CN108129144B - 一种低吸收/发射比自适应控温材料及其制备方法 - Google Patents
一种低吸收/发射比自适应控温材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种低吸收/发射比自适应，属于新材料领域，材料组分为BayAxTiO3，其中A为Sr、Sn、Ca、La、Nb、Y中一种或多种，其中x+y=1；本发明还公开了其制备方法，获得材料的红外发射率随外界热环境变化而在居里点附近发生变化，利用此方法制备的智能型自适应热控材料，具有低太阳吸收比，as<0.3，红外发射率变化幅度大的特性，ΔeH>0.2，可广泛应用于航天器热控***、建筑物节能减排、电子设备散热以及战术武器红外隐身等领域；特别是在建筑物节能减排、电子设备散热和航天器热控领域具有巨大的实用价值和应用前景。
Description
技术领域
本发明属于属于新材料领域，具体是指一种低吸收/发射比自适应控温材料 及其制备方法。
背景技术
智能型温控材料，是指材料本身在不同环境温度的激励作用下，通过自身结构物理性质的跃变实现红外发射率的突变，而自适应改变其热辐射性能，具有冬暖夏凉式的空调功能。智能温控材料在国防科技和民用节能减排领域具有极大的应用前景。可广泛应用于航天器热控、建筑物节能、智能玻璃/窗、发动机散热、电子产品散热、LED灯具散热等领域。实现智能温控的材料技术主要有电致变色材料、热致变色材料技术和热控百叶窗等。其中热致变色材料具有重量轻、无外加功耗、成本低、应用范围广等优点，成为当前热控技术领域最具前景的材料技术之一。然而，目前开发的VO2基和La1-xAxMnO3基热致相变可变发射率材料均存在突出的自身缺陷，严重限制了智能热控材料的应用。VO2材料在Tc=68℃发生由低温绝缘态（高发射率）向高温金属态（低发射率）快速可逆的热致相变，不符合传统低温保暖和高温散热的应用需求。尽管文献（吴春华等，一种用于改变智能热控材料控温能力的薄膜及其制备方法，中国专利CN104561897A）对VO2材料进行多层膜系设计，基本满足了应用需求，但存在结构复杂、成本较高、应用受限等缺点。另一种热致相变可变发射率材料La1-xAxMnO3则通常外观为深蓝色/黑色（张勇等，一种智能热辐射陶瓷材料的制备方法，中国专利CN101531513B），其太阳吸收比高达0.89，严重制约了其热控能力。因此，亟需探索开发具有低太阳吸收-半球发射比热环境响应特性的新型自适应热控材料。
发明内容
本发明针对现有技术中存在的问题，公开了一种低吸收/发射比自适应控温 材料及其制备方法，获得材料的红外发射率随外界热环境变化而在居里点附近发 生变化，利用此方法制备的智能型自适应热控材料，具有低太阳吸收比、红外发 射率变化幅度大的特性，解决了现有技术中存在的问题。
本发明是这样实现的：
一种低吸收/发射比自适应控温材料，其特征在于，所述的材料组分为 BayAxTiO3，其中A为Sr、Sn、Ca、La、Nb、Y其中一种或多种，x+y＝1。
进一步，所述的材料外观为白色；所述材料的居里温度点在-10～40℃范围内 可调，当环境温度低于居里点时，呈低发射率态；当环境温度高于居里点时，突 变为高红外发射率态,本发明自适应热控材料，具有低太阳吸收比，αs<0.3，红 外发射率变化幅度大的特性，ΔεH>0.2。
本发明还公开了一种低吸收/发射比自适应控温材料的制备方法，其特征在 于，具体步骤如下：
步骤一：分别称取1份TiO2粉末，x份A的氧化物或碳酸盐,y份Ba的氧 化物或碳酸盐，A为Sr(锶)、Sn(锡)、Ca(钙)、La(镧)、Nb(铌)、Y (钇)其中一种或多种，x+y＝1；
步骤二：将上述称量好试剂与玛瑙球、水或乙醇按体积比1：1：1混合放入 玛瑙球磨罐中，混合研磨24h，取出烘干；
步骤三：将步骤二中研磨后的粉末过100目筛，放入坩埚置于马弗炉中预烧；
步骤四：将预烧后的粉末取出，加入Al2O3、MnO2和纳米SiO2中的一种或多种， 通过加入三者中的一种或多种来改变发射率变化范围。加入后再次放入玛瑙罐中 球磨10h，取出烘干；
步骤五：将步骤四中的烘干后的粉末加入聚乙烯醇水溶液造粒(浓度1at％)， 聚乙烯醇水溶液加入量为粉末质量的5％，于100～200Mpa压力下压制成型， 然后烧结，烧结温度为1000～1400℃，保温时间1～3h。
进一步，所述的步骤一中的粉末纯度>99.9％，粒径分布在亚微米尺寸。
进一步，所述的步骤二中是采用行星式球磨机进行混合研磨。
进一步，所述的步骤三马弗炉预烧参数为：温度900～1200℃；预烧0.5～1h。
本发明与现有技术的有益效果在于：
1)本发明的方法是基于钙钛矿材料的金属-绝缘体转变原理，获得材料 的红外发射率随外界热环境变化而在居里点附近发生变化。居里温 度点在-10～40℃范围内可调，当环境温度低于居里点时，呈低发射 率态；当环境温度高于居里点时，突变为高红外发射率态；
2)利用此方法制备的智能型自适应热控材料，具有低太阳吸收比， αs<0.3，红外发射率变化幅度大的特性，ΔεH>0.2，可广泛应用于航 天器热控***、建筑物节能减排、电子设备散热以及战术武器红外 隐身等领域；特别是在建筑物节能减排、电子设备散热和航天器热 控领域具有巨大的实用价值和应用前景；
3)利用本发明方法制备的材料外观为白色，可有效反射太阳辐射热流， 同时其红外发射率随环境温度而自动调节，解决了当前热致变色材 料高太阳吸收比造成的温控能力差的问题，极大拓展了智能控温材 料的应用领域，适用于建筑物外墙冬保暖夏散热及航天器热控***；
4)本发明方法通过优化材料组分及工艺，优化后的工艺简单、成本低 廉，易于规模化生产，可做成涂层、陶瓷片、透明薄膜等形式，满 足不同领域的应用需求。
附图说明
图1为本发明实施例1制备的智能热控材料的扫描电子显微镜照片。
具体实施方式
为使本发明的目的、技术方案及效果更加清楚，明确，以及参照附图并举实 例对本发明进一步详细说明。应当指出此处所描述的具体实施仅用以解释本发明， 并不用于限定本发明。
实施例1
1)按化学计量比BayAxTiO3称取1mol TiO2粉，0.4mol碳酸锶(A组分),0.6mol 碳酸钡，三者的纯度>99.9％，粉末粒径在亚微米尺寸；
2)将步骤1)称量好的粉末与玛瑙球、水按体积比1：1：1混合放入玛瑙球 磨罐中，用行星式球磨机混合研磨24h，取出，100℃烘干；
3)将步骤2)中的粉末过100目筛，放入刚玉坩埚置于马弗炉，进行1000℃ 预烧1h，随炉冷却至室温；
4)将步骤3)中的粉末取出，放入0.005mol Al2O3和0.024mol纳米SiO2， 再次放入玛瑙罐中球磨10h，取出烘干
5)将步骤4)中的粉末加入聚乙烯醇水溶液造粒(浓度1at％)，聚乙烯醇水 溶液加入量为粉末质量的5％，于150Mpa压力下压制成型，然后烧结， 烧结温度为1350℃，保温时间3h。如图1所示，图1为本实施例制备的 材料的扫描电子显微镜照片。
6)将制备的智能热控陶瓷材料样品的居里温度为276K，太阳吸收比为0.25， 在270K时红外发射率为0.42，在300K时的红外发射率为0.67，ΔεH＝0.25。
实施例2
1)称取1mol TiO2粉，0.7mol Ba的碳酸盐(碳酸钡)，0.3mol Sr的碳酸盐(碳 酸锶A组分)，粉末纯度>99.9％，粒径在亚微米尺寸；
2)将步骤1)称量好的粉末与玛瑙球、乙醇按体积比1：1：1混合放入玛瑙 球磨罐中，用行星式球磨机混合研磨24h，取出，100℃烘干；
3)将步骤2)中的粉末过100目筛，放入坩埚置于马弗炉，进行1150℃预烧 0.5h，随炉冷却至室温；
4)将步骤3)中的粉末取出，放入0.003mol Al2O3，0.002mol MnO2和0.02mol 纳米SiO2，再次放入玛瑙罐中球磨10h，取出烘干
5)将步骤4)中的粉末加入聚乙烯醇水溶液造粒(浓度1at％)，聚乙烯醇水 溶液加入量为粉末质量的5％，于200Mpa压力下压制成型，然后烧结， 烧结温度为1380℃，保温时间2h；
6)本实施例制备的智能热控陶瓷材料样品的居里温度为290K，太阳吸收比 为0.25，在275K时红外发射率为0.45，在310K时的红外发射率为0.71， ΔεH＝0.26；
实施例3
1)称取1mol TiO2，0.6mol碳酸钡,0.3mol的碳酸锶，0.1mol碳酸锡，粉末 纯度>99.9％，粒径在亚微米尺寸；
2)将步骤1)称量好的粉末与玛瑙球、水或乙醇按体积比1：1：1混合放入 玛瑙球磨罐中，用行星式球磨机混合研磨24h，取出，100℃烘干；
3)将步骤2)中的粉末过100目筛，放入刚玉坩埚置于马弗炉，进行1100℃ 预烧1h，随炉冷却至室温
4)将步骤3)中的粉末取出，放入0.001mol Al2O3，0.002mol MnO2和0.03mol 纳米SiO2，再放入玛瑙罐中球磨10h，取出烘干，过100目筛。
5)将步骤4)中的粉末加入聚乙烯醇水溶液造粒(浓度1at％)，聚乙烯醇水 溶液加入量为粉末质量的5％，于200Mpa压力下压制成型，1050℃烧结 2h，用30分钟降温至800℃，然后随炉冷却至室温，得到热致变色可变 发射率材料组成为Ba0.6Sr0.3Sn0.1TiO3；
6)本实施例制备的粉末材料的居里温度为287K，太阳吸收比为0.26，在275K 时红外发射率为0.58，在310K时的红外发射率为0.79，ΔεH＝0.21；
实施例4
1)称取1mol TiO2粉，0.3mol氧化锡和0.1mol氧化钙(A组分),0.6mol氧 化钡，三者的纯度>99.9％，粉末粒径在亚微米尺寸；
2)将步骤1)称量好的粉末与玛瑙球、水按体积比1：1：1混合放入玛瑙球 磨罐中，用行星式球磨机混合研磨24h，取出，100℃烘干；
3)将步骤2)中的粉末过100目筛，放入刚玉坩埚置于马弗炉，进行1000℃ 预烧0.5h，随炉冷却至室温；
4)将步骤3)中的粉末取出，放入0.005mol Al2O3和0.024mol纳米SiO2， 再次放入玛瑙罐中球磨10h，取出烘干
5)将步骤4)中的粉末加入聚乙烯醇水溶液造粒(浓度1at％)，聚乙烯醇水 溶液加入量为粉末质量的5％，于150Mpa压力下压制成型，然后烧结， 烧结温度为1350℃，保温时间3h。
实施例5
1)称取1mol TiO2粉，0.3mol氧化锶和0.1mol氧化镧(A组分),0.6mol氧 化钡，三者的纯度>99.9％，粉末粒径在亚微米尺寸；
2)将步骤1)称量好的粉末与玛瑙球、乙醇按体积比1：1：1混合放入玛瑙 球磨罐中，用行星式球磨机混合研磨24h，取出，100℃烘干；
3)将步骤2)中的粉末过100目筛，放入刚玉坩埚置于马弗炉，进行1000℃ 预烧0.5h，随炉冷却至室温；
4)将步骤3)中的粉末取出，放入0.005mol Al2O3，0.002mol MnO2，0.024 mol纳米SiO2，再次放入玛瑙罐中球磨10h，取出烘干
5)将步骤4)中的粉末加入聚乙烯醇水溶液造粒(浓度1at％)，聚乙烯醇水 溶液加入量为粉末质量的5％，于150Mpa压力下压制成型，然后烧结， 烧结温度为1000℃，保温时间1h。
实施例6
1)称取1mol TiO2粉，0.3mol氧化钙和0.1mol氧化铌(A组分),0.6mol 氧化钡，粉末纯度>99.9％，粒径在亚微米尺寸；
2)将步骤1)称量好的粉末与玛瑙球、水按体积比1：1：1混合放入玛瑙球 磨罐中，用行星式球磨机混合研磨24h，取出，100℃烘干；
3)将步骤2)中的粉末过100目筛，放入坩埚置于马弗炉，进行1150℃预烧 0.5h，随炉冷却至室温；
4)将步骤3)中的粉末取出，放入0.003mol Al2O3，0.02mol纳米SiO2，再 次放入玛瑙罐中球磨10h，取出烘干
5)将步骤4)中的粉末加入聚乙烯醇水溶液造粒(浓度1at％)，聚乙烯醇水 溶液加入量为粉末质量的5％，于200Mpa压力下压制成型，然后烧结， 烧结温度为1400℃，保温时间1h。
实施例7
1)称取1mol TiO2粉，0.2mol氧化钇和0.2mol碳酸锡(A组分),0.6mol 碳酸钡，粉末纯度>99.9％，粒径在亚微米尺寸；
2)将步骤1)称量好的粉末与玛瑙球、乙醇按体积比1：1：1混合放入玛瑙 球磨罐中，用行星式球磨机混合研磨24h，取出，100℃烘干；
3)将步骤2)中的粉末过100目筛，放入坩埚置于马弗炉，进行1150℃预烧 0.5h，随炉冷却至室温；
4)将步骤3)中的粉末取出，放入0.003mol Al2O3，0.02mol纳米SiO2，再 次放入玛瑙罐中球磨10h，取出烘干
5)将步骤4)中的粉末加入聚乙烯醇水溶液造粒(浓度1at％)，聚乙烯醇水 溶液加入量为粉末质量的5％，于200Mpa压力下压制成型，然后烧结， 烧结温度为1200℃，保温时间2h。
Claims (2)
1.一种低吸收/发射比自适应控温材料的制备方法，其特征在于，所述的方法具体制备步骤如下：
1）、称取1mol TiO2粉，0.4mol碳酸锶, 0.6mol碳酸钡，三者的纯度>99.9%，粉末粒径在亚微米尺寸；
2）、将步骤1）称量好的粉末与玛瑙球、水按体积比1：1：1混合放入玛瑙球磨罐中，用行星式球磨机混合研磨24h，取出，100℃烘干；
3）、将步骤2）中的粉末过100目筛，放入刚玉坩埚置于马弗炉，进行1000℃预烧1h，随炉冷却至室温；
4）、将步骤3）中的粉末取出，放入0.005 mol Al2O3和0.024 mol 纳米SiO2，再次放入玛瑙罐中球磨10h，取出烘干；
5）、将步骤4）中的粉末加入聚乙烯醇水溶液造粒，聚乙烯醇水溶液加入量为粉末质量的5%，于150Mpa压力下压制成型，然后烧结，烧结温度为1350℃，保温时间3h。
2.根据权利要求1所述的一种低吸收/发射比自适应控温材料的制备方法制得的材料。
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