CN107188553B - 一种吸波铁氧体的制备方法 - Google Patents
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Abstract
本发明公开了一种吸波铁氧体的制备方法,包括如下步骤:S1、将Mn(NO3)2·4H2O、Zn(NO3)2·6H2O、Fe(NO3)3·9H2O加入水中溶解,然后加入十六烷基三甲基溴化铵混匀,滴加氢氧化钠水溶液至pH=10.5‑11.5,滴加过程中不断搅拌,升温至70‑75℃,保温2.5‑3h,过滤取滤饼,煅烧,球磨得到纳米铁氧体;S2、将S1中得到的纳米铁氧体加入乙醇中分散均匀得到铁氧体溶胶;将醋酸锌与乙醇混匀,超声得到溶液A;向溶液A中加入铁氧体溶胶混匀,超声,升温,滴加氢氧化钠水溶液,保温搅拌,过滤取滤饼,洗涤,然后调节温度,真空干燥得到吸波铁氧体。
Description
技术领域
本发明涉及铁氧体材料技术领域,尤其涉及一种吸波铁氧体的制备方法。
背景技术
吸波材料研究最初是为了提高武器在战场的生存率和战斗效果,但是随着现代社会的电子信息化,电磁波对空间的污染日趋严重,电磁辐射日益明显,对人类产生较大的损害。因此,吸波材料的应用已经远远超出了军事领域,目前吸波材料已广泛应用于广播、通讯、导航等许多民用领域。纳米铁氧体材料具有一定的吸波性能,但是其吸波性能并不高,因此需要提高其吸波性能,以扩展其使用范围。
发明内容
本发明提出了一种吸波铁氧体的制备方法,使得本发明制备得到的吸波铁氧体其具有良好的吸波性能,在频率为6GHz处,反射损耗达到了-31.5dB,在5-18GHz的频率范围内,-10dB带宽都超过了10GHz。
本发明提出的一种吸波铁氧体的制备方法,包括如下步骤:
S1、将Mn(NO3)2·4H2O、Zn(NO3)2·6H2O、Fe(NO3)3·9H2O加入水中溶解,然后加入十六烷基三甲基溴化铵混匀,滴加氢氧化钠水溶液至pH=10.5-11.5,滴加过程中不断搅拌,升温至70-75℃,保温2.5-3h,过滤取滤饼,升温至1150-1170℃,煅烧2.5-3h,球磨3-5h得到纳米铁氧体;
S2、将S1中得到的纳米铁氧体加入乙醇中分散均匀得到铁氧体溶胶;将醋酸锌与乙醇混匀,超声得到溶液A;向溶液A中加入铁氧体溶胶混匀,超声,升温,滴加氢氧化钠水溶液,保温搅拌,过滤取滤饼,洗涤,然后调节温度,真空干燥得到吸波铁氧体。
优选地,在S1中,Mn(NO3)2·4H2O、Zn(NO3)2·6H2O、Fe(NO3)3·9H2O的摩尔比为0.4-0.5:0.5-0.6:2。
优选地,在S1中,Mn(NO3)2·4H2O与水的重量体积(g/ml)比为1:20-30。
优选地,在S1中,十六烷基三甲基溴化铵与Fe(NO3)3·9H2O的摩尔比为0.9-1.1:2。
优选地,在S1中,氢氧化钠水溶液的浓度为1.5-2mol/l。
优选地,在S2中,将S1中得到的纳米铁氧体加入乙醇中分散均匀得到铁氧体溶胶;将醋酸锌与乙醇混匀,超声20-25min得到溶液A;向溶液A中加入铁氧体溶胶混匀,超声30-35min,升温至45-50℃,滴加氢氧化钠水溶液,保温搅拌6-6.5h,过滤取滤饼,用水洗涤6-8次,然后调节温度至50-60℃,真空干燥得到吸波铁氧体。
优选地,在S2中,在铁氧体溶胶中,纳米铁氧体和乙醇的重量体积(g/ml)比为1:10-14。
优选地,在S2中,氢氧化钠水溶液的浓度为0.2-0.25mol/l,氢氧化钠水溶液在50min内滴加完毕。
优选地,在S2中,保温搅拌的搅拌速度为200-250r/min。
优选地,在S2中,溶液A中,醋酸锌与乙醇的重量体积(g/ml)比为0.9-1:95-110。
优选地,在S2中,溶液A、铁氧体溶胶和氢氧化钠水溶液的体积比为100:1-1.4:25-30。
上述水均为去离子水。
本发明通过调整Mn、Zn、Fe元素的比例,并配合十六烷基三甲基溴化铵,结合合适的制备工艺,并配以合适的煅烧条件,阻止杂质相的生成,得到晶型均一、粒径均一的纳米铁氧体颗粒,且颗粒表面粗糙,可以促进氧化锌的附着,并且Mn、Zn、Fe与十六烷基三甲基溴化铵按合适比例相互配合,使得纳米铁氧体颗粒具有较好的吸波性能和分散性能,使得纳米铁氧体与醋酸锌、乙醇均匀分散,经合适的制备工艺,使得生成的氧化锌紧密、均匀的附着在纳米铁氧体表面,形成表面光滑,粒径大小均一的铁氧体,氧化锌与纳米铁氧体相互配合,使得本发明制备得到的铁氧体其具有良好的吸波性能,在频率为6GHz处,反射损耗达到了-31.5dB,在5-18GHz的频率范围内,-10dB带宽都超过了10GHz。
具体实施方式
实施例1
一种吸波铁氧体的制备方法,包括如下步骤:
S1、将Mn(NO3)2·4H2O、Zn(NO3)2·6H2O、Fe(NO3)3·9H2O加入水中溶解,然后加入十六烷基三甲基溴化铵混匀,滴加氢氧化钠水溶液至pH=11滴加过程中不断搅拌,升温至72℃,保温2.8h,过滤取滤饼,升温至1160℃,煅烧2.8h,球磨4h得到纳米铁氧体;
S2、将S1中得到的纳米铁氧体加入乙醇中分散均匀得到铁氧体溶胶;将醋酸锌与乙醇混匀,超声得到溶液A;向溶液A中加入铁氧体溶胶混匀,超声,升温,滴加氢氧化钠水溶液,保温搅拌,过滤取滤饼,洗涤,然后调节温度,真空干燥得到吸波铁氧体。
实施例2
一种吸波铁氧体的制备方法,包括如下步骤:
S1、将Mn(NO3)2·4H2O、Zn(NO3)2·6H2O、Fe(NO3)3·9H2O加入水中溶解,然后加入十六烷基三甲基溴化铵混匀,滴加浓度为1.5mol/l氢氧化钠水溶液至pH=11.5,滴加过程中不断搅拌,升温至70℃,保温3h,过滤取滤饼,升温至1150℃,煅烧3h,球磨3h得到纳米铁氧体,其中,Mn(NO3)2·4H2O、Zn(NO3)2·6H2O、Fe(NO3)3·9H2O的摩尔比为0.5:0.5:2,Mn(NO3)2·4H2O与水的重量体积(g/ml)比为1:30,十六烷基三甲基溴化铵与Fe(NO3)3·9H2O的摩尔比为0.9:2;
S2、将S1中得到的纳米铁氧体加入乙醇中分散均匀得到铁氧体溶胶,其中,纳米铁氧体和乙醇的重量体积(g/ml)比为1:14;将醋酸锌与乙醇混匀,超声20min得到溶液A,其中,醋酸锌与乙醇的重量体积(g/ml)比为1:95;向溶液A中加入铁氧体溶胶混匀,超声35min,升温至45℃,滴加浓度为0.25mol/l氢氧化钠水溶液,在50min内滴加完毕,以200r/min的速度保温搅拌6.5h,过滤取滤饼,用水洗涤6次,然后调节温度至60℃,真空干燥得到吸波铁氧体,其中,溶液A、铁氧体溶胶和氢氧化钠水溶液的体积比为100:1:25。
实施例3
一种吸波铁氧体的制备方法,包括如下步骤:
S1、将Mn(NO3)2·4H2O、Zn(NO3)2·6H2O、Fe(NO3)3·9H2O加入水中溶解,然后加入十六烷基三甲基溴化铵混匀,滴加浓度为2mol/l氢氧化钠水溶液至pH=10.5,滴加过程中不断搅拌,升温至75℃,保温2.5h,过滤取滤饼,升温至1170℃,煅烧2.5h,球磨5h得到纳米铁氧体,其中,Mn(NO3)2·4H2O、Zn(NO3)2·6H2O、Fe(NO3)3·9H2O的摩尔比为0.4:0.6:2,Mn(NO3)2·4H2O与水的重量体积(g/ml)比为1:20,十六烷基三甲基溴化铵与Fe(NO3)3·9H2O的摩尔比为1.1:2;
S2、将S1中得到的纳米铁氧体加入乙醇中分散均匀得到铁氧体溶胶,其中,纳米铁氧体和乙醇的重量体积(g/ml)比为1:10;将醋酸锌与乙醇混匀,超声25min得到溶液A,其中,醋酸锌与乙醇的重量体积(g/ml)比为0.9:110;向溶液A中加入铁氧体溶胶混匀,超声30min,升温至50℃,滴加浓度为0.2mol/l氢氧化钠水溶液,在50min内滴加完毕,以250r/min的速度保温搅拌6h,过滤取滤饼,用水洗涤8次,然后调节温度至50℃,真空干燥得到吸波铁氧体,其中,溶液A、铁氧体溶胶和氢氧化钠水溶液的体积比为100:1.4:30。
实施例4
一种吸波铁氧体的制备方法,包括如下步骤:
S1、将Mn(NO3)2·4H2O、Zn(NO3)2·6H2O、Fe(NO3)3·9H2O加入水中溶解,然后加入十六烷基三甲基溴化铵混匀,滴加浓度为1.6mol/l氢氧化钠水溶液至pH=11.3,滴加过程中不断搅拌,升温至71℃,保温2.9h,过滤取滤饼,升温至1155℃,煅烧2.9h,球磨3.5h得到纳米铁氧体,其中,Mn(NO3)2·4H2O、Zn(NO3)2·6H2O、Fe(NO3)3·9H2O的摩尔比为0.5:0.5:2,Mn(NO3)2·4H2O与水的重量体积(g/ml)比为1:28,十六烷基三甲基溴化铵与Fe(NO3)3·9H2O的摩尔比为1.05:2;
S2、将S1中得到的纳米铁氧体加入乙醇中分散均匀得到铁氧体溶胶,其中,纳米铁氧体和乙醇的重量体积(g/ml)比为1:13;将醋酸锌与乙醇混匀,超声21min得到溶液A,其中,醋酸锌与乙醇的重量体积(g/ml)比为0.98:100;向溶液A中加入铁氧体溶胶混匀,超声34min,升温至46℃,滴加浓度为0.23mol/l氢氧化钠水溶液,在50min内滴加完毕,以220r/min的速度保温搅拌6.3h,过滤取滤饼,用水洗涤7次,然后调节温度至57℃,真空干燥得到吸波铁氧体,其中,溶液A、铁氧体溶胶和氢氧化钠水溶液的体积比为100:1.1:28。
实施例5
一种吸波铁氧体的制备方法,包括如下步骤:
S1、将Mn(NO3)2·4H2O、Zn(NO3)2·6H2O、Fe(NO3)3·9H2O加入水中溶解,然后加入十六烷基三甲基溴化铵混匀,滴加浓度为1.8mol/l氢氧化钠水溶液至pH=10.7,滴加过程中不断搅拌,升温至73℃,保温2.7h,过滤取滤饼,升温至1165℃,煅烧2.7h,球磨4.5h得到纳米铁氧体,其中,Mn(NO3)2·4H2O、Zn(NO3)2·6H2O、Fe(NO3)3·9H2O的摩尔比为0.4:0.6:2,Mn(NO3)2·4H2O与水的重量体积(g/ml)比为1:22,十六烷基三甲基溴化铵与Fe(NO3)3·9H2O的摩尔比为1:2;
S2、将S1中得到的纳米铁氧体加入乙醇中分散均匀得到铁氧体溶胶,其中,纳米铁氧体和乙醇的重量体积(g/ml)比为1:11;将醋酸锌与乙醇混匀,超声23min得到溶液A,其中,醋酸锌与乙醇的重量体积(g/ml)比为0.92:105;向溶液A中加入铁氧体溶胶混匀,超声32min,升温至48℃,滴加浓度为0.21mol/l氢氧化钠水溶液,在50min内滴加完毕,以230r/min的速度保温搅拌6.1h,过滤取滤饼,用水洗涤7次,然后调节温度至53℃,真空干燥得到吸波铁氧体,其中,溶液A、铁氧体溶胶和氢氧化钠水溶液的体积比为100:1.3:26。
对实施例5所得吸波铁氧体进行性能测试,在频率为6GHz处,反射损耗达到了-31.5dB;实施例1-5所得吸波铁氧体,在5-18GHz的频率范围内,-10dB带宽都超过了10GHz。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (3)
1.一种吸波铁氧体的制备方法,其特征在于,包括如下步骤:
S1、将Mn(NO3)2·4H2O、Zn(NO3)2·6H2O、Fe(NO3)3·9H2O加入水中溶解,然后加入十六烷基三甲基溴化铵混匀,滴加氢氧化钠水溶液至pH=10.5-11.5,滴加过程中不断搅拌,升温至70-75℃,保温2.5-3h,过滤取滤饼,升温至1150-1170℃,煅烧2.5-3h,球磨3-5h得到纳米铁氧体;
S2、将S1中得到的纳米铁氧体加入乙醇中分散均匀得到铁氧体溶胶;将醋酸锌与乙醇混匀,超声得到溶液A;向溶液A中加入铁氧体溶胶混匀,超声,升温至45-50℃,滴加氢氧化钠水溶液,保温搅拌,过滤取滤饼,洗涤,然后调节温度,真空干燥得到吸波铁氧体;
在S1中,Mn(NO3)2·4H2O、Zn(NO3)2·6H2O、Fe(NO3)3·9H2O的摩尔比为0.4-0.5:0.5-0.6:2;
在S1中,Mn(NO3)2·4H2O与水的重量体积g/ml比为1:20-30;
在S1中,十六烷基三甲基溴化铵与Fe(NO3)3·9H2O的摩尔比为0.9-1.1:2;
在S1中,氢氧化钠水溶液的浓度为1.5-2mol/l;
在S2中,在铁氧体溶胶中,纳米铁氧体和乙醇的重量体积g/ml比为1:10-14;
在S2中,氢氧化钠水溶液的浓度为0.2-0.25mol/l,氢氧化钠水溶液在50min内滴加完毕;
在S2中,溶液A中,醋酸锌与乙醇的重量体积g/ml比为0.9-1:95-110;在S2中,溶液A、铁氧体溶胶和氢氧化钠水溶液的体积比为100:1-1.4:25-30。
2.根据权利要求1所述吸波铁氧体的制备方法,其特征在于,在S2中,将S1中得到的纳米铁氧体加入乙醇中分散均匀得到铁氧体溶胶;将醋酸锌与乙醇混匀,超声20-25min得到溶液A;向溶液A中加入铁氧体溶胶混匀,超声30-35min,升温至45-50℃,滴加氢氧化钠水溶液,保温搅拌6-6.5h,过滤取滤饼,用水洗涤6-8次,然后调节温度至50-60℃,真空干燥得到吸波铁氧体。
3.根据权利要求1或2所述吸波铁氧体的制备方法,其特征在于,在S2中,保温搅拌的搅拌速度为200-250r/min。
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