Fe（Ni）-N纳米粒子的制备及电磁性能
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摘要
本文以直流电弧等离子法制备的Fe和Fe1-xNix(x=0.43,0.65)纳米粒子为前躯体,在氨气气氛中,在不同的反应温度,通过固-气反应合成了FexN(x=4,3)纳米粒子,γ'Fe2.6Ni1.4N纳米粒子和γ'-Fe1.7Ni2.3N包覆γ-Fe1.7Ni2.3纳米复合粒子。利用X射线衍射仪(XRD)、透射电子显微镜(TEM)、X射线能谱仪(EDS)和振动样品强度计(VSM)对氮化产物的相结构、成分、微观形貌和磁性能进行表征。利用网络分析仪测试了2-18GHz范围内的电磁参数。
Fe纳米粒子的氮化结果表明：由于Fe纳米粒子存在大量的缺陷,促使Fe的氮化反应在低温进行；随着反应温度的升高,氮化产物从γ'-Fe4N相向ε-Fe3N相转变,产物颗粒出现轻微的烧结。氮化产物的微观结构和本征介电性能引起的多重极化使得纳米粒子的复介电常数显著的提高,并且表现出明显的多重介电弛豫峰。而复磁导率具有相似的变化规律,实部随频率增加而减小,在高频趋于稳定；虚部出现宽的自然共振峰,但其自然共振频率低于Fe纳米颗粒。微波吸收模拟结果显示,Fe4N/Fe和Fe3N/Fe4N纳米粒子分别在3.6-11.2GHz和4.6-13.6GHz范围内反射损耗值小于-10dB,对应的匹配厚度分别为1-2.99mm和0.83-2.49mm。在4.6-7.6GHz和7.0-9.2GHz范围内反射损耗值小于-20dB。
研究了FeNi合金纳米粒子中Ni含量对其氮化产物的相结构和电磁性能的影响。实验发现Fe1-xNix(x=0.43,0.65)的氮化产物分别为单相的γ'-Fe2.6Ni1.4N纳米粒子和γ'Fe1.7Ni2.3N包覆y-Fel.7Ni2.3纳米复合粒子,颗粒呈球形链状结构,保持了前躯体颗粒纳米形态,大小为10-100nm。FeNi合金的氮化产物的电磁性能表现出与Fe-N纳米粒子相近似的变化规律,γ'-Fe1.7Ni2.3N包覆γ-Fe1.7Ni2.3纳米复合粒子由于高的电导率和磁学性能导致其复介电常数和复磁导率大于γ'-Fe2.6Nil.4N纳米粒子。与Fe-N纳米粒子相比,镍的掺杂导致其自然共振频率向低频移动。γ'-Fe2.6Ni1.4N纳米粒子在2.6-18GHz范围内反射损耗值小于-10dB,对应的匹配厚度为0.74-4.4mm；在5.2GHz处出现最小的反射损耗值-39.9dB。不同含量的γ'-Fel.7Ni2.3N包覆γ-Fel.7Ni2.3纳米复合粒子分别在2-6.4GHz和3.6-7.8GHz范围内反射损耗值小于-10dB,最小的反射损耗值为-53.5dB和-35.4dB。可以通过前躯体的成分和氮化反应温度来控制反应产物,进而调节电磁参数来改变微波吸收频带,满足特定频带范围内的电磁波吸收要求。
The FexN(x=4,3) nanoparticles, Fe2.6Ni1.4N nanoparticles and Fe1.7Ni2.3N coated Fe1.7Ni2.3 nanocomposites are synthesised by solid-gas reaction in ammonia atmosphere at the different temperatures, using the Fe and Fe1-xNix(x=0.43,0.65) by DC arc-discharge plasma as a precursor. The phase struction, composition, morphology and magnetic properties are investigated by the X-ray diffraction (XRD), tansmission electron microscopy (TEM), energy dispersive spectroscopy (EDS) and vibrating sample magnetometer (VSM), respectively.The electromagnetic parameters also were studied in the 2-18GHz frequency range by vetor network analazer.
The results of nitridation of iron show nitridation reaction were processed at lower temperature duo to a large number of defects. The resultance products changed fromγ'-Fe4N structure toε-Fe3N phase with increasing temperature. The slightly sintering phenomenon can be found but the grain sizes still retain in the nanoscale ranges. The complex permittivity show notabilily enhancement valves and exhibit the muitiple dielectric relaxation resonance in 10-18GHz range, which attribute to the muitiple polarization affected by microstructure and intrinsic dielectronic. The permeability exhibit the similar varation trendency and the real part of permeability slightly decreased in the lower frequency and then retained a approximately constant. The abroad nature resonance peaks appear in the nitride products and the nature resonance frequency of products nanoparticles were lower than that of Fe nanopaiticles duo to smaller magnetocrystalline anisotropy. It is calculated that the nitride products exhibit the excellent the microwave absortion properties. For Fe4N/Fe and Fe3N/Fe4N nanoparticles, the reflection loss exceeding-10dB was observed in the 3.6-11.2GHz and 4.6-13.6GHz range for the thickness of 1-2.99mm and 0.83-2.49mm. The reflection loss was less than-20dB in the 4.6-7.6GHz and 7.0-9.2GHz, respectively.
The influence of Ni components on the phase and electromagnetic characteristics were investigated. It is found that nitride products are singleγ'-Fe2.6Ni1.4N nanoprticles andγ'-Fe1.7Ni2.3N coatedγ-Fe1.7Ni2.3 nanocomposites for Fe1-xNix(x=0.43,0.65), respectively. The products nanoparticles are spherial in shape like chain with its size ranges of 10-100nm and retain the morphology of the precuesor. The electromagnetic properties exhibit the similar variation trendency. The nanocomposites possess the higher the complex permittivity and the complex permeability than that the single nanoparticles duo to higher conductivity and magnetic properties. Comparaed to the Fe-N nanoparticles, the substituent of the Ni atoms resulted in the lower nature resonance frequency, which attribute to the lower magnetocrystalline anisotropy. For the singleγ'-Fe2.6Ni1.4N nanoprticles, the reflection loss less than -10 dB was obtained over the 2.6-18GHz with the thickness of 0.74-4.4 mm. An optical reflection loss of -39.9dB was observed at the 5.2GHz. The reflection loss exceeds-1OdB in the 2-6.4GHz and 3.6-7.8GHz and the minimum reflection loss was -53.5dB and-34.9dB for the nanocomposites with different y'-Fe1.7Ni2.3N components, respectively. Therefore, eleteromagnetic parameter adjusted by the precursor componenes and reaction temperature can tuned the frequency band of microwave absorption in order to meet the demands of electomagnetic absorption in the certain frequency range.
Fe纳米粒子的氮化结果表明：由于Fe纳米粒子存在大量的缺陷,促使Fe的氮化反应在低温进行；随着反应温度的升高,氮化产物从γ'-Fe4N相向ε-Fe3N相转变,产物颗粒出现轻微的烧结。氮化产物的微观结构和本征介电性能引起的多重极化使得纳米粒子的复介电常数显著的提高,并且表现出明显的多重介电弛豫峰。而复磁导率具有相似的变化规律,实部随频率增加而减小,在高频趋于稳定；虚部出现宽的自然共振峰,但其自然共振频率低于Fe纳米颗粒。微波吸收模拟结果显示,Fe4N/Fe和Fe3N/Fe4N纳米粒子分别在3.6-11.2GHz和4.6-13.6GHz范围内反射损耗值小于-10dB,对应的匹配厚度分别为1-2.99mm和0.83-2.49mm。在4.6-7.6GHz和7.0-9.2GHz范围内反射损耗值小于-20dB。
研究了FeNi合金纳米粒子中Ni含量对其氮化产物的相结构和电磁性能的影响。实验发现Fe1-xNix(x=0.43,0.65)的氮化产物分别为单相的γ'-Fe2.6Ni1.4N纳米粒子和γ'Fe1.7Ni2.3N包覆y-Fel.7Ni2.3纳米复合粒子,颗粒呈球形链状结构,保持了前躯体颗粒纳米形态,大小为10-100nm。FeNi合金的氮化产物的电磁性能表现出与Fe-N纳米粒子相近似的变化规律,γ'-Fe1.7Ni2.3N包覆γ-Fe1.7Ni2.3纳米复合粒子由于高的电导率和磁学性能导致其复介电常数和复磁导率大于γ'-Fe2.6Nil.4N纳米粒子。与Fe-N纳米粒子相比,镍的掺杂导致其自然共振频率向低频移动。γ'-Fe2.6Ni1.4N纳米粒子在2.6-18GHz范围内反射损耗值小于-10dB,对应的匹配厚度为0.74-4.4mm；在5.2GHz处出现最小的反射损耗值-39.9dB。不同含量的γ'-Fel.7Ni2.3N包覆γ-Fel.7Ni2.3纳米复合粒子分别在2-6.4GHz和3.6-7.8GHz范围内反射损耗值小于-10dB,最小的反射损耗值为-53.5dB和-35.4dB。可以通过前躯体的成分和氮化反应温度来控制反应产物,进而调节电磁参数来改变微波吸收频带,满足特定频带范围内的电磁波吸收要求。
The FexN(x=4,3) nanoparticles, Fe2.6Ni1.4N nanoparticles and Fe1.7Ni2.3N coated Fe1.7Ni2.3 nanocomposites are synthesised by solid-gas reaction in ammonia atmosphere at the different temperatures, using the Fe and Fe1-xNix(x=0.43,0.65) by DC arc-discharge plasma as a precursor. The phase struction, composition, morphology and magnetic properties are investigated by the X-ray diffraction (XRD), tansmission electron microscopy (TEM), energy dispersive spectroscopy (EDS) and vibrating sample magnetometer (VSM), respectively.The electromagnetic parameters also were studied in the 2-18GHz frequency range by vetor network analazer.
The results of nitridation of iron show nitridation reaction were processed at lower temperature duo to a large number of defects. The resultance products changed fromγ'-Fe4N structure toε-Fe3N phase with increasing temperature. The slightly sintering phenomenon can be found but the grain sizes still retain in the nanoscale ranges. The complex permittivity show notabilily enhancement valves and exhibit the muitiple dielectric relaxation resonance in 10-18GHz range, which attribute to the muitiple polarization affected by microstructure and intrinsic dielectronic. The permeability exhibit the similar varation trendency and the real part of permeability slightly decreased in the lower frequency and then retained a approximately constant. The abroad nature resonance peaks appear in the nitride products and the nature resonance frequency of products nanoparticles were lower than that of Fe nanopaiticles duo to smaller magnetocrystalline anisotropy. It is calculated that the nitride products exhibit the excellent the microwave absortion properties. For Fe4N/Fe and Fe3N/Fe4N nanoparticles, the reflection loss exceeding-10dB was observed in the 3.6-11.2GHz and 4.6-13.6GHz range for the thickness of 1-2.99mm and 0.83-2.49mm. The reflection loss was less than-20dB in the 4.6-7.6GHz and 7.0-9.2GHz, respectively.
The influence of Ni components on the phase and electromagnetic characteristics were investigated. It is found that nitride products are singleγ'-Fe2.6Ni1.4N nanoprticles andγ'-Fe1.7Ni2.3N coatedγ-Fe1.7Ni2.3 nanocomposites for Fe1-xNix(x=0.43,0.65), respectively. The products nanoparticles are spherial in shape like chain with its size ranges of 10-100nm and retain the morphology of the precuesor. The electromagnetic properties exhibit the similar variation trendency. The nanocomposites possess the higher the complex permittivity and the complex permeability than that the single nanoparticles duo to higher conductivity and magnetic properties. Comparaed to the Fe-N nanoparticles, the substituent of the Ni atoms resulted in the lower nature resonance frequency, which attribute to the lower magnetocrystalline anisotropy. For the singleγ'-Fe2.6Ni1.4N nanoprticles, the reflection loss less than -10 dB was obtained over the 2.6-18GHz with the thickness of 0.74-4.4 mm. An optical reflection loss of -39.9dB was observed at the 5.2GHz. The reflection loss exceeds-1OdB in the 2-6.4GHz and 3.6-7.8GHz and the minimum reflection loss was -53.5dB and-34.9dB for the nanocomposites with different y'-Fe1.7Ni2.3N components, respectively. Therefore, eleteromagnetic parameter adjusted by the precursor componenes and reaction temperature can tuned the frequency band of microwave absorption in order to meet the demands of electomagnetic absorption in the certain frequency range.
引文
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