CN103482709A - High-power ultrasound assisted controllable preparation method of nanoscale Fe3O4 powder - Google Patents

High-power ultrasound assisted controllable preparation method of nanoscale Fe3O4 powder Download PDF

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CN103482709A
CN103482709A CN201310404175.4A CN201310404175A CN103482709A CN 103482709 A CN103482709 A CN 103482709A CN 201310404175 A CN201310404175 A CN 201310404175A CN 103482709 A CN103482709 A CN 103482709A
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solution
naoh
fecl
preparation
powder
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于成龙
高丹鹏
郝欣
王斐
赵美娜
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a high-power ultrasound assisted controllable preparation method of nanoscale Fe3O4 powder. The method comprises the steps of respectively dissolving FeCl2 and NaOH into distilled water, and then, forming a FeCl2 solution and a NaOH solution; slowly dripping the FeCl2 solution into the NaOH solution so as to form a mixed solution, and carrying out magnetic stirring on the NaOH solution; processing the obtained mixed solution by using high-power ultrasound waves in an assisting manner until the mixed solution is light green; transferring the solution into a hydrothermal kettle for heat preservation; adding distilled water into a precipitate for flushing, carrying out centrifugation so as to obtain precipitates, and drying the precipitates, thereby obtaining nanoscale Fe3O4 powder. The method has the advantages that the operation is simple and convenient, the required raw materials are easily obtained, the synthesis cost is relatively low, the nucleating and growing processes are controllable, the degree of crystallinity of grains is high, the purity of a sample phase is high, and the grain size of the grains is relatively uniform.

Description

A kind of large power supersonic aided nano level Fe 3o 4the controllable method for preparing of powder
[technical field]
The invention belongs to wet chemistry method and prepare the nano-powder technical field, be specifically related to a kind of large power supersonic aided nano level Fe 3o 4the controllable method for preparing of powder.
[background technology]
Fe 3o 4it is a kind of well behaved ferrimagnetic material, owing to thering is biocompatibility, make it can be applicable to the biomedicine fields such as gene isolation, medicine directional transmissions, it also has unique electricity and magnetic performance, at aspects such as magnetic device, microwave material, magnetic inks, is widely used.
The Fe reported at present 3o 4the preparation method all can obtain thinner particle, but still can not obtain satisfied result aspect the controllability of simplifying preparation technology and nucleating growth.As, the people such as Y.Y.Zheng are with Fe (NO 3) 24H 2o, Fe (NO 3) 39H 2o is raw material, adopts hydrothermal method to prepare Fe 3o 4.Fixedly PEG concentration is 1.0 * 10 -3mol/L, Fe 2+, Fe 3+concentration is respectively 0.1mol/L and 0.2mol/L, has obtained the Fe of 30nm 3o 4nano particle.Chinese patent is announced a kind of reported synthesizing porous Fe 3 O 4 magnetic microballoon for No. CN102502877A method.It is raw material that the method be take ferrous ion, ferric ion salt, and urea is alkaline precipitating agent, and polyvinyl alcohol and acetic acid are stablizer, in the aqueous solution, with N under 80 ℃ of-95 ℃ of conditions 2protective reaction 20h-72h, the magnetic ferroferric oxide microballoon of formation porous.In above method, due to divalent iron salt (Fe 2+) very easily oxidized, want to obtain purer ferriferrous oxide particles, every batch sample preparation all needs to demarcate divalent iron salt concentration, and with trivalent iron salt mixing process in need N 2as shielding gas, cause the operating process complexity, production cost is high, is unfavorable for scale operation.
Reference:
Y.Y.Zheng,X.B.Wang,C.L.Li,et?al.Fabrication?of?shape?controlled?Fe 3O 4nanostructure[J].Materials?Characterization,2010,61:489-492.
Yan Husheng, etc. a kind of method of simple synthesizing porous Fe 3 O 4 magnetic microballoon. Chinese invention patent, CN102502877A, 2011.
[summary of the invention]
The purpose of this invention is to provide a kind of large power supersonic aided nano level Fe 3o 4the controllable method for preparing of powder, solved nucleation and the uncontrollable problem of growth, the nano-sized particles of preparing, and size distribution is very narrow, and phase purity is higher.
Concrete grammar of the present invention is as follows:
(1) by FeCl 2be dissolved in respectively in distilled water with NaOH, after dissolving, form the FeCl that concentration is 0.02～0.5mol/L 2the NaOH solution that solution and concentration are 16.00～20.00mol/L;
(2) by the FeCl of step (1) configuration 2solution slowly splashes in the NaOH solution of step (1) configuration and forms mixing solutions, the FeCl added 2solution is 2: 5 with NaOH liquor capacity ratio, in the dropping process, NaOH solution is carried out to magnetic agitation, and it is fully dissolved;
(3) with high-power ultrasonics auxiliary treatment step (2) gained mixing solutions, until mixed solution is light green;
(4) solution that will process through step (3) moves in water heating kettle, and at 120～240 ℃ of temperature, insulation 1-15h generates precipitation;
(5) add distilled water flushing in step (4) gained precipitation, and carry out centrifugal treating, after centrifugally operated completes, supernatant liquid is outwelled, repeatedly clean until supernatant liquid is neutral, be precipitated thing, throw out is carried out to drying, obtain nano level Fe 3o 4powder.
Controlling rate of addition in described step (2) is 0.1～0.5mL/min.
In described step (2), magnetic agitation speed is 600-2000r/min.
In described step (3), ultrasonic power is 120～200W, and ultrasonic frequency is 24～40KHz, and the supersound process time is 10～60min.
In described step (4), the packing ratio of solution in water heating kettle is 20～70%.
In described step (5), the centrifugal treating rotating speed is 8000～12000r/min, and centrifugation time is 5～10min.
In described step (5), the gained throw out, under 80 ℃ of conditions, carries out drying in air atmosphere.
Compared with prior art, the present invention at least has the following advantages:
1) Fe that prepared by the present invention 3o 4powder grows out under hydrothermal condition, and by changing titrating solution concentration and titration speed, nucleation and process of growth are controlled, and the particle crystallization degree is high.
2) adopt FeCl 2more easily generate nano particle as source of iron, use the high-power ultrasonics auxiliary treatment simultaneously, the Fe of formation 3o 4powder granularity is uniformly dispersed, and pattern is controlled.
3) Fe that prepared by the present invention 3o 4powder, technological operation is easy, and desired raw material is easy to get, and synthetic cost is lower.
4) Fe that prepared by the present invention 3o 4powder, sample phase purity is high, and grain graininess is more even, and particle size distribution range concentrates between 30～40nm.
[accompanying drawing explanation]
Fig. 1 is the Fe of example 1 preparation of the present invention 3o 4the X ray diffracting spectrum of powder;
Fig. 2 is the Fe of example 2 preparations of the present invention 3o 4the scanning electron microscope image of powder.
Fig. 3 is the Fe of example 3 preparations of the present invention 3o 4the scanning electron microscope image of powder.
Fig. 4 is with FeSO 47H 2o is Fe prepared by source of iron 3o 4the scanning electron microscope image of powder.
[concrete embodiment]
Below in conjunction with drawings and the specific embodiments, the present invention is described in further detail:
Embodiment 1
1) by FeCl 2be dissolved in respectively in distilled water with NaOH, after dissolving, form the FeCl that concentration is 0.10mol/L 2the NaOH solution that solution and concentration are 17.40mol/L;
2) the FeCl2 solution of step 1) configuration is slowly splashed in the NaOH solution of step 1) configuration to FeCl 2solution is 2: 5 with NaOH liquor capacity ratio, and the control rate of titration is 0.3mL/min.In the time of the dropping process, NaOH solution is carried out to magnetic agitation, the magnetic stirring apparatus rotating speed is controlled as 800r/min, and it is fully dissolved;
3) the use high-power ultrasonics auxiliary treatment step 2) mixing solutions of gained, ultrasonic power is 160W, and ultrasonic frequency is 32KHz, and ultrasonic time is 30min, until mixed solution is light green;
4) solution step 3) obtained moves in the Teflon water heating kettle, and packing ratio is 50%, at 120 ℃ of temperature, and insulation 15h;
5) add distilled water flushing in step 4) gained precipitation, and carry out centrifugal treating, centrifuge speed is 8000r/min, centrifugation time is 10min, after centrifugally operated completes, supernatant liquid is outwelled, and repeatedly cleans 7 times, until supernatant liquid is neutral (pH=7.0～7.5), be precipitated thing;
6) by step 5) gained throw out under 80 ℃ of conditions, carry out drying in air atmosphere, obtain product;
Product is carried out to the identification of phases by X-ray diffraction (XRD) analysis, and field emission scanning electron microscope (FE-SEM) carries out morphology observation, finally obtains nano level, and the Fe of even particle distribution 3o 4, as shown in Figure 1, gained Fe 3o 4the powder average particle size particle size is 36nm.
Embodiment 2
1) by FeCl 2be dissolved in respectively in distilled water with NaOH, after dissolving, form the FeCl that concentration is 0.02mol/L 2the NaOH solution that solution and concentration are 19.60mol/L;
2) by the FeCl of step 1) configuration 2solution slowly splashes in the NaOH solution of step 1) configuration, FeCl 2solution is 2: 5 with NaOH liquor capacity ratio, and the control rate of titration is 0.1mL/min.In the time of the dropping process, NaOH solution is carried out to magnetic agitation, the magnetic stirring apparatus rotating speed is controlled as 1200r/min, and it is fully dissolved;
3) the use high-power ultrasonics auxiliary treatment step 2) mixing solutions of gained, ultrasonic power is 180W, and ultrasonic frequency is 36KHz, and ultrasonic time is 45min, until mixed solution is light green;
4) solution step 3) obtained moves in the Teflon water heating kettle, and packing ratio is 70%, at 200 ℃ of temperature, and insulation 12h;
5) add distilled water flushing in step 4) gained precipitation, and carry out centrifugal treating, centrifuge speed is 10000r/min, centrifugation time is 5min, after centrifugally operated completes, supernatant liquid is outwelled, so repeatedly clean 9 times, until supernatant liquid is neutral (pH=7.0～7.5), be precipitated thing;
6) by step 5) gained throw out under 80 ℃ of conditions, carry out drying in air atmosphere, obtain product;
Product is carried out to the identification of phases by X-ray diffraction (XRD) analysis, and field emission scanning electron microscope (FE-SEM) carries out morphology observation, finally obtains nano level, and the Fe of even particle distribution 3o 4, as shown in Figure 2, gained Fe 3o 4the powder average particle size particle size is 38nm.
Embodiment 3
1) by FeCl 2be dissolved in respectively in distilled water with NaOH, after dissolving, form the FeCl that concentration is 0.05mol/L 2the NaOH solution that solution and concentration are 16.80mol/L;
2) by the FeCl of step 1) configuration 2solution slowly splashes in the NaOH solution of step 1) configuration, FeCl 2solution is 2: 5 with NaOH liquor capacity ratio, and the control rate of titration is 0.5mL/min.In the time of the dropping process, NaOH solution is carried out to magnetic agitation, the magnetic stirring apparatus rotating speed is controlled as 2000r/min, and it is fully dissolved;
3) the use high-power ultrasonics auxiliary treatment step 2) mixing solutions of gained, ultrasonic power is 200W, and ultrasonic frequency is 40KHz, and ultrasonic time is 20min, until mixed solution is light green;
4) solution step 3) obtained moves in the Teflon water heating kettle, and packing ratio is 20%, at 160 ℃ of temperature, and insulation 3h;
5) add distilled water flushing in step 4) gained precipitation, and carry out centrifugal treating, centrifuge speed is 12000r/min, centrifugation time is 7min, after centrifugally operated completes, supernatant liquid is outwelled, so repeatedly clean 8 times, until supernatant liquid is neutral (pH=7.0～7.5), be precipitated thing;
6) by step 5) gained throw out under 80 ℃ of conditions, carry out drying in air atmosphere, obtain product;
Product is carried out to the identification of phases by X-ray diffraction (XRD) analysis, and field emission scanning electron microscope (FE-SEM) carries out morphology observation, finally obtains nano level, and the Fe of even particle distribution 3o 4, as shown in Figure 3, gained Fe 3o 4the powder average particle size particle size is 34nm.
Embodiment 4
1) by FeCl 2be dissolved in respectively in distilled water with NaOH, after dissolving, form the FeCl that concentration is 0.50mol/L 2the NaOH solution that solution and concentration are 18.50mol/L;
2) by the FeCl of step 1) configuration 2solution slowly splashes in the NaOH solution of step 1) configuration, FeCl 2solution is 2: 5 with NaOH liquor capacity ratio, and the control rate of titration is 0.1mL/min.In the time of the dropping process, NaOH solution is carried out to magnetic agitation, the magnetic stirring apparatus rotating speed is controlled as 900r/min, and it is fully dissolved;
3) the use high-power ultrasonics auxiliary treatment step 2) mixing solutions of gained, ultrasonic power is 120W, and ultrasonic frequency is 24KHz, and ultrasonic time is 60min, until mixed solution is light green;
4) solution step 3) obtained moves in the Teflon water heating kettle, and packing ratio is 70%, at 240 ℃ of temperature, and insulation 1h;
5) add distilled water flushing in step 4) gained precipitation, and carry out centrifugal treating, centrifuge speed is 10000r/min, centrifugation time is 8min, after centrifugally operated completes, supernatant liquid is outwelled, so repeatedly clean 10 times, until supernatant liquid is neutral (pH=7.0～7.5), be precipitated thing;
6) by step 5) gained throw out under 80 ℃ of conditions, carry out drying in air atmosphere, obtain product;
Product is carried out to the identification of phases by X-ray diffraction (XRD) analysis, and field emission scanning electron microscope (FE-SEM) carries out morphology observation, finally obtains nano level, and the Fe of even particle distribution 3o 4, average particle size particle size is 41nm.
Embodiment 5
1) by FeCl 2be dissolved in respectively in distilled water with NaOH, after dissolving, form the FeCl that concentration is 0.15mol/L 2the NaOH solution that solution and concentration are 16.00mol/L;
2) by the FeCl of step 1) configuration 2solution slowly splashes in the NaOH solution of step 1) configuration, FeCl 2solution is 2: 5 with NaOH liquor capacity ratio, and the control rate of titration is 0.5mL/min.In the time of the dropping process, NaOH solution is carried out to magnetic agitation, the magnetic stirring apparatus rotating speed is controlled as 600r/min, and it is fully dissolved;
3) the use high-power ultrasonics auxiliary treatment step 2) mixing solutions of gained, ultrasonic power is 140W, and ultrasonic frequency is 28KHz, and ultrasonic time is 15min, until mixed solution is light green;
4) solution step 3) obtained moves in the Teflon water heating kettle, and packing ratio is 40%, at 180 ℃ of temperature, and insulation 6h;
5) add distilled water flushing in step 4) gained precipitation, and carry out centrifugal treating, centrifuge speed is 8000r/min, centrifugation time is 10min, after centrifugally operated completes, supernatant liquid is outwelled, so repeatedly clean 6 times, until supernatant liquid is neutral (pH=7.0～7.5), be precipitated thing;
6) by step 5) gained throw out under 80 ℃ of conditions, carry out drying in air atmosphere, obtain product;
Product is carried out to the identification of phases by X-ray diffraction (XRD) analysis, and field emission scanning electron microscope (FE-SEM) carries out morphology observation, finally obtains nano level, and the Fe3O4 of even particle distribution, and average particle size particle size is 33nm.
Embodiment 6
1) by FeCl 2be dissolved in respectively in distilled water with NaOH, after dissolving, form the FeCl that concentration is 0.5mol/L 2the NaOH solution that solution and concentration are 20.00mol/L;
2) by the FeCl of step 1) configuration 2solution slowly splashes in the NaOH solution of step 1) configuration, FeCl 2solution is 2: 5 with NaOH liquor capacity ratio, and the control rate of titration is 0.5mL/min.In the time of the dropping process, NaOH solution is carried out to magnetic agitation, the magnetic stirring apparatus rotating speed is controlled as 600r/min, and it is fully dissolved;
3) the use high-power ultrasonics auxiliary treatment step 2) mixing solutions of gained, ultrasonic power is 200W, and ultrasonic frequency is 40KHz, and ultrasonic time is 10min, until mixed solution is light green;
4) solution step 3) obtained moves in the Teflon water heating kettle, and packing ratio is 40%, at 220 ℃ of temperature, and insulation 3h;
5) add distilled water flushing in step 4) gained precipitation, and carry out centrifugal treating, centrifuge speed is 8000r/min, centrifugation time is 10min, after centrifugally operated completes, supernatant liquid is outwelled, so repeatedly clean 6 times, until supernatant liquid is neutral (pH=7.0～7.5), be precipitated thing;
6) by step 5) gained throw out under 80 ℃ of conditions, carry out drying in air atmosphere, obtain product;
Can find out in Fig. 4, adopt normally used FeSO 47H 2o etc. are as source of iron, gained Fe 3o 4particle size distribution is inhomogeneous, and powder is easily assembled the formation macrobead.Can be found out by Fig. 2 and Fig. 3, adopt FeCl in the present invention 2for source of iron, the gained particle size distribution is even, and powder dispersity is good, is nanometer Fe 3o 4particle.
Result shows, nanometer rice grain size distribution prepared by the method is narrower, between 30～40nm.As Fig. 1 is the X ray diffracting spectrum of example 1, the X-ray diffraction result shows, the nano-powder phase purity of preparation is higher, and degree of crystallinity is better.

Claims (7)

1. a large power supersonic aided nano level Fe 3o 4the controllable method for preparing of powder, other are characterised in that and comprise the following steps:
(1) by FeCl 2be dissolved in respectively in distilled water with NaOH, after dissolving, form the FeCl that concentration is 0.02～0.5mol/L 2the NaOH solution that solution and concentration are 16.00～20.00mol/L;
(2) by the FeCl of step (1) configuration 2solution slowly splashes in the NaOH solution of step (1) configuration and forms mixing solutions, the FeCl added 2solution is 2: 5 with NaOH liquor capacity ratio, in the dropping process, NaOH solution is carried out to magnetic agitation, and it is fully dissolved;
(3) with high-power ultrasonics auxiliary treatment step (2) gained mixing solutions, until mixed solution is light green;
(4) solution that will process through step (3) moves in water heating kettle, and at 120～240 ℃ of temperature, insulation 1-15h generates precipitation;
(5) add distilled water flushing in step (4) gained precipitation, and carry out centrifugal treating, after centrifugally operated completes, supernatant liquid is outwelled, repeatedly clean until supernatant liquid is neutral, be precipitated thing, throw out is carried out to drying, obtain nano level Fe 3o 4powder.
2. preparation method according to claim 1 is characterized in that: controlling rate of addition in described step (2) is 0.1～0.5mL/min.
3. preparation method according to claim 1 is characterized in that: in described step (2), magnetic agitation speed is 600-2000r/min.
4. preparation method according to claim 1 is characterized in that: in described step (3), ultrasonic power is 120～200W, and ultrasonic frequency is 24～40KHz, and the supersound process time is 10～60min.
5. preparation method according to claim 1 is characterized in that: in described step (4), the packing ratio of solution in water heating kettle is 20～70%.
6. preparation method according to claim 1 is characterized in that: in described step (5), centrifugal rotational speed is 8000～12000r/min, and centrifugation time is 5～10min.
7. preparation method according to claim 1 is characterized in that: in described step (5), the gained throw out, under 80 ℃ of conditions, carries out drying in air atmosphere.
CN201310404175.4A 2013-09-06 2013-09-06 High-power ultrasound assisted controllable preparation method of nanoscale Fe3O4 powder Pending CN103482709A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109455768A (en) * 2018-12-18 2019-03-12 合肥学院 It is a kind of to change the preparation controllable Fe of form using local magnetic field3O4The method of powder
CN115947379A (en) * 2022-12-30 2023-04-11 江苏理工学院 Paramagnetic micron material and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101323466A (en) * 2008-06-24 2008-12-17 杭州师范大学 Preparation of nano-ferriferrous oxide
CN102464358A (en) * 2010-11-05 2012-05-23 中国科学院生态环境研究中心 Ultrasonic auxiliary hydrothermal synthesizing water-soluble square ferrite magnetic nano-material method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101323466A (en) * 2008-06-24 2008-12-17 杭州师范大学 Preparation of nano-ferriferrous oxide
CN102464358A (en) * 2010-11-05 2012-05-23 中国科学院生态环境研究中心 Ultrasonic auxiliary hydrothermal synthesizing water-soluble square ferrite magnetic nano-material method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109455768A (en) * 2018-12-18 2019-03-12 合肥学院 It is a kind of to change the preparation controllable Fe of form using local magnetic field3O4The method of powder
CN115947379A (en) * 2022-12-30 2023-04-11 江苏理工学院 Paramagnetic micron material and preparation method thereof

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Application publication date: 20140101