CN111890764A - 复合材料、其制备方法及应用 - Google Patents
复合材料、其制备方法及应用 Download PDFInfo
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- CN111890764A CN111890764A CN201910367188.6A CN201910367188A CN111890764A CN 111890764 A CN111890764 A CN 111890764A CN 201910367188 A CN201910367188 A CN 201910367188A CN 111890764 A CN111890764 A CN 111890764A
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- composite material
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- dimensional graphene
- graphene film
- copper foil
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- 239000002131 composite material Substances 0.000 title claims abstract description 124
- 238000002360 preparation method Methods 0.000 title claims description 5
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 101
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 94
- 239000000835 fiber Substances 0.000 claims abstract description 93
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 39
- 239000004744 fabric Substances 0.000 claims description 34
- 239000000243 solution Substances 0.000 claims description 34
- 239000011889 copper foil Substances 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 25
- 238000005530 etching Methods 0.000 claims description 23
- 239000003292 glue Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 14
- 229910052802 copper Inorganic materials 0.000 claims description 13
- 239000010949 copper Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 11
- 238000002791 soaking Methods 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 239000011347 resin Substances 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- 238000005229 chemical vapour deposition Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- LPEKGGXMPWTOCB-UHFFFAOYSA-N 8beta-(2,3-epoxy-2-methylbutyryloxy)-14-acetoxytithifolin Natural products COC(=O)C(C)O LPEKGGXMPWTOCB-UHFFFAOYSA-N 0.000 claims description 2
- ODQWQRRAPPTVAG-GZTJUZNOSA-N doxepin Chemical compound C1OC2=CC=CC=C2C(=C/CCN(C)C)/C2=CC=CC=C21 ODQWQRRAPPTVAG-GZTJUZNOSA-N 0.000 claims description 2
- 229940057867 methyl lactate Drugs 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 229920000193 polymethacrylate Polymers 0.000 claims description 2
- 239000010410 layer Substances 0.000 description 84
- 239000004699 Ultra-high molecular weight polyethylene Substances 0.000 description 29
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 description 29
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 24
- 230000008569 process Effects 0.000 description 20
- 238000012360 testing method Methods 0.000 description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 12
- 229910052786 argon Inorganic materials 0.000 description 12
- 239000001257 hydrogen Substances 0.000 description 12
- 229910052739 hydrogen Inorganic materials 0.000 description 12
- 229920006262 high density polyethylene film Polymers 0.000 description 10
- 239000007789 gas Substances 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 9
- 238000005520 cutting process Methods 0.000 description 8
- 238000004804 winding Methods 0.000 description 8
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 7
- 239000000853 adhesive Substances 0.000 description 7
- 230000001070 adhesive effect Effects 0.000 description 7
- -1 graphite alkene Chemical class 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- LZCLXQDLBQLTDK-UHFFFAOYSA-N ethyl 2-hydroxypropanoate Chemical compound CCOC(=O)C(C)O LZCLXQDLBQLTDK-UHFFFAOYSA-N 0.000 description 6
- 150000002431 hydrogen Chemical class 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 6
- 239000004926 polymethyl methacrylate Substances 0.000 description 6
- 239000010453 quartz Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000004698 Polyethylene Substances 0.000 description 5
- 229920000573 polyethylene Polymers 0.000 description 5
- 238000000137 annealing Methods 0.000 description 4
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- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 3
- 235000011130 ammonium sulphate Nutrition 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005202 decontamination Methods 0.000 description 3
- 230000003588 decontaminative effect Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 229940116333 ethyl lactate Drugs 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 230000017525 heat dissipation Effects 0.000 description 3
- 239000004745 nonwoven fabric Substances 0.000 description 3
- 229920001778 nylon Polymers 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 239000002356 single layer Substances 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
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- 229910002804 graphite Inorganic materials 0.000 description 1
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- 238000010030 laminating Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
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- C01B32/186—Preparation by chemical vapour deposition [CVD]
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- F41H—ARMOUR; ARMOURED TURRETS; ARMOURED OR ARMED VEHICLES; MEANS OF ATTACK OR DEFENCE, e.g. CAMOUFLAGE, IN GENERAL
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Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
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- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Geometry (AREA)
- Composite Materials (AREA)
- General Engineering & Computer Science (AREA)
- Carbon And Carbon Compounds (AREA)
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Abstract
本发明提供一种复合材料,包括至少一个三维石墨烯层和至少一个纤维复合材料层,所述三维石墨烯层由三维石墨烯膜铺叠而成,所述三维石墨烯膜的至少一侧具有纤维复合材料层。本发明在复合材料中设置三维石墨烯层,利用三维石墨烯层的高导热特性在复合材料内部形成有效的导热通道,实现热量在复合材料上的快速传导,且本发明中的复合材料具有质量轻、强度高、柔韧性好、透气性好等特点,尤其适用于导热或防弹衣的设计。
Description
【技术领域】
本发明涉及复合材料领域,尤其涉及一种复合材料、其制备方法及应用。
【背景技术】
防弹衣的使用能有效地降低士兵的伤亡,对于警察甚至普通公民都是至关重要的防护装备。无纬布是制备防弹衣的主要材料,但在子弹侵彻无纬布的过程中,在子弹与无纬布作用的界面上会产生大量的热量,该热量直接加载在无纬布的局部区域,降低了无纬布在此区域对子弹的阻断性能。
石墨烯具有耐高温、柔软性好、质量轻、热传导率高等显著特点,在能源、电子、电力、导热、通信等领域已取得大量的应用。将石墨烯或导热填料添加到树脂和/或胶液中制备具有导热功能的复合材料,该方法可在一定程度上增强复合材料的导热性能,但由于石墨烯或导热填料在树脂和/或胶液中不易分散,且添加的石墨烯或导热填料在复合材料中很难形成连续有效的导热通道,因此上述方法制备的导热复合材料仍不满足防弹衣对局部区域的高散热要求。
【发明内容】
为解决上述技术问题,本发明提供一种复合材料,包括至少一个三维石墨烯层和至少一个纤维复合材料层,所述三维石墨烯层由三维石墨烯膜铺叠而成,所述三维石墨烯膜的至少一侧具有纤维复合材料层。本发明在复合材料中设置三维石墨烯层,利用三维石墨烯层的高导热特性在复合材料内部形成连续有效的导热通道,实现热量在复合材料上的快速传导,且本发明中的复合材料具有质量轻、强度高、柔韧性好、透气性好等特点,尤其适用于导热部件或防弹衣的设计。
在本发明中,复合材料可以是单一的纤维复合材料层与单一的三维石墨烯膜层,或多层纤维复合材料层与多层石墨烯膜层。当然,根据不同的使用环境和效果,可以将多层纤维复合材料层之间和/或相邻纤维复合材料层与三维石墨烯层之间通过粘接的方式使各层均固定或部分固定,也可以将多个纤维复合材料层与多个三维石墨烯层铺叠好的样品直接作为高强度导热复合材料使用。当然,将多个纤维复合材料层与多个三维石墨烯层铺叠好的样品直接作为高强度导热复合材料使用,在某些特殊应用下(例如防弹衣),未粘接固化的复合材料柔韧性和导热性更好,穿戴舒适,具有更好的散热效果和防弹阻隔性能,且方便对损坏后的片层进行替换。在本发明的另一些实施例中,当然还可将铺叠好的复合材料进一步进行压合固化,经固化后的复合材料具有更好的力学性能,使用更方便。
在本发明的一些实施例中,所述纤维复合材料层为纤维按预设方向在基板上铺叠而成,所述纤维上浸渍有树脂胶液,可使复合材料具有较好的工艺性和力学性能。例如,所述基板为高密度聚乙烯膜,所述纤维为超高分子量超高模量聚乙烯纤维,聚乙烯纤维浸胶后按0°、和/或30°、和/或60°、和/或90°等方向在高密度聚乙烯膜上铺层,经单层或多层铺叠压合后得到纤维复合材料层。
在本发明的一些实施例中,所述纤维复合材料层上浸有树脂胶液。在纤维复合材料层上浸渍和/或涂覆胶液有利于增加纤维复合材料层与三维石墨烯层界面处的作用力。在本发明中,可流动的树脂胶液还可在外力的作用下进入三维石墨烯孔洞内,经树脂胶液浸渍后的三维石墨烯层与纤维复合材料层固化后可显著提升纤维复合材料层与三维石墨烯之间的作用力,从而提高复合材料的力学性能和导热性能。
在本发明的一些实施例中,所述纤维复合材料层为超高分子量聚乙烯纤维复合材料层、尼龙纤维复合材料层、聚丙烯纤维复合材料层、基纶纤维复合材料层、碳纤维复合材料层、芳纶纤维复合材料层中的一种或多种,使用上述高性能纤维复合材料层可进一步提高复合材料的力学性能和耐高温性能。
在本发明的一些实施例中,所述纤维复合材料层为编织纤维复合材料层。在本发明中采用编织纤维复合材料层能使复合材料在不同的受力方向上均具有较强的强度和抗撕裂性能。
在本发明的一些实施例中,所述纤维复合材料层为无纬布层。所述无纬布包括尼龙无纬布,超高分子量无纬布和芳纶无纬布。
在本发明的一些实施例中,所述三维石墨烯薄膜与纤维复合材料层可通过胶液进行粘接固定,或用纤维穿过三维石墨烯膜与纤维复合材料进行编织固定。
在本发明的一些实施例中,所述单个三维石墨烯层的厚度为0.1mm~10mm。三维石墨烯合适的厚度有利于复合材料中热量的快速传递,当单个三维石墨烯层的厚度太小时,例如低于0.1mm容易导致散热效果不理想,厚度大于10mm不利于三维石墨烯层与纤维复合材料的固定,且在实际使用中容易造成产品尺寸太厚,限制其应用。
本发明还公开一种由上述或下述的复合材料在导热和/或防弹上的应用。
本发明还公开一种复合材料的制备方法,包括如下步骤:S1制备三维石墨烯膜;S2将至少一层三维石墨烯膜与至少一层纤维复合材料进行铺叠,所述三维石墨烯膜的至少一侧具有纤维复合材料层。在本发明中,多层铺叠好的样品即可作为高强度导热复合材料使用,当然还可对铺叠好的复合材料进一步进行压合固化,经铺叠固化后的复合材料具有更好的力学性能,使用更方便。
在本发明的一些实施例中,三维石墨烯膜的层数可以与纤维复合材料的层数相同,例如,复合材料按纤维复合材料层-三维石墨烯层为重复单元铺叠至预设厚度,在该实施例中,多个三维石墨烯层的间隔设置可使复合材料具有优异的散热效果。
在本发明的另一些实施例中,三维石墨烯膜层的数量也可以明显少于纤维复合材料层,例如,复合材料按先铺叠预设层数的纤维复合材料层,再铺叠一层三维石墨烯层,再铺叠预设层数的纤维复合材料层等的方式铺设至预设厚度,然后经固化得到,通过该方式得到的复合材料,通过设计适当数量的三维石墨烯层也可使本发明中的复合材料具有优异的散热效果。
在本发明的一些实施例中,所述步骤S2可以是直接将纤维复合材料层-三维石墨烯层-纤维复合材料层逐层铺叠至预设厚度后在进行压合固化得到本发明中的复合材料,也可以是先将一个三维石墨烯膜与一个或两个纤维复合材料层预先压合得到三维石墨烯/纤维复合材料,然后再将前述三维石墨烯/纤维复合材料铺叠至预设厚度后进行压合固化得到本发明中的复合材料。在本发明的另一些实施中,多层三维石墨烯膜/纤维复合材料可按相同方向进行铺叠,也可按不同方向进行铺叠。例如,当纤维复合材料层为编织纤维复合材料层时,多层三维石墨烯膜/纤维布即使按相同方向铺叠仍能使复合材料在不同的受力方向上具有较强的力学性能;当纤维复合材料层不是编织纤维复合材料层时,需要将多层三维石墨烯膜/纤维布按不相同的方向进行铺叠,从而使复合材料在不同都具有较强的力学性能。
在本发明的一些实施例中,所述步骤S1包括(1)对铜箔表面进行清洗干燥;(2)先对铜箔进行高温退火处理,然后采用高温CVD方法在铜箔表面生长石墨烯,得到铜箔-石墨烯复合物;(3)将铜箔-石墨烯复合物浸入固化液中浸泡,然后进行高温固化,冷却后得到固化物;(4)将固化物浸入刻蚀液中浸泡去除铜箔,然后用溶剂清洗干燥得到三维石墨烯膜。
在本发明的一些实施例中,所述固化液为聚甲基丙烯酸酯与乳酸甲酯的混合溶液。
在本发明的一些实施例中,所述三维石墨烯膜的厚度为0.5mm~10mm。
在本发明的一些实施例中,复合材料可以是单一的纤维复合材料层与单一的三维石墨烯膜层,或多层纤维复合材料层与多层石墨烯膜层。多层纤维复合材料层与多层石墨烯膜层的复合材料包括纤维复合材料层-三维石墨烯层的结构,和/或纤维复合材料层-三维石墨烯层-纤维复合材料层的结构,和/或纤维复合材料层-三维石墨烯膜层-三维石墨烯膜层-纤维复合材料层的结构。
本发明通过在复合材料中设置三维石墨烯层,利用三维石墨烯的高导热特性在复合材料内部形成有效的导热通道,实现热量在复合材料上的快速传导,从而增强复合材料在高温下的力学性能;且本发明中的复合材料具有耐高温性能、质量轻、强度高、柔韧性好、透气性好等特点,尤其适用于导热或防弹衣的设计。
【具体实施方式】
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
实施例1
采用30*30mm的25微米的铜箔作为反应基底,对铜箔表面进行去污处理,将铜箔放置在3%的Na2CO3溶液中浸泡10分钟,然后放在去离子水里进行超声冲洗10分钟,最后放置于80℃鼓风烘箱中干燥。
运用CVD法在铜箔表面生长石墨烯,将铜箔放在石英舟中,置于CVD系统的管式炉恒温区,首先将管式炉温度以20℃/min的速度加热升温到995℃,后再以5℃/min速度升至1050℃。在升温过程中以流量为50sccm通入氢气,以流量为300sccm通入氩气;接着,保持温度以及气体流量不变30min,对铜箔进行退火处理。然后,调节氢气流量到500sccm,并且保持氩气流量大小不变,再通入约50sccm甲烷作为碳源气体生长石墨烯,生长时间为25min,在此生长过程中,温度保持不变。
生长完毕后,关闭加热系统,并迅速关闭碳源和氢气,调气氩气流量至1000sccm约30s,此后在300sccm氩气和4sccm氢气保护下,以1℃/min的速度冷却至500℃左右,之后直接打开炉盖快速冷却至室温,整个生长过程结束,即得到铜箔-石墨烯复合物,整个生长过程都在常压下进行。
使用高分子化合物对铜箔-石墨烯复合物进行固化,采用的固化液以PMMA作为溶质、以乳酸乙酯作为溶剂,其中PMMA的质量含量为4%。将得到的铜箔-石墨烯复合物在固化液中浸泡10分钟;然后进行高温固化,固化温度为200℃,固化时间为4小时;冷却之后得到固化物。
将固化物浸入刻蚀液对金属进行刻蚀液为1mol/L的硫酸铵溶液,每次取用200ml刻蚀液对金属进行刻蚀,每2小时更换一次刻蚀液,直至刻蚀液颜色不再变蓝,刻蚀结束。
再将固化物放入丙酮中浸泡4小时,然后用丙酮进行清洗,烘干,最后在还原或者惰性气氛和350℃的温度下,进行退火处理60分钟,得到0.1mm厚度的三维石墨烯薄膜。
将高密度聚乙烯薄膜铺在自动控制辊筒卷绕机上,然后将超高分子量聚乙烯纤维卷筒放置到辊筒卷绕机的退绕架上。将超高分子量聚乙烯纤维的端头倒出,并经过张力调节架、展丝装置、胶槽,最后固定在辊筒一侧边缘。在辊筒卷绕机导轨的不断移动过程中,将超高分子量聚乙烯纤维经过胶槽后平铺在高密度聚乙烯薄膜上,导轨移动速度0.15-0.25m/min,缠绕速度为100-150m/min。当超高分子量聚乙烯纤维缠绕至设定宽度时,辊筒停止卷绕,割断超高分子量聚乙烯纤维。此时利用旋涂装置在超高分子量聚乙烯纤维表面均匀涂布一层丙烯酸胶粘剂,然后在它上面铺放1片厚度0.1mm的三维石墨烯膜,并用胶辊将三维石墨烯膜与超高分子量聚乙烯纤维紧密粘接。将辊筒重新转动至烘干的区域,转动辊筒直至辊筒表面的纤维全部烘干。沿着辊筒表面的凹槽割开无纬布取下。将上述聚乙烯无纬布进行4次正交复合,制成有4层纤维正交组成的30*30mm无纬布。
将上述制备的无纬布铺叠49层,将叠合成的整体制作成试样,并且对试样进行防弹性能测试。
参考GA141-2010对试样进行防弹性能测试。在常温下,用1951年式7.62mm铅心手枪弹以512m/s在0度下进行射击测试,试样中弹未穿透,试样的背衬材料的凹陷深度为6mm。
实施例2
采用30*30mm的25微米的铜箔作为反应基底,对铜箔表面进行去污处理,将铜箔放置在3%的Na2CO3溶液中浸泡10分钟,然后放在去离子水里进行超声冲洗10分钟,最后放置于80℃鼓风烘箱中干燥。
运用CVD法在铜箔表面生长石墨烯,将铜箔放在石英舟中,置于CVD系统的管式炉恒温区,首先将管式炉温度以20℃/min的速度加热升温到995℃,后再以5℃/min速度升至1050℃。在升温过程中以流量为50sccm通入氢气,以流量为300sccm通入氩气;接着,保持温度以及气体流量不变30min,对铜箔进行退火处理。然后,调节氢气流量到500sccm,并且保持氩气流量大小不变,再通入约800sccm甲烷作为碳源气体生长石墨烯,生长时间为4h,在此生长过程中,温度保持不变。
生长完毕后,关闭加热系统,并迅速关闭碳源和氢气,调气氩气流量至1000sccm约30s,此后在300sccm氩气和4sccm氢气保护下,以1℃/min的速度冷却至500℃左右,之后直接打开炉盖快速冷却至室温,整个生长过程结束,即得到铜箔-石墨烯复合物,整个生长过程都在常压下进行。
使用高分子化合物对铜箔-石墨烯复合物进行固化,采用的固化液以PMMA作为溶质、以乳酸乙酯作为溶剂,其中PMMA的质量含量为4%。将得到的铜箔-石墨烯复合物在固化液中浸泡10分钟;然后进行高温固化,固化温度为200℃,固化时间为4小时;冷却之后得到固化物。
将固化物浸入刻蚀液对金属进行刻蚀液为1mol/L的硫酸铵溶液,每次取用200ml刻蚀液对金属进行刻蚀,每2小时更换一次刻蚀液,直至刻蚀液颜色不再变蓝,刻蚀结束。
再将固化物放入丙酮中浸泡4小时,然后用丙酮进行清洗,烘干,最后在还原或者惰性气氛和350℃的温度下,进行退火处理60分钟,得到10mm厚度的三维石墨烯薄膜。
将高密度聚乙烯薄膜铺在自动控制辊筒卷绕机上,然后将超高分子量聚乙烯纤维卷筒放置到辊筒卷绕机的退绕架上。将超高分子量聚乙烯纤维的端头倒出,并经过张力调节架、展丝装置、胶槽,最后固定在辊筒一侧边缘。在辊筒卷绕机导轨的不断移动过程中,将超高分子量聚乙烯纤维经过胶槽后平铺在高密度聚乙烯薄膜上,导轨移动速度0.15-0.25m/min,缠绕速度为100-150m/min。当超高分子量聚乙烯纤维缠绕至设定宽度时,辊筒停止卷绕,割断超高分子量聚乙烯纤维。此时利用旋涂装置在超高分子量聚乙烯纤维表面均匀涂布一层丙烯酸胶粘剂,然后在它上面铺放一层厚度为10mm的三维石墨烯膜,并用胶辊将三维石墨烯膜与超高分子量聚乙烯纤维紧密粘接。将辊筒重新转动至烘干的区域,转动辊筒直至辊筒表面的纤维全部烘干。沿着辊筒表面的凹槽割开无纬布取下。将上述超高分子量聚乙烯无纬布进行4次正交复合,制成有4层纤维正交组成的30*30mm无纬布。
将48片不含三维石墨烯膜并且由4层纤维正交组成的30*30mm的无纬布与上述制备的1片含三维石墨烯膜的无纬布进行铺叠,含三维石墨烯膜的无纬布放在最中间,两边依次叠放24层其它无纬布,总共49层。将叠合成的整体制作成试样,并且对它进行防弹性能测试。
参考GA141-2010对试样进行防弹性能测试。在常温下,用1951年式7.62mm铅心手枪弹以515m/s在0度下进行射击测试,试样中弹未穿透,试样的背衬材料的凹陷深度为12mm。
实施例3
采用30*30mm的25微米的铜箔作为反应基底,对铜箔表面进行去污处理,将铜箔放置在3%的Na2CO3溶液中浸泡10分钟,然后放在去离子水里进行超声冲洗10分钟,最后放置于80℃鼓风烘箱中干燥。
运用CVD法在铜箔表面生长石墨烯,将铜箔放在石英舟中,置于CVD系统的管式炉恒温区,首先将管式炉温度以20℃/min的速度加热升温到995℃,后再以5℃/min速度升至1050℃。在升温过程中以流量为50sccm通入氢气,以流量为300sccm通入氩气;接着,保持温度以及气体流量不变30min,对铜箔进行退火处理。然后,调节氢气流量到500sccm,并且保持氩气流量大小不变,再通入约50sccm甲烷作为碳源气体生长石墨烯,生长时间为25min,在此生长过程中,温度保持不变。
生长完毕后,关闭加热系统,并迅速关闭碳源和氢气,调气氩气流量至1000sccm约30s,此后在300sccm氩气和4sccm氢气保护下,以1℃/min的速度冷却至500℃左右,之后直接打开炉盖快速冷却至室温,整个生长过程结束,即得到铜箔-石墨烯复合物,整个生长过程都在常压下进行。
使用高分子化合物对铜箔-石墨烯复合物进行固化,采用的固化液以PMMA作为溶质、以乳酸乙酯作为溶剂,其中PMMA的质量含量为4%。将得到的铜箔-石墨烯复合物在固化液中浸泡10分钟;然后进行高温固化,固化温度为200℃,固化时间为4小时;冷却之后得到固化物。
将固化物浸入刻蚀液对金属进行刻蚀液为1mol/L的硫酸铵溶液,每次取用200ml刻蚀液对金属进行刻蚀,每2小时更换一次刻蚀液,直至刻蚀液颜色不再变蓝,刻蚀结束。
再将固化物放入丙酮中浸泡4小时,然后用丙酮进行清洗,烘干,最后在还原或者惰性气氛和350℃的温度下,进行退火处理60分钟,得到0.1mm厚度的三维石墨烯薄膜。重复以上过程共制备49层厚度0.1mm厚度的三维石墨烯薄膜。
将高密度聚乙烯薄膜铺在自动控制辊筒卷绕机上,然后将超高分子量聚乙烯纤维卷筒放置到辊筒卷绕机的退绕架上。将超高分子量聚乙烯纤维的端头倒出,并经过张力调节架、展丝装置、胶槽,最后固定在辊筒一侧边缘。在辊筒卷绕机导轨的不断移动过程中,将超高分子量聚乙烯纤维经过胶槽后平铺在高密度聚乙烯薄膜上,导轨移动速度0.15-0.25m/min,缠绕速度为100-150m/min。当超高分子量聚乙烯纤维缠绕至设定宽度时,辊筒停止卷绕,割断超高分子量聚乙烯纤维。此时利用旋涂装置在超高分子量聚乙烯纤维表面均匀涂布一层丙烯酸胶粘剂,然后在它上面铺放1片厚度0.1mm的三维石墨烯膜,并用胶辊将三维石墨烯膜与超高分子量聚乙烯纤维紧密粘接。将辊筒重新转动至烘干的区域,转动辊筒直至辊筒表面的纤维全部烘干。沿着辊筒表面的凹槽割开无纬布取下。将上述聚乙烯无纬布进行4次正交复合,制成有4层纤维正交组成的30*30mm无纬布。
重复以上过程,制作40片30*30mm无纬布,并将它们叠合成一个整体成为一个试样,并且对试样进行防弹性能测试。
参考GA141-2010对试样进行防弹性能测试。在常温下,用1951年式7.62mm铅心手枪弹以515m/s在0度下进行射击测试,试样中弹未穿透,试样的背衬材料的凹陷深度为10mm。
对比例1
将高密度聚乙烯薄膜铺在自动控制辊筒卷绕机上,然后将超高分子量聚乙烯纤维卷筒放置到辊筒卷绕机的退绕架上。将超高分子量聚乙烯纤维的端头倒出,并经过张力调节架、展丝装置、胶槽,最后固定在辊筒一侧边缘。在辊筒卷绕机导轨的不断移动过程中,将超高分子量聚乙烯纤维经过胶槽后平铺在高密度聚乙烯薄膜上,导轨移动速度0.15-0.25m/min,缠绕速度为100-150m/min。当超高分子量聚乙烯纤维缠绕至设定宽度时,辊筒停止卷绕,割断超高分子量聚乙烯纤维。此时利用旋涂装置在超高分子量聚乙烯纤维表面均匀涂布一层丙烯酸胶粘剂,然后将辊筒重新转动至烘干的区域,转动辊筒直至辊筒表面的纤维全部烘干。沿着辊筒表面的凹槽割开无纬布取下。将上述聚乙烯无纬布进行4次正交复合,制成有4层纤维正交组成的30*30mm无纬布。
重复以上过程,制作49片30*30mm无纬布,并将它们叠合成一个整体成为一个试样,并且对试样进行防弹性能测试。
参考GA141-2010对试样进行防弹性能测试。在常温下,用1951年式7.62mm铅心手枪弹以515m/s在0度下进行射击测试,试样中弹未穿透,试样的背衬材料的凹陷深度为18mm。
在上述实施例中,仅对本发明进行了示范性描述,但是本领域技术人员在阅读本专利申请后可以在不脱离本发明的精神和范围的情况下对本发明进行各种修改。
Claims (10)
1.一种复合材料,其特征在于,所述复合材料包括至少一个三维石墨烯层和至少一个纤维复合材料层,所述三维石墨烯层由三维石墨烯膜铺叠而成,所述三维石墨烯膜的至少一侧具有纤维复合材料层。
2.如权利要求1所述的复合材料,其特征在于,所述纤维复合材料层为纤维按预设方向在基板上铺叠而成,所述纤维上浸渍有树脂胶液。
3.如权利要求1所述的复合材料,其特征在于,所述纤维复合材料层为无纬布层。
4.如权利要求1所述的复合材料,其特征在于,所述单个三维石墨烯层的厚度为0.1mm~10mm。
5.如权利要求1所述的复合材料,其特征在于,所述复合材料中三维石墨烯膜的层数与纤维复合材料的层数相同或三维石墨烯膜层的数量少于纤维复合材料层的数量。
6.如权利要求1至5任一项所述的复合材料在导热和/或防弹上的应用。
7.一种复合材料的制备方法,其特征在于,所述制备方法包括如下步骤:
S1制备三维石墨烯膜;
S2将至少一层三维石墨烯膜与至少一层纤维复合材料层进行铺叠,所述三维石墨烯膜的至少一侧具有纤维复合材料层。
8.如权利要求7所述的制备方法,其特征在于,所述步骤S1包括(1)对铜箔表面进行清洗干燥;(2)采用高温CVD方法在铜箔表面生长石墨烯,得到铜箔-石墨烯复合物;(3)将铜箔-石墨烯复合物浸入固化液中浸泡,然后进行高温固化,冷却后得到固化物;(4)将固化物浸入刻蚀液中浸泡去除铜箔,然后用溶剂清洗干燥得到三维石墨烯膜。
9.如权利要求7所述的制备方法,其特征在于,所述固化液为聚甲基丙烯酸酯与乳酸甲酯的混合溶液。
10.如权利要求7所述的制备方法,其特征在于,所述单个三维石墨烯膜的厚度为0.1mm~10mm。
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