CN112795832B - 一种稀土铁硼基磁制冷材料及其制备方法与应用 - Google Patents
一种稀土铁硼基磁制冷材料及其制备方法与应用 Download PDFInfo
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Abstract
本发明公开了一种稀土铁硼基磁制冷材料及其制备方法与应用,其特征在于化学通式为:La1‑xRExFe12‑yTyB6;为SrNi12B6型晶体结构,属于
Description
技术领域
本发明属于磁学材料技术领域,特别涉及一种稀土铁硼基磁制冷材料及其制备方法与其在磁制冷机中的应用。
背景技术
磁制冷是一种利用磁性材料的磁热效应(即magnetocaloric effect,又称磁卡效应或磁熵效应)实现制冷的一种无污染的制冷方式。磁制冷的原理是利用外加磁场而使磁工质的磁矩发生有序、无序的变化(相变)引起磁体吸热和放热作用而进行制冷循环。通过磁制冷工质进入高磁场区域,放出热量到周围环境;进入零/低磁场区域,温度降低,吸收热量达到制冷的目的;如此反复循环可连续制冷。与传统的制冷技术相比具有效率高、单元体积小、运行平稳、无噪音等优点。特别是相比较于氟利昂压缩制冷带来的种种环境问题,磁制冷技术是完全绿色无环境污染的制冷方式。磁制冷技术被认为是未来可能取代传统的气体压缩制冷,成为最有发展前景的制冷技术之一。而取决于这一技术能否走出实验室,走向商用化的关键之一是寻找不同温区的磁制冷材料。目前一方面高性能磁制冷材料相对较少,另一方面目前报道的高性能磁制冷材料,特别是中低温区磁制冷材料,一般均含有重稀土元素,由于重稀土元素价格昂贵且含量稀少,而限制了该类材料的实际应用。开发高丰度稀土低成本基磁性材料是稀土材料可持续发展战略至关重要。
根据研究,轻稀土La1-xRExFe12-yTyB6材料在各自磁转变温度附近部级具有较大的磁熵变。是一种优异的磁制冷材料,在磁制冷中具有较好的应用前景。
发明内容
本发明的目的是针对现有技术的不足,提供一种稀土铁硼基磁制冷材料及其制备方法与应用。
本发明一种稀土铁硼基磁制冷材料化学通式为:La1-xRExFe12-yTyB6;其中RE为轻稀土Pr、Nd、Sm中的一者或两者之间的混合,T为过渡金属Co、Ni、Mn、Cu、Al、Cr、Zn中的一种或者多种的混合,0.03≤x≤0.5,0≤y≤3;
所述的La1-xRExFe12-yTyB6材料为SrNi12B6型晶体结构,属于空间群,在0~5T的磁场变化下,等温磁熵变为10.2-16.8J/kgK;在0~7T的磁场变化下,等温磁熵变为12.5-20.3J/kgK。
所述的稀土铁硼基磁制冷材料的制备方法,其特征在于包括以下步骤:
步骤一:按照化学式La1-xRExFe12-yTyB6称量La、RE、Fe、T、B原料;
步骤二:在惰性气体保护或真空下,采用电弧放电、等离子放电、感应或电阻加热的方式将步骤一中的原料加热到熔化并保持1-3分钟;
步骤三:在惰性气体保护或真空下,将上一步骤所得产物翻转后,采用电弧、感应或电阻加热的方式再次加热至熔化并保持1-3分钟,此步骤可重复3-5次;
步骤四:将所得产物加热至800-1250摄氏度真空或惰性气体下保护下退火70-480小时,得到均匀的La1-xRExFe12-yTyB6磁制冷材料。
一种稀土铁硼基磁制冷材料在磁制冷机中的应用。
本发明相对现有技术具有的效果:本发明稀土铁硼材料采用常规技术手段制备,该方法工艺简单、原料价格低廉,适用于工业化生产与应用。
具体实施方式
下面对本发明做进一步的分析,但具体实施案例并不对本发明作任何限定。
实施例1:
本实施例制备化学式La0.9Pr0.1Fe12B6的磁制冷材料,其制备方法按以下具体步骤进行:
步骤一:按摩尔比La:Pr:Fe:B=0.9:0.1:12:6比例,分别称量纯度为99.9%的La、Pr、Fe、B原料;
步骤二:将称好的原料放入水冷坩埚中,在Ar气体保护下,采用电弧熔炼的原料加热到熔化并保持1分钟;
步骤三:在Ar气体保护下,将步骤二所得产物翻转后,再次利用电弧熔炼加热至熔化,并保持1分钟,重复此步骤5次;
步骤四:将所得得到La0.9Pr0.1Fe12B6锭子加热到1200摄氏度真空下退火80小时,获得多晶块体。
利用XRD和磁性测定表明La0.9Pr0.1Fe12B6材料为SrNi12B6型晶体结构,属于空间群,在0~5T的磁场变化下,等温磁熵变为10.8J/kgK;在0~7T的磁场变化下,等温磁熵变为13.5J/kgK。
实施例2:
本实施例制备化学式La0.8Nd0.2Fe12B6的磁制冷材料,其制备方法按以下具体步骤进行:
步骤一:按摩尔比La:Nd:Fe:B=0.8:0.2:12:6比例,分别称量纯度为99.9%的La、Nd、Fe、B原料;
步骤二:将称好的原料放入水冷坩埚中,在Ar气体保护下,采用感应熔炼的原料加热到熔化并保持2分钟;
步骤三:在Ar气体保护下,将步骤二所得产物翻转后,再次利用感应熔炼加热至熔化,并保持1.5分钟,重复此步骤3次;
步骤四:将所得得到La0.8Nd0.2Fe12B6锭子加热到1100摄氏度真空下退火120小时,获得多晶块体。
利用XRD和磁性测定表明La0.8Nd0.2Fe12B6材料为SrNi12B6型晶体结构,属于空间群,在0~5T的磁场变化下,等温磁熵变为11.2J/kgK;在0~7T的磁场变化下,等温磁熵变为14.3J/kgK。
实施例3:
本实施例制备化学式La0.6Pr0.3Nd0.1Fe12B6的磁制冷材料,其制备方法按以下具体步骤进行:
步骤一:按摩尔比La:Pr:Nd:Fe:B=0.6:0.3:0.1:12:6比例,分别称量纯度为99.9%的La、Pr、Nd、Fe、B原料;
步骤二:将称好的原料放入水冷坩埚中,在真空下,采用电阻丝熔炼的原料加热到熔化并保持3分钟;
步骤三:在Ar气体保护下,将步骤二所得产物翻转后,再次利用感应熔炼加热至熔化,并保持3分钟,重复此步骤3次;
步骤四:将所得得到La0.6Pr0.3Nd0.1Fe12B6锭子加热到800摄氏度真空下退火220小时,获得多晶块体。
利用XRD和磁性测定表明La0.6Pr0.3Nd0.1Fe12B6材料为SrNi12B6型晶体结构,属于空间群,在0~5T的磁场变化下,等温磁熵变为11.2J/kgK;在0~7T的磁场变化下,等温磁熵变为13.3J/kgK。
实施例4:
本实施例制备化学式La0.85Pr0.15Fe11CoB6的磁制冷材料,其制备方法按以下具体步骤进行:
步骤一:按摩尔比La:Pr:Fe:Co:B=0.85:0.15:11:1:6比例,分别称量纯度为99.9%的La、Pr、Fe、Co、B原料;
步骤二:将称好的原料放入水冷坩埚中,在真空下,采用电弧熔炼的原料加热到熔化并保持2分钟;
步骤三:在Ar气体保护下,将步骤二所得产物翻转后,再次利用感应熔炼加热至熔化,并保持2分钟,重复此步骤4次;
步骤四:将所得得到La0.85Pr0.15Fe11CoB6锭子加热到900摄氏度真空下退火300小时,获得多晶块体。
利用XRD和磁性测定表明La0.85Pr0.15Fe11CoB6材料为SrNi12B6型晶体结构,属于空间群,在0~5T的磁场变化下,等温磁熵变为15.4J/kgK;在0~7T的磁场变化下,等温磁熵变为19.2J/kgK。
实施例5:
本实施例制备化学式La0.6Pr0.2Sm0.2Fe10Ni2B6的磁制冷材料,其制备方法按以下具体步骤进行:
步骤一:按摩尔比La:Pr:Sm:Fe:Ni:B=0.6:0.2:0.2:10:2:6比例,分别称量纯度为99.9%的La、Pr、Nd、Fe、Ni、B原料;
步骤二:将称好的原料放入水冷坩埚中,在真空下,采用感应熔炼的原料加热到熔化并保持2.5分钟;
步骤三:在Ar气体保护下,将步骤二所得产物翻转后,再次利用感应熔炼加热至熔化,并保持2.5分钟,重复此步骤4次;
步骤四:将所得得到La0.6Pr0.2Sm0.2Fe10Ni2B6锭子加热到1100摄氏度真空下退火320小时,获得多晶块体。
利用XRD和磁性测定表明La0.6Pr0.2Sm0.2Fe10Ni2B6材料为SrNi12B6型晶体结构,属于空间群,在0~5T的磁场变化下,等温磁熵变为13.3J/kgK;在0~7T的磁场变化下,等温磁熵变为16.2J/kgK。
实施例6:
本实施例制备化学式La0.6Nd0.2Sm0.2Fe10CuMnB6的磁制冷材料,其制备方法按以下具体步骤进行:
步骤一:按摩尔比La:Nd:Sm:Fe:Cu:Mn:B=0.6:0.2:0.2:10:1:1:6比例,分别称量纯度为99.9%的La、Pr、Nd、Fe、Ni、B原料;
步骤二:将称好的原料放入水冷坩埚中,在真空下,采用感应熔炼的原料加热到熔化并保持2.5分钟;
步骤三:在Ar气体保护下,将步骤二所得产物翻转后,再次利用感应熔炼加热至熔化,并保持2.5分钟,重复此步骤4次;
步骤四:将所得得到La0.6Nd0.2Sm0.2Fe10CuMnB6锭子加热到1150摄氏度真空下退火400小时,获得多晶块体。
Claims (4)
1.一种稀土铁硼基磁制冷材料,其特征在于:化学通式为:La1-xRExFe12-yTyB6;其中RE为轻稀土Pr、Nd、Sm中的一者或两者之间的混合,T为过渡金属Co、Ni、Mn、Cu、Al、Cr、Zn中的一种或者多种的混合,0.03≤x≤0.5,0≤y≤3。
3.根据权利要求1所述的一种稀土铁硼基磁制冷材料的制备方法,其特征在于:包括以下步骤:
步骤一:按照化学式La1-xRExFe12-yTyB6称量La、RE、Fe、T、B原料;
步骤二:在惰性气体保护或真空下,采用电弧放电、等离子放电、感应或电阻加热的方式将步骤一中的原料加热到熔化并保持1-3分钟;
步骤三:在惰性气体保护或真空下,将上一步骤所得产物翻转后,采用电弧、感应或电阻加热的方式再次加热至熔化并保持1-3分钟,此步骤重复3-5次;
步骤四:将所得产物加热至800-1250摄氏度真空或惰性气体下保护下退火70-480小时,得到均匀的La1-xRExFe12-yTyB6磁制冷材料。
4.根据权利要求1所述的一种稀土铁硼基磁制冷材料在磁制冷机中的应用。
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