CN106745301B - 一种用聚酰胺-胺树形分子为模板制备铁磁性纯相Bi2Fe4O9纳米颗粒的方法 - Google Patents
一种用聚酰胺-胺树形分子为模板制备铁磁性纯相Bi2Fe4O9纳米颗粒的方法 Download PDFInfo
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Abstract
本发明涉及一种用聚酰胺‑胺树形分子为模板制备铁磁性纯相Bi2Fe4O9纳米颗粒的方法，其特征在于：以末端基团为酯基、羟基或羧基的聚酰胺‑胺（PAMAM）树形分子为模板，采用溶剂热法制得铁磁性纯相Bi2Fe4O9纳米颗粒。本发明采用了分散系数接近于1的球形聚酰胺‑胺树形分子为模板，制得的Bi2Fe4O9纳米颗粒为正交晶系，粒径小于10纳米，分散性好，饱和磁化强度达到18.4 emu/g，在可见光照射下具有高催化活性，可用作磁性回收可见光催化剂、传感器和磁流变液材料等领域。
Description
技术领域
本发明涉及一种用聚酰胺-胺树形分子为模板制备铁磁性纯相Bi2Fe4O9纳米颗粒的方法，属材料制备技术领域。
背景技术
Bi2Fe4O9是铁酸铋材料中一个重要的相，能带间隙大约为2.1eV，化学稳定性好，能够充分吸收利用可见光，在利用太阳能方面具有优势。Bi2Fe4O9在室温下具有弱铁磁性和良好的光催化活性，能将工业氨氧化为NO，在磁性回收光催化剂领域具有良好的应用前景。Bi2Fe4O9对乙醇和丙酮等气体有非常敏感，还可以作为半导体气敏传感器，是一种性能优良的功能材料。
Bi2Fe4O9的形貌、微观结构和尺寸对其光催化性能和磁性能影响很大，小尺寸的纳米颗粒具有更大的比表面积，更强的量子尺寸效应、小尺寸效应和宏观量子隧道效应，能表现出更强的光催化剂活性和磁化强度。因此，小尺寸的Bi2Fe4O9纳米颗粒可望成为一种新型的可磁性回收的窄带隙可见光催化剂，在可见光催化领域具有广泛的应用前景。
目前，科技人员研究了溶胶-凝胶法、共沉淀法和水热法等方法来合成Bi2Fe4O9材料，但要想制备出小尺寸的、高饱和磁化强度的纯相Bi2Fe4O9纳米颗粒仍然非常困难。聚酰胺-胺（PAMAM）树形分子具有单分散的球形分子结构，分子表面为密集的官能团，内部为纳米级空腔，在水和有机溶剂中均具有良好的溶解性能，在制备纳米颗粒时起到容器和载体的软模板作用，已经在制备纳米催化剂、检测试剂、生物医药制剂等高附加值产品上显示出了明显的性能优势，具有广阔的应用前景。为此，我们以PAMAM树形分子为模板，采用溶剂热法制备出直径在10 nm以下的铁磁性纯相Bi2Fe4O9纳米颗粒，在磁性回收可见光催化剂、传感器和磁流变液材料等领域具有很强的理论意义和应用价值。
发明内容
本发明的目的是提供一种能够制备出小尺寸的铁磁性纯相Bi2Fe4O9纳米颗粒的方法，其技术内容为：
一种用聚酰胺-胺树形分子为模板制备铁磁性纯相Bi2Fe4O9纳米颗粒的方法，其特征在于：以末端基团为酯基、羟基或羧基的聚酰胺-胺（PAMAM）树形分子为模板，采用溶剂热法制得铁磁性纯相Bi2Fe4O9纳米颗粒。
所述的一种用聚酰胺-胺树形分子为模板制备铁磁性纯相Bi2Fe4O9纳米颗粒的方法，其特征在于：包括以下步骤：（1）PAMAM/Fe(OH)3/Bi(OH)3前驱体制备：所述的PAMAM/Fe(OH)3/Bi(OH)3前驱体的制备步骤为：将物质的量比为2:1的Fe(NO3)3·9H2O和Bi(NO3)3·5H2O加入到有机溶剂中，边搅拌边缓慢滴加8～10%稀硝酸至Fe(NO3)3·9H2O和Bi(NO3)3·5H2O完全溶解，再加入PAMAM树形分子溶液，采用功率为50W的超声波清洗机震荡5min后，置于室温下搅拌2～4 h，使Fe3+和Bi3+与树形分子充分配位后，将搅拌速度调至800转/分以上，加入NaOH水溶液使反应体系的pH值为14，室温下搅拌反应1h后，即得到PAMAM/Fe(OH)3/Bi(OH)3前驱体悬浊液。（2）铁磁性纯相Bi2Fe4O9纳米颗粒制备：所述的铁磁性纯相Bi2Fe4O9纳米颗粒制备步骤为：将所述步骤（1）制得的PAMAM/Fe(OH)3/Bi(OH)3前驱体悬浊液转移至水热反应釜中，补充有机溶剂或NaOH水溶液使填充度为70%～75%，密封后将反应釜置于140～150℃的烘箱中，保温18～24h后取出，离心分离，用去离子水将沉淀物洗涤至PH值为中性后，在60℃以下烘干即得到铁磁性纯相Bi2Fe4O9纳米颗粒。
所述的一种用聚酰胺-胺树形分子为模板制备铁磁性纯相Bi2Fe4O9纳米颗粒的方法，其特征在于：PAMAM树形分子的代数为4～6代，末端基团为酯基、羟基或羧基，加入量以Fe3+与树形分子的物质的量比为140:1～10:1为标准，树形分子溶液的溶剂为水或乙醇，浓度为1×10-4～1×10-2 mol/L。
所述的一种用聚酰胺-胺树形分子为模板制备铁磁性纯相Bi2Fe4O9纳米颗粒的方法，其特征在于：有机溶剂为乙醇或丙酮，步骤（1）中Fe(NO3)3·9H2O的浓度为0.01～0.1mol/L，步骤（2）水热反应釜中有机溶剂与水的体积比为1:1～4:1。
所述的一种用聚酰胺-胺树形分子为模板制备铁磁性纯相Bi2Fe4O9纳米颗粒的方法，其特征在于：NaOH水溶液浓度为8～10 mol/L，步骤（1）中碱溶液分批加入，第一批加入量不少于体系中反应物Fe(NO3)3·9H2O、Bi(NO3)3·5H2O和硝酸的物质的量的总和，然后滴加至规定pH值。
本发明与现有技术相比，具有如下优点：
1、本发明采用分散系数接近于1的球形的聚酰胺-胺树形分子为模板，制得的Bi2Fe4O9纳米颗粒为纯相，正交晶系，尺寸均匀，粒径小于10 nm，分散性好，饱和磁化强度达到18.4 emu/g，在可见光照射下具有高催化活性；
2、本发明采用溶剂热法制备Bi2Fe4O9纳米颗粒，工艺简单，可用于磁性回收可见光催化剂、传感器和磁流变液材料等领域。
附图说明
图1是本发明制得的Bi2Fe4O9纳米颗粒的高分辨透射电子显微镜（HRTEM）照片，颗粒为球形，直径小于10 nm。
图2是本发明制得的Bi2Fe4O9纳米颗粒的磁滞回线，可以看出BiFeO3纳米颗粒具有铁磁性，饱和磁化强度为18.4 emu/g。
具体实施方式
实施例1：
步骤（1）：PAMAM/Fe(OH)3/Bi(OH)3前驱体制备：将物质的量比为2:1的Fe(NO3)3·9H2O和Bi(NO3)3·5H2O加入到丙酮中，边搅拌边缓慢滴加10%稀硝酸至Fe(NO3)3·9H2O和Bi(NO3)3·5H2O完全溶解，Fe3+的浓度为0.01 mol/L，再加入4代、末端基团为酯基的PAMAM树形分子水溶液，树形分子的浓度为1×10-2 mol/L，加入量以Fe3+与树形分子的物质的量比为10:1为标准，采用功率为50W的超声波清洗机震荡5min后，置于室温下搅拌2 h，使Fe3+和Bi3 +与树形分子充分配位后，将搅拌速度调至800转/分以上，加入8 mol/L 的NaOH水溶液使反应体系的pH值为14，室温下搅拌反应1h后，即得到PAMAM/Fe(OH)3/Bi(OH)3前驱体悬浊液。
步骤（2）：铁磁性纯相Bi2Fe4O9纳米颗粒制备：将步骤（1）制得的PAMAM/Fe(OH)3/Bi(OH)3前驱体悬浊液转移至水热反应釜中，补充丙酮或8 mol/L 的NaOH水溶液，使填充度为75%，丙酮与水的体积比为1:1，密封后将反应釜置于150℃的烘箱中，保温18h后取出，离心分离，用去离子水将沉淀物洗涤至PH值为中性后，在60℃以下烘干即得到铁磁性纯相Bi2Fe4O9纳米颗粒。
实施例2：
步骤（1）：PAMAM/Fe(OH)3/Bi(OH)3前驱体制备：将物质的量比为2:1的Fe(NO3)3·9H2O和Bi(NO3)3·5H2O加入到丙酮中，边搅拌边缓慢滴加10%稀硝酸至Fe(NO3)3·9H2O和Bi(NO3)3·5H2O完全溶解，Fe3+的浓度为0.05 mol/L，再加入5代、末端基团为羧基的PAMAM树形分子水溶液，树形分子的浓度为1×10-3 mol/L，加入量以Fe3+与树形分子的物质的量比为40:1为标准，采用功率为50W的超声波清洗机震荡5min后，置于室温下搅拌3 h，使Fe3+和Bi3 +与树形分子充分配位后，将搅拌速度调至800转/分以上，加入8 mol/L 的NaOH水溶液使反应体系的pH值为14，室温下搅拌反应1h后，即得到PAMAM/Fe(OH)3/Bi(OH)3前驱体悬浊液。
步骤（2）：铁磁性纯相Bi2Fe4O9纳米颗粒制备：将步骤（1）制得的PAMAM/Fe(OH)3/Bi(OH)3前驱体悬浊液转移至水热反应釜中，补充丙酮或8 mol/L 的NaOH水溶液，使填充度为70%，丙酮与水的体积比为2:1，密封后将反应釜置于150℃的烘箱中，保温18h后取出，离心分离，用去离子水将沉淀物洗涤至PH值为中性后，在60℃以下烘干即得到铁磁性纯相Bi2Fe4O9纳米颗粒。
实施例3：
步骤（1）：PAMAM/Fe(OH)3/Bi(OH)3前驱体制备：将物质的量比为2:1的Fe(NO3)3·9H2O和Bi(NO3)3·5H2O加入到乙醇中，边搅拌边缓慢滴加8%稀硝酸至Fe(NO3)3·9H2O和Bi(NO3)3·5H2O完全溶解，Fe3+的浓度为0.05 mol/L，再加入5代、末端基团为羟基的PAMAM树形分子乙醇溶液，树形分子的浓度为1×10-3 mol/L，加入量以Fe3+与树形分子的物质的量比为80:1为标准，采用功率为50W的超声波清洗机震荡5min后，置于室温下搅拌4 h，使Fe3+和Bi3+与树形分子充分配位后，将搅拌速度调至800转/分以上，加入8 mol/L 的NaOH水溶液使反应体系的pH值为14，室温下搅拌反应1h后，即得到PAMAM/Fe(OH)3/Bi(OH)3前驱体悬浊液。
步骤（2）：铁磁性纯相Bi2Fe4O9纳米颗粒制备：将步骤（1）制得的PAMAM/Fe(OH)3/Bi(OH)3前驱体悬浊液转移至水热反应釜中，补充乙醇或8 mol/L 的NaOH水溶液，使填充度为70%，乙醇与水的体积比为3:1，密封后将反应釜置于140℃的烘箱中，保温24h后取出，离心分离，用去离子水将沉淀物洗涤至PH值为中性后，在60℃以下烘干即得到铁磁性纯相Bi2Fe4O9纳米颗粒。
实施例4：
步骤（1）：PAMAM/Fe(OH)3/Bi(OH)3前驱体制备：将物质的量比为2:1的Fe(NO3)3·9H2O和Bi(NO3)3·5H2O加入到乙醇中，边搅拌缓慢滴加8%稀硝酸至Fe(NO3)3·9H2O和Bi(NO3)3·5H2O完全溶解，Fe3+的浓度为0.1 mol/L，再加入6代、末端基团为酯基的PAMAM树形分子乙醇溶液，树形分子的浓度为1×10-4 mol/L，加入量以Fe3+与树形分子的物质的量比为140:1为标准，采用功率为50W的超声波清洗机震荡5min后，置于室温下搅拌4 h，使Fe3+和Bi3+与树形分子充分配位后，将搅拌速度调至800转/分以上，加入10 mol/L 的NaOH水溶液使反应体系的pH值为14，室温下搅拌反应1h后，即得到PAMAM/Fe(OH)3/Bi(OH)3前驱体悬浊液。
步骤（2）：铁磁性纯相Bi2Fe4O9纳米颗粒制备：将步骤（1）制得的PAMAM/Fe(OH)3/Bi(OH)3前驱体悬浊液转移至水热反应釜中，补充乙醇或10 mol/L 的NaOH水溶液，使填充度为70%，乙醇与水的体积比为4:1，密封后将反应釜置于140℃的烘箱中，保温24h后取出，离心分离，用去离子水将沉淀物洗涤至PH值为中性后，在60℃以下烘干即得到铁磁性纯相Bi2Fe4O9纳米颗粒。
Claims (4)
1.一种用聚酰胺-胺树形分子为模板制备铁磁性纯相Bi2Fe4O9纳米颗粒的方法，其特征在于：以末端基团为酯基、羟基或羧基的聚酰胺-胺（PAMAM）树形分子为模板，采用溶剂热法制得铁磁性纯相Bi2Fe4O9纳米颗粒，包括以下步骤：（1）PAMAM/Fe(OH)3/Bi(OH)3前驱体制备：所述的PAMAM/Fe(OH)3/Bi(OH)3前驱体的制备步骤为：将物质的量比为2:1的Fe(NO3)3·9H2O和Bi(NO3)3·5H2O加入到有机溶剂中，边搅拌边缓慢滴加8～10%稀硝酸至Fe(NO3)3·9H2O和Bi(NO3)3·5H2O完全溶解，再加入PAMAM树形分子溶液，采用功率为50W的超声波清洗机震荡5min后，置于室温下搅拌2～4 h，使Fe3+和Bi3+与树形分子充分配位后，将搅拌速度调至800转/分以上，加入NaOH水溶液使反应体系的pH值为14，室温下搅拌反应1h后，即得到PAMAM/Fe(OH)3/Bi(OH)3前驱体悬浊液；（2）铁磁性纯相Bi2Fe4O9纳米颗粒制备：所述的铁磁性纯相Bi2Fe4O9纳米颗粒制备步骤为：将所述步骤（1）制得的PAMAM/Fe(OH)3/Bi(OH)3前驱体悬浊液转移至水热反应釜中，补充有机溶剂或NaOH水溶液使填充度为70%～75%，密封后将反应釜置于140～150℃的烘箱中，保温18～24h后取出，离心分离，用去离子水将沉淀物洗涤至pH值为中性后，在60℃以下烘干即得到铁磁性纯相Bi2Fe4O9纳米颗粒。
2.如权利要求1所述的一种用聚酰胺-胺树形分子为模板制备铁磁性纯相Bi2Fe4O9纳米颗粒的方法，其特征在于：PAMAM树形分子的代数为4～6代，末端基团为酯基、羟基或羧基，加入量以Fe3+与树形分子的物质的量比为140:1～10:1为标准，树形分子溶液的溶剂为水或乙醇，浓度为1×10-4～1×10-2 mol/L。
3.如权利要求1所述的一种用聚酰胺-胺树形分子为模板制备铁磁性纯相Bi2Fe4O9纳米颗粒的方法，其特征在于：有机溶剂为乙醇或丙酮，步骤（1）中Fe(NO3)3·9H2O的浓度为0.01～0.1 mol/L，步骤（2）水热反应釜中有机溶剂与水的体积比为1:1～4:1。
4.如权利要求1所述的一种用聚酰胺-胺树形分子为模板制备铁磁性纯相Bi2Fe4O9纳米颗粒的方法，其特征在于： NaOH水溶液浓度为8～10 mol/L，步骤（1）中碱溶液分批加入，第一批加入量不少于体系中反应物Fe(NO3)3·9H2O、Bi(NO3)3·5H2O和硝酸的物质的量的总和，然后滴加至规定pH值。
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