CN110218095A - 一种基于等级孔陶瓷的高效储热单元的制备方法 - Google Patents

一种基于等级孔陶瓷的高效储热单元的制备方法 Download PDF

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CN110218095A
CN110218095A CN201910261014.1A CN201910261014A CN110218095A CN 110218095 A CN110218095 A CN 110218095A CN 201910261014 A CN201910261014 A CN 201910261014A CN 110218095 A CN110218095 A CN 110218095A
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徐晓虹
张晨
李昱
吴建锋
周军辉
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Wuhan University of Technology WUT
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Abstract

本发明涉及一种基于等级孔陶瓷的高效储热单元的制备方法，其特征在于它包括以下步骤：1)设计等级孔结构参数：依据默里定律设计选取等级孔结构参数，一个完整的等级孔结构储热单元由多级孔构成，每一级孔分成kn个次级孔，各级孔的孔径D的关系满足默里定律(Dn 3＝kn·Dn+1 3)；2)制备等级孔陶瓷基体：以金属陶瓷TiB2粉体为主要原料，另添加1～3wt％的Si3N4，采用陶瓷3D打印成型等级孔结构陶瓷坯体，于氩气气氛中经1600～1750℃烧成，得到等级孔结构陶瓷基体；3)构筑储热单元：将上述等级孔结构陶瓷基体作为骨架，填充相变温度在500℃～700℃的熔盐或合金，封装，得到基于等级孔陶瓷的高效储热单元。该方法制备的储热单元具有储热密度大、传热换热效率高的优点。

Description

一种基于等级孔陶瓷的高效储热单元的制备方法
技术领域
本发明涉及一种基于等级孔陶瓷的高效储热单元的制备方法，主要用于采暖等各种储热领域，属于能源领域。
背景技术
自然界中存在的等级孔结构物质具有高效的物质与能量传输与交换能力，已成为研究热点。等级孔结构最早发现于生命体(如血管、植物根茎等)中，而等级孔结构材料是由孔隙结构的等级、形貌结构的等级、成分组成的等级三个方面共同构建而形成的。目前国内外在等级孔材料的制备与应用方面已开展了一些工作，如中国发明专利《一种具有等级孔结构的Y型分子筛制备方法》(CN108408736A)利用等级孔结构的Y型分子筛极大地提升了重油的汽油收率，并降低了焦炭的产率，具有显著的经济效益；中国发明专利《一种呈等级孔结构且宏孔单向排列氧化硅陶瓷的制备方法》(CN102295472B)制备的等级孔氧化硅陶瓷结合了微孔/介孔的高比表面积和宏孔网络快速传质的优点，可作为吸附剂、催化剂载体和多孔电极等；又如《Impregnation of porous material with phase change material forthermal energy storage》一文利用多孔珍珠岩、多孔硅藻、介孔γ-Al2O3等为原料，合成的等级孔结构相变复合材料在四次循环之后，仍然能够维持75％的质量储存密度(Nomura Tetc,Materials Chemistry and Physics,2009,115(2-3):846-850)。
陶瓷储热材料具有优良的热物理化学稳定性和耐侵蚀性，尤其当其与高储热密度的合金或熔盐等相变材料(PCM)复合构成陶瓷基储热单元时，往往具有更高的储热密度。中国发明专利《刚玉莫来石质蜂窝陶瓷蓄热体》(CN102399082B)公开了一种以刚玉、莫来石、氧化铝和粘土为原料制备的刚玉莫来石质蜂窝陶瓷蓄热体；中国发明专利《一种利用石墨尾矿制备蜂窝陶瓷蓄热体的方法》(CN201710212094.2)以固体废弃物石墨尾矿为主要原料，制备了低成本低烧成温度的蜂窝陶瓷储热材料，但以上两项专利中储热材料的储热密度有待提高；中国发明专利《一种低成本的太阳能热发电显热-潜热复合储热陶瓷及其制备方法》(CN201711066294.8)制备了一种以SiC-刚玉质蜂窝陶瓷封装Al-Si合金相变材料构成的复合储热单元，储热密度可达1500kJ/kg(室温～1000℃)，然而其热导率有待提高。
发明内容
本发明的目的是提供一种基于等级孔陶瓷的高效储热单元的制备方法，该方法制备的储热单元具有储热密度大、传热换热效率高的优点。
为实现上述目的，本发明所采取的技术方案是，一种基于等级孔陶瓷的高效储热单元的制备方法，其特征在于它包括以下步骤：
1)设计等级孔结构参数：依据默里定律设计选取等级孔结构参数，一个完整的等级孔结构储热单元由多级孔构成，相邻同级孔夹角为锐角，孔形状为圆形，每一级孔分成kn个次级孔，各级孔的孔径D的关系满足默里定律式中，n表示第n级孔，kn表示第n级孔分成kn个第n+1级孔，Dn表示第n级孔的孔径，Dn+1表示第n+1级孔的孔径；
2)制备等级孔陶瓷基体：依据所设计选取的等级孔结构参数，以金属陶瓷TiB2粉体(粒度≤2μm)为主要原料，另添加TiB2粉体质量1～3wt％的粒径小于0.2μm的Si3N4作为烧结助剂，混合，采用陶瓷3D打印成型等级孔结构陶瓷坯体(可提高TiB2陶瓷的抗高温氧化性能)，于氩气气氛中经1600～1750℃烧成，温度制度为：≤1200℃升温速率为1℃/min，温度＞1200℃升温速率为3℃/min，最高烧成温度保温1h，得到等级孔结构陶瓷基体；
3)构筑储热单元：将上述等级孔结构陶瓷基体作为骨架，填充相变温度在500℃～700℃的熔盐或合金中的一种于等级孔结构陶瓷基体外，然后将整个储热单元封装于绝热保温功能的高铝纤维箱体中，得到基于等级孔陶瓷的高效储热单元。
经测试，该基于等级孔陶瓷的高效储热单元的储热密度大于1800kJ/kg，导热系数大于15W/(m·K)。
所述多级孔为≥3级(如3-7级)。
所述kn为4-8。
所述熔盐为LiF/MgF2、LiF/NaF中的中的一种；合金为Al-Si合金、Al-Cu合金中的一种。
本发明的有益效果：
1.储热密度大。首先，本发明所采用的TiB2陶瓷体积密度高达4.5g·cm-3，远高于目前常用的SiC(3.2g·cm-3)、Al2O3(3.97g·cm-3)等储热陶瓷，意味着单位体积的储热材料具有更大的储热密度；另外，等级孔结构可提供更多的相界面，界面处非均相态可提高材料潜热，大大提高了储热密度。
2.传热换热效率高。首先，等级孔结构陶瓷储热单元相对于传统的直通孔结构，换热面积更大，显著提高了传热换热效率；其次，本发明采用的陶瓷基体材料为金属陶瓷TiB2，不仅常温下热导率高(25℃：96W/m·K)，而且高温下依然较高(1000℃：76W/m·K)，该特性显著优于高温下热导率衰减明显的Al2O3、SiC等，大幅提高了储热单元在200～1000℃工作区间的传热换热效率。
3.目前，对于新一代的高效储热单元的要求是兼具高储热密度、优良的高温服役性能和较快的储放热效率，但是已有的储热材料均无法同时兼具这三个特性。因此本发明提出将等级孔结构应用于陶瓷基储热单元的创新设计与制备，是一项变革性的技术，是一种在高温热循环条件下高效储热、高效传热换热的新型储热单元。
附图说明
图1是本发明等级孔结构陶瓷基体的实物图。
图2是本发明基于等级孔陶瓷的高效储热单元的示意图。
具体实施方式
为使本领域技术人员更好地理解本发明的技术方案，下面结合附图对本发明作进一步详细描述。
实施例1：
一种基于等级孔陶瓷的高效储热单元的制备方法，它包括以下步骤：
1)设计等级孔结构参数：依据默里定律设计选取等级孔结构参数。一个完整的等级孔结构储热单元由4级孔构成，依据孔径由大到小依次编号为第A1、A2、A3、A4级等级孔，孔径依次为D1＝100mm、D2＝55.03mm、D3＝30.29mm、D4＝16.67mm，相邻同级孔夹角为47°，孔形状为圆形，每一级孔分成6个次级孔(kn＝6)，各级孔的孔径D满足默里定律
2)制备等级孔陶瓷基体：依据所设计选取的等级孔结构参数，以金属陶瓷TiB2粉体(粒度＝2μm)为主要原料，另添加TiB2粉体质量1.5wt％的粒径为0.15μm的Si3N4粉体作为烧结助剂，同时可提高TiB2陶瓷的抗高温氧化性能，采用陶瓷3D打印成型等级孔结构陶瓷坯体，于氩气气氛中经1600℃烧成，温度制度为：≤1200℃升温速率为1℃/min，温度＞1200℃升温速率为3℃/min，最高烧成温度保温1h，得到等级孔结构陶瓷基体(即图2中枝状等级孔结构陶瓷材料)，实物图如附图1所示。
3)构筑储热单元：以上述等级孔结构陶瓷基体作为骨架，填充相变温度为572℃的Al-Si合金(即图2中PCM相变储热材料)于基体外，最终将整个储热单元封装于绝热保温功能的高铝纤维箱体(即图2中绝热保温复合陶瓷)中，得到基于等级孔陶瓷的高效储热单元，如附图2所示。
经测试，该储热单元的储热密度为2010kJ/kg，导热系数27W/(m·K)。
实施例2：
与实施例1基本相同，不同之处在于：Si3N4粉体的添加量为TiB2粉体质量1.0wt％，氩气气氛中经1650℃烧成；填充相变温度为620℃的Al-Cu合金于等级孔结构陶瓷基体外。
经测试，该基于等级孔陶瓷的高效储热单元的储热密度为1944kJ/kg，导热系数28W/(m·K)。
实施例3：
与实施例1基本相同，不同之处在于：Si3N4粉体的添加量为TiB2粉体质量3.0wt％，氩气气氛中经1750℃烧成。
经测试，该基于等级孔陶瓷的高效储热单元的储热密度为1877kJ/kg，导热系数21W/(m·K)。
实施例4：
与实施例1基本相同，不同之处在于；填充相变温度为650℃的LiF/MgF2熔盐于等级孔结构陶瓷基体外。
经测试，该基于等级孔陶瓷的高效储热单元的储热密度大于1823kJ/kg，导热系数16W/(m·K)。

Claims (4)

1.一种基于等级孔陶瓷的高效储热单元的制备方法，其特征在于它包括以下步骤：
1)设计等级孔结构参数：依据默里定律设计选取等级孔结构参数，一个完整的等级孔结构储热单元由多级孔构成，相邻同级孔夹角为锐角，孔形状为圆形，每一级孔分成kn个次级孔，各级孔的孔径D的关系满足默里定律(Dn 3＝kn·Dn+1 3)，式中，n表示第n级孔，kn表示第n级孔分成kn个第n+1级孔，Dn表示第n级孔的孔径，Dn+1表示第n+1级孔的孔径；
2)制备等级孔陶瓷基体：依据所设计选取的等级孔结构参数，以金属陶瓷TiB2粉体为主要原料，金属陶瓷TiB2粉体的粒度≤2μm，另添加TiB2粉体质量1～3wt％的粒径小于0.2μm的Si3N4作为烧结助剂，混合，采用陶瓷3D打印成型等级孔结构陶瓷坯体，于氩气气氛中经1600～1750℃烧成，温度制度为：≤1200℃升温速率为1℃/min，温度＞1200℃升温速率为3℃/min，最高烧成温度保温1h，得到等级孔结构陶瓷基体；
3)构筑储热单元：将上述等级孔结构陶瓷基体作为骨架，填充相变温度在500℃～700℃的熔盐或合金中的一种于等级孔结构陶瓷基体外，然后将整个储热单元封装于绝热保温功能的高铝纤维箱体中，得到基于等级孔陶瓷的高效储热单元。
2.根据权利要求1所述的一种基于等级孔陶瓷的高效储热单元的制备方法，其特征在于：所述多级孔为≥3级。
3.根据权利要求1所述的一种基于等级孔陶瓷的高效储热单元的制备方法，其特征在于：所述kn为4～8。
4.根据权利要求1所述的一种基于等级孔陶瓷的高效储热单元的制备方法，其特征在于：所述熔盐为LiF/MgF2、LiF/NaF中的一种；合金为Al-Si合金、Al-Cu合金中的一种。
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