CN104495943A - Preparation method of manganese ferrite nano powder - Google Patents

Preparation method of manganese ferrite nano powder Download PDF

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CN104495943A
CN104495943A CN201410737543.1A CN201410737543A CN104495943A CN 104495943 A CN104495943 A CN 104495943A CN 201410737543 A CN201410737543 A CN 201410737543A CN 104495943 A CN104495943 A CN 104495943A
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microwave
microwave hydrothermal
preparation
ferrite nano
reaction
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CN104495943B (en
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刘桂香
罗庆平
徐光亮
白玉洁
孟平原
李胜男
赖振宇
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Jiangsu Shangshan Environmental Protection Technology Co ltd
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Southwest University of Science and Technology
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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; adding a surface modifier sodium dodecyl benzene sulfonate into the mixed solution 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

A kind of preparation method of Mn ferrite nano-powder
Technical field
The invention belongs to technical field of chemistry and chemical engineering, be specifically related to a kind of preparation method of Mn ferrite nano-powder.
Background technology
Magneticsubstance is one of critical material promoted social development, and is mainstay and the basis of national economy and national defense industry, is widely used in electronic information component field, have broad application prospects in daily life, national defence, military affairs etc.
The develop rapidly of nanosecond science and technology is that the better application of magneticsubstance provides good opportunity.Nanostructured manganese ferrite is the high-quality soft magnetic materials with features such as high saturation and magnetic intensity, high initial permeability, low-coercivities, is widely used in various electronic information, electromagnetic shielding, biological medicine and nucleus magnetic resonance, water treatment and the field such as magnetic resolution, magnetic fluid.Thus the ferritic preparation method of nanostructured manganese receives much concern.
The preparation method of nano oxide powder is a lot, common are: sol-gel method, the precipitator method, microemulsion method, Low Temperature Solid-Phase chemical method, hydrothermal method etc.Wherein the method such as sol-gel method, the precipitator method, microemulsion method, Low Temperature Solid-Phase chemical method can relate to calcination process when preparing Mn ferrite, makes the preparation process of oxide compound complicated.Water heat transfer legal system is low for the temperature of reaction of powder, powder granularity and morphology controllable, and the powder that simultaneously prepared by hydrothermal method has the advantages such as better crystallinity degree, chemical constitution are even, but the reaction times needed for conventional hydrothermal 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 has the advantages 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, specifically implements according to following steps:
Step 1, by MnCl 24H 2o and Fe (NO 3) 39H 2o is dissolved in deionized water and is configured to mixing solutions, wherein, and Mn in this mixed solution 2+concentration be 0.12mol/L;
Add surface-modifying agent Sodium dodecylbenzene sulfonate in step 2, the mixing solutions that obtains in step 1 to dissolve, and mix;
Step 3, ammoniacal liquor is slowly added in the mixing solutions of step 2 gained, regulate the pH value of microwave hydrothermal reaction system; Add in micro-wave diminishing pot by the solution mixing up pH value again, sealing is placed on microwave dissolver, carries out microwave hydrothermal reaction;
After step 4, reaction terminate, stop heating, take out solution, filter, precipitation distilled water and dehydrated alcohol are repeatedly washed rear drying, obtains microwave hydrothermal product, be Mn ferrite nano-powder.
Feature of the present invention is also,
Mn in step 1 in mixing solutions 2+with Fe 3+mol ratio is 1:1.9-1:2.1.
Sodium dodecylbenzene sulfonate and MnCl in step 2 24H 2o and Fe (NO 3) 39H 2the mass ratio of O total 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 conditions is: drying temperature is 65 DEG C-75 DEG C; Time of drying is 1.5h-2.5h.
The invention has the beneficial effects as follows: traditional hydrothermal synthesis method combines with microwave field by the present invention, utilize the dielectric effect of microwave to water to carry out transmission ofenergy, and heat-processed is from material is inner, can produce the thermograde contrary with conventional heat transfer process.The present invention have rate of heating fast, be quick on the draw, be heated evenly, a lot of reaction system had to the advantage accelerating chemical reaction, in preparation evenly, there is unique advantage in the nano-powder of narrow particle size distribution.The present invention adopts microwave-hydrothermal method to synthesize Mn ferrite, shortens the microwave reaction time, avoids calcination process, simplify experimental procedure, finally obtains the Mn ferrite that degree of crystallinity is good, saturation magnetization is higher, coercive force is little.
Accompanying drawing explanation
Fig. 1 is the XRD spectra (T=130 DEG C, t=10min) of products therefrom under the different microwave hydrothermal system pH of the present invention;
The VSM curve (T=130 DEG C, t=10min) of gained Mn ferrite when Fig. 2 is the present invention's difference microwave hydrothermal system pH;
Fig. 3 is the XRD spectra (pH=12, t=10min) of products therefrom under the different microwave hydrothermal temperature of reaction of the present invention;
Fig. 4 is the VSM curve (pH=12, t=10min) of gained Mn ferrite under the different microwave hydrothermal temperature of reaction of the present invention;
Fig. 5 is that the embodiment of the present invention 1 synthesizes MnFe 2o 4sEM photo.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
The invention provides a kind of preparation method of Mn ferrite nano-powder, specifically implement according to following steps:
Step 1, by Mn 2+with Fe 3+mol ratio is 1:1.9-1:2.1, by MnCl 24H 2o and Fe (NO 3) 39H 2o is dissolved in deionized water and is configured to mixing solutions, wherein, and Mn in this mixed solution 2+concentration be 0.12mol/L;
Step 2, in above-mentioned solution, add surface-modifying agent Sodium dodecylbenzene sulfonate, wherein, Sodium dodecylbenzene sulfonate and MnCl 24H 2o and Fe (NO 3) 39H 2the mass ratio of O total amount is 1:100-1:10, dissolves and mixes;
Step 3, be that the ammoniacal liquor of 10wt% slowly adds in the mixing solutions of step 2 gained by concentration, regulate the pH value of microwave hydrothermal reaction system to 9-13; Add in micro-wave diminishing pot by the solution mixing up pH value again, sealing is placed on microwave dissolver, and be warming up to 100 DEG C ~ 145 DEG C and carry out microwave hydrothermal reaction, the reaction times is 8min-12min;
After step 4, reaction terminate, stop heating, take out solution, filter, precipitation distilled water and dehydrated alcohol are repeatedly washed rear drying, obtains microwave hydrothermal product, be Mn ferrite nano-powder, wherein, drying temperature is 65 DEG C-75 DEG C; Time of drying is 1.5h-2.5h.
Adopt microwave heating than conventional hydrothermal method rate of heating faster evenly, efficiency is higher, the reaction times only needs 8-12min, and microwave hydrothermal product is target product Mn ferrite, without the need to high-temperature calcination, simplifies experimental procedure and decreases energy consumption; Microwave hydrothermal reaction environment is a kind of supercritical state, in this condition, raw molecule, ion be Quick Casting under microwave heating action, is conducive to forming a large amount of nucleus instantaneously, thus reduce the granularity of product, finally obtain the little and nano particle of better crystallinity degree of granularity.
MnCl in the present invention 24H 2o, Fe (NO 3) 39H 2o is respectively microwave hydrothermal product MnFe 2o 4mn is provided 2+with Fe 3+; Ammoniacal liquor one side and Mn 2+and Fe 3+reaction generates the intermediate product of Mn ferrite, on the one hand in order to regulate the pH value of microwave reaction system; Sodium dodecylbenzene sulfonate is a kind of surface-modifying agent, and its effect is the MnFe to generating in microwave hydrothermal reaction system 2o 4particle carries out surface modification, stops or weakens the reunion between particle.
Adopt microwave hydrothermal reaction method all can generate ZnO product 80 DEG C ~ 150 DEG C temperature ranges, the product particle size wherein during lesser temps is larger.When microwave hydrothermal reaction system pH value lower than 10 time, the MnFe that degree of crystallinity is good can not be obtained 2o 4nano-powder, as the MnFe of preparation 2o 4the pH value of reaction system too high time, microwave hydrothermal product MnFe can be made 2o 4grain fineness number become large.
The beneficial effect of the Mn ferrite nano-powder that the present invention prepares is described below in conjunction with experimental result:
D/max – RB II type X-ray diffractometer (XRD) is adopted to analyze the thing phase of microwave hydrothermal product; Zeiss, Germany ULTRA55 type field emission scanning electron microscope (SEM) is adopted to observe the pattern of microwave product; The magnetic hysteresis loop of microwave hydrothermal product measured by BKT-4500Z type vibrating sample magnetometer (VSM).
By the grain fineness number of Scherrer formulae discovery microwave hydrothermal product.
1, microwave hydrothermal pH value of reaction system is on the impact of its product property
Microwave hydrothermal temperature be 130 DEG C, soaking time be 10min time, change the XRD spectra of pH value of reaction system gained microwave hydrothermal product and experimental result data as shown in figure 1 and table 1.
When microwave hydrothermal temperature be 130 DEG C, microwave soaking time be 10min time, change the magnetic hysteresis loop of pH value of reaction system gained microwave hydrothermal product and experimental result data as shown in Fig. 2 and table 2.
The grain fineness number of gained microwave hydrothermal product and material phase analysis result during table 1 different pH value
From Fig. 1, table 1, microwave hydrothermal temperature is 130 DEG C, soaking time is under 10min condition, and when microwave hydrothermal pH value of reaction system equals 9, products therefrom is amorphous substance.When pH value of reaction system is at 10-13, microwave hydrothermal product is the Mn ferrite MnFe of Spinel 2o 4, and X-ray diffraction peak shape is sharp-pointed, better crystallinity degree.Through Scherrer formulae discovery, when microwave hydrothermal pH value of reaction system is 10-13, the grain fineness number of gained Spinel Mn ferrite is between 17.4nm-25.7nm.
It can thus be appreciated that, can the Mn ferrite of one-step synthesis Spinel under suitable experiment condition by microwave-hydrothermal method, eliminate general wet chemistry method and first obtain the step that Mn ferrite precursor needs calcining.And the time of microwave-hydrothermal method one-step synthesis Spinel Mn ferrite is short, degree of crystallinity good, grain-size is nano level.
The magnetic parameter of microwave hydrothermal product under table 2 different PH
From Fig. 2, table 2, microwave hydrothermal temperature is 130 DEG C, soaking time is under 10min condition, when microwave hydrothermal pH value of reaction system equals 9, because products therefrom is amorphous substance, so its saturation magnetization is very low, only has 3.34emu.g -1.When pH value of reaction system is at 10-13, the saturation magnetization of the Mn ferrite product of Spinel is greatly improved, and their remanent magnetism and coercive force are also very little.Wherein, as pH=12, the saturation magnetization of Mn ferrite product reaches maximum value 53.56441emu.g -1.
2, microwave hydrothermal temperature of reaction is on the impact of its product property
When microwave hydrothermal pH value of reaction system be 12, soaking time be 10min time, change the XRD spectra of microwave hydrothermal temperature of reaction products therefrom and experimental result data as shown in Fig. 3 and table 3.
When microwave hydrothermal pH value of reaction system be 12, soaking time be 10min time, change the magnetic hysteresis loop of microwave hydrothermal temperature of reaction products therefrom and experimental result data as shown in Fig. 4 and table 4.
Table 3 microwave hydrothermal temperature of reaction is on the impact of product property
From Fig. 3, table 3, microwave hydrothermal pH value of reaction system is 12, soaking time is under 10min condition, and microwave hydrothermal temperature of reaction all a step can generate the Mn ferrite MnFe of Spinel between 100 DEG C-145 DEG C 2o 4, its grain fineness number is between 17.4nm-31nm.Wherein the degree of crystallinity of microwave hydrothermal temperature of reaction gained Spinel Mn ferrite product between 115 DEG C-145 DEG C is good.
The magnetic parameter of gained Mn ferrite under the different microwave hydrothermal temperature of reaction of table 4
From Fig. 4, table 4, microwave hydrothermal pH value of reaction system is 12, soaking time is under 10min condition, microwave hydrothermal temperature of reaction is that the saturation magnetization of gained Mn ferrite between 100 DEG C-145 DEG C is in falling " V " shape, occurring maximum value when microwave hydrothermal temperature of reaction is 130 DEG C, is 53.56441emug -1.Their remanent magnetism and coercive force are also very little.
Embodiment 1
A preparation method for Mn ferrite nano-powder, specifically implements according to following steps:
Step 1, take 1.1875gMnCl 24H 2o, 4.8480gFe (NO 3) 39H 2o is placed in same beaker, the two kinds of salt taken with deionized water dissolving, makes the total amount of solution be 50ml.
Step 2, take 0.2414g Sodium dodecylbenzene sulfonate, be dissolved in the solution configured in step 1.
Step 3, be the ammoniacal liquor instillation step 2 gained solution of 10wt% by concentration under rapid mixing conditions, and regulate its pH value to be 12 with the ammoniacal liquor of this concentration, obtain suspension.
Step 4, step 3 gained suspension load microwave dissolver reaction vessels-micro-wave diminishing pot in, microwave dissolver is put into after sealing, arrange that microwave hydrothermal temperature of reaction is 130 DEG C, the reaction times is 10min, microwave hydrothermal reaction product deionized water and dehydrated alcohol respectively wash twice, filter, then put into baking oven at 70 DEG C of dry 2h, products therefrom is Mn ferrite powder.
Gained MnFe under this reaction conditions 2o 4as shown in Figure 5, the grain fineness number of obtained Mn ferrite powder is 17.4nm to scanning electron photomicrograph, and saturation magnetization is 53.56441emu.g -1, remanent magnetism is 0.73913emu.g -1, coercive force is 6.81553Oe.
Embodiment 2
A preparation method for Mn ferrite nano-powder, specifically implements according to following steps:
Step 1, take 1.1875gMnCl 24H 2o, 4.6056gFe (NO 3) 39H 2o is placed in same beaker, the two kinds of salt taken with deionized water dissolving, makes the total amount of solution be 50ml.
Step 2, take 0.057931g Sodium dodecylbenzene sulfonate, be dissolved in the solution configured in step 1.
Step 3, be the ammoniacal liquor instillation step 2 gained solution of 10wt% by concentration under rapid mixing conditions, and regulate its pH value to be 9 with the ammoniacal liquor of this concentration, obtain suspension.
Step 4, step 3 gained suspension load microwave dissolver reaction vessels-micro-wave diminishing pot in, microwave dissolver is put into after sealing, arrange that microwave hydrothermal temperature of reaction is 100 DEG C, the reaction times is 8min, microwave hydrothermal reaction product deionized water and dehydrated alcohol respectively wash twice, filter, then baking oven is put 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 1.1875gMnCl 24H 2o, 5.0904gFe (NO 3) 39H 2o is placed in same beaker, the two kinds of salt taken with deionized water dissolving, makes the total amount of solution be 50ml.
Step 2, take 0.6278g Sodium dodecylbenzene sulfonate, be dissolved in the solution configured in step 1.
Step 3, be the ammoniacal liquor instillation step 2 gained solution of 10wt% by concentration under rapid mixing conditions, and regulate its pH value to be 13 with the ammoniacal liquor of this concentration, obtain suspension.
Step 4, step 3 gained suspension load microwave dissolver reaction vessels-micro-wave diminishing pot in, microwave dissolver is put into after sealing, arrange that microwave hydrothermal temperature of reaction is 145 DEG C, the reaction times is 12min, microwave hydrothermal reaction product deionized water and dehydrated alcohol respectively wash twice, filter, then put into baking oven at 75 DEG C of dry 2.5h, products therefrom is Mn ferrite powder.

Claims (6)

1. a preparation method for Mn ferrite nano-powder, is characterized in that, specifically implements according to following steps:
Step 1, by MnCl 24H 2o and Fe (NO 3) 39H 2o is dissolved in deionized water and is configured to mixing solutions, wherein, and Mn in this mixed solution 2+concentration be 0.12mol/L;
Add surface-modifying agent Sodium dodecylbenzene sulfonate in step 2, the mixing solutions that obtains in step 1 to dissolve, and mix;
Step 3, ammoniacal liquor is slowly added in the mixing solutions of step 2 gained, regulate the pH value of microwave hydrothermal reaction system; Add in micro-wave diminishing pot by the solution mixing up pH value again, sealing is placed on microwave dissolver, carries out microwave hydrothermal reaction;
After step 4, reaction terminate, stop heating, take out solution, filter, precipitation distilled water and dehydrated alcohol are repeatedly washed rear drying, obtains microwave hydrothermal product, be Mn ferrite nano-powder.
2. the preparation method of Mn ferrite nano-powder according to claim 1, is characterized in that, the Mn in described step 1 in mixing solutions 2+with Fe 3+mol ratio is 1:1.9-1:2.1.
3. the preparation method of Mn ferrite nano-powder according to claim 1, is characterized in that, Sodium dodecylbenzene sulfonate and MnCl in described step 2 24H 2o and Fe (NO 3) 39H 2the mass ratio of O total amount is 1:100-1:10.
4. the preparation method of Mn ferrite nano-powder according to claim 1, is characterized in that, in described step 3, the concentration of ammoniacal liquor is 10wt%; The pH value of described microwave hydrothermal reaction system is 9 ~ 13.
5. the preparation method of Mn ferrite nano-powder according to claim 1, is characterized in that, the condition of described microwave hydrothermal reaction is: temperature is 100 DEG C ~ 145 DEG C; Time is 8min-12min.
6. the preparation method of Mn ferrite nano-powder according to claim 1, is characterized in that, in described step 4, drying conditions is: drying temperature is 65 DEG C-75 DEG C; Time of drying is 1.5h-2.5h.
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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN113511732A (en) * 2021-04-09 2021-10-19 安徽中科索纳新材料科技有限公司 Capacitive deionization selective adsorption electrode, capacitive deionization device and application
CN114105210A (en) * 2021-10-19 2022-03-01 中南大学 Amorphous iron-manganese oxide and preparation and application thereof
CN115448373A (en) * 2022-10-20 2022-12-09 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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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113511732A (en) * 2021-04-09 2021-10-19 安徽中科索纳新材料科技有限公司 Capacitive deionization selective adsorption electrode, capacitive deionization device and application
CN114105210A (en) * 2021-10-19 2022-03-01 中南大学 Amorphous iron-manganese oxide and preparation and application thereof
CN115448373A (en) * 2022-10-20 2022-12-09 横店集团东磁股份有限公司 Preparation method of manganese ferrite material
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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