CN110892037B - 相变材料及其生产方法 - Google Patents

相变材料及其生产方法 Download PDF

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CN110892037B
CN110892037B CN201880045950.2A CN201880045950A CN110892037B CN 110892037 B CN110892037 B CN 110892037B CN 201880045950 A CN201880045950 A CN 201880045950A CN 110892037 B CN110892037 B CN 110892037B
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phase change
change material
scaffold
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CN110892037A (zh
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约翰·亚历山大·诺埃尔
玛丽·安妮·怀特
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Ma LiAnniHuaite
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Abstract

一种用于生产形状稳定的相变材料的方法包括：冷冻固体和溶剂的浆料以提供冷冻的浆料，将所述冷冻的浆料暴露于引起所述冷冻的溶剂升华的条件以除去溶剂并提供其中具有空位的主体，烧结所述主体以提供支架，并且将熔融的相变材料添加到所述支架中以提供所述形状稳定的相变材料。当研磨时，相同的支架充当相变成核助剂。

Description

相变材料及其生产方法
技术领域
本披露涉及用于例如绝缘、热能储存、或热管理的相变材料。
发明背景
当相变材料发生相变时，相变材料以热的形式吸收或释放能量。结果，这些材料适合于储存和释放热能。此类材料可以用于各种各样的应用中，例如用于绝缘或热能储存，或者用于热管理，例如在电子应用中。
相变材料的缺点是此类材料的包装或封装昂贵。尽管此类材料的潜在应用是广泛的，但是相变材料的使用受到成本的限制。相变材料还具有低热导率的缺点。低的热导率限制了热量可以被带入或带出相变材料的速率。
对相变材料的封装和热导率的改进是希望的。
发明概述
根据本发明的一个方面，一种用于生产形状稳定的相变材料的方法包括：冷冻固体和溶剂的浆料以提供冷冻的浆料，将所述冷冻的浆料暴露于引起所述冷冻浆料溶剂升华的条件以提供其中具有空位的主体，烧结所述主体以提供支架，并且将熔融的相变材料添加到所述支架中以提供所述形状稳定的相变材料。
可以将冷冻的浆料冷冻干燥以引起所述冷冻的溶剂升华。
可以在冷冻之前将粘合剂添加到浆料中。所使用的溶剂可以是水。
定向进行冷冻，例如通过将所述浆料倒入模具中并将所述模具放置在冷板上以在冷冻期间提供温度梯度。
所述主体可以包括陶瓷、碳、金属或它们的组合。
所述浆料包括粘合剂、表面活性剂、分散剂、冰点降低剂、和结构改性剂中的一种或多种。
任选地，将支架的表面功能化或活化。
可以在添加熔融的相变材料的同时加热支架，使得当将所述熔融的相变材料添加到所述支架中时，所述支架的温度大于所述相变材料的熔点。
任选地，通过将熔融的相变材料的液滴添加到支架中，将所述熔融的相变材料添加到所述支架中以提供所述形状稳定的相变材料。可以例如在大气压下添加相变材料，直到支架饱和。
根据另一方面，一种形状稳定的相变材料包括支架，所述支架包括大体上规则的固体结构，所述结构包括在其中具有相变材料的空位。
任选地，将支架研磨并直接添加到相变材料中。
附图
现在将参考附图和以下描述，通过举例来描述本发明的实施例，其中：
图1是说明根据实施例用于生产形状稳定的相变材料的方法的简化流程图；
图2是在生产图1的形状稳定的相变材料的方法中冷冻的示意图；
图3A至图3E是生产图1的形状稳定的相变材料的方法中的材料的图；并且
图4是说明根据另一个实施例用于生产相变材料的方法的简化流程图。
具体实施方式
为了说明的简明和清楚起见，可能在图中重复参考号以指示相对应或类似的元件。阐述了许多细节以提供对本文描述的实例的理解。所述实例可以在没有这些细节的情况下实践。在其他情况下，未详细描述熟知方法、程序以及部件以免妨碍对所描述的实例的理解。所述描述不应被认为限制本文描述的实例的范围。
本披露总体上涉及一种用于生产形状稳定的相变材料的方法。所述方法包括：冷冻固体和溶剂的浆料以提供冷冻的浆料，将所述冷冻的浆料暴露于引起所述冷冻的溶剂升华的条件以除去溶剂并提供其中具有空位的主体，烧结所述主体以提供支架，并且将熔融的相变材料添加到所述支架中以提供所述形状稳定的相变材料。
参考图1，示出了说明用于生产形状稳定的相变材料的方法的流程图。所述方法可以包含比示出和描述的更多或更少的过程，并且所述方法的部分可以以不同的顺序进行。
由浆料制备冷冻浇铸支架。首先在102中制备浆料并且所述浆料的基础是溶剂，如蒸馏水。可以将添加剂添加到溶剂中并施加热通过搅拌溶解，所述添加剂包括粘合剂、表面活性剂或分散剂、冰点降低剂、和结构改性剂中的一种或多种。将固体材料，如陶瓷、碳、金属、聚合物、氧化物、或其他材料、或材料的组合的固体颗粒添加到水性混合物中。所述固体材料用于形成支架。所使用的添加剂和数量取决于诸如所希望的结构和固体颗粒的材料等因素。
例如，用磁力搅拌棒搅拌溶液以使颗粒悬浮并形成浆料。根据组成，可以使用行星式研磨机而不是磁力搅拌棒来帮助颗粒的悬浮以产生浆料。还可以使用添加表面活性剂或其他分散剂来帮助颗粒的悬浮，并且可以添加粘合剂或其他改性剂。
将浆料在104中冷冻。用于在生产形状稳定的相变材料的方法中冷冻的设备的示意图在图2中示出。可以例如通过将浆料倒入具有导热底部的模具中，并在提供温度梯度的冷板或其他装置上从下到上定向冷冻而将所述浆料定向冷冻。以这种方式、以适合实际组成和条件的速率冷冻产生了单向的冷冻的溶剂柱，所述柱迫使悬浮的固体颗粒进入间隙。可以使用冰点降低添加剂来调节固体溶剂生长的形态。
然后将冷冻的复合材料在106中升华以除去固体溶剂，如呈冰形式的水。可以将冷冻的复合材料冷冻干燥以除去冷冻的溶剂，留下生坯(原型支架)。在固体溶剂(如冰)先前存在的地方保留了空位。包含在浆料中的任选的结构改性添加剂可能影响固体溶剂的几何形状，例如平面、六边形等，并且因此改变所得的孔几何形状。
然后在108中烧结生支架。根据材料的不同，可以在空气或惰性气氛中烧结支架，以使固体强化和致密，从而形成更刚性的支架。如果支架没有充分烧结，则支架可能在热循环下塌陷。因此，为每种支架材料确定适当的制备和烧结工艺和条件，包括时间、温度、粘合剂等。
在110中通过添加相变材料来制备形状稳定的相变结构。为了制备形状稳定的相变材料，在本文中也称为形状稳定的相变材料(PCM)复合材料，将支架加热至高于相变材料的熔点的温度。相变材料可以包括脂肪酸、糖醇、脂肪醇、酯、聚合物、石蜡、水合盐和其他以及它们的组合。将熔融的PCM逐滴添加至支架的表面，并且通过毛细管作用将熔融的PCM吸入支架中。可以在大气压下添加PCM。如果支架的表面温度不高于PCM的熔点，则PCM可能在支架的表面上结晶并且因此无法完全吸收。当支架达到饱和，并且不再吸收相变材料时，相变材料的添加完成。
现在参考图3A至图3E，其示出了形状稳定的相变材料的示意性生产。
浆料在图3A中示出。如图所示，固体颗粒悬浮在浆料中。从底部开始并且以受控的速率将浆料冷冻，产生规则的冷冻的溶剂结构。此类结构的一个实例在图3B中示出。如图3C所示，将冷冻的浆料冷冻干燥，除去所有冷冻的溶剂并留下所有其他固体颗粒。如图3D所示，烧结支架以增加强度和致密化，并除去任何有机添加剂。如图3E所示，支架渗透有PCM，提供了形状稳定的相变材料。
现在参考图4来描述生产根据另一个实施例的相变材料的方法。所述方法可以包含比示出和描述的更多或更少的过程，并且所述方法的部分可以以不同的顺序进行。生产成核助剂(也称为成核剂)，而不是形状稳定的相变材料，并用于使相变材料成核。
图4的方法的许多过程类似于以上参考图1描述的那些，并且因此不再详细描述。
由浆料制备冷冻浇铸支架。在102中第一次制备浆料。在104中将浆料冷冻并且将冷冻的复合材料在106中升华以除去固体溶剂，如呈冰形式的水。在108中烧结生支架。
然后在410中将烧结的支架研磨成粉末并撒粉。在412中，通过将粉末混合到熔融的相变材料中，所述粉末被用作相变材料中的成核助剂。将粉末与熔融的相变材料混合，例如，约5wt.％或更多的粉末。
实例
提交以下实例来进一步说明本发明的各种实施例。这些实例旨在仅是说明性的并非旨在限制本发明的范围。
通过冷冻浇铸生产包括渗透有PCM的多孔固体支架的形状稳定的(FS)相变材料(PCM)。使用氧化铝、氧化铝和碳、二氧化钛、炭黑、壳聚糖和石墨化壳聚糖制造支架。预期其他陶瓷材料、金属、聚合物和氧化物也适用于此类支架。进行了实验室实验，证实了聚合物和其他氧化物适用于制造这种支架。金属支架也是合适的，因为金属也易于进行冷冻浇铸。
支架成功地渗透有PCM，如十二烷酸(在室温下为固体)、辛酸(在室温下为液体)、赤藓糖醇、石蜡、三水合乙酸钠和聚乙二醇。使用水作为溶剂。然而，可以成功地使用其他溶剂。
基于所使用的PCM，也可以使用其他PCM，包括但不限于其他长链脂肪酸、其他糖醇、长链烷烃、长链酯、长链脂肪醇、长链脂肪酰胺、各种蜡、水合盐以及甘油单酯、甘油二酯和甘油三酯。
表1总结了迄今为止制备的支架。表2总结了制备的FS PCM组成以及每种的特性。另外，确定氧化铝/十二烷酸FS PCM的维氏硬度为40。
表1.冷冻浇铸支架
Figure BDA0002360949060000061
*碳支架太脆而无法在填充PCM之前处理，但可以在负载PCM的情况下处理。
Figure BDA0002360949060000062
相对于支架的体积密度计算的支架孔隙率(％孔隙率对应于可用于负载的体积分数)
表2.形状稳定的相变材料组成
Figure BDA0002360949060000063
Figure BDA0002360949060000071
Figure BDA0002360949060000081
a 实验值
b 测量的
C稳定性没有变化的循环次数(-表示未尝试)
d用NaOH处理的支架
e用NaOH处理的支架，研磨成粉末，并以按质量计5％添加
支架的制备：
氧化铝：
所制备的浆料中列出的比例以全部浆料的％质量报告。还可以成功地使用其他比例和组成。将去离子水(37.8％)、乙酸锆(14.1％，基于在稀乙酸中的16％溶液，奥德里奇公司(Aldrich))和蔗糖(1.2％)；>99％，BDH化学品公司)用磁力搅拌棒混合。乙酸锆用于诱导冰的六角柱状生长。添加蔗糖以降低冰的熔点。然后将溶液加热至40℃，并添加聚甲基丙烯酸甲酯(PMMA)(0.66％；100目，奥德里奇公司)。PMMA用于帮助将氧化铝颗粒悬浮在浆料中。然后添加两种粒度的氧化铝，0.25至0.45μm(44.25％；99.95％，阿法埃莎公司(AlfaAesar))和40至50nm(1.9％；99.5％，阿法埃莎公司)，并搅拌浆料直至氧化铝粉末完全悬浮。将浆料倒入铜底塑料模具中。使用两个具有11mm和7mm直径的模具，并将所述模具填充至6至20mm的深度，并在珀耳帖(Peltier)冷却的冷板上定向地、从下到上冷冻。然后将冷冻的氧化铝主体在Edwards Modulyo冷冻干燥机中在约-40℃和约2×10-3巴下冷冻干燥24小时。将生坯氧化铝块在空气中以5℃ min-1加热至500℃并保持1小时以燃烧掉有机化合物，然后在1500℃下烧结2小时。
氧化铝+碳：
以与氧化铝相同的方式制备浆料，除了用等质量的炭黑(Black Pearls 2000)替代0.5至0.45μm的量的氧化铝(按质量计1％或5％)。还使用了不同的烧结过程：将生坯氧化铝+碳块在氩气下以5℃ min-1加热至1500℃，并烧结2小时。
炭黑：
通过将PVA水溶液(24g L-1)(75.6％)与乙酸锆(14.1％)和蔗糖(1.2％)混合来制备碳浆料。然后将溶液加热至40℃，并添加聚甲基丙烯酸甲酯(PMMA)(0.8％；100目，奥德里奇公司)。然后加入炭黑(8.3％)，并搅拌溶液直至所有碳悬浮。将浆料倒入铜底塑料模具(直径为11mm或7mm，填充至6至20mm的深度)中，并在珀尔帖冷却的冷板上从下到上冷冻。然后将冷冻的主体在Edwards Modulyo冷冻干燥机中在约-40℃和约2×10-3巴下冷冻干燥24小时。
壳聚糖：
通过剧烈混合去离子水(95.7％)、壳聚糖(2.4％；奥德里奇公司)和冰乙酸(1.9％)来制备壳聚糖凝胶。将凝胶倒入铜底塑料模具(直径为11mm或7mm，填充至6至20mm的深度)中，并在珀尔帖冷却的冷板上从下到上冷冻。然后将冷冻的壳聚糖主体在EdwardsModulyo冷冻干燥机中在约-40℃和约2×10-3巴下冷冻干燥24小时。
石墨化壳聚糖：
通过在氩气下以5℃ min-1加热至800℃并在所述温度下保持3小时，将制得的壳聚糖支架石墨化。
将一些石墨化壳聚糖支架样品用1摩尔氢氧化钠水溶液饱和，并在100℃下保持24小时以使表面功能化。然后将支架用去离子水冲洗5次，并在100℃下干燥24小时。
将其他功能化的石墨化壳聚糖支架样品研磨成粉末，并作为成核助剂添加到PCM中。
制备形状稳定的PCM：
以两种尺寸制备支架：11mm直径和7mm直径。支架的长度在从6mm至20mm的范围内，这取决于模具用于冷冻浇注的填充高度。为了产生形状稳定的PCM，将选择的支架加热到高于所使用的PCM的熔点约10℃，然后将熔融的PCM逐滴添加到支架的上表面，直至不再被吸收。然后将FS PCM复合材料放在其侧面，并在高于PCM熔点10℃下保持30分钟，以除去已经沉积在支架表面上的任何PCM而不被吸收。
所生产的冷冻浇铸支架容纳相变材料并在许多热循环中保持其形状。因此，所得的相变材料可用于可逆的热能储存。
支架材料能够容纳不同的相变材料。因此，可以为支架材料选择不同的相变材料。基于应用选择相变材料，以确保相变材料的熔点和结晶温度落在应用的温度范围内。在基于应用合适的那些相变材料中，可以通过选择相对于其他相变材料具有高焓变的相变材料，或者通过选择实现高相变材料负载(产生相对于能够相对降低相变材料负载的支架的高焓变)的支架，来选择具有最高热能储存密度的相变材料。
在所研究的PCM中，赤藓糖醇具有最高的熔融焓变，并且壳聚糖和碳化壳聚糖支架具有最高的负载。氧化铝支架提供了最高的热导率增强，这在热导率是重要的应用中是有益的。氧化铝支架也是最坚固的，这在强度可能是重要的应用中是有益的。在PCM的熔点中的滞后是重要的应用中，经NaOH处理的碳化壳聚糖支架成功地降低了一些PCM的滞后。冷冻浇注碳支架具有相对较差的机械和热特性。
上述实例旨在仅是说明性的。本领域技术人员可以对具体实例进行改变、修改和变型。因此，权利要求书的范围不应受在实例中列出的实施例限制，而是应当被给予与说明书总体相一致的最宽泛的解释。

Claims (16)

1.一种用于生产形状稳定的相变材料的方法，所述方法包括：
定向冷冻固体和溶剂的浆料，提供冷冻的浆料，所述冷冻的浆料包括迫使悬浮的固体颗粒进入间隙的单向的冷冻的溶剂柱；
将所述冷冻的浆料暴露于引起所述冷冻的浆料的所述溶剂升华的条件以除去冷冻的溶剂并提供其中具有空位的主体；
烧结所述主体以提供支架，所述支架包括在其中的空位柱；并且
将熔融的相变材料添加到所述支架中，使得通过毛细管作用将所述熔融的相变材料吸入所述空位中，以提供所述形状稳定的相变材料；
其中，所述支架是NaOH处理的石墨化壳聚糖，所述NaOH处理包括将石墨化壳聚糖支架用1摩尔NaOH水溶液饱和，在100℃下保持24小时以使表面功能化，将支架用去离子水冲洗并干燥；并且
所述相变材料是赤藓糖醇。
2.根据权利要求1所述的方法，其中，将所述冷冻的浆料暴露于引起升华的条件包括冷冻干燥。
3.根据权利要求1所述的方法，其中，冷冻包括将所述浆料倒入模具中并将所述模具放置在冷板上以在冷冻期间提供温度梯度。
4.根据权利要求1所述的方法，其中，所述浆料包括粘合剂。
5.根据权利要求1所述的方法，其中，所述浆料包含结构改性添加剂。
6.根据权利要求1所述的方法，该方法包括在添加所述熔融的相变材料的同时加热所述支架。
7.根据权利要求1所述的方法，其中，当将所述熔融的相变材料添加到所述支架中时，所述支架的温度大于所述相变材料的熔点。
8.根据权利要求1所述的方法，其中，将熔融的相变材料添加到所述支架中以提供所述形状稳定的相变材料包括将熔融的相变材料的液滴添加到所述支架中。
9.根据权利要求1所述的方法，其中，添加熔融的相变材料包括添加所述熔融的相变材料直到所述支架饱和。
10.根据权利要求1所述的方法，该方法包括在冷冻之前形成所述浆料。
11.根据权利要求10所述的方法，其中，形成所述浆料包括搅拌和行星式研磨中的至少一种。
12.根据权利要求11所述的方法，其中，形成所述浆料包括添加至少一种粘合剂、表面活性剂、分散剂、冰点降低剂、或结构改性剂。
13.根据权利要求1所述的方法，其中，添加所述熔融的相变材料包括在大气压下添加所述熔融的相变材料。
14.一种通过根据权利要求1所述的方法制备的形状稳定的相变材料。
15.一种形状稳定的相变材料，其包括：
多孔固体支架，所述多孔固体支架包括空位柱，其中所述支架的孔隙率是大于或等于74体积％；以及
渗透在所述支架的空位柱中的相变材料，其中所述相变材料具有在从-55℃至118℃温度范围的熔点；
其中包括所述相变材料的所述多孔固体支架在多个所述相变材料熔点左右的热循环内保持其形状；
其中，所述支架是NaOH处理的石墨化壳聚糖，所述NaOH处理包括将石墨化壳聚糖支架用1摩尔NaOH水溶液饱和，在100℃下保持24小时以使表面功能化，将支架用去离子水冲洗并干燥；并且
所述相变材料是赤藓糖醇。
16.一种生产用于相变材料的成核剂的方法，所述方法包括：
定向冷冻壳聚糖、溶剂和至少一种添加剂的浆料，提供冷冻的浆料，所述冷冻的浆料包括迫使悬浮的固体颗粒进入间隙的单向的冷冻的溶剂柱；
将所述冷冻的浆料暴露于引起所述冷冻的浆料的所述溶剂升华的条件以除去冷冻的溶剂并提供其中具有空位柱的主体；
烧结所述主体以提供石墨化壳聚糖支架；
用NaOH处理所述支架，所述NaOH处理包括将石墨化壳聚糖支架用1摩尔NaOH水溶液饱和，在100℃下保持24小时以使表面功能化，将支架用去离子水冲洗并干燥；并且
将所述支架研磨成粉末，用作相变材料成核助剂，所述相变材料是赤藓糖醇。
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