CN104495943B - Preparation method of manganese ferrite nano powder - Google Patents
Preparation method of manganese ferrite nano powder Download PDFInfo
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Abstract
The invention discloses a preparation method of manganese ferrite nano powder, which is implemented according to the following steps: mixing MnCl2·4H2O and Fe (NO)3)3·9H2Dissolving O in deionized water to prepare a mixed solution; in the above mixed solutionAdding a surface modifier sodium dodecyl benzene sulfonate for dissolving, and uniformly mixing; adjusting the pH value of a microwave hydrothermal reaction system; adding the solution with the adjusted pH value into a microwave digestion tank, sealing and placing the tank in a microwave digestion instrument for microwave hydrothermal reaction; and after the reaction is finished, taking out the solution, filtering, washing the precipitate for multiple times by using distilled water and absolute ethyl alcohol, and drying to obtain a microwave hydrothermal product, namely the manganese ferrite nano powder. According to the invention, the manganese ferrite is synthesized by adopting a microwave hydrothermal method, so that the microwave reaction time is shortened, the calcination process is avoided, the experimental procedures are simplified, and the manganese ferrite with good crystallinity, higher saturation magnetization and small coercive force is finally obtained.
Description
Technical field
The invention belongs to technical field of chemistry and chemical engineering, be specifically related to a kind of system of Mn ferrite nano-powderPreparation Method.
Background technology
Magnetic material is one of critical material promoting social development, and is national economy and national defense industryMainstay and basis, be widely used in electronic information component field, daily life, national defence,The aspects such as military affairs have broad application prospects.
The better application that the develop rapidly of nanosecond science and technology is magnetic material provides good opportunity. NanometerMn ferrite is the high-quality with features such as high saturation and magnetic intensity, high initial permeability, low-coercivitiesSoft magnetic materials, be widely used in various electronic information, electromagnetic shielding, biological medicine and nuclear magnetic resonance,The fields such as water treatment and Magnetic Isolation, magnetic fluid. Thereby the ferritic preparation method of nanostructured manganese enjoys passNote.
The preparation method of nano oxide powder is a lot, common are: sol-gel process, the precipitation method,Microemulsion method, Low Temperature Solid-Phase chemical method, hydro-thermal method etc. Wherein sol-gel process, the precipitation method, micro emulsionThe methods such as liquid method, Low Temperature Solid-Phase chemical method can relate to calcination process in the time preparing Mn ferrite, make oxygenThe preparation process of compound is complicated. Reaction temperature that hydro-thermal method synthetic method is prepared powder is low, powder granularityControlled with pattern, the powder that simultaneously prepared by hydro-thermal method has the advantages such as better crystallinity degree, chemical composition are even,But traditional required reaction time of hydro-thermal method synthetic powder is longer.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of Mn ferrite nano-powder, the method toolThere is the feature that preparation process is simple, chemical time is short.
The technical solution adopted in the present invention is, a kind of preparation method of Mn ferrite nano-powder, toolBody is implemented according to following steps:
Step 1, by MnCl2·4H2O and Fe (NO3)3·9H2O is dissolved in deionized water and configuresBecome mixed solution, wherein, Mn in this mixed liquor2+Concentration be 0.12mol/L;
In step 2, the mixed solution that obtains, add surface modifier DBSA in step 1Sodium dissolves, and mixes;
Step 3, ammoniacal liquor is slowly added in the mixed solution of step 2 gained, regulate microwave hydrothermal reactionThe pH value of system; The solution that mixes up pH value is added in micro-wave diminishing pot, sealing is placed on microwave againCounteract appearance, carries out microwave hydrothermal reaction;
Step 4, reaction finish after, stop heating, take out solution, filter, will precipitate use distilled water withAbsolute ethyl alcohol repeatedly washs rear dry, obtains microwave hydrothermal product, is Mn ferrite nano-powder.
Feature of the present invention is also,
Mn in step 1 in mixed solution2+With Fe3+Mol ratio is 1:1.9-1:2.1.
Neopelex and MnCl in step 22·4H2O and Fe (NO3)3·9H2O is totalThe mass ratio of amount is 1:100-1:10.
In step 3, the concentration of ammoniacal liquor is 10wt%; The pH value of described microwave hydrothermal reaction system is 9～13。
The condition of microwave hydrothermal reaction is: temperature is 100 DEG C～145 DEG C; Time is 8min-12min.
In step 4, drying condition is: baking temperature is 65 DEG C-75 DEG C; Be 1.5h-2.5h drying time.
The invention has the beneficial effects as follows: the present invention combines traditional hydrothermal synthesis method and microwave field,Utilize microwave to carry out energy transmission to the dielectric effect of water, and heating process is from material is inner,Can produce the thermograde contrary with conventional diabatic process. The present invention has that firing rate is fast, reaction spiritQuick, be heated evenly, a lot of reaction systems had advantages of to the chemical reaction of acceleration, preparation evenly,The nano-powder aspect of narrow particle size distribution has unique advantage. The present invention adopts microwave-hydrothermal method syntheticMn ferrite, has shortened the microwave reaction time, has avoided calcination process, has simplified experiment operation,Obtain eventually the Mn ferrite that degree of crystallinity is good, saturation magnetization is higher, coercivity is little.
Brief description of the drawings
Fig. 1 is the XRD spectra (T=130 of products therefrom under the different microwave hydrothermal system pH of the present invention℃，t＝10min)；
The VSM curve of gained Mn ferrite when Fig. 2 is the different microwave hydrothermal system pH of the present invention(T＝130℃，t＝10min)；
Fig. 3 be products therefrom under the different microwave hydrothermal reaction temperatures of the present invention XRD spectra (pH=12,t＝10min)；
Fig. 4 is the VSM curve of gained Mn ferrite under the different microwave hydrothermal reaction temperatures of the present invention(pH＝12，t＝10min)；
Fig. 5 is the synthetic MnFe of the embodiment of the present invention 12O4SEM photo.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in detail.
The invention provides a kind of preparation method of Mn ferrite nano-powder, specifically real according to following stepsExecute:
Step 1, press Mn2+With Fe3+Mol ratio is 1:1.9-1:2.1, by MnCl2·4H2O and Fe (NO3)3·9H2O is dissolved in deionized water and is configured to mixed solution, wherein, and Mn in this mixed liquor2+ConcentrationFor 0.12mol/L;
Step 2, in above-mentioned solution, add surface modifier neopelex, wherein, 12Sodium alkyl benzene sulfonate and MnCl2·4H2O and Fe (NO3)3·9H2The mass ratio of O total amount is1:100-1:10, dissolves and mixes;
Step 3, the ammoniacal liquor that is 10wt% by concentration slowly add in the mixed solution of step 2 gained, adjustThe pH value of joint microwave hydrothermal reaction system is to 9-13; Again the solution that mixes up pH value is added to micro-wave digestionIn tank, sealing is placed on microwave dissolver, and be warming up to 100 DEG C～145 DEG C and carry out microwave hydrothermal reaction,Reaction time is 8min-12min;
Step 4, reaction finish after, stop heating, take out solution, filter, will precipitate use distilled water withAbsolute ethyl alcohol repeatedly washs rear dry, obtains microwave hydrothermal product, is Mn ferrite nano-powder,Wherein, baking temperature is 65 DEG C-75 DEG C; Be 1.5h-2.5h drying time.
Adopt heating using microwave than traditional hydro-thermal method firing rate sooner, more evenly, efficiency is higher, reactionTime only needs 8-12min, and microwave hydrothermal product is target product Mn ferrite, without high temperatureCalcining, has simplified experiment operation and has reduced energy consumption; Microwave hydrothermal reaction environment is a kind of overcritical shapeState, under this state, raw molecule, ion be restructuring fast under microwave heating action, is conducive to winkBetween form a large amount of nucleus, thereby reduce the granularity of product, finally obtain granularity little and better crystallinity degreeNano particle.
MnCl in the present invention2·4H2O、Fe(NO3)3·9H2O is respectively microwave hydrothermal product MnFe2O4Mn is provided2+With Fe3+; Ammoniacal liquor one side and Mn2+And Fe3+Reaction generates the intermediate product of Mn ferrite,On the one hand in order to regulate the pH value of microwave reaction system; Neopelex is a kind of surface modificationAgent, its effect is the MnFe generating in microwave hydrothermal reaction system2O4Particle carries out surface modification,Stop or weaken the reunion between particle.
Adopt microwave hydrothermal reaction method all can generate ZnO product 80 DEG C～150 DEG C temperature ranges, itsProduct granularity when middle lower temperature is larger. When the pH of microwave hydrothermal reaction system value is lower than 10 time,Can not obtain the good MnFe of degree of crystallinity2O4Nano-powder, as the MnFe of preparation2O4Reaction systemPH value when too high, can make microwave hydrothermal product MnFe2O4Grain size become large.
Below in conjunction with experimental result, the useful of Mn ferrite nano-powder that the present invention prepares is describedEffect:
Adopt D/max – RB II type X-ray diffractometer (XRD) to analyze the thing phase of microwave hydrothermal product;Adopt Zeiss, Germany ULTRA55 type field emission scanning electron microscope (SEM) to observe the shape of microwave productLooks; BKT-4500Z type vibrating specimen magnetometer (VSM) is measured the hysteresis curve of microwave hydrothermal product.
Calculate the grain size of microwave hydrothermal product by Scherrer formula.
1, the impact of microwave hydrothermal pH value of reaction system on its product property
Be 130 DEG C, temperature retention time while being 10min in microwave hydrothermal temperature, change pH value of reaction systemThe XRD spectra of gained microwave hydrothermal product and experimental result data are as shown in Fig. 1 and table 1.
When microwave hydrothermal temperature is 130 DEG C, microwave temperature retention time while being 10min, change reaction systemThe hysteresis curve of pH value gained microwave hydrothermal product and experimental result data are as shown in Fig. 2 and table 2.
Grain size and the material phase analysis result of gained microwave hydrothermal product when the different pH value of table 1
From Fig. 1, table 1, microwave hydrothermal temperature is that 130 DEG C, temperature retention time are under 10min condition,In the time that microwave hydrothermal pH value of reaction system equals 9, products therefrom is amorphous substance. Work as reaction systemPH value in the time of 10-13, the Mn ferrite MnFe that microwave hydrothermal product is Spinel2O4, and X penetratesLine diffraction peak shape is sharp-pointed, better crystallinity degree. Calculate microwave hydrothermal pH value of reaction system through Scherrer formulaDuring for 10-13, the grain size of gained Spinel Mn ferrite is between 17.4nm-25.7nm.
Hence one can see that, can one-step synthesis spinelle under suitable experiment condition by microwave-hydrothermal methodThe Mn ferrite of phase, has removed general wet chemistry method from and has first obtained the step that Mn ferrite predecessor need to be calcinedSuddenly. And the time of microwave-hydrothermal method one-step synthesis Spinel Mn ferrite is short, degree of crystallinity good,Crystallite dimension is nanoscale.
The magnetic parameter of microwave hydrothermal product under table 2 different PH
From Fig. 2, table 2, microwave hydrothermal temperature is that 130 DEG C, temperature retention time are under 10min condition,In the time that microwave hydrothermal pH value of reaction system equals 9, because products therefrom is amorphous substance, so it is fullVery low with the intensity of magnetization, only have 3.34emu.g-1. When pH value of reaction system is during at 10-13, point is brilliantThe saturation magnetization of the Mn ferrite product of stone phase is greatly improved, and their remanent magnetism and strongStupid power is also very little. Wherein, in the time of pH=12, the saturation magnetization of Mn ferrite product reaches the utmost pointLarge value 53.56441emu.g-1。
2, the impact of microwave hydrothermal reaction temperature on its product property
When microwave hydrothermal pH value of reaction system is 12, temperature retention time is while being 10min, changes Microwave WaterThe XRD spectra of thermal response temperature products therefrom and experimental result data are as shown in Fig. 3 and table 3.
When microwave hydrothermal pH value of reaction system is 12, temperature retention time is while being 10min, changes Microwave WaterThe hysteresis curve of thermal response temperature products therefrom and experimental result data are as shown in Fig. 4 and table 4.
The impact of table 3 microwave hydrothermal reaction temperature on product property
From Fig. 3, table 3, microwave hydrothermal pH value of reaction system is 12, temperature retention time is 10minUnder condition, microwave hydrothermal reaction temperature all can one between 100 DEG C-145 DEG C step generate the manganese of SpinelFerrite MnFe2O4, its grain size is between 17.4nm-31nm. Wherein microwave hydrothermal reaction temperatureBetween 115 DEG C-145 DEG C, the degree of crystallinity of gained Spinel Mn ferrite product is good.
The magnetic parameter of gained Mn ferrite under the different microwave hydrothermal reaction temperatures of table 4
From Fig. 4, table 4, microwave hydrothermal pH value of reaction system is 12, temperature retention time is 10minUnder condition, microwave hydrothermal reaction temperature is that the saturated magnetization of gained Mn ferrite between 100 DEG C-145 DEG C is strongDegree is down " V " shape, occurs maximum in the time that microwave hydrothermal reaction temperature is 130 DEG C, for53.56441emu·g-1. Their remanent magnetism and coercivity are also very little.
Embodiment 1
A preparation method for Mn ferrite nano-powder, specifically implements according to following steps:
Step 1, take 1.1875gMnCl2·4H2O、4.8480gFe(NO3)3·9H2O is placed inIn same beaker, two kinds of salt that take with deionized water dissolving, the total amount that makes solution is 50ml.
Step 2, take 0.2414g neopelex, be dissolved in configure in step 1 moltenIn liquid.
Step 3, the ammoniacal liquor that is 10wt% by concentration under rapid stirring condition splash into step 2 gained solution,And to regulate its pH value with the ammoniacal liquor of this concentration be 12, obtain suspension.
Step 4, step 3 gained suspension is packed into the reaction vessels-micro-wave diminishing pot of microwave dissolverIn, after sealing, put into microwave dissolver, microwave hydrothermal reaction temperature is set is 130 DEG C, reaction time and be10min, microwave hydrothermal product use deionized water and the each washed twice of absolute ethyl alcohol, filtration, thenPut into baking oven at 70 DEG C of dry 2h, products therefrom is Mn ferrite powder.
Gained MnFe under this reaction condition2O4Scanning electron micrograph as shown in Figure 5, the manganese makingThe grain size of ferrite powder is 17.4nm, and saturation magnetization is 53.56441emu.g-1, remanent magnetism is0.73913emu.g-1, coercivity is 6.81553Oe.
Embodiment 2
A preparation method for Mn ferrite nano-powder, specifically implements according to following steps:
Step 1, take 1.1875gMnCl2·4H2O、4.6056gFe(NO3)3·9H2O is placed inIn same beaker, two kinds of salt that take with deionized water dissolving, the total amount that makes solution is 50ml.
Step 2, take 0.057931g neopelex, be dissolved in and configure in step 1In solution.
Step 3, the ammoniacal liquor that is 10wt% by concentration under rapid stirring condition splash into step 2 gained solution,And to regulate its pH value with the ammoniacal liquor of this concentration be 9, obtain suspension.
Step 4, step 3 gained suspension is packed into the reaction vessels-micro-wave diminishing pot of microwave dissolverIn, after sealing, put into microwave dissolver, microwave hydrothermal reaction temperature is set is 100 DEG C, reaction time and be8min, microwave hydrothermal product use deionized water and the each washed twice of absolute ethyl alcohol, filtration, thenPut into baking oven at 65 DEG C of dry 1.5h, products therefrom is Mn ferrite powder, belongs to amorphous substance.
Embodiment 3
A preparation method for Mn ferrite nano-powder, specifically implements according to following steps:
Step 1, take 1.1875gMnCl2·4H2O、5.0904gFe(NO3)3·9H2O is placed inIn same beaker, two kinds of salt that take with deionized water dissolving, the total amount that makes solution is 50ml.
Step 2, take 0.6278g neopelex, be dissolved in configure in step 1 moltenIn liquid.
Step 3, the ammoniacal liquor that is 10wt% by concentration under rapid stirring condition splash into step 2 gained solution,And to regulate its pH value with the ammoniacal liquor of this concentration be 13, obtain suspension.
Step 4, step 3 gained suspension is packed into the reaction vessels-micro-wave diminishing pot of microwave dissolverIn, after sealing, put into microwave dissolver, microwave hydrothermal reaction temperature is set is 145 DEG C, reaction time and be12min, microwave hydrothermal product use deionized water and the each washed twice of absolute ethyl alcohol, filtration, thenPut into baking oven at 75 DEG C of dry 2.5h, products therefrom is Mn ferrite powder.
Claims (1)
1. a preparation method for Mn ferrite nano-powder, is characterized in that, specifically according toLower step is implemented:
Step 1, by MnCl2·4H2O and Fe (NO3)3·9H2O is dissolved in deionized water and configuresBecome mixed solution, wherein, Mn in this mixed liquor2+Concentration be 0.12mol/L, Mn2+With Fe3+Mol ratio is 1:1.9-1:2.1;
In step 2, the mixed solution that obtains, add surface modifier dodecyl in step 1Benzene sulfonic acid sodium salt dissolves, and mixes neopelex and MnCl2·4H2O andFe(NO3)3·9H2The mass ratio of O total amount is 1:100-1:10;
Step 3, ammoniacal liquor is slowly added in the mixed solution of step 2 gained, regulate Microwave WaterThe pH value of thermal response system; Again the solution that mixes up pH value is added in micro-wave diminishing pot, closeBe honored as a queen and be placed in microwave dissolver, carry out microwave hydrothermal reaction; The concentration of ammoniacal liquor is 10wt%;The pH value of described microwave hydrothermal reaction system is 9～13; The bar of described microwave hydrothermal reactionPart is: temperature is 100 DEG C～145 DEG C; Time is 8min-12min;
After step 4, reaction finish, stop heating, take out solution, filter, will precipitate with steamingHeat up in a steamer water and absolute ethyl alcohol and repeatedly wash rear being dried, obtain microwave hydrothermal product, be Mn ferriteNano-powder; Drying condition is: baking temperature is 65 DEG C-75 DEG C; Be drying time1.5h-2.5h。
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| CN114105210B (en) * | 2021-10-19 | 2023-03-24 | 中南大学 | Amorphous iron-manganese oxide and preparation and application thereof |
| CN115448373B (en) * | 2022-10-20 | 2024-03-05 | 横店集团东磁股份有限公司 | Preparation method of manganese ferrite material |
| CN115838187A (en) * | 2022-12-14 | 2023-03-24 | 西安超磁纳米生物科技有限公司 | Microwave-assisted organic phase ultra-small ferrite nano-particles and preparation method thereof |
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