CN106086828B - 一种ZnOw晶须表面复合层的制备方法 - Google Patents
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 27
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- 239000002105 nanoparticle Substances 0.000 claims abstract description 19
- 238000005234 chemical deposition Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000011777 magnesium Substances 0.000 claims description 23
- 239000008367 deionised water Substances 0.000 claims description 22
- 229910021641 deionized water Inorganic materials 0.000 claims description 22
- MCDLETWIOVSGJT-UHFFFAOYSA-N acetic acid;iron Chemical compound [Fe].CC(O)=O.CC(O)=O MCDLETWIOVSGJT-UHFFFAOYSA-N 0.000 claims description 18
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- XNSQZBOCSSMHSZ-UHFFFAOYSA-K azane;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxymethyl)amino]acetate;iron(3+) Chemical compound [NH4+].[Fe+3].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O XNSQZBOCSSMHSZ-UHFFFAOYSA-K 0.000 claims description 6
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- 238000001035 drying Methods 0.000 claims description 6
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- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 6
- 229940071125 manganese acetate Drugs 0.000 claims description 6
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 6
- 239000012286 potassium permanganate Substances 0.000 claims description 6
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 6
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- 235000010265 sodium sulphite Nutrition 0.000 claims description 5
- 238000002242 deionisation method Methods 0.000 claims description 4
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- PQUCIEFHOVEZAU-UHFFFAOYSA-N Diammonium sulfite Chemical compound [NH4+].[NH4+].[O-]S([O-])=O PQUCIEFHOVEZAU-UHFFFAOYSA-N 0.000 claims description 3
- QDMGKUOANLJICG-UHFFFAOYSA-N [Mg].[N+](=O)(O)[O-] Chemical compound [Mg].[N+](=O)(O)[O-] QDMGKUOANLJICG-UHFFFAOYSA-N 0.000 claims description 3
- VJGJZVCKMKGZKS-UHFFFAOYSA-N iron;oxalic acid;hydrate Chemical compound O.[Fe].OC(=O)C(O)=O VJGJZVCKMKGZKS-UHFFFAOYSA-N 0.000 claims description 3
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- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims 2
- 239000012295 chemical reaction liquid Substances 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
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- 229910052938 sodium sulfate Inorganic materials 0.000 claims 1
- 235000011152 sodium sulphate Nutrition 0.000 claims 1
- 239000011358 absorbing material Substances 0.000 abstract description 8
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- 238000005516 engineering process Methods 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
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- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
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Abstract
本发明涉及一种ZnOw晶须表面复合层的制备方法，通过在金属镍纳米颗粒表面沉积MnxMgyZn1‑x‑yFe2O4铁氧体，从而形成核壳结构纳米颗粒；然后在四针ZnOw晶须表面实现金属铁的局域化学沉积的基础上进行核壳结构纳米颗粒的复合共沉积，从而在四针ZnOw晶须表面制备了铁及镍核@MnxMgyZn1‑x‑yFe2O4铁氧体壳结构复合层，其充分发挥了四针ZnOw晶须在用作吸波材料时具有较大介电损耗的特点，并结合了尖晶石型MnxMgyZn1‑x‑yFe2O4铁氧体具有的宽频带和兼容性好的吸波特性以及镍纳米颗粒优良的磁滞和涡流损耗的优点。
Description
技术领域
本发明涉及吸波材料技术领域，特别是一种ZnOw晶须表面复合层的制备方法。
背景技术
随着科学技术的发展，广播电视、通讯及电力产生的电磁福射污染越来越严重；此外，在军事领域，武器装备的隐身技术要求也越来越高，因而，研发一种高性能的吸波材料具有重要意义。四针ZnOw晶须作为一种极性单体具有独特的吸波特性，其具有四角针状结构，在吸波过程中具有较大的介电损耗，且四针ZnOw晶须有压电效应，能将入射电磁波能量转化为电能或其它能量从而达到使电磁波耗散消失的目的。但是，现有技术中制备的四针ZnOw晶须的低频吸波特性能差，不能有效满足低频波段吸波性能。
发明内容
为了克服现有技术的不足，本发明提供了一种ZnOw晶须表面复合层的制备方法，该制备方法包括镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构纳米颗粒的制备以及四针ZnOw晶须表面铁及镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构复合层的制备，本发明制备方法使得镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构纳米颗粒弥散分布于四针ZnOw晶须表面的金属铁层，充分发挥了四针ZnOw晶须在用作吸波材料时具有较大介电损耗的特点，并集合了尖晶石型MnxMgyZn1-x-yFe2O4铁氧体具有的宽频带和兼容性好的吸波特性以及镍纳米颗粒优良的磁滞和涡流损耗的优点。
本发明解决其技术问题所采用的技术方案是：一种ZnOw晶须表面复合层的制备方法，由以下制备步骤组成：
步骤一：镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构纳米颗粒的制备；
步骤二：四针ZnOw晶须表面局域铁的化学沉积；
步骤三：四针ZnOw晶须表面铁与镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构纳米颗粒的复合共沉积。
优选的，所述步骤一具体为：
①配制反应液：将浓度为分析纯的乙酸锰、硝酸镁和乙酸亚铁加入去离子水中，形成乙酸锰浓度为50-280g/L、硝酸镁浓度为80-320g/L和乙酸亚铁浓度为35-410g/L的混合液，随后向混合液中依次加入60％的磷酸、分析纯的磷酸氢二钠和高锰酸钾，形成60％的磷酸浓度为60-90mL/L、磷酸氢二钠浓度为15-40g/L和高锰酸钾浓度为60-160g/L的反应液。
②制备镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构纳米颗粒：将镍纳米颗粒加入去离子水，使其重量百分比为10％-40％，在室温下以超声波分散1-1.5小时形成稳定的镍纳米颗粒去离子水分散体系；将50-120mL前述配制的反应液与1L镍纳米颗粒去离子水分散体系充分混合，反应1-1.5小时后过滤烘干，所得到的颗粒粉体即为镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构纳米颗粒。
优选的，所述步骤二具体为：
①配备化学沉积液：将浓度为分析纯的乙酸亚铁、三乙酰丙酮铁、三水合草酸铁铵和亚硫酸钠加入去离子水中形成乙酸亚铁、三乙酰丙酮铁、三水合草酸铁铵和亚硫酸钠的浓度分别为35-80g/L、90-270g/L、5-30g/L、20-50g/L的化学沉积液。
②四针ZnOw晶须表面局域铁的化学沉积：将四针ZnOw晶须加入去离子水，使其重量的百分比为30-60％，在室温下以超声波分散0.5-1小时形成稳定的四针ZnOw晶须去离子水分散体系A；取该分散体系300-500mL加入500mL所述化学沉积液中并充分混合，反应10-30分钟后即实现四针ZnOw晶须表面金属铁的局域沉积。
优选的，所述步骤三具体为：
①配制沉积基础液：将浓度为分析纯的硝酸铁、乙酸亚铁、乙二胺四乙酸铁铵、硫酸氢钠和硅酸钠加入去离子水中形成硝酸铁、乙酸亚铁、乙二胺四乙酸铁铵、硫酸氢钠和硅酸钠的浓度分别为130-280g/L、90-320g/L、5-20g/L、10-45mL/L和160-310g/L的沉积基础液。
②四针ZnOw晶须表面的复合共沉积：将表面已局域沉积金属的四针ZnOw晶须加入去离子水，使其重量百分比为50％-80％，在室温下以超声波分散10-20分钟形成稳定的四针ZnOw晶须去离子水分散体系B；取该分散体系500mL与500mL沉积基础液充分混合，共沉积0.5-2小时后过过滤烘干，即在四针ZnOw晶须表面形成铁及镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构复合层。
本发明的积极效果：根据本发明方法制备的四针ZnOw晶须表面铁及镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构复合层，一方面充分发挥了四针ZnOw晶须的复介电常数虚部在一定范围内具有较大数值，在用作吸波材料时具有较大介电损耗的特点，另一方面结合了尖晶石型MnxMgyZn1-x-yFe2O4铁氧体具有的宽频带和兼容性好的吸波特性以及镍纳米颗粒优良的磁滞和涡流损耗的优点，因而制备的四针ZnOw晶须表面铁及镍核@MnxMgyZn1-x- yFe2O4铁氧体壳结构复合层是具有优良宽频带和高吸收率的吸波材料。
附图说明
图1是本发明所述复合层制备方法的流程示意图；
图2是本发明所述复合层的结构示意图。
具体实施方式
下面结合附图对本发明的优选实施例进行详细说明。
参照图1至图2，本发明优选实施例提供一种ZnOw晶须表面复合层的制备方法，由以下制备步骤组成：
步骤一：镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构纳米颗粒的制备；
步骤二：四针ZnOw晶须表面局域铁的化学沉积；
步骤三：四针ZnOw晶须表面铁与镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构纳米颗粒的复合共沉积。
所述步骤一具体为：
①配制反应液：将浓度为分析纯的乙酸锰、硝酸镁和乙酸亚铁加入去离子水中，形成乙酸锰浓度为70g/L、硝酸镁浓度为220g/L和乙酸亚铁浓度为60g/L的混合液，随后向混合液中依次加入60％的磷酸、分析纯的磷酸氢二钠和高锰酸钾，形成60％的磷酸浓度为80mL/L、磷酸氢二钠浓度为40g/L和高锰酸钾浓度为110g/L的反应液。
②制备镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构纳米颗粒：将镍纳米颗粒加入去离子水，使其重量百分比为30％，在室温下以超声波分散1小时形成稳定的镍纳米颗粒去离子水分散体系；将80mL前述配制的反应液与1L镍纳米颗粒去离子水分散体系充分混合，反应1.5小时后过滤烘干，所得到的颗粒粉体即为镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构纳米颗粒。
所述步骤二具体为：
①配备化学沉积液：将浓度为分析纯的乙酸亚铁、三乙酰丙酮铁、三水合草酸铁铵和亚硫酸钠加入去离子水中形成乙酸亚铁、三乙酰丙酮铁、三水合草酸铁铵和亚硫酸钠的浓度分别为60g/L、130g/L、20g/L、40g/L的化学沉积液。
②四针ZnOw晶须表面局域铁的化学沉积：将四针ZnOw晶须加入去离子水，使其重量的百分比为40％，在室温下以超声波分散1小时形成稳定的四针ZnOw晶须去离子水分散体系A；取该分散体系400mL加入500mL所述化学沉积液中并充分混合，反应20分钟后即实现四针ZnOw晶须表面金属铁的局域沉积。
所述步骤三具体为：
①配制沉积基础液：将浓度为分析纯的硝酸铁、乙酸亚铁、乙二胺四乙酸铁铵、硫酸氢钠和硅酸钠加入去离子水中形成硝酸铁、乙酸亚铁、乙二胺四乙酸铁铵、硫酸氢钠和硅酸钠的浓度分别为150g/L、240g/L、5g/L、25mL/L和170g/L的沉积基础液。
②四针ZnOw晶须表面的复合共沉积：将表面已局域沉积金属的四针ZnOw晶须加入去离子水，使其重量百分比为70％，在室温下以超声波分散15分钟形成稳定的四针ZnOw晶须去离子水分散体系B；取该分散体系500mL与500mL沉积基础液充分混合，共沉积1.5小时后过过滤烘干，即在四针ZnOw晶须表面形成铁及镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构复合层。
将相同质量本实施例制备的ZnOw晶须表面铁及镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构复合层吸波材料与相同质量的普通四针ZnOw晶须加入涂料，加入普通四针ZnOw涂料的吸波带宽实验结果为10-18GHz，而加入本实施例制备的ZnOw晶须表面铁及镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构复合层吸波材料涂料的吸波带宽实验结果为3-18GHz。显然，依据本发明制备的ZnOw晶须表面铁及镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构复合层吸波材料结合了尖晶石型MnxMgyZn1-x-yFe2O4铁氧体具有的宽频带和兼容性好的吸波特性以及镍纳米颗粒优良的磁滞和涡流损耗的优点，具有优良宽频带和高吸收率的吸波性能。
以上所述的仅为本发明的优选实施例，所应理解的是，以上实施例的说明只是用于帮助理解本发明的方法及其核心思想，并不用于限定本发明的保护范围，凡在本发明的思想和原则之内所做的任何修改、等同替换等等，均应包含在本发明的保护范围之内。
Claims (4)
1.一种ZnOw晶须表面复合层的制备方法，其特征在于，由以下制备步骤组成：
步骤一：镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构纳米颗粒的制备；
步骤二：四针ZnOw晶须表面局域铁的化学沉积；
步骤三：四针ZnOw晶须表面铁与镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构纳米颗粒的复合共沉积；
所述步骤一具体为：
①配制反应液：将浓度为分析纯的乙酸锰、硝酸镁和乙酸亚铁加入去离子水中，形成混合液，随后向混合液中依次加入60％的磷酸、分析纯的磷酸氢二钠和高锰酸钾，形成反应液；
②制备镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构纳米颗粒：将镍纳米颗粒加入去离子水，使其重量百分比为10％-40％，在室温下以超声波分散1-1.5小时形成稳定的镍纳米颗粒去离子水分散体系；将50-120mL前述配制的反应液与1L镍纳米颗粒去离子水分散体系充分混合，反应1-1.5小时后过滤烘干，所得到的颗粒粉体即为镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构纳米颗粒；
所述步骤二具体为：
①配备化学沉积液：将浓度为分析纯的乙酸亚铁、三乙酰丙酮铁、三水合草酸铁铵和亚硫酸钠加入去离子水中形成化学沉积液；
②四针ZnOw晶须表面局域铁的化学沉积：将四针ZnOw晶须加入去离子水，使其重量的百分比为30-60％，在室温下以超声波分散0.5-1小时形成稳定的四针ZnOw晶须去离子水分散体系A；取该分散体系300-500mL加入500mL所述化学沉积液中并充分混合，反应10-30分钟后即实现四针ZnOw晶须表面金属铁的局域沉积；
所述步骤三具体为：
①配制沉积基础液：将浓度为分析纯的硝酸铁、乙酸亚铁、乙二胺四乙酸铁铵、硫酸氢钠和硅酸钠加入去离子水中形成沉积基础液；
②四针ZnOw晶须表面的复合共沉积：将表面已局域沉积金属的四针ZnOw晶须加入去离子水，使其重量百分比为50％-80％，在室温下以超声波分散10-20分钟形成稳定的四针ZnOw晶须去离子水分散体系B；取该分散体系500mL与500mL沉积基础液充分混合，共沉积0.5-2小时后过滤烘干，即在四针ZnOw晶须表面形成铁及镍核@MnxMgyZn1-x-yFe2O4铁氧体壳结构复合层。
2.根据权利要求1所述的一种ZnOw晶须表面复合层的制备方法，其特征在于：所述混合液中乙酸锰浓度为50-280g/L，硝酸镁浓度为80-320g/L，乙酸亚铁浓度为35-410g/L，所述反应液中60％的磷酸浓度为60-90mL/L，磷酸氢二钠浓度为15-40g/L，高锰酸钾浓度为60-160g/L。
3.根据权利要求1所述的一种ZnOw晶须表面复合层的制备方法，其特征在于：所述化学沉积液中乙酸亚铁、三乙酰丙酮铁、三水合草酸铁铵和亚硫酸钠的浓度分别为35-80g/L、90-270g/L、5-30g/L、20-50g/L。
4.根据权利要求1所述的一种ZnOw晶须表面复合层的制备方法，其特征在于：所述沉积基础液中硝酸铁、乙酸亚铁、乙二胺四乙酸铁铵、硫酸氢钠和硅酸钠的浓度分别为130-280g/L、90-320g/L、5-20g/L、10-45mL/L和160-310g/L。
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