CN117070127B - 一种高导热防冰涂料的制备及应用 - Google Patents
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Abstract
本发明提供了一种高导热防冰涂料的制备及应用,包括如下步骤:S1:将粘结剂、固化剂溶于溶剂中,搅拌得到混合溶液,将基底材料浸入到混合溶液中,将基底材料从混合溶液中提出静置,将六方氮化硼颗粒洒在基底材料上,静置烘干,得到半成品基底材料;S2:将步骤S1得到的半成品基底材料浸入到润滑剂中,将半成品基底材料静从润滑剂中提出静置,得到涂抹高导热防冰涂料的固体成品。本专利具有很好的导热性,不影响基材的传热,氮化硼除了赋予涂层良好的导热性外,形成的微纳米结构可以更好的锁住聚硼硅氧烷,防止聚硼硅氧烷在静置时溢出。
Description
技术领域
本发明属于涂料制备技术领域,尤其是涉及一种高导热防冰涂料的制备及应用。
背景技术
现有技术如CN116040962A,多为先构造一个粗糙的微纳米结构表面,然后将润滑油注入到上述粗糙表面中,润滑液由于毛细力的作用会被锁在微纳结构的骨架中,因此,冰或者霜不会再光滑的润滑油上凝结。但专利采用低导热性的高分子作为骨架材料,该材料难以应用于如换热器翅片等需要高导热的环境中,并且当风力较大或者有灰尘撞击时,润滑油很容易干涸。
发明内容
有鉴于此,本发明旨在提出一种高导热防冰涂料的制备及应用,以解决基材在高温环境中,风力较大或者有灰尘撞击时,润滑油很容易干涸的问题。
为达到上述目的,本发明的技术方案是这样实现的:
一种高导热防冰涂料的制备,包括如下步骤:
S1:将粘结剂、固化剂溶于溶剂中,搅拌得到混合溶液,将基底材料浸入到混合溶液中,将基底材料从混合溶液中提出静置,将六方氮化硼颗粒洒在基底材料上,静置烘干,得到半成品基底材料;
S2:将步骤S1得到的半成品基底材料浸入到润滑剂中,将半成品基底材料静从润滑剂中提出静置,得到涂抹高导热防冰涂料的固体成品。
进一步的,所述步骤S1中的粘结剂包括环氧树脂、硅胶、丙烯酸树脂、酚醛树脂、醇酸树脂中的一种。不同的粘结剂,对应使用不同的固化剂。
进一步的,所述步骤S1中的溶剂包括二甲苯、四氢呋喃、乙醇、乙酸乙酯、庚烷中的一种。
进一步的,所述步骤S1中的胶粘剂:固化剂:溶剂的质量比为1:0-1:1-100。
进一步的,所述步骤S1中的六方氮化硼粒径为0.01-100微米;涂层厚度为10-500微米。
进一步的,所述步骤S1中的基底材料浸入到混合溶液中的时间至少为10分钟,将基底材料从混合溶液中提出静置的时间为30-100分钟。
进一步的,所述步骤S1中将六方氮化硼颗粒洒在基底材料上包括将六方氮化硼颗粒放置在筛网中,抖动筛网,将颗粒均匀的撒在未固化的环氧树脂表面,静置10-60分钟,放置到80-100℃的烘箱固化1.5-2.5小时,固化后,用刷子将未被粘连的氮化硼刷掉。
进一步的,所述步骤S2在润滑剂中静置的时间为1小时,将铝板缓慢提出,静置1小时。
进一步的,所述步骤S2的润滑剂包括聚硼硅氧烷、硅油、氟硅油、食用油、矿物油中的一种。
一种高导热防冰涂料的制备的应用,应用于具有高频震动的防冰敷的涂层处理,例如应用于换热器翅片、发电风机扇面、飞机表面的涂层处理。
使用高导热的氮化硼作为微纳结构,使得该涂料具有很好的导热性。使用聚硼硅氧烷或其他油状物质做润滑层,当聚硼硅氧烷受到风或者灰尘的撞击时会高频震动而转变成固体,从而避免的聚硼硅氧烷的流失,当聚硼硅氧烷不受外力时会转变成液体,使涂层表面恢复光滑,防止了冰的附着。基于该涂料的频率响应性,特别适合换热器翅片、发电风机扇面、飞机表面等既有高频震动又有静置的场景下去做防冰应用。
猪笼草植物由于其特殊的微结构及近乎完美的表面超滑属性,近年来引起了科研人员的广泛专注。猪笼草的瓶状捕虫笼内壁具有多孔的微结构并填充有润滑液,正是利用内壁的这种超滑属性,猪笼草可以阻止滑落进笼内的昆虫逃脱。
受到猪笼草启发,人们将润滑油注入到多孔的基材内,制备了类似猪笼草的超润滑表面,该表面具有防污、防冰敷的功能,原理如图1所示。Philseok等人收到猪笼草启发,用电沉积的方法在铝基表面制备了聚吡咯(PPy)微结构,在用全氟辛基三氯硅烷氟化以后,使用杜邦的GPL100润滑油浸入制备得到超润滑表面。并研究了这种超润滑表面的防冰性能。由测试结果可知这种超润滑表面可以有效抑制冰霜在表面的生长,且具有很低的冰粘附力。
六方氮化硼具有高导热系数。六方氮化硼的平面内热导率高达550 W/(m·K),它具有高度的导热各向异性,面外热导率为5 W/(m·K)。自然丰度的六方氮化硼具有19.78%的B10和80.22%的B11,由于B10和B11质量的不同,导致原子振动差异,发生同位素声子散射现象,因此,高丰度的六方氮化硼具有更优良的导热性。
聚硼硅氧烷(PBS)是通过反应使硼原子替代聚硅氧烷主链上的部分氧原子而形成的高分子聚硅氧烷衍生物,其结构简式如化学式(Ⅰ)所示。
(Ⅰ)
其中,R1、R2为氧、氢、烷基、芳基等;R3为氧、芳基等。该结构赋予PBS固液性能,即低频应力下为液态高频应力下为固态。这是由于硼原子最外层空轨道可以容纳其他主链上氧原子的孤对电子形成电子桥,引起分子间微弱的配位键合,构成物理交联。除这种配位键合外,PBS中还可能存在动态氢键,这两者共同作为交联点使其具有超分子结构。动态配位键缔合/解离的速率与频率相关,因而PBS具有固态与液态的转变。除此之外,由于配位键的动态性,PBS具有良好的室温自修复性能。然而想要使PBS在较低应力频率下也保持形状。其方法通常分为两方面:第一种是使用纳米填料与PBS共混以克制PBS的流动性,另一种方法是通过构建双网络体系实现结构优化。
相对于现有技术,本发明所述的一种高导热防冰涂料的制备及应用具有以下优势:
1、本专利具有很好的导热性,不影响基材的传热,氮化硼除了赋予涂层良好的导热性外,形成的微纳米结构可以更好的锁住聚硼硅氧烷,防止聚硼硅氧烷在静置时溢出。
2、本专利由于聚硼硅氧烷具有固液性能和自修复性能,当涂层高速震动(如风吹)时,聚硼硅氧烷会表现出固体性质,不易被风或者灰尘带落,当涂层静置时,聚硼硅氧烷的流动性使表面划痕得到恢复,形成光滑的防冰面。
附图说明
构成本发明的一部分的附图用来提供对本发明的进一步理解,本发明的示意性实施例及其说明用于解释本发明,并不构成对本发明的不当限定。在附图中:
图1为超润滑涂层防污、防冰敷原理的示意图;
图2为本发明实施例所述的冰附着力强度测试设备示意图;
图3为本发明实施例1所述的冰附着力强度随冰附次数变化示意图;
图4为本发明实施例2所述的冰附着力强度随冰附次数变化示意图;
图5为本发明实施例3所述的冰附着力强度随冰附次数变化示意图;
图6为本发明对比例1所述的冰附着力强度随冰附次数变化示意图;
图7为本发明实施例3所述的冰附着力强度随冰附次数变化示意图。
具体实施方式
需要说明的是,在不冲突的情况下,本发明中的实施例及实施例中的特征可以相互组合。
下面将参考附图并结合实施例来详细说明本发明。
实施例1:
粗糙结构的制备:将10g环氧树脂和1g环氧树脂固化剂(环氧树脂固化剂的型号为590环氧固化剂)溶解在100g二甲苯中,搅拌均匀,将铝片浸入环氧溶液中静置10分钟,缓慢提出,静置10分钟,等待溶剂挥发,将平均粒径为0.5微米的六方氮化硼用筛网撒在未固化的环氧树脂表面,静置30分钟,将其放入80℃烘箱固化2小时。
聚硼硅氧烷的注入:将上述涂有环氧树脂/氮化硼涂层的铝板缓慢浸入到聚硼硅氧烷中,静置1小时,将铝板缓慢提出,得到防冰涂层。
将制备的防冰敷涂层的铝板放置在冰箱冷冻层约为-20℃的环境下一小时,将一个长方形硅胶模具(1cm*1cm*2cm)置于涂层之上,并向硅胶模具中滴入少量去离子水,水量刚好铺满硅胶模具底部,将其放置在冰箱冷冻层冷冻10min,让模具底部的水结冰。继续向模具中加入去离子水,至磨具中充满水,然后将其放置冰箱冷冻层冷冻1h。
附着力强度测试:将推力测力器固定在可移动平台上,并将推力测力器垂直对准已冻结的模具下半部分,移动移动平台,当冰脱离涂层表面时,记录此时推力测力器的数值,冰的附着力强度=推力测力器示数/冷冻面积。该过程装置如图2所示。
过程装置包括固定平台,将防冰敷涂层的铝板放在固定平台上,移动平台设置在固定平台的一侧,移动平台上固定设有推力测力器,移动平台和固定平台在同一水平面上,移动平台沿着水平面移动。
实验结果:防冰敷涂层的厚度为2微米,防冰敷涂层的导热系数为5W/(m·K),冰附着力强度随冰附次数变化如图3所示。
实施例2:
粗糙结构的制备:将10g硅胶(硅胶的型号为道康宁184)和1g硅胶固化剂溶解在80g二甲苯中,搅拌均匀,将铝片浸入环氧溶液中静置10分钟,缓慢提出,静置10分钟,等待溶剂挥发,将平均粒径为10微米的六方氮化硼用筛网撒在未固化的环氧树脂表面,静置30分钟,将其放入80℃烘箱固化2小时。
聚硼硅氧烷的注入:将上述涂有硅胶/氮化硼涂层的铝板缓慢浸入到聚硼硅氧烷中,静置1小时,将铝板缓慢提出,得到防冰涂层。
将制备的防冰敷涂层的铝板放置在冰箱冷冻层约为-20℃的环境下一小时,将一个长方形硅胶模具(1cm*1cm*2cm)置于涂层之上,并向硅胶模具中滴入少量去离子水,水量刚好铺满硅胶模具底部,将其放置在冰箱冷冻层冷冻10min,让模具底部的水结冰。继续向模具中加入去离子水,至磨具中充满水,然后将其放置冰箱冷冻层冷冻1h。
附着力强度测试:将推力测力器固定在可移动平台上,并将推力测力器垂直对准已冻结的模具下半部分,移动移动平台,当冰脱离涂层表面时,记录此时推力测力器的数值,冰的附着力强度=推力测力器示数/冷冻面积。
实验结果:防冰敷涂层的厚度为20微米,防冰敷涂层的导热系数为6W/(m·K),冰附着力强度随冰附次数变化如图4所示。
实施例3:
粗糙结构的制备:将10g丙烯酸树脂溶解在50g二甲苯中,搅拌均匀,将铝片浸入环氧溶液中静置10分钟,缓慢提出,静置10分钟,等待溶剂挥发,将平均粒径为60微米的六方氮化硼用筛网撒在未固化的环氧树脂表面,静置30分钟,将其放入80℃烘箱固化2小时。
聚硼硅氧烷的注入:将上述涂有丙烯酸/氮化硼涂层的铝板缓慢浸入到聚硼硅氧烷中,静置1小时,将铝板缓慢提出,得到防冰涂层。
将制备的防冰敷涂层的铝板放置在冰箱冷冻层约为-20℃的环境下一小时,将一个长方形硅胶模具(1cm*1cm*2cm)置于涂层之上,并向硅胶模具中滴入少量去离子水,水量刚好铺满硅胶模具底部,将其放置在冰箱冷冻层冷冻10min,让模具底部的水结冰。继续向模具中加入去离子水,至磨具中充满水,然后将其放置冰箱冷冻层冷冻1h。
附着力强度测试:将推力测力器固定在可移动平台上,并将推力测力器垂直对准已冻结的模具下半部分,移动移动平台,当冰脱离涂层表面时,记录此时推力测力器的数值,冰的附着力强度=推力测力器示数/冷冻面积。
实验结果:防冰敷涂层的厚度为100微米,防冰敷涂层的导热系数为4W/(m·K),冰附着力强度随冰附次数变化如图5所示。
对比例1:
粗糙结构的制备:将10g环氧树脂和1g环氧树脂固化剂(环氧树脂固化剂的型号为590环氧固化剂)溶解在100g二甲苯中,搅拌均匀,将铝片浸入环氧溶液中静置10分钟,缓慢提出,静置10分钟,等待溶剂挥发,将平均粒径为0.5微米的六方氮化硼用筛网撒在未固化的环氧树脂表面,静置30分钟,将其放入80℃烘箱固化2小时。
聚硼硅氧烷的注入:将上述涂有环氧树脂/氮化硼涂层的铝板缓慢浸入到硅油中,静置1小时,将铝板缓慢提出,得到防冰涂层。
将制备的防冰敷涂层的铝板放置在冰箱冷冻层约为-20℃的环境下一小时,将一个长方形硅胶模具(1cm*1cm*2cm)置于涂层之上,并向硅胶模具中滴入少量去离子水,水量刚好铺满硅胶模具底部,将其放置在冰箱冷冻层冷冻10min,让模具底部的水结冰。继续向模具中加入去离子水,至磨具中充满水,然后将其放置冰箱冷冻层冷冻1h。
附着力强度测试:将推力测力器固定在可移动平台上,并将推力测力器垂直对准已冻结的模具下半部分,移动移动平台,当冰脱离涂层表面时,记录此时推力测力器的数值,冰的附着力强度=推力测力器示数/冷冻面积。
实验结果:防冰敷涂层的厚度为1.7微米,防冰敷涂层的导热系数为5W/(m·K),冰附着力强度随冰附次数变化如图6所示。
重新制备实施例1和对比例1的样品,并放置在通风橱中,风速为0.4m/s,累计吹风240小时。然后,用上述方法测试附着力强度,结果如下表所示:
表1 实施例1和对比例1的附着力强度
由上述结果可知,当润滑剂为聚硼硅氧烷时,长时间吹风后,冰附着力变化很小;当润滑剂为硅油时,长时间吹风后,冰附着力变大6倍。这是因为聚硼硅氧烷具有频率应变性,当受到吹风时,表现为固体特性,不易干涸;而硅油则一直为液体特性,较容易干涸,导致冰附着力增大。
对比例2:
涂层的制备:将10g硅胶(硅胶的型号为道康宁184)、1g硅胶固化剂、10g聚硼硅氧烷和5g六方氮化硼加入80g二甲苯中搅拌均匀,将其涂敷在铝片表面,然后放入80℃烘箱固化2小时。
将制备的防冰敷涂层的铝板放置在冰箱冷冻层约为-20℃的环境下一小时,将一个长方形硅胶模具(1cm*1cm*2cm)置于涂层之上,并向硅胶模具中滴入少量去离子水,水量刚好铺满硅胶模具底部,将其放置在冰箱冷冻层冷冻10min,让模具底部的水结冰。继续向模具中加入去离子水,至磨具中充满水,然后将其放置冰箱冷冻层冷冻1h。
附着力强度测试:将推力测力器固定在可移动平台上,并将推力测力器垂直对准已冻结的模具下半部分,移动移动平台,当冰脱离涂层表面时,记录此时推力测力器的数值,冰的附着力强度=推力测力器示数/冷冻面积。
实验结果:防冰敷涂层的厚度为2微米,防冰敷涂层的导热系数为0.5W/(m·K),冰附着力强度:200KPa。可见,将底表层和表层混合后涂敷,其对冰的附着力较大,不具备防冰效果。
对比例3:
将聚硼硅氧烷直接涂于铝片上,用上述方法测试冰敷着力强度,冰附着力强度随冰附次数变化如下图7所示。聚硼硅氧烷不能被很好固定,三次冰敷实验后涂层基本消失。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (3)
1.一种高导热防冰涂层的制备方法,其特征在于:包括如下步骤:
S1:将粘结剂、固化剂溶于溶剂中,搅拌得到混合溶液,将基底材料浸入到混合溶液中,将基底材料从混合溶液中提出静置,将六方氮化硼颗粒洒在基底材料上,静置烘干,得到半成品基底材料;
粘结剂为环氧树脂;
所述步骤S1中的粘结剂:固化剂:溶剂的质量比为10:1:100;
S2:将步骤S1得到的半成品基底材料浸入到润滑剂中,将半成品基底材料从润滑剂中提出静置即得;
所述步骤S1中将六方氮化硼颗粒洒在基底材料上包括将六方氮化硼颗粒放置在筛网中,抖动筛网,将颗粒均匀的撒在未固化的环氧树脂表面,静置10-60分钟,放置到80-100℃的烘箱固化1.5-2.5小时,固化后,用刷子将未被粘连的氮化硼刷掉;
所述基底材料为铝板;
六方氮化硼的平均粒径为0.5微米;
润滑剂为聚硼硅氧烷。
2.根据权利要求1所述的一种高导热防冰涂层的制备方法,其特征在于:所述步骤S1中的溶剂包括二甲苯、四氢呋喃、乙醇、乙酸乙酯、庚烷中的一种。
3.根据权利要求1或权利要求2所述的一种高导热防冰涂层的制备方法制备得到的涂层在换热器翅片、发电风机扇面的防冰应用。
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