CN108383491B - 高岭土基储热陶瓷及其制备方法 - Google Patents

高岭土基储热陶瓷及其制备方法 Download PDF

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CN108383491B
CN108383491B CN201810186085.5A CN201810186085A CN108383491B CN 108383491 B CN108383491 B CN 108383491B CN 201810186085 A CN201810186085 A CN 201810186085A CN 108383491 B CN108383491 B CN 108383491B
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刘松阳
韩杰
王鲁男
李海军
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Liaoning Shihua University
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Abstract

本发明公开一种用于热能存储系统的高岭土基储热陶瓷及其制备方法，以高岭土为主要原料，通过添加造孔剂的方法制备多孔陶瓷预制体，多孔陶瓷预制体中组分含量重量比是：高岭土：氢氧化铝：外加氟化铝：石墨为3‑7：3‑7：1：1。通过改变原料中高岭土的添加量从而对多孔陶瓷预制体中莫来石的形貌进行调控，以多孔陶瓷预制体为基体，将其完全置入相变材料碳酸钠中，通过熔融浸渍法制备高岭土基储热陶瓷。本发明可提高天然高岭土的附加值，制备方法简单。所制备的高岭土基储热陶瓷具有储热容量大、抗折强度高、抗热震特性好等特点。本发明能够有效提高热能存储系统工作时的稳定性和连续性，表现出较高的储热容量和抗热震性能。

Description

高岭土基储热陶瓷及其制备方法
技术领域
本发明涉及复合相变储热材料领域，具体是高岭土基储热陶瓷及其制备方法。
背景技术
太阳能作为一种开发潜力巨大的新能源和可再生能源，早已引起了世界各国的广泛关注。但是在太阳能的转化和使用过程中，时间和空间上存在供需不匹配的矛盾，限制了太阳能资源的高效利用。储能技术可以很好的解决能源供需平衡问题，实现能量的存储，提高能源利用效率。然而我国能源利用率很低，大约30％左右，与发达国家的40％～50％相比，还有很大差距。而能源的紧张和能源在利用中所造成的环境污染问题使得人们强烈要求使用具有间歇性的太阳能等清洁能源。与此同时，为了克服电力负荷峰谷差严重的状况，在全国实行峰谷电价政策来鼓励工业和民间在采暖、空调制冷、热水工业及其它方面使用谷期电力，这都对储能技术的实际应用提出了严峻的考验。
作为储热技术的核心已被广泛应用于太阳能光热领域：太阳能热发电、建筑节能、太阳能热水系统等节能减排产业。然而，储热材料的高成本制备限制这些终端产业的发展，从而影响太阳能光热技术的广泛应用。因此，迫切需求高性能储热材料的低成本制备技术。由于储热材料的基础研究欠缺，未能建立储热材料微结构与储热性能之间的关系，无法掌握储热材料性能调控的关键技术。我国高岭土矿产资源储量丰富，分布广泛，在经济建设中起着十分重要的作用。高岭土具有独特的孔道结构和优良的物理化学特性，具有十分广阔的应用前景和研究价值。然而目前我国对于高岭土矿产资源开发和利用水平相对较低，因此对其进行精细化加工和研究至关重要。由于高岭土矿物具有独特的结构、丰富的形貌、良好的热稳定性等原料优势，同时具备简单易得、价格低廉的成本优势。因此，通过发掘高岭土的储热特性，将矿高岭土与储热材料结合有望低成本获得高性能矿物基复合储热材料，并建立微结构与性能之间的联系，实现储热性能的调控。
发明内容
本发明选用天然的高岭土为主要原料，制备具有较高气孔率及抗折强度的多孔陶瓷预制体(PCP)。以多孔陶瓷预制体为基体材料，融化浸渍相变材料碳酸钠，制备高岭土基储热陶瓷。利用高岭土在高温环境下的结构演变，考察高岭土的结构对储热陶瓷抗热震性能的影响机制，制备成本低廉、耐高温、抗热震性能良好的储热陶瓷，解决上述背景技术中提出的问题。
为实现上述目的，本发明提供如下技术方案：高岭土基储热陶瓷及其制备方法：高岭土基储热陶瓷,其特征在于:多孔陶瓷预制体中组分含量重量比是：高岭土：氢氧化铝：外加氟化铝：石墨为3-7：3-7：1：1。
优选方案一:多孔陶瓷预制体中组分含量是高岭土70g，氢氧化铝30g，外加氟化铝10g，石墨10g。
优选方案二:多孔陶瓷预制体中组分含量是高岭土30g，氢氧化铝70g，外加氟化铝10g，石墨10g。
高岭土基储热陶瓷的制备方法，其特征在于:
a)、将权利要求1所述含量的高岭土、氢氧化铝、氟化铝和石墨混合后搅拌2小时；
b)、将5wt％的水做为结合剂加入混合均匀的粉末中，继而装入成型模具中，成型压力20-80kN，保压时间为30s，即生坯；
c)、将生坯置于80℃的干燥箱中干燥24小时备用；
d)、最高烧结温度1400-1500℃，设定烧成制度如下：从室温升温至850℃的升温速率为2℃/min，温度高于850℃时升温速率为5℃/min，升至最高烧结温度，制备多孔陶瓷预制体。
f)、以多孔陶瓷预制体为基体，Na2CO3为相变材料，将基体材料完全置于Na2CO3中，当外界环境温度高于Na2CO3熔点时，Na2CO3相变材料融化、浸渍于多孔陶瓷预制体中，从而制备储热陶瓷，浸渍温度为900-1100℃，浸渍时间为0.5-2.5h。
当样品中高岭土添加量从70wt％增加至30wt％时，PCP中莫来石形貌从针状转变为片状，如附图2(a)、(b)所示。当浸渍Na2CO3后，其绝大部分孔隙被凝固的Na2CO3堵住，如附图3(a)、(b)所示。此外，在经过三十次抗热震实验后，高岭土基储热陶瓷其线收缩基本没有发生变化，表面没有裂痕形成，表明在长期应用中具有良好的可靠性；而表面裂纹较为明显，这表明Na2CO3相变材料在热循环过程中可能从PCP中泄露出来，从而失去储放热能力，如图4所示。
本发明的有益效果是：
本发明是高岭土基储热陶瓷及其制备方法，以天然的高岭土为主要原材料制备储热陶瓷，成本低廉，具有广阔的应用前景。通过改变原料中高岭土和氢氧化铝的比例调控多孔陶瓷预制体中莫来石的形貌，从而影响储热陶瓷的储热性能。所制备的储热陶瓷具有更高的相变潜热及抗热震特性，其相变温度和相变焓分别为874.93℃和52.59J/g。在经过三十次抗热震循环实验后，储热陶瓷表面基本没有发生变化，其相变焓为52.47J/g，仅仅改变了0.12J/g，展现出极为良好的可靠性。
附图说明
图1为高岭土基储热陶瓷制备流程图；
图2(a)、(b)分别为PCP-1及PCP-2的扫描电镜照片；
图3(a)、(b)分别为PCP-1/Na2CO3及PCP-2/Na2CO3的扫描电镜照片；
图4为PCP-1/Na2CO3及PCP-2/Na2CO3抗热震循环前后表观形貌图。
具体实施方式:
实施例1
高岭土基储热陶瓷及其制备方法，其具体制备步骤为：
步骤一、实验设计两种制备多孔陶瓷预制体的配方。1号多孔陶瓷预制体(PCP-1)中各组分含量分别为：高岭土70g，氢氧化铝30g，外加氟化铝10g，石墨10g；2号多孔陶瓷预制体(PCP-2)中各组分含量分别为：高岭土30g，氢氧化铝70g，外加氟化铝10g，石墨10g；
步骤二、将PCP-1或PCP-2中的高岭土、氢氧化铝、氟化铝和石墨混合后搅拌2小时；
步骤三、将5wt％的结合剂(水)加入混合均匀的粉末中，继而装入成型模具中，成型压力20kN，保压时间为30s，即生坯；
步骤四、将生坯置于80℃的干燥箱中干燥24小时备用；
步骤五、最高烧结温度1400℃，设定烧成制度如下：从室温升温至850℃的升温速率为2℃/min，温度从850℃升高至1400℃时升温速率为5℃/min，制备二种多孔陶瓷预制体PCP-1及PCP-2。
步骤六、以PCP-1或PCP-2为基体，Na2CO3相变材料，将二种基体材料完全置于Na2CO3中。当外界环境温度高于Na2CO3熔点时，Na2CO3相变材料融化、浸渍于二种多孔陶瓷预制体中，从而制备PCP-1/Na2CO3和PCP-2/Na2CO3储热陶瓷，浸渍温度为900℃，浸渍时间为0.5h。
实施例2
高岭土基储热陶瓷及其制备方法，其具体制备步骤为：
步骤一、实验设计两种制备多孔陶瓷预制体的配方。1号多孔陶瓷预制体(PCP-1)中各组分含量分别为：高岭土70g，氢氧化铝30g，外加氟化铝10g，石墨10g；2号多孔陶瓷预制体(PCP-2)中各组分含量分别为：高岭土30g，氢氧化铝70g，外加氟化铝10g，石墨10g；
步骤二、将PCP-1或PCP-2中的高岭土、氢氧化铝、氟化铝和石墨混合后搅拌2小时；
步骤三、将5wt％的结合剂(水)加入混合均匀的粉末中，继而装入成型模具中，成型压力50kN，保压时间为30s，即生坯；
步骤四、将生坯置于80℃的干燥箱中干燥24小时备用；
步骤五、最高烧结温度1450℃，设定烧成制度如下：从室温升温至850℃的升温速率为2℃/min，温度从850℃升高至1450℃时升温速率为5℃/min，制备二种多孔陶瓷预制体PCP-1及PCP-2。
步骤六、以PCP-1或PCP-2为基体，Na2CO3相变材料，将二种基体材料完全置于Na2CO3中。当外界环境温度高于Na2CO3熔点时，Na2CO3相变材料融化、浸渍于二种多孔陶瓷预制体中，从而制备PCP-1/Na2CO3和PCP-2/Na2CO3储热陶瓷，浸渍温度为950℃，浸渍时间为1.5h。
实施例3
高岭土基储热陶瓷其制备方法，其具体制备步骤为：
步骤一、实验设计两种制备多孔陶瓷预制体的配方。1号多孔陶瓷预制体(PCP-1)中各组分含量分别为：高岭土70g，氢氧化铝30g，外加氟化铝10g，石墨10g；2号多孔陶瓷预制体(PCP-2)中各组分含量分别为：高岭土30g，氢氧化铝70g，外加氟化铝10g，石墨10g；
步骤二、将PCP-1或PCP-2中的高岭土、氢氧化铝、氟化铝和石墨混合后搅拌2小时；
步骤三、将5wt％的结合剂(水)加入混合均匀的粉末中，继而装入成型模具中，成型压力80kN，保压时间为30s，即生坯；
步骤四、将生坯置于80℃的干燥箱中干燥24小时备用；
步骤五、最高烧结温度1500℃，设定烧成制度如下：从室温升温至850℃的升温速率为2℃/min，温度从850℃升高至1500℃时升温速率为5℃/min，制备二种多孔陶瓷预制体PCP-1及PCP-2。
步骤六、以PCP-1或PCP-2为基体，Na2CO3相变材料，将二种基体材料完全置于Na O3中。当外界环境温度高于Na2CO3熔点时，Na2CO3相变材料融化、浸渍于二种多孔陶瓷预制体中，从而制备PCP-1/Na2CO3和PCP-2/Na2CO3储热陶瓷，浸渍温度为1000℃，浸渍时间为2.5h。

Claims (1)

1.高岭土基储热陶瓷的制备方法，其特征在于:
a)、将高岭土、氢氧化铝、氟化铝和石墨混合后搅拌 2 小时；其中高岭土 30 g，氢氧化铝 70 g，外加氟化铝10 g，石墨 10 g；
b)、 将 5 wt%的水作为结合剂加入混合均匀的粉末中，继而装入成型模具中，成型压力 20-80 kN，保压时间为 30 s，即得生坯；
c)、将生坯置于 80 °C 的干燥箱中干燥 24 小时备用；
d)、最高烧结温度 1400-1500 °C，设定烧成制度如下：从室温升温至 850 °C 的升温速率为 2 °C/min，温度高于 850 °C 时升温速率为5 °C/min，升至最高烧结温度，制备多孔陶瓷预制体；
f）、以多孔陶瓷预制体为基体， Na2CO3 为相变材料，将基体材料完全置于 Na2CO3 中，当外界环境温度高于 Na2CO3 熔点时，Na2CO3 相变材料融化、浸渍于多孔陶瓷预制体中，从而制备储热陶瓷，浸渍温度为 900-1100 °C，浸渍时间为 0.5-2.5 h。
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