CN106856119A - 一种多元结构宽带片状吸收剂的制备方法 - Google Patents

一种多元结构宽带片状吸收剂的制备方法 Download PDF

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CN106856119A
CN106856119A CN201611116478.6A CN201611116478A CN106856119A CN 106856119 A CN106856119 A CN 106856119A CN 201611116478 A CN201611116478 A CN 201611116478A CN 106856119 A CN106856119 A CN 106856119A
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吴赛
程红飞
张昳
张丹丹
杨东方
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BEIJING INSTITUTE OF AERONAUTICAL MATERIALS CHINA AVIATION INDUSTRY GROUP Corp
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    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
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    • H01F1/12Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
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    • H01F1/14716Fe-Ni based alloys in the form of sheets
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    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
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Abstract

本发明属于微波吸波材料技术领域,具体涉及一种具有轻质、高磁导率、磁谱和介电谱特性良好的多元结构宽带片状吸收剂的制备方法。本发明提出了新颖的过程可控机械合金化方法制备一种轻质、高磁导率、磁谱和介电谱特性良好的Fe‑Ni‑SiO2多元结构宽带片状吸收剂。形状各向异性的片状磁性金属材料的退磁场不为零,其磁导率和频散特性较传统球形羰基铁粉有显著的改善。同时,Fe元素和Ni元素进行合金化制备片状Fe‑Ni合金化粉末的谐振频率向低频偏移,进一步地在合金化粉末表面包覆SiO2可在不降低吸收剂磁导率的前提下提高其阻抗匹配特性,从而为制备轻质、高磁导率、磁谱和介电谱特性良好的宽带片状吸收剂提供理想方案。

Description

一种多元结构宽带片状吸收剂的制备方法
技术领域:
本发明属于微波吸波材料技术领域,具体涉及一种具有轻质、高磁导率、磁谱和介电谱特性良好的多元结构宽带片状吸收剂的制备方法。
背景技术
吸收剂是决定吸波材料性能优劣的关键组成部分,而目前研制的吸收剂主要为球形羰基铁粉和铁氧体,由于结构简单或饱和磁化强度小,磁导率数值不够大、频散特性差,无法达到吸波材料“簿、轻、宽、强”的要求。
发明内容
本发明的目的是针对上述存在的问题,提出一种多元结构宽带片状吸收剂的制备方法。
本发明的目的是通过以下技术方案实现的:
步骤1:将磨球和Fe粉、Ni粉按比例投入到转速和工作气氛可控的高能搅拌球磨机中,并加入过程控制剂;将所述的球磨机抽真空后冲入氩气,在氩气保护下先进行低速分散混合,后提高转速进行金属粉末快速塑性变形、合金化;然后加入气相SiO2对上述合金化粉末进行包覆,完成后停机、冷却;磨球选用直径5~12mm的氧化锆,选用D50为5μm、分布1-20μm的Fe粉,选用D50为3μm、分布1-5μm的Ni粉,选用D≤20nm的气相SiO2,选用的过程控制剂为硬脂酸;其中Fe粉、Ni粉和气相SiO2的质量比为50~70:10~20:10~15,球料比为10~50;低速分散的时间为0.5~2h,球磨机转速为50~150rpm,高速分散的时间为10~30h,球磨机转速为160~300rpm,氩气流量为50~100ml/min;
步骤2:将上述经过机械合金化及包覆完成后的合金化粉末进行球料分离,然后使用旋风分级分离设备,在氮气保护气体下进行粒度分级,得到平均长度为10~15μm,厚度小于等于0.3μm的Fe-Ni-SiO2多元结构宽带片状吸收剂,其中,氮气进气工作压力为0.5~0.8MPa。
本发明技术方案的优点是:
本发明提出了新颖的过程可控机械合金化方法制备一种轻质、高磁导率、磁谱和介电谱特性良好的Fe-Ni-SiO2多元结构宽带片状吸收剂。形状各向异性的片状磁性金属材料的退磁场不为零,其磁导率和频散特性较传统球形羰基铁粉有显著的改善。同时,Fe元素和Ni元素进行合金化制备片状Fe-Ni合金化粉末的谐振频率向低频偏移,进一步地在合金化粉末表面包覆SiO2可在不降低吸收剂磁导率的前提下提高其阻抗匹配特性,从而为制备轻质、高磁导率、磁谱和介电谱特性良好的宽带片状吸收剂提供理想方案。
附图说明
图1实施例一中Fe-Ni-SiO2多元结构宽带片状吸收剂SEM形貌图。
图2实施例一中Fe-Ni-SiO2多元结构宽带片状吸收剂TEM形貌图。
具体实施方式
以下将结合实施例对本发明技术方案做进一步地详述:
步骤1:将磨球和Fe粉、Ni粉按照一定质量比投入到转速和工作气氛可控的高能搅拌球磨机中,并加入适量的过程控制剂;
步骤2:将所述的球磨机抽真空后冲入氩气,在氩气保护下先进行低速分散混合,后提高转速进行金属粉末快速塑性变形、合金化;
步骤3:通过加料装置加入气相SiO2对上述合金化粉末进行包覆,完成后停机、冷却。
步骤4:将上述经过机械合金化及包覆完成后的合金化粉末进行球料分离,然后使用旋风分级分离设备,在氮气保护气体下进行粒度分级,得到平均长度约为10~15μm,厚度小于等于0.3μm的Fe-Ni-SiO2多元结构宽带片状吸收剂。
本发明所述的Fe粉、Ni粉和气相SiO2的质量比为50~70:10~20:10~15,球料比为10~50;选用直径5~12mm的氧化锆作为磨球,选用D50为5μm、分布1-20μm的Fe粉,D50为3μm、分布1-5μm的Ni粉和D≤20nm气相SiO2;选用的过程控制剂为硬脂酸。
本发明所述的高能搅拌球磨机转速控制在50~300rpm范围内,氩气流量为50~100ml/min,金属粉末合金化时间为10~30h,无机粉末包覆时间为5~10h。
本发明所述的粉末旋风分级分离在氮气保护下进行,氮气进气工作压力为0.5~0.8MPa。
实施例1
(1)将2.1Kg的Fe粉(D50为5μm、分布1-20μm)、0.3Kg的Ni粉(D50为3μm、分布1-5μm)和60Kg的氧化锆(直径为8mm)加入转速和工作气氛可控的高能搅拌球磨机中,然后加入10g硬脂酸。
(2)将上述加料后的球磨机进行抽真空,并冲入氩气作为保护气体进行机械合金化。氩气流量为80ml/min,球磨机首先在100rpm的低转速下对金属粉末进行分散混合,时间为0.5h,然后提高转速至300rpm对金属粉末进行快速塑性变形、合金化,时间为23h。
(3)通过加料装置加入0.3Kg气相SiO2(D≤20nm)对上述合金化粉末进行包覆,时间为5h,完成后停机、使合金化粉末冷却至室温。
(4)将上述经过机械合金化及包覆完成后的合金化粉末进行球料分离,然后使用旋风分级分离设备,在氮气保护气体下进行粒度分级,氮气进气工作压力为0.6MPa。
制备获得的Fe-Ni-SiO2多元结构宽带片状吸收剂SEM形貌图和TEM形貌图如图示1、2。
实施例2
(1)将2.1Kg的Fe粉(D50为5μm、分布1-20μm)、0.3KgNi粉(D50为3μm、分布1-5μm)和90Kg的氧化锆(直径为8mm)加入转速和工作气氛可控的高能搅拌球磨机中,然后加入10g硬脂酸。
(2)将上述加料后的球磨机进行抽真空,并冲入氩气作为保护气体进行干法球磨,氩气流量为80ml/min,球磨机首先在100rpm的低转速下对金属粉末进行分散混合,时间为0.5h,然后提高转速至300rpm对金属粉末进行快速塑性变形、合金化,时间为23h。
(3)通过加料装置加入0.3Kg气相SiO2(D≤20nm)对上述合金化粉末进行包覆,时间为5h,完成后停机、使合金化粉末冷却至室温。
(4)将上述经过机械合金化及包覆完成后的合金化粉末进行球料分离,然后使用旋风分级分离设备,在氮气保护气体下进行粒度分级,氮气进气工作压力为0.6MPa。

Claims (1)

1.一种多元结构宽带片状吸收剂的制备方法,其步骤如下:
步骤1:将磨球和Fe粉、Ni粉按照比例投入到转速和工作气氛可控的高能搅拌球磨机中,并加入过程控制剂;将所述的球磨机抽真空后冲入氩气,在氩气保护下先进行低速分散混合,后提高转速进行金属粉末快速塑性变形、合金化;然后加入气相SiO2对上述合金化粉末进行包覆,完成后停机、冷却;磨球选用直径5~12mm的氧化锆,选用D50为5μm、分布1-20μm的Fe粉,选用D50为3μm、分布1-5μm的Ni粉,选用D≤20nm的气相SiO2,选用的过程控制剂为硬脂酸;其中Fe粉、Ni粉和气相SiO2的质量比为50~70:10~20:10~15,球料比为10~50;低速分散的时间为0.5~2h,球磨机转速为50~150rpm,高速分散的时间为10~30h,球磨机转速为160~300rpm,氩气流量为50~100ml/min;
步骤2:将上述经过机械合金化及包覆完成后的合金化粉末进行球料分离,然后使用旋风分级分离设备,在氮气保护气体下进行粒度分级,得到平均长度为10~15μm,厚度小于等于0.3μm的Fe-Ni-SiO2多元结构宽带片状吸收剂,其中,氮气进气工作压力为0.5~0.8MPa。
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