶Si(OH)4在烘干阶段发生陶瓷化,形成包覆在碳纤维表面的SiO2玻璃层,从而提高碳纤维的绝缘性,优化其吸波消光性能。
优选的,所述预处理包括:将聚丙烯酰胺、硅烷偶联剂、碳纤维在去离子水中分散均匀,进行水浴加热。
本优选方案的有益效果为:聚丙烯酰胺作为分散剂能够提高碳纤维的疏水性和分散性;硅烷偶联剂的活性基团在溶液中可水解,与碳纤维表面的羟基和羧基结合,定向构建羟基官能团,附着在碳纤维的表面。经烘干脱水后,硅烷偶联剂在碳纤维表面形成醚键,可以在无机和有机物质界面间架起“分子桥”,把两种性质悬殊的材料连接在一起,提高碳纤维的分散性,有利于解决碳纤维易发生团聚的问题。
优选的,所述碳纤维与去离子水的质量比为:(10-11):(300-500),碳纤维的长度为1.5-4mm,
所述聚丙烯酰胺为碳纤维质量的0.5-1%,所述硅烷偶联剂为碳纤维质量的5-10%。
优选的,所述水浴加热的温度为80-100℃,水浴加热过程中以400-600r的转速搅拌15-25min。
本发明还设计了一种基于碳纤维陶瓷化的烟幕干扰材料,所述烟幕干扰材料应用上述的制备方法制备得到。
与现有技术相比,本发明的有益效果为:本发明通过表面微纳绝缘功能层界面构筑,调控关键技术,制备的烟幕干扰材料成功解决了传统材料干扰波段单一、遮蔽时间短、武器装备电子元器件电击穿的问题,同时石英陶瓷化负载碳纤维解决了碳纤维易团聚的问题。
附图说明
图1为本发明实施例2烟幕干扰材料的电镜图。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚,下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述。
实施例1
本实施例提供了一种基于碳纤维陶瓷化的烟幕干扰材料制备方法,包括以下步骤:
S1:碳纤维预处理:取200g的1.5mm长的碳纤维、1g聚丙烯酰胺、10g硅烷偶联剂在6L的去离子水中分散均匀,进行水浴加热。
S2:将S1的溶液在80℃的温度下进行水浴加热,水浴加热过程中以400r的转速搅拌15min,得到第一混合物。
S3:按5:32的质量比,将50g氨水和400mL乙醇混合,得到溶液A;
按11:16的质量比,将220g正硅酸乙酯和400mL乙醇混合,得到溶液B。
S4:将溶液A和溶液B滴加至S2的第一混合物中,得到第二混合物,将第二混合物加热至60℃,反应时间为2h。
S5:对加热后的第二混合物进行抽滤、洗涤、烘干处理,其中烘干温度为80℃,得到SiO2包覆碳纤维的烟幕干扰材料。
本实施例检测到包覆碳纤维的陶瓷层厚度为0.7μm,对陶瓷化后的单丝碳纤维电阻率进行测试,其电阻率不小于10 5欧米,证明陶瓷化可解决碳纤维导电的问题。
实施例2
本实施例提供了一种基于碳纤维陶瓷化的烟幕干扰材料制备方法,包括以下步骤:
S1:碳纤维预处理:取210g的3mm长的碳纤维、1.47g聚丙烯酰胺、14.7g硅烷偶联剂在8L的去离子水中分散均匀,进行水浴加热。
S2:将S1的溶液在90℃的温度下进行水浴加热,水浴加热过程中以500r的转速搅拌20min,得到第一混合物。
S3:按6:40的质量比,将60g氨水和500mL乙醇混合,得到溶液A;
按12:20的质量比,将240g正硅酸乙酯和500mL乙醇混合,得到溶液B。
S4:将溶液A和溶液B滴加至S2的第一混合物中,得到第二混合物,将第二混合物加热至70℃,反应时间为3h。
S5:对加热后的第二混合物进行抽滤、洗涤、烘干处理,其中烘干温度为90℃,得到SiO2包覆碳纤维的烟幕干扰材料。
本实施例制得的烟幕干扰材料的电镜图如图1所示,其中a、b、c、d图分别为不同放大倍数下的烟幕干扰材料,由图1可知,SiO2包覆在碳纤维表面,形成了较为均匀的陶瓷层,为进一步验证碳纤维表面确实有SiO2层附着,本实施例在烟幕干扰材料上任选了三个扫描点进行检测,检测结果如表1-3所示:
表1
Element | Weight% | Atomic% | Net Int. | Error% | Kratio | Z | A | F |
C K | 88.54 | 92.68 | 354.68 | 3.41 | 0.7239 | 0.9422 | 0.8678 | 1.0000 |
O K | 6.46 | 5.08 | 12.51 | 25.81 | 0.0148 | 0.9054 | 0.2525 | 1.0000 |
Si K | 5.00 | 2.24 | 39.16 | 6.89 | 0.0413 | 0.8319 | 0.9888 | 1.0044 |
表2
Element | Weight% | Atomic% | Net Int. | Error% | Kratio | Z | A | F |
C K | 84.82 | 90.58 | 572.08 | 4.38 | 0.5983 | 0.9446 | 0.7468 | 1.0000 |
O K | 7.19 | 5.77 | 27.84 | 20.18 | 0.0169 | 0.9079 | 0.2581 | 1.0000 |
Si K | 7.99 | 3.65 | 122.44 | 4.12 | 0.0661 | 0.8344 | 0.9884 | 1.0035 |
表3
Element | Weight% | Atomic% | Net Int. | Error% | Kratio | Z | A | F |
C K | 88.79 | 92.94 | 248.05 | 3.86 | 0.7213 | 0.9422 | 0.8623 | 1.0000 |
O K | 6.04 | 4.75 | 8.18 | 38.64 | 0.0138 | 0.9054 | 0.2516 | 1.0000 |
Si K | 5.17 | 2.31 | 28.45 | 8.00 | 0.0427 | 0.8319 | 0.9895 | 1.0043 |
其中,表1为Spot 1的EDS扫描结果,表2为Spot 2的EDS扫描结果,表3为Spot 3的EDS扫描结果,由表1-3可知,Si和O的EDS误差偏差较小,即SiO2均匀包覆在碳纤维表面形成了陶瓷层。
本实施例检测到包覆碳纤维的陶瓷层厚度为0.8μm,对陶瓷化后的单丝碳纤维电阻率进行测试,其电阻率不小于10 5欧米,证明陶瓷化可解决碳纤维导电的问题。
实施例3
本实施例提供了一种基于碳纤维陶瓷化的烟幕干扰材料制备方法,包括以下步骤:
S1:碳纤维预处理:取220g的4mm长的碳纤维、2.2g聚丙烯酰胺、22g硅烷偶联剂在10L的去离子水中分散均匀,进行水浴加热。
S2:将S1的溶液在100℃的温度下进行水浴加热,水浴加热过程中以600r的转速搅拌25min,得到第一混合物。
S3:按7:48的质量比,将70g氨水和600mL乙醇混合,得到溶液A;
按13:24的质量比,将260g正硅酸乙酯和600mL乙醇混合,得到溶液B。
S4:将溶液A和溶液B滴加至S2的第一混合物中,得到第二混合物,将第二混合物加热至80℃,反应时间为4h。
S5:对加热后的第二混合物进行抽滤、洗涤、烘干处理,其中烘干温度为100℃,得到SiO2包覆碳纤维的烟幕干扰材料。
本实施例检测到包覆碳纤维的陶瓷层厚度为0.9μm,对陶瓷化后的单丝碳纤维电阻率进行测试,其电阻率不小于10 5欧米,证明陶瓷化可解决碳纤维导电的问题。
以上实施例仅用以说明本发明的技术方案,而非对其限制;基于本发明的实施例,本领域普通技术人员在没有作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。尽管参照前述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精神和范围。
Claims (10)
1.一种基于碳纤维陶瓷化的烟幕干扰材料制备方法,其特征在于,包括以下步骤:
对碳纤维进行预处理,得到第一混合物;
向第一混合物加入正硅酸乙酯、氨水、乙醇,得到第二混合物;
对第二混合物进行烘干处理,得到SiO2包覆碳纤维的烟幕干扰材料。
2.根据权利要求1所述的制备方法,其特征在于,所述正硅酸乙酯、氨水、乙醇的质量比为(22-26):(5-7):(60-100)。
3.根据权利要求1所述的制备方法,其特征在于,将氨水和乙醇混合,得到溶液A;
将正硅酸乙酯和乙醇混合,得到溶液B;
将溶液A和溶液B滴加至第一混合物中,得到第二混合物。
4.根据权利要求3所述的制备方法,其特征在于,所述溶液A中的氨水与乙醇的质量比为:(5-7):(30-48);
所述溶液B中的正硅酸乙酯与乙醇的质量比为:(11-13):(15-24)。
5.根据权利要求1所述的制备方法,其特征在于,所述烘干处理的加热温度为60-80℃,加热时间为2-4h。
6.根据权利要求1所述的制备方法,其特征在于,对加热后的第二混合物进行抽滤、洗涤、烘干处理,得到SiO2包覆碳纤维的烟幕干扰材料;
所述烘干温度为80-100℃。
7.根据权利要求1所述的制备方法,其特征在于,所述预处理包括:将聚丙烯酰胺、硅烷偶联剂、碳纤维在去离子水中分散均匀,进行水浴加热。
8.根据权利要求7所述的制备方法,其特征在于,所述碳纤维与去离子水的质量比为:(10-11):(300-500),
所述聚丙烯酰胺为碳纤维质量的0.5-1%,所述硅烷偶联剂为碳纤维质量的5-10%。
9.根据权利要求7所述的制备方法,其特征在于,所述水浴加热的温度为80-100℃,水浴加热过程中以400-600r的转速搅拌15-25min。
10.一种基于碳纤维陶瓷化的烟幕干扰材料,其特征在于,所述烟幕干扰材料应用权利要求1-9任一所述的制备方法制备得到。
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