CN102491428A - Method for preparing hexagonal BeFe12O19 (barium ferrite) magnetic nano powder by microwave-hydrothemal method - Google Patents

Method for preparing hexagonal BeFe12O19 (barium ferrite) magnetic nano powder by microwave-hydrothemal method Download PDF

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CN102491428A
CN102491428A CN2011103631007A CN201110363100A CN102491428A CN 102491428 A CN102491428 A CN 102491428A CN 2011103631007 A CN2011103631007 A CN 2011103631007A CN 201110363100 A CN201110363100 A CN 201110363100A CN 102491428 A CN102491428 A CN 102491428A
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microwave
nano powder
magnetic nano
hydrothermal
befe
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蒲永平
石轩
刘丹
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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 provides a method for preparing hexagonal BeFe12O19 (barium ferrite) magnetic nano powder by a microwave-hydrothemal method, which includes the steps of utilizing iron nitrate nonahydrate and barium nitrate as precursors to be dissolved in deionized water; then dropwise adding sodium hydroxide into liquor and adjusting pH (potential of hydrogen) within the range from 9 to 14 so that uniform precursor liquor is generated; pouring the precursor liquor into a hydrothermal reaction kettle prior to sealing; and performing microwave-hydrothermal synthesis for the hydrothermal reaction kettle placed in a microwave digestion system prior to cooling the reaction kettle to the room temperature, scrubbing products with deionized water and absolute ethyl alcohol for several times and calcining the scrubbed products at the temperature ranging from 800 DEG C to 1000 DEG C so that the hexagonal BeFe12O19 magnetic nano powder is obtained. The method for preparing the hexagonal BeFe12O19 magnetic nano powder by the microwave-hydrothemal method is low in preparing cost, simple in operation, short in reaction period and high in purity after the products are calcined, and crystal grains are complete in growth and uniform in distribution.

Description

A kind of microwave-hydrothermal method prepares hexagonal BeFe 12O 19The method of magnetic nano powder
Technical field
The present invention relates to a kind of preparation method of nano-magnetic powder, particularly a kind of microwave-hydrothermal method prepares hexagonal BeFe 12O 19The method of magnetic nano powder.
Background technology
GP 500 (the BeFe of Magnetoplumbate-type 12O 19) be a kind of ferromagnetic material with hex crystal structure; Monadic magnetocrystalline anisotropy with good chemicalstability and erosion resistance; The c axle is easy to magnetization; Have bigger coercive force and magnetic energy product, obtained to use widely mainly as magnetic recording material, absorbing material and permanent magnet material etc.
In recent years, along with the particularly continuous development of nanosecond science and technology of Materials science, the performance of Ferrite Material has had very big improving.Because nano material has special surface effects, volume effect and quantum tunneling effect, significant for the further research of this type nanoparticle magnetic properties with application, so the exploitation of ferrite nano powder is more and more paid attention to.The performance of GP 500 is with its purity, particle shape, state of aggregation, particle size and distribute relevant.Therefore, hope to obtain as far as possible little particle size, narrow size distribution and en plaque particle.Particle diameter is little in order to obtain, homogeneous, the better dispersed and GP 500 that has excellent magnetic characteristics, has adopted chemical precipitation method, sol-gel method, hydrothermal method in succession, has spread method and molten-salt growth method etc. certainly.Above method or complicated operation perhaps are exactly complex process, and the cycle is long, poor repeatability.
Summary of the invention
Technical problem to be solved by this invention provide a kind of simple to operate, grain-size is little, crystal grain is grown complete, even particle size distribution and the higher microwave-hydrothermal method of purity prepares hexagonal BeFe 12O 19The method of magnetic nano powder.
For realizing above-mentioned purpose, the invention provides a kind of microwave-hydrothermal method and prepare hexagonal BeFe 12O 19The method of magnetic nano powder is a precursor with nine water iron nitrates and nitrate of baryta, is dissolved in the deionized water, and regulator solution pH is 9～14 then, forms uniform precursor liquid; Precursor liquid is poured in the hydrothermal reaction kettle and sealing, put then into to carry out microwave hydrothermal in the microwave dissolver synthetic, be cooled to room temperature, product with deionized water and absolute ethanol washing neutrality extremely, is promptly got 800～1000 ℃ of calcinings at last.
As the preferred embodiments of the present invention, after said nine water iron nitrates and nitrate of baryta were dissolved in the deionized water, its concentration was respectively 0.06～0.1mol/L and 0.01mol/L;
As the preferred embodiments of the present invention, said nine water iron nitrates and nitrate of baryta are dissolved in the iron nitrate solution of back formation in the deionized water and the ratio of the Ba/Fe mole in the nitrate of baryta solution is 1: (6～10);
As the preferred embodiments of the present invention, the compactedness of said hydrothermal reaction kettle is 40%;
As the preferred embodiments of the present invention, said microwave hydrothermal synthetic step is: at first at 100 ℃ of insulation 5min, then at 125 ℃ of insulation 5min, then at 150 ℃ of insulation 10min, again at 175 ℃ of insulation 15min, at last at 180 ℃ of insulation 30min.
Microwave-hydrothermal method of the present invention prepares hexagonal BeFe 12O 19The method of magnetic nano powder has the following advantages at least: the present invention adopts microwave-hydrothermal method to prepare BeFe 12O 19Magnetic nano powder.Because to have speed fast for microwave reaction, advantages such as no thermograde, not only preparation cost is low, simple to operate, reaction time is short, product purity is high, the crystal grain growth is complete and be evenly distributed.Final calcining at a lower temperature promptly gets the BeFe of even compact 12O 19Magnetic powder.
Description of drawings
Fig. 1 is the BeFe by the present invention's preparation 12O 19The X-ray diffraction of magnetic powder (XRD) figure;
Fig. 2 is the BeFe by the present invention's preparation 12O 19The SEM figure of magnetic powder.
Embodiment
Embodiment 1:
Step 1: the homogeneous solution A and the homogeneous solution B that analytically pure nitrate of baryta and nine water iron nitrates are configured to 0.01mol/L and 0.06mol/L respectively;
Step 2: by the Ba/Fe mol ratio is 1: 6, and B solution is added A solution, stirs, and regulating the pH value is 8～13, forms uniform co-precipitation precursor C;
Step 3: the co-precipitation precursor C is poured in the microwave hydrothermal reaction kettle, and compactedness is controlled at 40%; The sealed reaction jar puts it into and carries out polystep reaction in the microwave dissolver then, and respectively at 100 ℃ of insulation 5min, at 125 ℃ of insulation 5min, at 150 ℃ of insulation 10min, at 175 ℃ of insulation 15min, at 180 ℃ of insulation 30min, reaction is accomplished postcooling to room temperature;
Step 4: the thermal response of fetching boiling water jar, take out to use deionized water rinsing to be 7 the material in the retort to pH after, 900 ℃ down calcining promptly got hexagonal plate BeFe in two hours 12O 19Magnetic nano powder.
Embodiment 2:
Step 1: the homogeneous solution A and the homogeneous solution B that analytically pure nitrate of baryta and nine water iron nitrates are configured to 0.01mol/L and 0.07mol/L respectively;
Step 2: by the Ba/Fe mol ratio is 1: 7, and B solution is added A solution, stirs, and regulates the pH value and is respectively 9～12, forms uniform co-precipitation precursor C;
Step 3: the co-precipitation precursor C is poured in the microwave hydrothermal reaction kettle, and compactedness is controlled at 40%; The sealed reaction jar puts it into and carries out polystep reaction in the microwave dissolver then, and respectively at 100 ℃ of insulation 5min, at 125 ℃ of insulation 5min, at 150 ℃ of insulation 1min, at 175 ℃ of insulation 15min, at 180 ℃ of insulation 30min, reaction is accomplished postcooling to room temperature;
Step 4: the thermal response of fetching boiling water jar, it is 7 to pH that the material in the retort is taken out the use deionized water rinsing, last, calcining promptly got hexagonal plate BeFe in two hours under 800 ℃ 12O 19Magnetic nano powder.
Embodiment 3:
Step 1: the homogeneous solution A and the homogeneous solution B that analytically pure nitrate of baryta and nine water iron nitrates are configured to 0.01mol/L and 0.08mol/L respectively;
Step 2: by the Ba/Fe mol ratio is 1: 8, and B solution is added A solution, stirs, and regulates the pH value and is respectively 10～13, forms uniform co-precipitation precursor C;
Step 3: the co-precipitation precursor C is poured in the microwave hydrothermal reaction kettle, and compactedness is controlled at 40%; The sealed reaction jar puts it into and carries out polystep reaction in the microwave dissolver then, and respectively at 100 ℃ of insulation 5min, at 125 ℃ of insulation 5min, at 150 ℃ of insulation 1min, at 175 ℃ of insulation 15min, at 180 ℃ of insulation 30min, reaction is accomplished postcooling to room temperature;
Step 4: the thermal response of fetching boiling water jar, take out to use deionized water rinsing to be 7 the material in the retort to pH after, 1000 ℃ down calcining promptly got hexagonal plate BeFe in two hours 12O 19Magnetic nano powder.
Embodiment 4:
Step 1: the homogeneous solution A and the homogeneous solution B that analytically pure nitrate of baryta and nine water iron nitrates are configured to 0.01mol/L and 0.09mol/L respectively;
Step 2: by the Ba/Fe mol ratio is 1: 9, and B solution is added A solution, stirs, and regulates the pH value and is respectively 8～11, forms uniform co-precipitation precursor C;
Step 3: the co-precipitation precursor C is poured in the microwave hydrothermal reaction kettle, and compactedness is controlled at 40%; The sealed reaction jar puts it into and carries out polystep reaction in the microwave dissolver then, and holding temperature and soaking time are respectively at 100 ℃ of insulation 5min; At 125 ℃ of insulation 5min, at 150 ℃ of insulation 1min, at 175 ℃ of insulation 15min; At 180 ℃ of insulation 30min, reaction is accomplished postcooling to room temperature;
Step 4: the thermal response of fetching boiling water jar, take out to use deionized water rinsing to be 7 the material in the retort to pH after, 950 ℃ down calcining promptly got hexagonal plate BeFe in two hours 12O 19Magnetic nano powder.
Embodiment five
Step 1: the homogeneous solution A and the homogeneous solution B that analytically pure nitrate of baryta and nine water iron nitrates are configured to 0.01mol/L and 0.10mol/L respectively;
Step 2: by the Ba/Fe mol ratio is 1: 10, and B solution is added A solution, stirs, and regulates the pH value and is respectively 8～10, forms uniform co-precipitation precursor C;
Step 3: the co-precipitation precursor C is poured in the microwave hydrothermal reaction kettle, and compactedness is controlled at 40%; The sealed reaction jar puts it into and carries out polystep reaction in the microwave dissolver then, and holding temperature and soaking time are respectively at 100 ℃ of insulation 5min; At 125 ℃ of insulation 5min, at 150 ℃ of insulation 1min, at 175 ℃ of insulation 15min; At 180 ℃ of insulation 30min, reaction is accomplished postcooling to room temperature;
Step 4: the thermal response of fetching boiling water jar, take out to use deionized water rinsing to be 7 the material in the retort to pH after, 900 ℃ down calcining promptly got hexagonal plate BeFe in two hours 12O 19Magnetic nano powder.
Embodiment six
Step 1: the homogeneous solution A homogeneous solution B that analytically pure nitrate of baryta and nine water iron nitrates is configured to 0.01mol/L and 0.06～0.08mol/L respectively;
Step 2: by the Ba/Fe mol ratio is 1: (7～9), B solution is added A solution, stir, regulate the pH value and be respectively 13, form uniform co-precipitation precursor C;
Step 3: the co-precipitation precursor C is poured in the microwave hydrothermal reaction kettle, and compactedness is controlled at 40%; The sealed reaction jar puts it into and carries out polystep reaction in the microwave dissolver then, and holding temperature and soaking time are respectively at 100 ℃ of insulation 5min; At 125 ℃ of insulation 5min, at 150 ℃ of insulation 1min, at 175 ℃ of insulation 15min; At 200 ℃ of insulation 30min, reaction is accomplished postcooling to room temperature;
Step 4: the thermal response of fetching boiling water jar, take out to use deionized water rinsing to be 7 the material in the retort to pH after, 850 ℃ down calcining promptly got hexagonal plate BeFe in two hours 12O 19Magnetic nano powder.
Embodiment seven
Step 1: the homogeneous solution A homogeneous solution B that analytically pure nitrate of baryta and nine water iron nitrates is configured to 0.01mol/L and 0.07～0.1mol/L respectively;
Step 2: by the Ba/Fe mol ratio is 1: (8～10), B solution is added A solution, stir, regulate the pH value and be respectively 11～13, form uniform co-precipitation precursor C;
Step 3: the co-precipitation precursor C is poured in the microwave hydrothermal reaction kettle, and compactedness is controlled at 40%; The sealed reaction jar puts it into and carries out polystep reaction in the microwave dissolver then, and holding temperature and soaking time are respectively at 100 ℃ of insulation 5min; At 125 ℃ of insulation 5min, at 150 ℃ of insulation 1min, at 175 ℃ of insulation 15min; At 200 ℃ of insulation 30min, reaction is accomplished postcooling to room temperature;
Step 4: the thermal response of fetching boiling water jar, take out to use deionized water rinsing to be 7 the material in the retort to pH after, 800～1000 ℃ down calcining promptly got hexagonal plate BeFe in two hours 12O 19Magnetic nano powder.
See also shown in Figure 1, with prepared BeFe 12O 19Powder is with Japanese D/max2000PC x-ray diffractometer analytic sample of science, and its product is the BeFe that JCPDS is numbered 27-1029 12O 19
See also shown in Figure 2, the hexagonal plate nanometer BeFe for preparing by the inventive method 12O 19Magnetic powder, the particle surface rule, particle is grown complete, and component is even.
The above is merely one embodiment of the present invention; It or not whole or unique embodiment; The conversion of any equivalence that the logical technician in this area takes technical scheme of the present invention through reading specification sheets of the present invention is claim of the present invention and contains.

Claims (9)

1. a microwave-hydrothermal method prepares hexagonal BeFe 12O 19The method of magnetic nano powder is characterized in that: with nine water iron nitrates and nitrate of baryta is precursor, is dissolved in the deionized water, and regulator solution pH is 9～14 then, forms uniform precursor liquid; Precursor liquid is poured in the hydrothermal reaction kettle and sealing, put then into to carry out microwave hydrothermal in the microwave dissolver synthetic, be cooled to room temperature, product with deionized water and absolute ethanol washing neutrality extremely, is promptly got 800～1000 ℃ of calcinings at last.
2. microwave-hydrothermal method as claimed in claim 1 prepares hexagonal BeFe 12O 19The method of magnetic nano powder is characterized in that: after said nine water iron nitrates and nitrate of baryta were dissolved in the deionized water, its concentration was respectively 0.06～0.1mol/L and 0.01mol/L.
3. microwave-hydrothermal method as claimed in claim 2 prepares hexagonal BeFe 12O 19The method of magnetic nano powder is characterized in that: said nine water iron nitrates and nitrate of baryta are dissolved in the iron nitrate solution of back formation in the deionized water and the Ba/Fe mol ratio in the nitrate of baryta solution is: 1: (6～10).
4. microwave-hydrothermal method as claimed in claim 1 prepares hexagonal BeFe 12O 19The method of magnetic nano powder is characterized in that: the compactedness of said hydrothermal reaction kettle is 40%.
5. microwave-hydrothermal method as claimed in claim 1 prepares hexagonal BeFe 12O 19The method of magnetic nano powder is characterized in that: said microwave hydrothermal synthetic step is: at first at 100 ℃ of insulation 5min, then at 125 ℃ of insulation 5min, then at 150 ℃ of insulation 10min, again at 175 ℃ of insulation 15min, at last at 180 ℃ of insulation 30min.
6. a microwave-hydrothermal method prepares hexagonal BeFe 12O 19The method of magnetic nano powder is characterized in that: may further comprise the steps:
Step 1: getting concentration is the nitrate of baryta homogeneous solution A of 0.01mol/L and the iron nitrate homogeneous solution B that concentration is 0.06～0.1mol/L;
Step 2: according to the Ba/Fe mol ratio is 1: the ratio of (6～10) joins homogeneous solution B among the homogeneous solution A, stirs, and is adjusted to alkalescence, forms uniform co-precipitation precursor C;
Step 3: the co-precipitation precursor C is poured in the microwave hydrothermal reaction kettle, and the control compactedness is 40%, sealed reaction, and reaction is cooled to room temperature after accomplishing;
Step 4: the material water that takes out in the reaction kettle washes to neutrality, and calcining promptly gets the BeFe of hexagonal plate 12O 19Magnetic nano powder.
7. microwave-hydrothermal method as claimed in claim 6 prepares hexagonal BeFe 12O 19The method of magnetic nano powder is characterized in that: the pH when being adjusted to alkalescence in the said step 2 is 8～13.
8. microwave-hydrothermal method as claimed in claim 6 prepares hexagonal BeFe 12O 19The method of magnetic nano powder; It is characterized in that: in the said step 3; The step of sealed reaction is in microwave hydrothermal reaction kettle: at first at 100 ℃ of insulation 5min, then at 125 ℃ of insulation 5min, then at 150 ℃ of insulation 10min; Again at 175 ℃ of insulation 15min, at last at 180 ℃ of insulation 30min.
9. microwave-hydrothermal method as claimed in claim 6 prepares hexagonal BeFe 12O 19The method of magnetic nano powder is characterized in that: the calcining temperature of said step 4 is 800～1000 ℃.
CN2011103631007A 2011-11-16 2011-11-16 Method for preparing hexagonal BeFe12O19 (barium ferrite) magnetic nano powder by microwave-hydrothemal method Pending CN102491428A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103787420A (en) * 2014-01-25 2014-05-14 陕西科技大学 Method for preparing SrFe12O19 magnetic nano powder by using microwave hydrothermal method
CN105460977A (en) * 2015-11-23 2016-04-06 电子科技大学 Preparation method of morphology controllable M-type barium ferrite powder
CN105645944A (en) * 2015-12-30 2016-06-08 陕西科技大学 Bi2Fe4O9/BaFe12O19 (bismuth ferrite/barium ferrite) composite ceramic and preparation method thereof
CN105645476A (en) * 2016-03-24 2016-06-08 陕西科技大学 Method for preparing nano Sr(Fe0.5Nb0.5)O3 powder by microwave-hydrothermal method
CN106587971A (en) * 2016-12-15 2017-04-26 陕西科技大学 Multiferroic composite ceramics with softened magnetic hysteresis loops and preparation method for multiferroic composite ceramics

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CN101698608A (en) * 2009-10-28 2010-04-28 上海应用技术学院 Method for synthesizing nanocrystalline M-type ferrite powder

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103787420A (en) * 2014-01-25 2014-05-14 陕西科技大学 Method for preparing SrFe12O19 magnetic nano powder by using microwave hydrothermal method
CN105460977A (en) * 2015-11-23 2016-04-06 电子科技大学 Preparation method of morphology controllable M-type barium ferrite powder
CN105645944A (en) * 2015-12-30 2016-06-08 陕西科技大学 Bi2Fe4O9/BaFe12O19 (bismuth ferrite/barium ferrite) composite ceramic and preparation method thereof
CN105645944B (en) * 2015-12-30 2018-05-15 陕西科技大学 A kind of Bi2Fe4O9/BaFe12O19Composite ceramics and preparation method thereof
CN105645476A (en) * 2016-03-24 2016-06-08 陕西科技大学 Method for preparing nano Sr(Fe0.5Nb0.5)O3 powder by microwave-hydrothermal method
CN106587971A (en) * 2016-12-15 2017-04-26 陕西科技大学 Multiferroic composite ceramics with softened magnetic hysteresis loops and preparation method for multiferroic composite ceramics

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Application publication date: 20120613