镍/铁基电磁波屏蔽涂料的研究
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摘要
随着电子信息技术的发展，电磁干扰影响人们的健康和隐身及保密工作，因此电磁波屏蔽已成为研究的热点。在各类电磁屏蔽方法中，以镍、铁为金属填料的电磁屏蔽涂料因其成本低、工艺简便、适用性强、无需特殊设备等优点，在电磁屏蔽材料中最受青睐。但是常规铁粉容易被氧化，制备而成的电磁屏蔽涂料效果差；而用镍粉不容易被氧化，由微米镍粉制备而成的涂料导电性能虽然较好，但可屏蔽的电磁波频率比较窄。针对上述问题，论文作了三方面的工作：(1)选用化学镀在铁粉上面进行镍包覆，解决常规铁粉的氧化问题。(2)在微米镍粉里面加入纳米镍粉形成复合粉末，提高涂料的导电和屏蔽性能，展宽屏蔽电磁波的频率。(3)用纳米／微米混合镍粉制备电磁波屏蔽涂料，优化工艺，探讨各组分对电磁波屏蔽涂层屏蔽性能的影响机理。并采用先进的测试分析手段研究了屏蔽涂料在300KHz～1.5GHz电磁波频段范围的电磁波屏蔽性能。
为了解决铁粉作为涂料中金属填料易氧化的缺点，提高铁粉的电磁屏蔽效能，我们研究了一种优化铁粉性能，提高抗氧化能力以及吸波性能的化学镀制备镍包覆铁的方法。该法是利用镍的耐氧化和镍／铁双金属吸波效果，通过还原反应，在铁粉表面包覆一层镍保护层。试验选取了5个主要参数，并以此设计了L_(25)(5~5)型正交试验。获得的优化工艺参数为pH值：12，硫酸镍初始质量浓度：2.5g／100mL，联胺初始体积浓度：8ml／100mL，镀覆温度：75℃，铁粉加载量：1.5g／100mL。采用SEM、XRD对选用上述参数制取的镍包铁粉进行了分析测试。结果表明，复合粉末表面较原始粉末粗糙，颗粒明显长大，包覆层未引入杂质元素，包覆效果较好。实验验证，用镍包铁粉比用纯铁粉制备成的涂料的导电性能好。
为提高镍、铁电磁屏蔽涂料的性能，论文分析了各组分的作用，影响电磁波屏蔽涂料导电性能的关键因素在于粒子之间的接触数目和粒子间接近的程度，即所形成导电网络的完整性和密实程度。各种影响因素包括丙烯酸树脂、导电填料、钛酸酯偶联剂、硅烷偶联剂和有机膨润土等对涂料的导电性能和电磁屏蔽性能的影响。丙烯酸树脂使得涂料具有粘贴力，能附着在基板上，是填料和偶联剂、分散剂共存的基础；偶联剂使得无机填料和成膜树脂相互融合，改善填料的抗氧化性；有机膨润土提高了填料在涂料中的分散性。
用微米镍粉和纳米镍粉的混合粉末制备成的电磁屏蔽涂料的导电性能比用纯微米镍粉制备成的涂料的导电性能更好，并且展宽屏蔽电磁波的频率。
电磁波屏蔽性能的测定结果表明，用微米镍粉和混合粉末所制成涂料的电磁波屏蔽率在300kHz～1.5GHz可达95％～99％，用镍包覆铁制成涂料的电磁波屏蔽率在低频时达到99％，屏蔽效果较好。
With the rapid development of the electronic industry, electromagnetic interference (EMI) is becoming an increasing problem that affects people's health and work.So the electromagnetic interference shielding is increasingly required.Among all the shielding methods, the electromagnetic safety conductive paints have a bright future in this realm because of its low cost, simple process, good applicability, and without special equipments etc. Studies on the development of the EMI shielding coating is particularly important. The normal iron particle is easily oxidized, so the electromagnetic shielding effectivenesss is bad, while the electric conductivity of coating based on the micron nickel particles is better because these particles are not easy to be oxidized, However, the frequency of electromagnetic wave is narrow. Aiming at the above-mentioned problems,The present thesis designed experiments as follows:(1)nickel was coated on iron by the electroless plating in order to improve the oxidization of iron powder;(2) To improve the effect of the electromagnetic shielding and the electric conductivity, nanometer nickel powder combined micron nickel powder was used ,which was able to widen the frequency range of electromagnetic shielding wave;(3)The Ni / acrylic resin electromagnetic shielding coating was prepared, and the effect of every component on properties was also investigated.The electromagnetic shielding effectivenesss of the above composites have been studied systematically at the frequency range from 300KHz to 1.5GHz.
Due to its poor function as the metals filler in the coating,the iron powder was modified using the electroless plating which prepared nickel coating around iron powder by means of oxidization resistance of nickel and the ability of absorbing electromagnetic wave.Five major parameters were selected for experimental investigation of powder preparation: initial concentration of nickelion, initial concentration of hydrazine, its pH value, plating temperature, and added amount of Iron powder, and an orthogonal array test L_(25)(5~5)was designed accordingly. A great number of experiments were performed to get optimal technological parameters as follows: Initial concentration of nickel sulfate was 2.5 g/100mL, initial concentration of hydrazine 8ml/100mL, pH value 12, plating temperature 75℃,added amount of Iron powder 1.5 g/100mL. SEM and XRD were used to analyze the power for nickel plating aroundiron. The results showed that the surface of coating around such powder was rougher than that of original powder and the particles of the powder grew greatly. There was also no inclusion inside the coating layer .It suggested that the plating effect was preferable. The experiment prove that the electric conductivity of the coating with the Ni/Fe was better than that with the pure iron powder.
In order to increse the electromagnetic shielding effectivenesss,the thesis analyzed the function of each component.The number of contacting particles and the distance among particles were the key factors, which decided the completeness and denseness of the framework.We studied systematically the influence of manifold factors,such as acrylic resin,the conductive filling and organobentonite, the aminosilane coupling agent and coupling agent of organic titanate.Acrylic resin is cohensive and helpful to combine because the conductive filling blended with resin through coupling agent ,the oxidation resistivity improved. Organobentonite can improve the dispersion of the coating.
The electromagnetic shielding coating based on the nanometer nickel powder combined the micron nickel powder, has raised the electromagnetic shielding effectivenesss and the electric conductivity, also has widened the frequency range of electromagnetic shielding wave.
The resultant coating based on nickel powder and combined powder showed that 95%～99%of the electromagnetic wave was shielding at the frequency range from 300KHz to 1.5GHz,while the coating based on Ni/Fe the shielding was 95% at the low frequency.
为了解决铁粉作为涂料中金属填料易氧化的缺点，提高铁粉的电磁屏蔽效能，我们研究了一种优化铁粉性能，提高抗氧化能力以及吸波性能的化学镀制备镍包覆铁的方法。该法是利用镍的耐氧化和镍／铁双金属吸波效果，通过还原反应，在铁粉表面包覆一层镍保护层。试验选取了5个主要参数，并以此设计了L_(25)(5~5)型正交试验。获得的优化工艺参数为pH值：12，硫酸镍初始质量浓度：2.5g／100mL，联胺初始体积浓度：8ml／100mL，镀覆温度：75℃，铁粉加载量：1.5g／100mL。采用SEM、XRD对选用上述参数制取的镍包铁粉进行了分析测试。结果表明，复合粉末表面较原始粉末粗糙，颗粒明显长大，包覆层未引入杂质元素，包覆效果较好。实验验证，用镍包铁粉比用纯铁粉制备成的涂料的导电性能好。
为提高镍、铁电磁屏蔽涂料的性能，论文分析了各组分的作用，影响电磁波屏蔽涂料导电性能的关键因素在于粒子之间的接触数目和粒子间接近的程度，即所形成导电网络的完整性和密实程度。各种影响因素包括丙烯酸树脂、导电填料、钛酸酯偶联剂、硅烷偶联剂和有机膨润土等对涂料的导电性能和电磁屏蔽性能的影响。丙烯酸树脂使得涂料具有粘贴力，能附着在基板上，是填料和偶联剂、分散剂共存的基础；偶联剂使得无机填料和成膜树脂相互融合，改善填料的抗氧化性；有机膨润土提高了填料在涂料中的分散性。
用微米镍粉和纳米镍粉的混合粉末制备成的电磁屏蔽涂料的导电性能比用纯微米镍粉制备成的涂料的导电性能更好，并且展宽屏蔽电磁波的频率。
电磁波屏蔽性能的测定结果表明，用微米镍粉和混合粉末所制成涂料的电磁波屏蔽率在300kHz～1.5GHz可达95％～99％，用镍包覆铁制成涂料的电磁波屏蔽率在低频时达到99％，屏蔽效果较好。
With the rapid development of the electronic industry, electromagnetic interference (EMI) is becoming an increasing problem that affects people's health and work.So the electromagnetic interference shielding is increasingly required.Among all the shielding methods, the electromagnetic safety conductive paints have a bright future in this realm because of its low cost, simple process, good applicability, and without special equipments etc. Studies on the development of the EMI shielding coating is particularly important. The normal iron particle is easily oxidized, so the electromagnetic shielding effectivenesss is bad, while the electric conductivity of coating based on the micron nickel particles is better because these particles are not easy to be oxidized, However, the frequency of electromagnetic wave is narrow. Aiming at the above-mentioned problems,The present thesis designed experiments as follows:(1)nickel was coated on iron by the electroless plating in order to improve the oxidization of iron powder;(2) To improve the effect of the electromagnetic shielding and the electric conductivity, nanometer nickel powder combined micron nickel powder was used ,which was able to widen the frequency range of electromagnetic shielding wave;(3)The Ni / acrylic resin electromagnetic shielding coating was prepared, and the effect of every component on properties was also investigated.The electromagnetic shielding effectivenesss of the above composites have been studied systematically at the frequency range from 300KHz to 1.5GHz.
Due to its poor function as the metals filler in the coating,the iron powder was modified using the electroless plating which prepared nickel coating around iron powder by means of oxidization resistance of nickel and the ability of absorbing electromagnetic wave.Five major parameters were selected for experimental investigation of powder preparation: initial concentration of nickelion, initial concentration of hydrazine, its pH value, plating temperature, and added amount of Iron powder, and an orthogonal array test L_(25)(5~5)was designed accordingly. A great number of experiments were performed to get optimal technological parameters as follows: Initial concentration of nickel sulfate was 2.5 g/100mL, initial concentration of hydrazine 8ml/100mL, pH value 12, plating temperature 75℃,added amount of Iron powder 1.5 g/100mL. SEM and XRD were used to analyze the power for nickel plating aroundiron. The results showed that the surface of coating around such powder was rougher than that of original powder and the particles of the powder grew greatly. There was also no inclusion inside the coating layer .It suggested that the plating effect was preferable. The experiment prove that the electric conductivity of the coating with the Ni/Fe was better than that with the pure iron powder.
In order to increse the electromagnetic shielding effectivenesss,the thesis analyzed the function of each component.The number of contacting particles and the distance among particles were the key factors, which decided the completeness and denseness of the framework.We studied systematically the influence of manifold factors,such as acrylic resin,the conductive filling and organobentonite, the aminosilane coupling agent and coupling agent of organic titanate.Acrylic resin is cohensive and helpful to combine because the conductive filling blended with resin through coupling agent ,the oxidation resistivity improved. Organobentonite can improve the dispersion of the coating.
The electromagnetic shielding coating based on the nanometer nickel powder combined the micron nickel powder, has raised the electromagnetic shielding effectivenesss and the electric conductivity, also has widened the frequency range of electromagnetic shielding wave.
The resultant coating based on nickel powder and combined powder showed that 95%～99%of the electromagnetic wave was shielding at the frequency range from 300KHz to 1.5GHz,while the coating based on Ni/Fe the shielding was 95% at the low frequency.
引文
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