CN116217216B - 可变太阳吸收率铁酸镧陶瓷粉体及其制备方法和应用 - Google Patents

可变太阳吸收率铁酸镧陶瓷粉体及其制备方法和应用 Download PDF

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CN116217216B
CN116217216B CN202310175702.2A CN202310175702A CN116217216B CN 116217216 B CN116217216 B CN 116217216B CN 202310175702 A CN202310175702 A CN 202310175702A CN 116217216 B CN116217216 B CN 116217216B
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solar absorptivity
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王忠阳
陈灿
童丽萍
范同祥
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Shanghai Jiaotong University
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Abstract

本发明提供了一种可变太阳吸收率铁酸镧陶瓷粉体及其制备方法和应用,所述的可变太阳吸收率铁酸镧陶瓷粉体的通式为La1‑xScxFeO3,其中,0.025≤x≤0.125,所述的可变太阳吸收率铁酸镧陶瓷粉体在25℃下对太阳波段吸收率不高于0.51、在270℃下对太阳波段吸收率不低于0.68。本发明提供的可变太阳吸收率铁酸镧陶瓷粉体或块体,为室温至270℃之间太阳吸收率变化值0.3的智能热控陶瓷材料;本发明提供的可变太阳吸收率铁酸镧陶瓷粉体或块体的制备方法,通过对铁酸镧的镧位进行钪掺杂使铁酸镧在25℃‑270℃的太阳吸收率变化增大,并通过调节钪的掺杂量使所述材料的25℃‑270℃可变太阳吸收率最大达到0.3(x=0.1),同时降低了铁酸镧体系相同温度水平下的太阳吸收率/红外发射率比值。

Description

可变太阳吸收率铁酸镧陶瓷粉体及其制备方法和应用
技术领域
本发明涉及智能材料技术领域,具体地,涉及可变太阳吸收率铁酸镧陶瓷粉体及其制备方法和应用。
背景技术
智能热控材料根据温度水平的变化调整自身的热物性参数从而实现对热控对象的温度控制,智能热控材料的太阳吸收率αs、红外发射率ε是两个重要的性能参数,通过改变材料的太阳吸收率,可以在不同条件下实现智能热控。
现有的智能热控材料大都从调控红外发射率入手,如钙钛矿型锰氧化物、二氧化钒等。但基于钙钛矿型锰氧化物和二氧化钒的智能热控陶瓷材料几乎已到达其自身性能极限,钙钛矿型锰氧化物需进行表面的精加工和多层膜系设计来降低其过高的太阳吸收率,而二氧化钒制备方法复杂,因此目前智能热控领域对新型材料有迫切需求,缺乏制备方法简便的可变太阳吸收率的智能热控材料。
发明内容
针对现有技术中的缺陷,本发明的目的是一种可变太阳吸收率铁酸镧陶瓷粉体及块体,通过Sc掺杂对铁酸镧材料的太阳吸收率进行调控,获得室温至270℃之间太阳吸收率变化值0.3的智能热控陶瓷材料,同时降低了铁酸镧体系相同温度水平下的太阳吸收率/红外发射率比值,在热控领域有广阔的应用前景;此外,本发明还提供了该可变太阳吸收率铁酸镧陶瓷粉体和块体的制备方法及应用。
本发明第一方面提供了一种可变太阳吸收率铁酸镧陶瓷粉体,所述的可变太阳吸收率铁酸镧陶瓷粉体的通式为La1-xScxFeO3,其中,0.025≤x≤0.125,所述的可变太阳吸收率铁酸镧陶瓷粉体在25℃下对太阳波段吸收率不高于0.51、在270℃下对太阳波段吸收率不低于0.68。
在本发明的一实施方式中,所述的可变太阳吸收率铁酸镧陶瓷粉体为正交相。
本发明第二方面提供了上述可变太阳吸收率铁酸镧陶瓷粉体的制备方法,包括以下步骤:
(1)将硝酸镧水合物、硝酸铁水合物、硝酸钪水合物溶于去离子水中,再加入络合剂,反应形成凝胶;
(2)将步骤(1)中反应形成的凝胶降温至室温,干燥,研磨,煅烧,得到可变太阳吸收率铁酸镧陶瓷粉体。
在本发明的一实施方式中,基于安全性、简便性的考虑,步骤(1)中的络合剂为柠檬酸;
步骤(1)中,硝酸铁水合物、硝酸镧水合物和硝酸钪水合物的摩尔量总和与柠檬酸的摩尔比为1:1.1;
步骤(1)中,反应温度为80℃~90℃。
在本发明的一实施方式中,步骤(2)中干燥温度为100℃;
步骤(2)中的煅烧具体步骤为:以5℃/min的升温速度升至600℃保温3小时,以5℃/min的升温速度升至800℃保温5小时,然后以5℃/min的降温速度降至500℃,自然冷却至室温;本发明中上述煅烧步骤,可以确保完全完全反应,成分均匀,粉体颗粒大小均匀。
本发明第三方面提供了采用上述制备方法制得的可变太阳吸收率铁酸镧陶瓷粉体制备可变太阳吸收率铁酸镧陶瓷块体的方法,包括以下步骤:将可变太阳吸收率铁酸镧陶瓷粉体压制成片,煅烧,得到可变太阳吸收率铁酸镧陶瓷块体。
在本发明的一实施方式中,变太阳吸收率铁酸镧陶瓷粉体压制成片后,煅烧,煅烧的具体步骤为:以5℃/min的升温速度升至550℃保温2小时,以5℃/min的升温速度升至1250℃保温5小时,然后以5℃/min的降温速度降至500℃,自然冷却至室温;本申请中上述煅烧具体步骤,可以确保块体陶瓷不过烧(过于致密,晶界消失)或欠烧(粉体颗粒间未形成结合力,块体松散不成型)。
本发明第四方面提供了上述可变太阳吸收率铁酸镧陶瓷粉体在制备智能热控材料中的应用或作为智能热控材料在智能热控领域的应用。
本发明第五方面提供了上述可变太阳吸收率铁酸镧陶瓷块体在制备智能热控材料中的应用或作为智能热控材料在智能热控领域的应用。
与现有技术相比,本发明的实施例具有如下的有益效果:
1、本发明实施例提供的可变太阳吸收率铁酸镧陶瓷粉体或块体,为室温至270℃之间太阳吸收率变化值0.3的智能热控陶瓷材料,在热控领域有广阔的应用前景。
2、本发明实施例提供的可变太阳吸收率铁酸镧陶瓷粉体或块体的制备方法,通过对铁酸镧的镧位进行钪掺杂使铁酸镧在25℃-270℃的太阳吸收率变化增大,并通过调节钪的掺杂量使所述材料的25℃-270℃可变太阳吸收率最大达到0.3(x=0.1),同时降低了铁酸镧体系相同温度水平下的太阳吸收率/红外发射率比值,在热控领域有广阔的应用前景。
3、本发明实施例提供的可变太阳吸收率铁酸镧陶瓷粉体或块体的制备方法,解决了目前缺乏调控太阳吸收率的智能热控材料的问题,提出了通过调控太阳吸收率从而实现智能热控的新思路。
4、本发明实施例提供的可变太阳吸收率铁酸镧陶瓷粉体或块体用于制备智能热控材料或直接作为智能热控材料应用,在建筑、电子和个人热管理等领域热控具有重要的应用价值。
当然,实施本发明的任一产品并不一定需要同时达到以上所述的所有优点。
附图说明
通过阅读参照以下附图对非限制性实施例所作的详细描述,本发明的其它特征、目的和优点将会变得更明显:
图1为实施例1、实施例2、实施例3及对比例1中所制得的陶瓷块体的外观图;
图2为实施例1、实施例2、实施例3及对比例1中所制得的陶瓷粉体的XRD图谱;
图3为实施例1、实施例2、实施例3及对比例1中所制得的陶瓷块体的XRD图谱;
图4为实施例1、实施例2、实施例3及对比例1中所制得的陶瓷块体的SEM图像;其中,图4(a)为对比例1中所制得的陶瓷块体的SEM图像,图4(b)为实施例1中所制得的陶瓷块体的SEM图像,图4(c)为实施例2中所制得的陶瓷块体的SEM图像,图4(d)为实施例3中所制得的陶瓷块体的SEM图像;
图5为实施例1、实施例2、实施例3及对比例1中所制得的陶瓷块体的可见光吸收光谱;
图6为对比例1中所制得的陶瓷块体在25℃、270℃的反射率图谱;
图7为实施例1中所制得的陶瓷块体在25℃、270℃的反射率图谱;
图8为实施例2中所制得的陶瓷块体在25℃、270℃的反射率图谱;
图9为实施例3中所制得的陶瓷块体在25℃、270℃的反射率图谱。
具体实施方式
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明,但不以任何形式限制本发明。应当指出的是,对本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变化和改进。这些都属于本发明的保护范围。
此外,下面所描述的本发明不同实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互结合。
实施例1
本实施例提供了一种可变太阳吸收率铁酸镧陶瓷粉体的制备方法,包括以下步骤:
分别称取La(NO3)3·6H2O(99.99%)25.3336g、Fe(NO3)3·9H2O(AR)24.4848g和Sc(NO3)3·5H2O(99.99%)0.3465g溶于去离子水中,搅拌使其混合均匀,称取柠檬酸(AR)34.7554g溶于去离子水中,加入硝酸盐溶液中,水浴恒温90℃同时通过磁力搅拌6h,形成凝胶;冷却至室温,在100℃干燥24h,研磨,以5℃/min的升温速率升至600℃煅烧3h,再以5℃/min的升温速率升至800℃煅烧5h,以5℃/min的降温速率降至500℃,冷却至室温,得到可变太阳吸收率铁酸镧陶瓷粉体。
本实施例中还提供了一种将上述所得可变太阳吸收率铁酸镧陶瓷粉体制作为可变太阳吸收率铁酸镧陶瓷块体的方法,包括以下步骤:
将上述的陶瓷粉体称取4g置于Φ30mm的模具中,使用液压机将其压成圆片,以5℃/min的升温速率升至550℃保温2h,再以5℃/min的升温速率升至1250℃煅烧5h,以5℃/min的降温速率降至500℃,冷却至室温,得到可变太阳吸收率铁酸镧陶瓷块体。
本实施例所得可变太阳吸收率铁酸镧陶瓷块体的相组成为La0.975Sc0.025FeO3
实施例2
本实施例提供了一种可变太阳吸收率铁酸镧陶瓷粉体的制备方法,包括以下步骤:
分别称取La(NO3)3·6H2O(99.99%)23.3849g、Fe(NO3)3·9H2O(AR)24.4848g和Sc(NO3)3·5H2O(99.99%)1.3860g溶于去离子水中,搅拌使其混合均匀,称取柠檬酸(AR)34.7554g溶于去离子水中,加入硝酸盐溶液中,水浴恒温90℃同时通过磁力搅拌6h,形成凝胶。冷却至室温,在100℃干燥24h,研磨,以5℃/min的升温速率升至600℃煅烧3h,再以5℃/min的升温速率升至800℃煅烧5h,以5℃/min的降温速率降至500℃,冷却至室温,得到可变太阳吸收率铁酸镧陶瓷粉体。
本实施例中还提供了一种将上述所得可变太阳吸收率铁酸镧陶瓷粉体制作为可变太阳吸收率铁酸镧陶瓷块体的方法,包括以下步骤:
将上述的陶瓷粉体称取4g置于Φ30mm的模具中,使用液压机将其压成圆片,以5℃/min的升温速率升至550℃保温2h,再以5℃/min的升温速率升至1250℃煅烧5h,以5℃/min的降温速率降至500℃,冷却至室温,得到可变太阳吸收率铁酸镧陶瓷块体。
本实施例所得可变太阳吸收率铁酸镧陶瓷块体的相组成为La0.9Sc0.1FeO3
实施例3
本实施例提供了一种可变太阳吸收率铁酸镧陶瓷粉体的制备方法,包括以下步骤:
分别称取La(NO3)3·6H2O(99.99%)22.7353g、Fe(NO3)3·9H2O(AR)24.4848g和Sc(NO3)3·5H2O(99.99%)1.7324g溶于去离子水中,搅拌使其混合均匀,称取柠檬酸(AR)34.7554g溶于去离子水中,加入硝酸盐溶液中,水浴恒温90℃同时通过磁力搅拌6h,形成凝胶。冷却至室温,在100℃干燥24h,研磨,以5℃/min的升温速率升至600℃煅烧3h,再以5℃/min的升温速率升至800℃煅烧5h,以5℃/min的降温速率降至500℃,冷却至室温,得到可变太阳吸收率铁酸镧陶瓷粉体。
本实施例中还提供了一种将上述所得可变太阳吸收率铁酸镧陶瓷粉体制作为可变太阳吸收率铁酸镧陶瓷块体的方法,包括以下步骤:
将上述的陶瓷粉体称取4g置于Φ30mm的模具中,使用液压机将其压成圆片,以5℃/min的升温速率升至550℃保温2h,再以5℃/min的升温速率升至1250℃煅烧5h,以5℃/min的降温速率降至500℃,冷却至室温,得到可变太阳吸收率铁酸镧陶瓷块体。
本实施例所得可变太阳吸收率铁酸镧陶瓷块体的相组成为La0.875Sc0.125FeO3
对比例1
本对比例提供了一种铁酸镧陶瓷粉体的制备方法,包括以下步骤:
分别称取La(NO3)3·6H2O(99.99%)25.9832g、Fe(NO3)3·9H2O(AR)24.4848g溶于去离子水中,搅拌使其混合均匀,称取柠檬酸(AR)34.7554g溶于去离子水中,加入硝酸盐溶液中,水浴恒温90℃同时通过磁力搅拌6h,形成凝胶。冷却至室温,在100℃干燥24h,研磨,以5℃/min的升温速率升至600℃煅烧3h,再以5℃/min的升温速率升至800℃煅烧5h,以5℃/min的降温速率降至500℃,冷却至室温,得到铁酸镧陶瓷粉体。
本对比例还提供了一种将上述所得铁酸镧陶瓷粉体制备为铁酸镧陶瓷块体的方法,包括以下步骤:
将上述的陶瓷粉体称取4g置于Φ30mm的模具中,使用液压机将其压成圆片,以5℃/min的升温速率升至550℃保温2h,再以5℃/min的升温速率升至1250℃煅烧5h,以5℃/min的降温速率降至500℃,冷却至室温,得到铁酸镧陶瓷块体。
本对比例所得铁酸镧陶瓷块体的相组成为LaFeO3
试验例
本试验例对实施例1-3及对比例1中所制得的陶瓷材料进行表征,使用X射线衍射图谱(XRD,德国Bruker公司,D8 focus)表征可变太阳吸收率粉体和块体的晶体结构和物相,使用扫描电镜(SEM,TESCAN,MIRA3)表征块体陶瓷表面形貌,使用紫外-可见-近红外分光光度计系统(国产,Lamda 950)表征样品的太阳吸收率。
从可变太阳吸收率陶瓷粉体和块体的XRD图谱(图2、图3)可以确认样品为标准正交相(PDF#74-2203)。图中显示的所有峰都与铁酸镧的峰匹配得很好。随着Sc3+掺杂浓度的增加,没有发现任何新的衍射峰,包括氧化镧、三氧化二铁和氧化钪峰。说明,Sc3+进入了铁酸镧钙钛矿的晶格形成了稳定正交相。因此,各实施例和对比例中块体陶瓷的物相应如表1中所示。
表1可变太阳吸收率陶瓷块体物相组成
块体 实施例1 实施例2 实施例3 对比例1
相组成 La0.975Sc0.025FeO3 La0.9Sc0.1FeO3 La0.875Sc0.125FeO3 LaFeO3
从可变太阳吸收率陶瓷块体的扫描电镜图像(图4)可以观察到所述陶瓷块体的陶瓷晶粒以及晶粒间空隙,空隙是由于氧在烧结过程中逸出而产生的。掺杂Sc后所述陶瓷块体的空隙减少,陶瓷体更为致密,晶粒变大。
从可变太阳吸收率陶瓷块体的可见光吸收光谱(图5)可以看出实施例1-3和对比例1的样品均有较强的可见光吸收,掺杂后的吸收边缘清晰可见。
图6-图9显示出25℃、270℃下可变太阳吸收率陶瓷块体的太阳(0.25μm~2.5μm)光谱图。通过光谱计算出的太阳吸收率如表2所示。可以看出,掺杂Sc后,25℃下的太阳吸收率从0.76下降到约0.5,高温下的太阳吸收率也有一定的降低。在x=0.1的掺杂水平下,从25℃到270℃的太阳吸收率(Δαs)增量增加到0.3。说明钪掺杂可以有效提升铁酸镧材料的可变太阳吸收率范围。
表2可变太阳吸收率陶瓷块体在不同温度下的太阳吸收率
以上对本发明的具体实施例进行了描述。需要理解的是,本发明并不局限于上述特定实施方式,本领域技术人员可以在权利要求的范围内做出各种变化或修改,这并不影响本发明的实质内容。在不冲突的情况下,本申请的实施例和实施例中的特征可以任意相互组合。

Claims (7)

1.一种可变太阳吸收率铁酸镧陶瓷粉体,其特征在于,所述的可变太阳吸收率铁酸镧陶瓷粉体的通式为La1-xScxFeO3,其中,0.025≤x≤0.125,所述的可变太阳吸收率铁酸镧陶瓷粉体在25℃下对太阳波段吸收率不高于0.51、在270℃下对太阳波段吸收率不低于0.68;
所述可变太阳吸收率铁酸镧陶瓷粉体的制备方法,包括以下步骤:
(1)将硝酸镧水合物、硝酸铁水合物、硝酸钪水合物溶于去离子水中,再加入络合剂,反应形成凝胶;
(2)将步骤(1)中反应形成的凝胶降温至室温,干燥,研磨,煅烧,得到可变太阳吸收率铁酸镧陶瓷粉体;
其中,步骤(2)中干燥温度为100℃;步骤(2)中的煅烧具体步骤为:以5℃/min 的升温速度升至600℃保温3小时,以5℃/min 的升温速度升至800℃保温5小时,然后以5℃/min的降温速度降至500℃,自然冷却至室温。
2.根据权利要求1所述的可变太阳吸收率铁酸镧陶瓷粉体,其特征在于,所述的可变太阳吸收率铁酸镧陶瓷粉体为正交相。
3.根据权利要求1所述的可变太阳吸收率铁酸镧陶瓷粉体,其特征在于,步骤(1)中的络合剂为柠檬酸;
步骤(1)中,硝酸铁水合物、硝酸镧水合物和硝酸钪水合物的摩尔量总和与柠檬酸的摩尔比为1:1.1;
步骤(1)中,反应温度为80℃~90℃。
4.一种利用权利要求1~3任一项所述可变太阳吸收率铁酸镧陶瓷粉体制备可变太阳吸收率铁酸镧陶瓷块体的方法,其特征在于,包括以下步骤:将可变太阳吸收率铁酸镧陶瓷粉体压制成片,煅烧,得到可变太阳吸收率铁酸镧陶瓷块体。
5.根据权利要求4所述的制备可变太阳吸收率铁酸镧陶瓷块体的方法,其特征在于,可变太阳吸收率铁酸镧陶瓷粉体压制成片后,煅烧,煅烧的具体步骤为:以5℃/min 的升温速度升至550℃保温2小时,以5℃/min 的升温速度升至1250℃保温5小时,然后以5℃/min的降温速度降至500℃,自然冷却至室温。
6.权利要求1~3任一项所述的可变太阳吸收率铁酸镧陶瓷粉体在制备智能热控材料中的应用或作为智能热控材料在智能热控领域中的应用。
7.由权利要求4~5任一项所述的制备可变太阳吸收率铁酸镧陶瓷块体的方法制备得到的可变太阳吸收率铁酸镧陶瓷块体在制备智能热控材料中的应用或作为智能热控材料在智能热控领域中的应用。
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