CN114824826A - 一种YFe4B4合金磁性吸波材料及其制备工艺 - Google Patents
一种YFe4B4合金磁性吸波材料及其制备工艺 Download PDFInfo
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Abstract
本发明提供一种YFe4B4合金磁性吸波材料及其制备工艺，涉及吸波材料技术领域。所述合金磁性吸波材料按照原子配比为YFe4‑x‑ yMnxSnyB4‑zSiz，其中0.1≤x≤0.8、0.2≤y≤0.6、0.1≤z≤0.8，且所述合金磁性吸波材料的制备方法主要包括配料、熔炼、球磨、成型、烧结、研磨等步骤，本发明克服了现有技术的不足，所制得的金磁性吸波材料在2‑8GHz内具有吸收频带宽、吸波性能优异的优点，且该材料的制备工艺容易掌握、生产成本低，适宜大规模的生产使用，提升市场的经济效益。
Description
技术领域
本发明涉及吸波材料技术领域，具体涉及一种YFe4B4合金磁性吸波材料及其制备工艺。
背景技术
近年来，随着各类电子产品的广泛应用，微波辐射已经成为一种新的污染源，对人类的健康造成了严重威胁,为此人们开发了各种吸波材料来防护微波辐射，同时军事上隐身技术开发，都促进了吸波材料的发展。
传统的吸波材料主要有铁氧体和磁性金属(合金)微粉等，虽然铁氧体是应用最广和最有效的抗电磁干扰材料，然而由于其饱和磁化强度低，热稳定性和耐腐蚀性差，因此铁氧体材料的应用受到很大的局限。而磁性金属微粉由于居里温度高，热稳定性好，有较好的饱和磁化强度以及颗粒形状效应，具有较高的复磁导率和较低的涡流损耗，匹配厚度较小(毫米级)，作为电磁波吸收剂具有很好的应用前景。
目前应用最多的软磁合金微粉主要是Fe、Co、Ni及其合金微粉等，由于Fe的资源比较丰富，价格相对于Co和Ni都比较低廉，而且Fe基合金吸波材料的吸波性能也较好，应用较为广泛，多应用于在2-18GHz频段，但是目前研制出的Fe基合金吸波材料在S(2-4GHz)和C(4-8GHz)波段特别是在S波段的吸波性能仍不理想，因而开发一种在2-8GHz范围内吸波性能好的吸波材料具有重要的意义。
发明内容
针对现有技术不足，本发明提供一种YFe4B4合金磁性吸波材料及其制备工艺，使得所制得的金磁性吸波材料在2-8GHz内具有吸收频带宽、吸波性能优异的优点，且该材料的制备工艺容易掌握、生产成本低，适宜大规模的生产使用，提升市场的经济效益。
为实现以上目的，本发明的技术方案通过以下技术方案予以实现：
一种YFe4B4合金磁性吸波材料，所述合金磁性吸波材料按照原子配比的比例为：YFe4-x-yMnxSnyB4-zSiz。
所述合金磁性吸波材料的制备方法包括：配料、熔炼、球磨、成型、烧结、研磨等步骤。
优选的，所述配料为：选取金属Y、Fe、Mn、Sn、Si、B为原料，按照YFe4-x-yMnxSnyB4-zSiz(0.1≤x≤0.8；0.2≤y≤0.6；0.1≤z≤0.8)，的原子配比配料，得原料混合物。
优选的，所述熔炼为：将原料混合物置于真空熔炼炉中在氩气保护下进行熔炼，浇铸获得合金锭。
优选的，所述球磨为：将合金锭破碎成颗粒度均小于0.5mm的粗粉，然后于50目筛下过筛获得合金粗粉；将破碎的合金粗粉与氧化锆球按18:1的质量比放入氧化锆罐中，在无水乙醇保护下球磨10-24h，球磨机转速为200-350r/min，得球磨粉末。
优选的，所述成型为：将球磨粉末在氮气保护的手套箱中取出晾干后压制成直径20mm，高度10mm的坯料。
优选的，所述烧结为：将坯料放入真空微波烧结炉中进行高温烧结，烧结温度1000-1060℃，保温20-40min，微波频率为2.0-3.2kW，获得烧结坯料；
优选的，所述研磨为：将烧结坯料破碎，使用玛瑙研钵将其研磨成细粉，然后于200目筛下过筛获得合金吸波粉上述烧结胚料取出后破碎，再研磨过筛，得合金吸波粉。
本发明提供一种YFe4B4合金磁性吸波材料及其制备工艺，与现有技术相比优点在于：
(1)本申请中所制得的合金磁性吸波材料能够在2-8GHz频段具有优良的微波吸收效果和频带宽度，有效保证材料的性能，提升材料的使用范围；
(2)本申请中材料经过配料、熔炼、球磨、成型、烧结、研磨即可得到，工序较为简单，且操作便捷，适合规模性生产，且有效降低生产成本。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面结合本发明实施例对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1：
一种YFe4B4合金磁性吸波材料：
(1)以纯度≥99.9％的金属Y、Fe、Mn、Sn、Si、B为原料，按YFe3.2Mn0.5Sn0.3B3.8Si0.2原子配比进行配料；
(2)在氩气保护下于标准的真空熔炼炉中熔炼，浇铸获得合金锭；
(3)将得到的合金锭破碎成颗粒度均小于0.5mm的粗粉，然后于50目筛下过筛获得合金粗粉；将破碎的合金粗粉与氧化锆球按18:1的质量比放入氧化锆罐中，在无水乙醇保护下球磨24h，球磨机转速为350r/min；
(4)将球磨的粉末在氮气保护的手套箱中取出晾干后压制成直径20mm，高度10mm的坯料；
(5)将坯料放入真空微波烧结炉中进行高温烧结，烧结温度1040℃，保温30min，微波频率为3.2kW，获得烧结坯料；
(6)将得到的烧结坯料破碎，使用玛瑙研钵将其研磨成细粉,然后于200目筛下过筛获得合金吸波粉。
实施例2：
一种YFe4B4合金磁性吸波材料：
(1)以纯度≥99.9％的金属Y、Fe、Mn、Sn、Si、B为原料，按YFe3.1Mn0.8Sn0.1B3.5Si0.5原子配比进行配料；
(2)在氩气保护下于标准的真空熔炼炉中熔炼，浇铸获得合金锭；
(3)将得到的合金锭破碎成颗粒度均小于0.5mm的粗粉，然后于50目筛下过筛获得合金粗粉；将破碎的合金粗粉与氧化锆球按18:1的质量比放入氧化锆罐中，在无水乙醇保护下球磨16h，球磨机转速为250r/min；
(4)将球磨的粉末在氮气保护的手套箱中取出晾干后压制成直径20mm,高度10mm的坯料；
(5)将坯料放入真空微波烧结炉中进行高温烧结，烧结温度1000℃，保温40min，微波频率为2.7kW，获得烧结坯料；
(6)将得到的烧结坯料破碎,使用玛瑙研钵将其研磨成细粉,然后于200目筛下过筛获得合金吸波粉。
实施例3：
一种YFe4B4合金磁性吸波材料：
(1)以纯度≥99.9％的金属Y、Fe、Mn、Sn、Si、B为原料，按YFe3.2Mn0.2Sn0.6B3.1Si0.9原子配比进行配料；
(2)在氩气保护下于标准的真空熔炼炉中熔炼，浇铸获得合金锭；
(3)将得到的合金锭破碎成颗粒度均小于0.5mm的粗粉，然后于50目筛下过筛获得合金粗粉；将破碎的合金粗粉与氧化锆球按18:1的质量比放入氧化锆罐中，在无水乙醇保护下球磨10h，球磨机转速为300r/min；
(4)将球磨的粉末在氮气保护的手套箱中取出晾干后压制成直径20mm,高度10mm的坯料；
(5)将坯料放入真空微波烧结炉中进行高温烧结，烧结温度1060℃，保温20min，微波频率为2.0kW，获得烧结坯料；
(6)将得到的烧结坯料破碎，使用玛瑙研钵将其研磨成细粉,然后于200目筛下过筛获得合金吸波粉。
检测：
将上述实施例1-3所得的合金吸波粉分别与石蜡按照质量比17：3的比例混合，制成内径和外径分别为3mm和7mm，厚度分别为1.0mm、1.3mm、1.6mm、1.9mm、2.2mm、2.5mm的同轴试样,将同轴试样分别采用HP8722ES微波矢量网络分析仪测量2-8GHz频段的复磁导率、复介电常数。
将测量的复磁导率、复介电常数数据按照式(1)计算出单层吸波材料的反射率R；
式中εr、μr和d分别为吸波材料的相对介电常数、相对磁导率和厚度，f为电磁波的频率，C为电磁波在自由空间的传播速度(即光速)，j为虚数单位。
其中实施例1中YFe3.2Mn0.5Sn0.3B3.8Si0.2合金吸波粉体测试结果见图2，从图2中可知：在所有的厚度中，最小反射率峰值均小于-10dB(吸收率大于90％)，且具有较好的宽频效果，当复合物厚度为1.0mm时，在4.8GHz频率处最小反射率峰值达到-31.9dB左右；当复合物厚度为1.3mm时，在4.1GHz频率处最小反射率峰值达到-28.3dB左右；当厚度为1.6mm时，在3.6GHz处其最小反射率峰值达到-29.8dB左右；当复合物厚度为1.9mm时，在3.2GHz处其最小反射率峰值达-30.2dB左右；当复合物厚度为2.2mm时，在2.8GHz处其最小反射率峰值达到-30.0dB左右；当复合物厚度为2.5mm时，在2.6GHz处其最小反射率峰值达到-26.4dB左右；当复合物厚度在1.6-2.5mm时，此复合物最小反射率都落在S波段(2-4GHz)之间，具有优良的微波吸收效果和频带宽度。
实施例2中YFe3.1Mn0.8Sn0.1B3.5Si0.5合金吸波粉体测试结果见图3，从图3中可知：在所有的厚度中，最小反射率峰值均小于-10dB(吸收率大于90％)，且具有较好的宽频效果，当复合物厚度为1.0mm时，在5.6GHz频率处最小反射率峰值达到-28.4dB左右；当复合物厚度为1.3mm时，在4.5GHz频率处最小反射率峰值达到-39.3dB左右；当厚度为1.6mm时，在3.84GHz处其最小反射率峰值达到-36.3dB左右；当复合物厚度为1.9mm时，在3.3GHz处其最小反射率峰值达到-36.5dB左右；当复合物厚度为2.2mm时，在2.8GHz处其最小反射率峰值达到-46.9dB左右；当复合物厚度为2.5mm时，在2.4GHz处其最小反射率峰值达到-29.6dB左右；当复合物厚度在1.6-2.5mm时，此复合物最小反射率都落在S波段(2-4GHz)之间，具有优良的微波吸收效果和频带宽度。
实施例3中YFe3.2Mn0.2Sn0.6B3.1Si0.9合金吸波粉体测试结果见图3，从图3中可知：在所有的厚度中，最小反射率峰值均小于-10dB(吸收率大于90％)，且具有较好的宽频效果，当复合物厚度为1.0mm时，在5.4GHz频率处最小反射率峰值达到-28.9dB左右；当复合物厚度为1.3mm时，在4.6GHz频率处最小反射率峰值达到-28.7dB左右；当厚度为1.6mm时，在3.80GHz处其最小反射率峰值达到-27.9dB左右；当复合物厚度为1.9mm时，在3.2GHz处其最小反射率峰值达到-28.1dB左右；当复合物厚度为2.2mm时，在2.8GHz处其最小反射率峰值达到-30.4dB左右；当复合物厚度为2.5mm时，在2.5GHz处其最小反射率峰值达到-29.3dB左右；当复合物厚度在1.6-2.5mm时，此复合物最小反射率都落在S波段(2-4GHz)之间，具有优良的微波吸收效果和频带宽度。
需要说明的是，在本文中，诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来，而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且，术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含，从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素，而且还包括没有明确列出的其他要素，或者是还包括为这种过程、方法、物品或者设备所固有的要素。在没有更多限制的情况下，由语句“包括一个……”限定的要素，并不排除在包括所述要素的过程、方法、物品或者设备中还存在另外的相同要素。
以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (8)
1.一种YFe4B4合金磁性吸波材料，其特征在于，所述合金磁性吸波材料按照原子配比的比例为：YFe4-x-yMnxSnyB4-zSiz。
2.一种如权利要求1所述的YFe4B4合金磁性吸波材料的制备方法，其特征在于，所述合金磁性吸波材料的制备方法包括以下步骤：
(1)配料：选取金属Y、Fe、Mn、Sn、Si、B为原料，按照YFe4-x-yMnxSnyB4-zSiz，的原子配比配料，得原料混合物备用；
(2)熔炼：将上述混合物置于真空熔炼炉中熔炼，浇铸获得合金锭；
(3)球磨：将上述合金锭破碎制备合金粗粉，后将合金粗粉进行球磨，得球磨粉末备用；
(4)成型：将上述球磨粉末在氮气保护的手套箱中取出晾干后压制成胚料；
(5)烧结：将上述坯料进行高温烧结，获得烧结坯料备用；
(6)研磨：将上述烧结胚料取出后破碎，再研磨过筛，得合金吸波粉。
3.根据权利要求2所述的一种YFe4B4合金磁性吸波材料的制备方法，其特征在于：所述步骤(1)中原子配比中0.1≤x≤0.8；0.2≤y≤0.6；0.1≤z≤0.8。
4.根据权利要求2所述的一种YFe4B4合金磁性吸波材料的制备方法，其特征在于：所述步骤(2)中熔炼需在氩气保护下进行。
5.根据权利要求2所述的一种YFe4B4合金磁性吸波材料的制备方法，其特征在于：所述步骤(3)中合金粗粉过50目筛，且球磨时将合金粗粉和氧化锆球按18:1的质量比放入氧化锆罐中，在无水乙醇保护下球磨24h，其中球磨机转速为350r/min。
6.根据权利要求2所述的一种YFe4B4合金磁性吸波材料的制备方法，其特征在于：所述步骤(4)中胚料的直径为20mm，高度为10mm。
7.根据权利要求2所述的一种YFe4B4合金磁性吸波材料的制备方法，其特征在于：所述步骤(5)中采用真空微波烧结炉对胚料进行烧结，其中烧结温度为1000-1060℃，烧结时间为20-40min，微波频率为2.0-3.2kW。
8.根据权利要求2所述的一种YFe4B4合金磁性吸波材料的制备方法，其特征在于：所述步骤(6)中合金吸波粉需过200目筛。
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