CN104774590B - 一种复合材料及其制备方法 - Google Patents

一种复合材料及其制备方法 Download PDF

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CN104774590B
CN104774590B CN201510197778.0A CN201510197778A CN104774590B CN 104774590 B CN104774590 B CN 104774590B CN 201510197778 A CN201510197778 A CN 201510197778A CN 104774590 B CN104774590 B CN 104774590B
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张伟
孔祥春
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BOE Technology Group Co Ltd
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Abstract

本发明公开了一种复合材料及其制备方法。该复合材料由TiO2和BaZn1.2Co0.8Fe16O27构成。本发明的复合材料具有吸收频段高、兼容性优良和频带宽的优点，有望应用在手机和电视外壳保护材料，吸收对人体伤害最大的电磁波段而又不影响正常手机等电子设备通讯功能。

Description

一种复合材料及其制备方法
技术领域
本发明涉及一种复合材料及其制备方法，尤其涉及W型钡铁氧体/TiO2复合材料及其制备方法。
背景技术
在日常生活中电磁波无处不在，无线电广播、电视、移动通讯、无线电遥控、导航、高压送配电线等均向周围辐射强大的电磁波能量。自电子工业问世以来，的确使科学技术和工业生产发生了革命性的变革，给人们生活带来了极大的便利，但各种电子产品辐射出的电磁波，有时会对环境造成污染，成为重要的环境污染要素之一，并有可能危及人体健康，从而成为继废气、废水、废渣和噪声之后的人类环境的又一大公害。其中3MHz～30MHz是军队使用的短波波段，跟公众关系不大，我们不必关心。而日常生活中由于手机、电视、高压电等设备的普及我们生活中电磁波频段为30MHz～30GHz范围内，其中频率越大，对人体伤害越大，目前对减小电子产品辐射(如手机、电视等)研究较少，高频辐射产品应用范围也受到一定限制，开发新型吸波材料显得十分必要。二氧化钛(TiO2)具有较高的介电常数，且稳定性好，是一种重要的介电材料，能够依靠介电损耗吸收电磁波。将TiO2与W型钡铁氧体进行复合，有望获得介电损耗能力和磁损耗能力均较好的复合吸波材料。
申请号为201110328815.9中国发明专利申请公开了一种氧化锌包覆钡铁氧体的复合吸波材料及其制备方法。所述的复合吸波材料由氧化锌包覆钡铁氧体颗粒构成，其制备方法如下：将硝酸铁、硝酸钡、柠檬酸按摩尔比配成溶液，调节溶液pH值，蒸干至凝胶之后加热进行自蔓燃反应，并进行焙烧，得到钡铁氧体颗粒；将醋酸锌溶于二甘醇并加入聚乙烯吡咯烷酮表面活性剂，配制成溶液1。将钡铁氧体粉末按铁锌摩尔比加入溶液1中，在一定温度下反应制得氧化锌包覆钡铁氧体粉末。
发明内容
本发明涉及一种复合材料，其分子式为(BaZn1.2Co0.8Fe16O27)/TiO2。在下文中，BaZn1.2Co0.8Fe16O27简写为BaW。本发明的复合材料具有高吸收、兼容性优良和频带宽的优点。
本发明的复合材料，由TiO2和BaZn1.2Co0.8Fe16O27构成，具体的是TiO2包覆BaZn1.2Co0.8Fe16O27颗粒构成。其中TiO2与BaZn1.2Co0.8Fe16O27的重量比为(0.1-10):(1-10)，优选(0.1-1):(5-10)；如在本发明的一个实施例中，二者的重量比为0.469:7.94。
其中，所述复合材料为微米级的复合材料。
所述复合材料在7.76-13.68GHz的反射损耗小于-10dB，并且在10.3GHz反射损耗达到-47.6dB。
本发明还提供了一种复合材料的制备方法，包括如下步骤：
将Ba(NO3)2、Zn(NO3)2·6H2O、Co(NO3)2·6H2O和Fe(NO3)3·9H2O按摩尔比为1:1.2:0.8:16溶解于蒸馏水中，向其中加入与Ba(NO3)2摩尔比为10:1的柠檬酸搅拌至完全溶解，并调节溶液的pH至中性；将上述溶液蒸发制得溶胶，干燥得到凝胶，然后焙烧，得到BaZn1.2Co0.8Fe16O27；
称取BaZn1.2Co0.8Fe16O27加入到TiO2溶胶中，搅拌、过滤；滤渣洗涤、干燥得到前驱体，将该前躯体干燥得到所述复合材料。其中，TiO2与BaZn1.2Co0.8Fe16O27的重量比为(0.1-10):(1-10)，优选(0.1-1):(5-10)；如在本发明的一个实施例中，二者的重量比为0.469:7.94。
其中，所述Ba(NO3)2、Zn(NO3)2·6H2O、Co(NO3)2·6H2O和Fe(NO3)3·9H2O为分析纯Ba(NO3)2、分析纯Zn(NO3)2·6H2O、分析纯Co(NO3)2·6H2O和分析纯Fe(NO3)3·9H2O。
其中，所述溶液蒸发的条件为70℃水浴中恒温蒸发。
其中，在于1300℃下焙烧之前，所述凝胶被研磨成粉体。
其中，所述滤渣用无水乙醇洗涤。
其中，经过无水乙醇洗涤的滤渣在80℃干燥。
其中，所述TiO2溶胶按照如下方法制备：将2重量份的钛酸丁酯和1重量份冰醋酸溶于10重量份无水乙醇中，搅拌得到透明溶液，将体积分数为75％的4重量份乙醇溶液缓慢滴入上述透明溶液中，搅拌，得到TiO2溶胶。
其中，所述焙烧在1300℃下进行。
本发明的复合材料可以用于制作手机等电子设备的外壳的材料，从而可以吸收对人体伤害最大的电磁波段而又不影响正常手机等电子设备通讯功能。
本发明的另一个目的是提供一种电子设备外壳，所述电子设备外壳由包括所述复合材料的原料制成。
其中，所述电子设备为手机。
本发明将TiO2与BaW材料进行复合，获得了介电损耗能力和磁损耗能力均较好的复合材料。本发明的复合材料具有吸收频段高、兼容性优良和频带宽的优点，可用于手机等电子设备的外壳的材料，从而可以吸收对人体伤害最大的电磁波段而又不影响正常手机等电子设备通讯功能。
附图说明
图1表示实施例1的BaW/TiO2复合材料、BaW、TiO2的XRD图。
图2表示实施例1的BaW/TiO2复合材料样品的SEM图。
图3实施例1的BaW/TiO2复合材料和BaW的反射损失曲线。
具体实施方式
本发明实施方式的复合材料，其分子式为(BaZn1.2Co0.8Fe16O27)/TiO2。该复合材料为微米级的复合材料，在7.76-13.68GHz的反射损耗小于-10dB，并且在10.3GHz反射损耗达到-47.6dB。
本发明实施方式的复合材料具有吸收频段高、兼容性优良和频带宽的优点，可用于手机等电子设备的外壳的材料，从而可以吸收对人体伤害最大的电磁波段而又不影响正常手机等电子设备通讯功能。
下面将结合附图和实施例，对本发明的具体实施方式作进一步详细描述。以下实施例用于说明本发明，但不用来限制本发明的范围。
实施例1
1.制备BaZn1.2Co0.8Fe16O27：
第一步：将2.61g Ba(NO3)2、2.97g Zn(NO3)2·6H2O、2.91g Co(NO3)2·6H2O和3.42gFe(NO3)3·9H2O溶解于50mL蒸馏水中，待其充分溶解后向其中加入19.5g的分析纯柠檬酸，充分搅拌使之完全溶解，再用乙二胺调节溶液的pH至中性。
第二步：将上述溶液置于70℃水浴中恒温蒸发制得溶胶，干燥后得到凝胶。研磨凝胶成粉体，于1300℃下焙烧3h得到所需样品BaW。
第三步：将2mg钛酸丁酯和1mg冰醋酸溶于10mg无水乙醇中，充分搅拌得到透明溶液A，将4mg体积分数为75％的乙醇溶液滴入A液中，搅拌30min得到淡黄色TiO2溶胶。称7.94g的BaW粉末加入溶胶中，室温搅拌3h后将体系在80℃干燥10h得前驱体，将此前躯体在500℃干燥3h得到TiO2包覆BaZn1.2Co0.8Fe16O27颗粒构成的BaW/TiO2复合材料粉体，该粉体的粒径为微米级(1-1000um)。
2.复合材料BaW/TiO2的结构、组成、形貌、磁性能及其吸波性能：
将BaW/TiO2复合材料与石蜡以质量比为2.4:1混合，用模具压制成外径为7mm、内径为3mm、厚度约为4mm的环形样品。
扫描电子显微镜观察BaW/TiO2复合材料样品，结果如图2所示，BaW/TiO2复合材料为微米级的吸波材料。
X射线衍射分析BaW/TiO2复合材料样品，结果如图1所示，表明获得的复合材料确实为BaW/TiO2复合材料。
采用矢量网络分析仪在2-18GHz范围内测试其电磁参数:磁导率实部(μ')、磁导率虚部(μ")、介电常数实部(ε')、介电常数虚部(ε")。
由复磁导率μr＝μ'-jμ",复介电常数εr＝ε'-jε"，及公式最终模拟出样品的反射率R(dB)。
测得产物在7.76-13.68GHz的反射损耗小于-10dB，并在10.3GHz反射损耗达到-47.6dB(如图3所示)。产物电磁波反射率小于-10dB的频宽可达3.92GHz,最小反射率为-47.6dB，说明BaW/TiO2复合材料具有高吸收、兼容性优良和频带宽的优点。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明实施方式技术原理的前提下，还可以做出若干改进和替换，这些改进和替换也应视为本发明的保护范围。

Claims (13)

1.一种复合材料，其特征在于，由TiO2和BaZn1.2Co0.8Fe16O27构成，TiO2与BaZn1.2Co0.8Fe16O27的重量比为(0.1-10):(1-10)。
2.根据权利要求1所述的复合材料，其特征在于，所述复合材料为微米级的复合材料。
3.根据权利要求1所述的复合材料，其特征在于，所述复合材料在7.76-13.68GHz的反射损耗小于-10dB，并且在10.3GHz反射损耗达到-47.6dB。
4.一种复合材料的制备方法，包括如下步骤：
将Ba(NO3)2、Zn(NO3)2·6H2O、Co(NO3)2·6H2O和Fe(NO3)3·9H2O按摩尔比为1:1.2:0.8:16溶解于蒸馏水中，向其中加入与Ba(NO3)2摩尔比为10:1的柠檬酸搅拌至完全溶解，并调节溶液的pH至中性；将上述溶液蒸发制得溶胶，干燥得到凝胶，然后焙烧，得到BaZn1.2Co0.8Fe16O27；
称取BaZn1.2Co0.8Fe16O27加入到TiO2溶胶中，搅拌、过滤；滤渣洗涤、干燥得到前驱体，将该前躯体干燥得到所述复合材料；其中，TiO2与BaZn1.2Co0.8Fe16O27颗粒的重量比为(0.1-10):(1-10)。
5.根据权利要求4所述的方法，其特征在于，所述Ba(NO3)2、Zn(NO3)2·6H2O、Co(NO3)2·6H2O和Fe(NO3)3·9H2O为分析纯Ba(NO3)2、分析纯Zn(NO3)2·6H2O、分析纯Co(NO3)2·6H2O和分析纯Fe(NO3)3·9H2O。
6.根据权利要求4所述的方法，其特征在于，所述溶液蒸发的条件为70℃水浴中恒温蒸发。
7.根据权利要求4所述的方法，其特征在于，在于1300℃下焙烧之前，所述凝胶被研磨成粉体。
8.根据权利要求4所述的方法，其特征在于，所述滤渣用无水乙醇洗涤。
9.根据权利要求8所述的方法，其特征在于，经过无水乙醇洗涤的滤渣在80℃干燥。
10.根据权利要求4所述的方法，其特征在于，所述TiO2溶胶按照如下方法制备：将2重量份的钛酸丁酯和1重量份冰醋酸溶于10重量份无水乙醇中，搅拌得到透明溶液，将4重量份体积分数为75％的乙醇溶液缓慢滴入上述透明溶液中，搅拌，得到TiO2溶胶。
11.根据权利要求4所述的方法，其特征在于，所述焙烧在1300℃下进行。
12.一种电子设备外壳，所述电子设备外壳由包括权利要求1-3中任一项所述复合材料为原料制成。
13.根据权利要求12所述的电子设备外壳，其特征在于，所述电子设备为手机。
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