CN111943275A - 一种磁性Fe3S4纳米晶材料的制备方法 - Google Patents
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- 238000000034 method Methods 0.000 title abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 239000002243 precursor Substances 0.000 claims abstract description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 62
- 239000012498 ultrapure water Substances 0.000 claims description 20
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 19
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 14
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- 229960000583 acetic acid Drugs 0.000 claims description 7
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- 239000001301 oxygen Substances 0.000 claims description 2
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- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims 1
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- 238000002441 X-ray diffraction Methods 0.000 description 1
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Abstract
本发明公开了一种磁性Fe3S4纳米晶材料的制备方法，包括前体溶液配制、pH调节以及后处理步骤。本发明操作简单，不采用高毒性溶剂和其他有机表面活性剂，制成品的粒径在100 nm以下，无其它杂质，质量稳定且纯度高，有良好的生物相容性；本发明所采用的原料价格低，大大降低了生产成，可规模化生产；采用本发明方法获得的产品在低温保存下，经12个月后仍然稳定存在，适合长期存储。
Description
技术领域
本发明属于纳米材料制备技术领域，具体涉及一种磁性Fe3S4纳米晶材料的制备方法。
背景技术
近些年来Fe3S4磁性纳米粒子由于其独特的物理化学性质，如量子尺寸效应、电磁学特性，在环境治理、能源储存、催化剂、生物医学应用等方面展示出了其巨大的潜力。Fe3S4纳米粒子的制备方法主要有共沉淀法、水热法（溶液热法）、热分解法和模板法。其中水热法、热解法等由于操作复杂，生产成本高等缺点，不适用于工业生产。而共沉淀法由于其制备过程简单、消耗低、粒径小等优点，适合于工业规模生产。
Fe3S4与Fe3O4同作为磁小体，具有相似的晶格结构，最早被Skinner等人作为一种矿物报道出来。但与Fe3O4纳米材料相比，对Fe3S4的研究了解还比较少，由于Fe3S4的亚稳态性质，导致对成功合成出Fe3S4纳米材料的报道较少，合成出相对稳定、结晶度高的Fe3S4纯相纳米材料较困难。
沉淀法是一种操作简单的制备金属纳米颗粒的一种方法。根据溶液中含有的化合物离子的价态，沉淀法可以分为共沉淀法、氧化还原沉淀法。由于Fe3S4的亚稳态性质，利用沉淀法制备Fe3S4纳米材料比较困难。为此，研发一种制备简单、质量稳定的磁性Fe3S4纳米晶材料的制备方法是非常必要的。
发明内容
本发明的目的在于提供一种磁性Fe3S4纳米晶材料的制备方法。
本发明的目的是这样实现的，包括以下步骤：
S1、在N2保护的条件下，将铁源FeSO4·7H2O按1：1摩尔比溶解在无氧超纯水中，得到浓度为0.1~0.5mol·L-1的溶液，将铁源Na2S·9H2O按1：1摩尔比溶解在无氧超纯水中，得到浓度为0.1~0.5mol·L-1的溶液；
S2、在N2保护的条件下，将S1步骤得到的两种溶液等体积混合均匀，得到前体溶液；
S3、对前体溶液逐滴滴加冰醋酸，调节溶液pH至2.9~3.1；
S4、将S3步骤调节pH后的溶液强力搅拌4~6min，再离心4~6min，移除多余液体，再经冻干处理除去水分，得到直径在20~100 nm磁性Fe3S4纳米晶材料。
与现有技术相比，本发明具有以下技术效果：
1、本发明操作简单，不采用高毒性溶剂和其他有机表面活性剂，制成品的粒径在100nm以下，无其它杂质，质量稳定且纯度高，有良好的生物相容性；
2、本发明所采用的原料价格低，大大降低了生产成，可规模化生产；
3、采用本发明方法获得的产品在低温保存下，经12个月后仍然稳定存在，适合长期存储。
附图说明
图1为本发明实施例1制得的磁性Fe3S4纳米晶材料的X射线衍射图谱。
图2为本发明实施例1制得的磁性Fe3S4纳米晶材料的磁铁测试图。
图3为本发明实施例1制得的磁性Fe3S4纳米晶材料的投射电镜图。
图4为本发明实施例1制得的磁性Fe3S4纳米晶材料的高倍扫描电镜图。
具体实施方式
下面结合附图对本发明作进一步的说明，但不以任何方式对本发明加以限制，基于本发明教导所作的任何变换或替换，均属于本发明的保护范围。
如附图1~图4所示本发明包括以下步骤：
S1、在N2保护的条件下，将铁源FeSO4·7H2O按1：1摩尔比溶解在无氧超纯水中，得到浓度为0.1~0.5mol·L-1的溶液，将铁源Na2S·9H2O按1：1摩尔比溶解在无氧超纯水中，得到浓度为0.1~0.5mol·L-1的溶液；
S2、在N2保护的条件下，将S1步骤得到的两种溶液等体积混合均匀，得到前体溶液；
S3、对前体溶液逐滴滴加冰醋酸，调节溶液pH至2.9~3.1；
S4、将S3步骤调节pH后的溶液强力搅拌4~6min，再离心4~6min，移除多余液体，再经冻干处理除去水分，得到直径在20~100 nm磁性Fe3S4纳米晶材料。
本发明用共沉淀法，将Fe2+、Fe3+与S2-按比例混合，调节pH进行反应，然后经搅拌、离心、冻干处理，其反应原理为：
最后得到制得Fe3S4纳米晶材料。
优选地，S1步骤的无氧超纯水是先将超纯水煮沸，然后通入N2，去除超纯水中的氧，即可。
优选地，S3步骤调节溶液pH至3.0。
优选地，S4步骤离心是在5000~8000 rpm下条件下离心。
优选地，S4步骤强力搅拌5min，再离心5min。
下面结合实施例1~实施例4对本发明作进一步说明。
实施例1
磁性Fe3S4纳米晶材料的制备方法，包括以下步骤：
S1、在N2保护的条件下，将铁源FeSO4·7H2O按1：1摩尔比溶解在无氧超纯水中，得到浓度为0.1mol·L-1的溶液，将铁源Na2S·9H2O按1：1摩尔比溶解在无氧超纯水中，得到浓度为0.1mol·L-1的溶液；
S2、在N2保护的条件下，将S1步骤得到的两种溶液等体积混合均匀，得到前体溶液；
S3、对前体溶液逐滴滴加冰醋酸，调节溶液pH至3.0；
S4、将S3步骤调节pH后的溶液强力搅拌5min，再在7000rpm条件下离心5min，移除多余液体，再经冻干处理除去水分，得到直径在20nm磁性Fe3S4纳米晶材料。
实施例2
磁性Fe3S4纳米晶材料的制备方法，包括以下步骤：
S1、在N2保护的条件下，将铁源FeSO4·7H2O按1：1摩尔比溶解在无氧超纯水中，得到浓度为0.1mol·L-1的溶液，将铁源Na2S·9H2O按1：1摩尔比溶解在无氧超纯水中，得到浓度为0.1mol·L-1的溶液；
S2、在N2保护的条件下，将S1步骤得到的两种溶液等体积混合均匀，得到前体溶液；
S3、对前体溶液逐滴滴加冰醋酸，调节溶液pH至2.9；
S4、将S3步骤调节pH后的溶液强力搅拌4min，再在5000 rpm条件下离心4min，移除多余液体，再经冻干处理除去水分，得到直径在100nm磁性Fe3S4纳米晶材料。
实施例3
磁性Fe3S4纳米晶材料的制备方法，包括以下步骤：
S1、在N2保护的条件下，将铁源FeSO4·7H2O按1：1摩尔比溶解在无氧超纯水中，得到浓度为0.5mol·L-1的溶液，将铁源Na2S·9H2O按1：1摩尔比溶解在无氧超纯水中，得到浓度为0.5mol·L-1的溶液；
S2、在N2保护的条件下，将S1步骤得到的两种溶液等体积混合均匀，得到前体溶液；
S3、对前体溶液逐滴滴加冰醋酸，调节溶液pH至3.1；
S4、将S3步骤调节pH后的溶液强力搅拌6min，再在8000 rpm条件下离心6min，移除多余液体，再经冻干处理除去水分，得到直径在50 nm磁性Fe3S4纳米晶材料。
实施例4
磁性Fe3S4纳米晶材料的制备方法，包括以下步骤：
S1、在N2保护的条件下，将铁源FeSO4·7H2O按1：1摩尔比溶解在无氧超纯水中，得到浓度为0.3mol·L-1的溶液，将铁源Na2S·9H2O按1：1摩尔比溶解在无氧超纯水中，得到浓度为0.3mol·L-1的溶液；
S2、在N2保护的条件下，将S1步骤得到的两种溶液等体积混合均匀，得到前体溶液；
S3、对前体溶液逐滴滴加冰醋酸，调节溶液pH至3.0；
S4、将S3步骤调节pH后的溶液强力搅拌5min，再在6500rpm条件下离心5min，移除多余液体，再经冻干处理除去水分，得到直径在60nm磁性Fe3S4纳米晶材料。
Claims (5)
1.一种磁性Fe3S4纳米晶材料的制备方法，其特征在于包括以下步骤：
S1、在N2保护的条件下，将铁源FeSO4·7H2O按1：1摩尔比溶解在无氧超纯水中，得到浓度为0.1~0.5mol·L-1的溶液，将铁源Na2S·9H2O按1：1摩尔比溶解在无氧超纯水中，得到浓度为0.1~0.5mol·L-1的溶液；
S2、在N2保护的条件下，将S1步骤得到的两种溶液等体积混合均匀，得到前体溶液；
S3、对前体溶液逐滴滴加冰醋酸，调节溶液pH至2.9~3.1；
S4、将S3步骤调节pH后的溶液强力搅拌4~6min，再离心4~6min，移除多余液体，再经冻干处理除去水分，得到直径在20~100 nm磁性Fe3S4纳米晶材料。
2.根据权利要求1所述的磁性Fe3S4纳米晶材料的制备方法，其特征在于S1步骤的无氧超纯水是先将超纯水煮沸，然后通入N2，去除超纯水中的氧，即可。
3.根据权利要求1所述的磁性Fe3S4纳米晶材料的制备方法，其特征在于S3步骤调节溶液pH至3.0。
4.根据权利要求1所述的磁性Fe3S4纳米晶材料的制备方法，其特征在于S4步骤离心是在5000~8000 rpm下条件下离心。
5.根据权利要求1所述的磁性Fe3S4纳米晶材料的制备方法，其特征在于S4步骤强力搅拌5min，再离心5min。
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| CN102817081A (zh) * | 2012-08-22 | 2012-12-12 | 兰州大学 | 一种片状四硫化三铁纳米单晶的制备方法 |
| CN102874879A (zh) * | 2012-10-12 | 2013-01-16 | 中国科学技术大学 | 一种Fe3S4纳米晶材料的制备方法 |
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| YO-SHENG CHANG等: "Fabrication, characterization, and application of greigite nanoparticles for cancer hyperthermia", 《JOURNAL OF COLLOID AND INTERFACE SCIENCE》 * |
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