CN1657490A - Method for preparing cobalt ferrite by co-precipitation method - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 29
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 28
- 239000010941 cobalt Substances 0.000 title claims abstract description 24
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 24
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000000975 co-precipitation Methods 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000000725 suspension Substances 0.000 claims abstract description 26
- 239000002244 precipitate Substances 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 239000002105 nanoparticle Substances 0.000 claims abstract description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000009835 boiling Methods 0.000 claims abstract description 7
- 150000001868 cobalt Chemical class 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 150000002505 iron Chemical class 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 5
- 238000009775 high-speed stirring Methods 0.000 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 229910003321 CoFe Inorganic materials 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 230000005415 magnetization Effects 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical group Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- UAWMFRUMUMAZOE-UHFFFAOYSA-N [Co]=O.[Cl] Chemical group [Co]=O.[Cl] UAWMFRUMUMAZOE-UHFFFAOYSA-N 0.000 claims 1
- 239000002585 base Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 17
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 238000004108 freeze drying Methods 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000004886 process control Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 239000006249 magnetic particle Substances 0.000 description 2
- 238000000593 microemulsion method Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 0 CC*1C(**)*2(C3C)C3C1*2 Chemical compound CC*1C(**)*2(C3C)C3C1*2 0.000 description 1
- 229910020599 Co 3 O 4 Inorganic materials 0.000 description 1
- 229910021094 Co(NO3)2-6H2O Inorganic materials 0.000 description 1
- 229910002518 CoFe2O4 Inorganic materials 0.000 description 1
- 229910016870 Fe(NO3)3-9H2O Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011553 magnetic fluid Substances 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000003921 particle size analysis Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
本发明涉及一种制备纳米钴铁氧体的方法。共沉淀法制备钴铁氧体的方法，其特征是它包括如下步骤：1)按Fe/Co摩尔比为1.8－2.2的比例称取计算量的水溶性铁盐和水溶性钴盐混合溶解在水中，然后在高速搅拌下将碱或酸缓慢倒入，调节溶液pH值至11－13，搅拌30－60min后，形成悬浮液；2)在沸水浴中浸渍；3)去离子水洗，过滤得到褐色沉淀物；4)热处理，形成悬浮液；5)分散，在真空下进行冷冻干燥，得到钴铁氧体纳米颗粒。本发明所制得的纳米钴铁氧体粒径小，且分布范围窄，磁性能良好，容易操作和控制过程。
The invention relates to a method for preparing nano cobalt ferrite. The method for preparing cobalt ferrite by co-precipitation is characterized in that it includes the following steps: 1) weighing the calculated amount of water-soluble iron salt and water-soluble cobalt salt according to the ratio of Fe/Co molar ratio of 1.8-2.2, mixing and dissolving in water, then pour alkali or acid slowly under high-speed stirring, adjust the pH value of the solution to 11-13, and stir for 30-60 minutes to form a suspension; 2) Soak in a boiling water bath; 3) Wash with deionized water and filter to obtain brown precipitate; 4) heat treatment to form a suspension; 5) dispersion and freeze-drying under vacuum to obtain cobalt ferrite nanoparticles. The prepared nano-cobalt ferrite has small particle size, narrow distribution range, good magnetic properties, and easy operation and process control.
Description
技术领域technical field
本发明涉及一种制备纳米钴铁氧体的方法。The invention relates to a method for preparing nano cobalt ferrite.
背景技术Background technique
近年来，由于尖晶石纳米铁氧体具有良好的电磁性质并广泛的应用于信息存储系统，医疗诊断技术，磁流体技术，磁致热和致冷作用，因此，人们对这方面的研究也越来越关注。其中钴铁氧体CoFe2O4具有高的磁晶各向异性，高的矫顽力和磁饱和强度而引起广大研究者的兴趣。In recent years, because spinel nano-ferrite has good electromagnetic properties and is widely used in information storage systems, medical diagnostic technology, magnetic fluid technology, magneto-caloric and refrigeration effects, people's research on this aspect is also growing concern. Among them, cobalt ferrite CoFe 2 O 4 has high magnetocrystalline anisotropy, high coercive force and magnetic saturation strength, which has attracted the interest of many researchers.
目前，合成CoFe2O4纳米颗粒的方法有很多种。Pileni等人利用O/W(水包油型)胶态粒子合成2-5nm的钴铁氧体，Shah和Ahn采用W/O(油包水型)微乳液法通过热处理分别合成了粒径为50nm和4.9nm的纳米颗粒；另外，Morais等人在95℃的水溶液中，通过控制搅拌速率来控制纳米颗粒的尺寸；Rajendrain等人证明了在室温下水溶液中共沉淀Fe3+和Co2+合成粒径为6-20nm的钴铁氧体纳米颗粒；J.Ding将Co3O4和Fe3O4混合球磨后煅烧到700℃以上得到钴铁氧体纳米颗粒。虽然通过微乳液法制备的纳米颗粒比在水溶液中采用化学共沉淀法能更好地控制颗粒的粒径。但是，由于在微乳液中表面活性剂包裹在铁氧体纳米颗粒外面很难去除，而影响到磁性材料的应用。Currently, there are many ways to synthesize CoFe2O4 nanoparticles. Pileni et al. used O/W (oil-in-water type) colloidal particles to synthesize 2-5nm cobalt ferrite, and Shah and Ahn used W/O (water-in-oil type) microemulsion method to synthesize the particle size by heat treatment respectively. 50nm and 4.9nm nanoparticles; In addition, Morais et al. controlled the size of the nanoparticles by controlling the stirring rate in aqueous solution at 95 °C; Rajendrain et al. demonstrated the co-precipitation of Fe3 + and Co2 + synthesis in aqueous solution at room temperature Cobalt ferrite nanoparticles with a particle size of 6-20nm; J. Ding mixed Co 3 O 4 and Fe 3 O 4 by ball milling and calcined to above 700°C to obtain cobalt ferrite nanoparticles. Although the nanoparticles prepared by the microemulsion method can better control the particle size than the chemical co-precipitation method in aqueous solution. However, it is difficult to remove the surfactant wrapped around the ferrite nanoparticles in the microemulsion, which affects the application of magnetic materials.
[专利文献]：[Patent Document]:
1.国别：中国 分类号：CO4B35/26；CO4B35/32；CO1G51/00；HO1F1/44；申请日：2002.09.29 公开日：2003.04.30 申请号：02133864.7。1. Country: China Classification number: CO4B35/26; CO4B35/32; CO1G51/00; HO1F1/44; Application date: 2002.09.29 Publication date: 2003.04.30 Application number: 02133864.7.
2.国别：中国 分类号：CO4B35/38 申请日：1994.12.26 公开日：1995.09.06，申请号：94114251.5。2. Country: China Classification number: CO4B35/38 Application date: 1994.12.26 Publication date: 1995.09.06, application number: 94114251.5.
发明内容Contents of the invention
本发明的目的是提供一种粒径小、磁性能好的共沉淀法制备钴铁氧体的方法，该方法避免了表面活性剂对纳米钴铁氧体磁性颗粒表面的影响，有利于纳米钴铁氧体磁性材料的应用。The purpose of the present invention is to provide a method for preparing cobalt ferrite by co-precipitation method with small particle size and good magnetic properties, which avoids the influence of surfactant on the surface of nano-cobalt ferrite magnetic particles, and is beneficial to Application of ferrite magnetic materials.
为了实现上述目的，本发明的技术方案是：共沉淀法制备钴铁氧体的方法，其特征是它包括如下步骤：In order to achieve the above object, the technical scheme of the present invention is: the method for preparing cobalt ferrite by co-precipitation method is characterized in that it comprises the steps:
1).首先按Fe/Co摩尔比为1.8-2.2的比例称取计算量的水溶性铁盐和水溶性钴盐混合溶解在水中，在搅拌条件下，配制成水溶性铁盐浓度为0.5-1.0M和水溶性钴盐浓度为0.23-0.56M的混合溶液，然后在高速搅拌下将碱或酸缓慢倒入，高速搅拌速度为2500-3500r/min，调节溶液pH值至11-13，搅拌30-60min后，形成悬浮液A；1). First, weigh the calculated amount of water-soluble iron salt and water-soluble cobalt salt according to the ratio of Fe/Co molar ratio of 1.8-2.2, mix and dissolve them in water, and prepare the water-soluble iron salt with a concentration of 0.5- A mixed solution of 1.0M and water-soluble cobalt salt with a concentration of 0.23-0.56M, then pour the alkali or acid slowly under high-speed stirring, the high-speed stirring speed is 2500-3500r/min, adjust the pH value of the solution to 11-13, stir After 30-60min, a suspension A is formed;
2).将步骤1)得到的悬浮液A在沸水浴中浸渍1-3小时，得到沉淀物；2). Soak the suspension A obtained in step 1) in a boiling water bath for 1-3 hours to obtain a precipitate;
3).将步骤2)得到的沉淀物用去离子水水洗10-20次，直至pH为6-8为止，过滤得到褐色沉淀物；3). Wash the precipitate obtained in step 2) with deionized water for 10-20 times until the pH is 6-8, and filter to obtain a brown precipitate;
4).将步骤3)得到的褐色沉淀物在90-110℃热处理1-3小时，冷却后加蒸馏水搅拌形成悬浮液B；4). Heat-treat the brown precipitate obtained in step 3) at 90-110° C. for 1-3 hours, add distilled water after cooling and stir to form a suspension B;
5).将步骤4)得到的悬浮液B在强力超声清洗仪中分散30-60min后，置于低温冰箱中冷冻，待成冰后，在真空下进行冷冻干燥，得到CoFe2O4纳米颗粒。5). After dispersing the suspension B obtained in step 4) for 30-60 minutes in a powerful ultrasonic cleaner, place it in a low-temperature refrigerator and freeze it. After it becomes ice, freeze-dry it under vacuum to obtain CoFe 2 O 4 nanoparticles .
所述的水溶性铁盐，可以是氯化铁、硝酸铁中的一种。The water-soluble iron salt can be one of ferric chloride and ferric nitrate.
所述的水溶性钴盐，可以是氯化钴、硝酸钴中的一种。The water-soluble cobalt salt can be one of cobalt chloride and cobalt nitrate.
所述的碱可以是NaOH、KOH、NH4OH中的一种。The alkali may be one of NaOH, KOH, NH 4 OH.
所述的酸可以是HNO3、HCl中的一种。The acid may be one of HNO 3 and HCl.
本发明的特点是：避免表面活性剂对纳米磁性颗粒表面的影响，有利于铁氧体磁性能在生物医学发面的应用；合成的颗粒较小，在10-14nm，且分布范围窄，磁性能良好，饱和磁化强度为44-50emu/g，剩余磁化强度为20-23emu/g；工艺简单，便于操作和控制。The characteristics of the present invention are: avoiding the influence of surfactant on the surface of nano-magnetic particles, which is beneficial to the application of ferrite magnetic properties in biomedicine; the synthesized particles are small, at 10-14nm, and the distribution range is narrow, and the magnetic The performance is good, the saturation magnetization is 44-50emu/g, and the residual magnetization is 20-23emu/g; the process is simple, easy to operate and control.
附图说明Description of drawings
图1为本发明的流程图；Fig. 1 is a flowchart of the present invention;
图2为100℃热处理后CoFe2O4的X射线衍射图谱图；Figure 2 is the X-ray diffraction pattern of CoFe 2 O 4 after heat treatment at 100°C;
图3为100℃热处理后CoFe2O4的磁滞回线图；Figure 3 is the hysteresis loop diagram of CoFe 2 O 4 after heat treatment at 100°C;
图4为100℃热处理后CoFe2O4的透射电镜图；Figure 4 is a transmission electron microscope image of CoFe 2 O 4 after heat treatment at 100°C;
图5为100℃热处理后CoFe2O4的激光粒度分析分布情况图。Fig. 5 is a laser particle size analysis distribution diagram of CoFe 2 O 4 after heat treatment at 100°C.
具体的实施方法specific implementation method
实施例1：Example 1:
共沉淀法制备钴铁氧体的方法，如图1所示，步骤如下：Co-precipitation method prepares the method for cobalt ferrite, as shown in Figure 1, and the steps are as follows:
1).称取21.6gFeCl3·6H2O(0.08mol)和9.5gCoCl2·6H2O(0.04mol)溶解在120ml的蒸馏水中，Fe/Co摩尔比为2.0，搅拌得到混合溶液，然后在高速(3500r/min)搅拌下将浓度为6.0M的NaOH溶液缓慢倒入，调节溶液pH值至12.0，搅拌30min后，形成悬浮液A；1). Weigh 21.6g FeCl 3 6H 2 O (0.08mol) and 9.5g CoCl 2 6H 2 O (0.04mol) and dissolve them in 120ml of distilled water, the Fe/Co molar ratio is 2.0, stir to obtain a mixed solution, and then Slowly pour the NaOH solution with a concentration of 6.0M under high-speed (3500r/min) stirring, adjust the pH value of the solution to 12.0, and stir for 30 minutes to form a suspension A;
2).将步骤1)得到的悬浮液A在沸水浴中浸渍2小时，得到沉淀物；2). Soak the suspension A obtained in step 1) in a boiling water bath for 2 hours to obtain a precipitate;
3).将步骤2)得到的沉淀物用去离子水水洗15次，直至pH为7.0为止，过滤得到褐色沉淀物；3). Wash the precipitate obtained in step 2) with deionized water for 15 times until the pH is 7.0, and filter to obtain a brown precipitate;
4).将步骤3)得到的褐色沉淀物在100℃热处理2小时，冷却后加蒸馏水搅拌形成悬浮液B；4). Heat-treat the brown precipitate obtained in step 3) at 100°C for 2 hours, add distilled water after cooling and stir to form a suspension B;
5).将步骤4)得到的悬浮液B在强力超声清洗仪中分散45min后，置于低温冰箱中冷冻，待成冰后，在真空下进行冷冻干燥，将得到的颗粒进行X-射线衍射分析如图2所示为CoFe2O4。由图4的统计和图5激光粒度分析仪的分析，制得的CoFe2O4平均粒径为12nm。图3可知该钴铁氧体颗粒的饱和磁化强度为46.6emu/g，剩余磁化强度为21.3emu/g。5). After dispersing the suspension B obtained in step 4) in a powerful ultrasonic cleaner for 45 minutes, place it in a low-temperature refrigerator and freeze it. After it becomes ice, perform freeze-drying under vacuum, and perform X-ray diffraction on the obtained particles The analysis is shown in Figure 2 as CoFe 2 O 4 . According to the statistics in Figure 4 and the analysis of the laser particle size analyzer in Figure 5, the average particle size of the prepared CoFe 2 O 4 is 12nm. It can be seen from FIG. 3 that the saturation magnetization of the cobalt ferrite particles is 46.6 emu/g, and the residual magnetization is 21.3 emu/g.
实施例2：Example 2:
共沉淀法制备钴铁氧体的方法，如图1所示，步骤如下：Co-precipitation method prepares the method for cobalt ferrite, as shown in Figure 1, and the steps are as follows:
1).称取19.44gFeCl3·6H2O(0.072mol)和9.5gCoCl2·6H2O(0.04mol)溶解在100ml的蒸馏水中，Fe/Co摩尔比为1.8，搅拌得到混合溶液，然后在高速(2500r/min)搅拌下将浓度为5.0M的KOH溶液缓慢倒入，调节溶液pH值至13.0，搅拌30min后，形成悬浮液A；1). Weigh 19.44g FeCl 3 6H 2 O (0.072mol) and 9.5g CoCl 2 6H 2 O (0.04mol) and dissolve them in 100ml of distilled water, the molar ratio of Fe/Co is 1.8, stir to obtain a mixed solution, and then Slowly pour the KOH solution with a concentration of 5.0M under high-speed (2500r/min) stirring, adjust the pH value of the solution to 13.0, and form a suspension A after stirring for 30 minutes;
2).将步骤1)得到的悬浮液A在沸水浴中浸渍3小时，得到沉淀物；2). Soak the suspension A obtained in step 1) in a boiling water bath for 3 hours to obtain a precipitate;
3).将步骤2)得到的沉淀物用去离子水水洗10次，直至pH为8.0为止，过滤得到褐色沉淀物；3). Wash the precipitate obtained in step 2) with deionized water for 10 times until the pH is 8.0, and filter to obtain a brown precipitate;
4).将步骤3)得到的褐色沉淀物在100℃热处理3小时，冷却后加蒸馏水搅拌形成悬浮液B；4). Heat-treat the brown precipitate obtained in step 3) at 100°C for 3 hours, add distilled water after cooling and stir to form a suspension B;
5).将步骤4)得到的悬浮液B在强力超声清洗仪中分散30min后，置于低温冰箱中冷冻，待成冰后，在真空下进行冷冻干燥，在真空下进行冷冻干燥，制得的CoFe2O4平均粒径为11nm。颗粒的饱和磁化强度为49.8emu/g，剩余磁化强度为22.8emu/g。5). After dispersing the suspension B obtained in step 4) for 30 minutes in a powerful ultrasonic cleaner, place it in a low-temperature refrigerator to freeze, and after it is frozen, freeze-dry it under vacuum, and then freeze-dry it under vacuum to obtain The average particle size of CoFe 2 O 4 is 11nm. The saturation magnetization of the particles was 49.8 emu/g, and the residual magnetization was 22.8 emu/g.
实施例3：Example 3:
共沉淀法制备钴铁氧体的方法，如图1所示，步骤如下：Co-precipitation method prepares the method for cobalt ferrite, as shown in Figure 1, and the steps are as follows:
1).称取23.76gFeCl3·6H2O(0.088mol)和9.5gCoCl2·6H2O(0.04mol)溶解在150ml的蒸馏水中，Fe/Co摩尔比为2.2，搅拌得到混合溶液，然后在高速(3500r/min)搅拌下将氨水缓慢倒入，调节溶液pH值至11.0，搅拌60min后，形成悬浮液A；1). Weigh 23.76g FeCl 3 6H 2 O (0.088mol) and 9.5g CoCl 2 6H 2 O (0.04mol) and dissolve them in 150ml of distilled water, the Fe/Co molar ratio is 2.2, stir to obtain a mixed solution, and then Slowly pour ammonia water under high-speed (3500r/min) stirring, adjust the pH value of the solution to 11.0, and form suspension A after stirring for 60 minutes;
2).将步骤1)得到的悬浮液A在沸水浴中浸渍1小时，得到沉淀物；2). Soak the suspension A obtained in step 1) in a boiling water bath for 1 hour to obtain a precipitate;
3).将步骤2)得到的沉淀物用去离子水水洗20次，直至pH为6.0为止，过滤得到褐色沉淀物；3). Wash the precipitate obtained in step 2) with deionized water for 20 times until the pH is 6.0, and filter to obtain a brown precipitate;
4).将步骤3)得到的褐色沉淀物在100℃热处理1小时，冷却后加蒸馏水搅拌形成悬浮液B；4). Heat-treat the brown precipitate obtained in step 3) at 100°C for 1 hour, add distilled water after cooling and stir to form a suspension B;
5).将步骤4)得到的悬浮液B在强力超声清洗仪中分散60min后，置于低温冰箱中冷冻，待成冰后，在真空下进行冷冻干燥，在真空下进行冷冻干燥，制得的CoFe2O4平均粒径为13nm。颗粒的饱和磁化强度为44.3emu/g，剩余磁化强度为20.1emu/g。5). After dispersing the suspension B obtained in step 4) in a powerful ultrasonic cleaner for 60 minutes, place it in a low-temperature refrigerator to freeze, and after it becomes ice, freeze-dry it under vacuum, and then freeze-dry it under vacuum to obtain The average particle size of CoFe 2 O 4 is 13nm. The saturation magnetization of the particles was 44.3 emu/g, and the residual magnetization was 20.1 emu/g.
实施例4：Example 4:
共沉淀法制备钴铁氧体的方法，如图1所示，步骤如下：Co-precipitation method prepares the method for cobalt ferrite, as shown in Figure 1, and the steps are as follows:
1).称取32.32gFe(NO3)3·9H2O(0.08mol)和11.64gCo(NO3)2·6H2O(0.04mol)溶解在120ml的蒸馏水中，Fe/Co摩尔比为2.0，搅拌得到混合溶液，然后在高速(3500r/min)搅拌下将浓度为6.0M的NaOH溶液缓慢倒入，调节溶液pH值至12.0，搅拌30min后，形成悬浮液A；1). Weigh 32.32g Fe(NO 3 ) 3 9H 2 O (0.08mol) and 11.64g Co(NO 3 ) 2 6H 2 O (0.04mol) and dissolve them in 120ml of distilled water, the Fe/Co molar ratio is 2.0 , stirred to obtain a mixed solution, then slowly poured the NaOH solution with a concentration of 6.0M under high-speed (3500r/min) stirring, adjusted the pH value of the solution to 12.0, and stirred for 30min to form a suspension A;
2).将步骤1)得到的悬浮液A在沸水浴中浸渍2小时，得到沉淀物；2). Soak the suspension A obtained in step 1) in a boiling water bath for 2 hours to obtain a precipitate;
3).将步骤2)得到的沉淀物用去离子水水洗15次，直至pH为7.0为止，过滤得到褐色沉淀物；3). Wash the precipitate obtained in step 2) with deionized water for 15 times until the pH is 7.0, and filter to obtain a brown precipitate;
4).将步骤3)得到的褐色沉淀物在100℃热处理2小时，冷却后加蒸馏水搅拌形成悬浮液B；4). Heat-treat the brown precipitate obtained in step 3) at 100°C for 2 hours, add distilled water after cooling and stir to form a suspension B;
5).将步骤4)得到的悬浮液B在强力超声清洗仪中分散45min后，置于低温冰箱中冷冻，待成冰后，在真空下进行冷冻干燥，制得的CoFe2O4纳米颗粒平均粒径为13nm。颗粒的饱和磁化强度为47.3emu/g，剩余磁化强度为21.9emu/g。5). After dispersing the suspension B obtained in step 4) in a powerful ultrasonic cleaner for 45 minutes, place it in a low-temperature refrigerator and freeze it. After ice formation, freeze-dry it under vacuum to obtain CoFe 2 O 4 nanoparticles The average particle diameter is 13nm. The saturation magnetization of the particles was 47.3 emu/g, and the residual magnetization was 21.9 emu/g.
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| CN100336732C (en) * | 2006-04-13 | 2007-09-12 | 上海交通大学 | Microwave synthetic method for water soluble magnetic cobalt-ferrite CoFe2O4 nano crystal |
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| CN100336732C (en) * | 2006-04-13 | 2007-09-12 | 上海交通大学 | Microwave synthetic method for water soluble magnetic cobalt-ferrite CoFe2O4 nano crystal |
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