CN103193472A - Method for synthesizing subsphaeroidal barium ferrite superfine powder by using ultrasound-assisted coprecipitation method - Google Patents
Method for synthesizing subsphaeroidal barium ferrite superfine powder by using ultrasound-assisted coprecipitation method Download PDFInfo
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- CN103193472A CN103193472A CN2013101376277A CN201310137627A CN103193472A CN 103193472 A CN103193472 A CN 103193472A CN 2013101376277 A CN2013101376277 A CN 2013101376277A CN 201310137627 A CN201310137627 A CN 201310137627A CN 103193472 A CN103193472 A CN 103193472A
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Abstract
The invention provides a preparation method for synthesizing subsphaeroidal barium ferrite superfine powder by using an ultrasound-assisted coprecipitation method. The preparation method comprises the following steps of: preparing a mixed salt solution from raw materials of soluble barium salt and ferric salt according to a barium-iron molar ratio; selecting an appropriate precipitant, and dropwise adding the precipitant into the mixed salt solution under the action of external ultrasounds; fully reacting; centrifuging and drying to obtain a precursor; grinding the precursor and putting the precursor into a crucible; and putting the crucible into a muffle furnace to carry out heat treatment at a certain temperature to obtain the subsphaeroidal barium ferrite superfine powder. By adopting the preparation method, the mixing uniformity of barium and iron ions in the precursor is improved, the synthesis temperature is reduced, the shape of synthesized particles is controlled to tend to an equal subsphaeroidal shape, the particle size distribution is relatively concentrated, and the obtained barium ferrite particles can be used as a high-quality microwave absorbing medium.
Description
Technical field
The present invention relates to the method for the synthetic subsphaeroidal barium ferrite superfine powder of a kind of ultrasonic auxiliary coprecipitation method, belong to advanced functional materials preparing technical field.
Background technology
The hexagonal barium ferrite is because having higher magnetocrystalline anisotropy field, coercive field and saturation magnetization and good characteristics such as chemical erosion resistance are widely used in permanent-magnet ferrite, fields such as microwave, millimeter wave gyromagnetic material and perpendicular recording material, especially in recent years, because the concern that people pollute hertzian wave, receive much concern as the hexagonal barium ferrite of excellent microwave-absorbing body.Yet, owing to be subjected to the restriction of Growth Habit, particle is many in the general resultant barium ferrite powder exists with the hexagonal plate form, anisotropy on this granule-morphology makes it be affected as the raising of inhaling absorptive character in the use of ripple medium and the even character of absorbed performance to a certain extent, so synthetic barium ferrite superfine powder with isotropy pattern (as spherical morphology) becomes particularly important.
The method of synthesizing barium ferrite is mainly by solid reaction process, reverse microemulsion process, and coprecipitation method, hydrothermal synthesis method and sol-gel method etc., it differs from one another.Current, industrial for the preparation of high quality barium ferrite superfine powder mainly be coprecipitation method, have spherical or subglobose barium ferrite superfine powder yet adopt this method still to be difficult to preparation.
At present, the existing institute of work that adopts ultrasonic aids precipitation legal system to be equipped with the simple compounds superfine powder report, but for applications of ultrasound to coprecipitation method, and further effectively control property such as product powder granule pattern is tending towards and do not appear in the newspapers as yet.
Summary of the invention
The present invention put forth effort to solve have subsphaeroidal pattern, the uniform barium ferrite superfine powder of particle diameter prepares problem, has proposed the method that a kind of ultrasonic auxiliary coprecipitation method prepares subsphaeroidal barium ferrite superfine powder.In coprecipitation process, introduce ultrasonic auxiliary, impel on the one hand that barium, iron ion evenly distribute in the co-precipitation presoma, on the other hand, utilize ultrasonic air to turn usefulness into, presoma to homogenizing is cut apart, and in addition, ultrasonication has promoted precipitin reaction to take place to a certain extent and reacted completely, make to obtain pattern homogeneous, the uniform product powder of particle size in follow-up heat treatment process, the product powder that obtains can be applicable to use as the efficient microwave absorbing medium.
The present invention is achieved through the following technical solutions,
Be raw material with soluble barium salt and molysite, according to barium iron mol ratio preparation mixing salt solution; Select suitable precipitation agent again, adding under the ultrasonication, be added dropwise to precipitation agent, fully reaction; By centrifugal, dry, obtain presoma, and with its thermal treatment under the certain temperature in retort furnace, can obtain subsphaeroidal barium ferrite superfine powder at last.The present invention improves presoma intermediate ion distributing homogeneity by choose reasonable, optimization ultrasonic power and time, the ultrasonic auxiliary chemical coprecipitation technique of employing of precipitation agent, can obtain the preparation of subsphaeroidal barium ferrite superfine powder through thermal treatment, its concrete steps are as follows:
Step 1: be raw material with solubility barium, molysite, barium ion and iron ion are prepared barium, ferrous metal salts solution according to the mol ratio of 1:10～12, the concentration of barium ion is at 0.01～0.10mol/L in the solution, and described solubility barium, molysite comprise bariumchloride, iron(ic) chloride, nitrate of baryta, iron nitrate;
Step 2: selective precipitation agent, excessive 0%～100% according to the total amount of metal ion, the preparation precipitant solution, and under ultrasonic auxiliary condition, drip precipitant solution, simultaneously, the water-bath magnetic agitation keeps reaction system to be in room temperature, wait to dropwise, continue to stir 1～5 hour, it is fully reacted, guarantee that barium, ferrous metal ion precipitate fully;
Step 3: gained precipitated product, through centrifugation, centrifugal rotational speed: 2500rpm～10000 rev/min, centrifugation time: 5～20 minutes, the washing of gained precipitated product and centrifugation were cleaned 2～3 times, products therefrom carries out vacuum-drying under 60 ℃～80 ℃ conditions, to constant weight, general 12～24 hours time of drying, obtain presoma;
Step 4: the gained presoma, be placed in the crucible through grinding, put into retort furnace and heat-treat, select thermal treatment temp 700～1000
oC, generated time 1～8 hour obtains the subsphaeroidal barium ferrite superfine powder of product.
Preferably, adopt the method for ultrasonic auxiliary coprecipitation reaction in the step 2, ultrasonic output rating is 9.5W～104.5W interval, the ultrasonic amplitude transformer diameter is 6mm, 10mm, ultrasonic power adopts intermittent type, ultrasonic time 1～5 second, 2～10 seconds pitch times, be aided with stirring in water bath, system temperature is constant in the maintenance ultrasonic procedure.
Preferably, in the step 2 at the ultrasonic precipitation agent that adds simultaneously, precipitation agent is chosen as one or more the combination in sodium hydroxide, ammoniacal liquor, volatile salt and the yellow soda ash, contained precipitation agent amount of substance is according to the additional excessive value of precipitating ion theoretical consumption in its solution, as to adopt ammoniacal liquor be precipitation agent precipitated iron ion, its target product is ironic hydroxide, so the amount of substance of ammoniacal liquor is: the iron ion amount of substance multiply by 3 and multiply by (the excessive ratio of 1+).
The present invention introduces ultrasonic auxiliary cleverly in coprecipitation process, impels that barium, iron ion evenly distribute in the co-precipitation presoma, and gained barium ferrite particle has and is subsphaeroidal form, distribution of sizes and characteristics such as concentrates, and can be used as the high-quality microwave absorbing medium and uses.Compare with traditional co-precipitation method, method thinking novelty provided by the invention, greatly improve the mixing uniformity of barium iron ion in the presoma, reduced synthesis temperature, controlled property forms such as synthetic granule-morphology is tending towards, particle size distribution is concentrated relatively, specifically comprises as follows:
1, in the coprecipitation reaction process, adopts ultrasonic assisting, improved barium iron ion mixing uniformity in the presoma on the one hand, also accelerated the generation of precipitin reaction on the other hand to a certain extent, make precipitin reaction complete;
2, the prepared subsphaeroidal form that obtains property such as barium ferrite is tending towards has important help for improving its microwave absorbing property;
3, related instrument is simple in the preparation process, is easy to control, for synthetic other complex oxide nano-powder reference function is energetically arranged.
Description of drawings
The XRD figure spectrum of Fig. 1 ultrasound assisted chemical coprecipitation method synthesizing barium ferrite superfine powder.
The FE-SEM photo of Fig. 2 ultrasound assisted chemical coprecipitation method synthesizing barium ferrite superfine powder.
The magnetic hysteresis loop of Fig. 3 ultrasound assisted chemical coprecipitation method synthesizing barium ferrite superfine powder.
The XRD figure spectrum of Fig. 4 ultrasound assisted chemical coprecipitation method synthesizing barium ferrite superfine powder.
The FE-SEM photo of Fig. 5 ultrasound assisted chemical coprecipitation method synthesizing barium ferrite superfine powder.
The magnetic hysteresis loop of Fig. 6 ultrasound assisted chemical coprecipitation method synthesizing barium ferrite superfine powder.
Embodiment
Adopting ultrasonic auxiliary coprecipitation method to synthesize subsphaeroidal barium ferrite ultrafine powder, is raw material with soluble barium salt and molysite, according to barium iron mol ratio preparation mixing salt solution; Select suitable precipitation agent again, adding under the ultrasonication, be added dropwise to precipitation agent, fully reaction; By centrifugal, dry, obtain presoma at last, the presoma grinding is placed in the crucible, put into retort furnace and carry out heat-treating with certain temperature, can obtain subsphaeroidal barium ferrite superfine powder.The present invention is described in detail below by specific embodiment.
Embodiment 1
Be raw material with analytical pure bariumchloride and iron(ic) chloride, according to Ba
2+: Fe
3+The mol ratio of=1:10.5 takes by weighing bariumchloride and iron(ic) chloride, is dissolved in the proper amount of deionized water, obtains bariumchloride and ferric chloride Solution, and its concentration is respectively: [Ba
2+]=0.01mol/L, [Fe
3+]=0.105mol/L;
Ultrasonic cell pulverization instrument parameter is set: horn diameter 6mm, power are 19W, ultrasonic 2.0s, the ultrasonic pass 8.0s of opening;
Add precipitation agent volatile salt and ammoniacal liquor in above-mentioned solution, add-on drips by Calculation of chemical equilibrium excessive 50%, under 25 ℃ of conditions, stirs in the time of ultrasonic then, reacts constant to the pH value, the precursor solution that obtains reacting completely;
Above-mentioned solution is poured in the centrifuge tube centrifugal, the throw out after centrifugal is carried out vacuum-drying under-0.08MPa, 80 ℃ condition, obtain reddish brown presoma after 24 hours;
The gained presoma ground be placed in the retort furnace calcining 2 hours, temperature is 800 ℃, and the product after the calcining is the barium ferrite of single thing phase, its XRD spectrum as shown in Figure 1, Fig. 2 is its SEM photo, Fig. 3 is its barium ferrite powder magnetic hysteresis loop.
By analyzing as can be known, the barium ferrite pattern of the single thing phase of present embodiment is bordering on sphere, and median size is 80～120nm, and grain diameter is even.
Embodiment 2
Be raw material with analytical pure bariumchloride and iron(ic) chloride, press Ba
2+: Fe
3+The mol ratio of=1:10.5 takes by weighing bariumchloride and iron(ic) chloride, is dissolved in the proper amount of deionized water, obtains bariumchloride and ferric chloride Solution, and concentration is respectively: [Ba
2+]=0.01M/L, [Fe
3+]=0.105M/L;
Ultrasonic cell pulverization instrument parameter is set: power is 47.5W, ultrasonic 2.0s, the ultrasonic pass 8.0s of opening;
Add precipitation agent volatile salt and ammoniacal liquor in above-mentioned solution, add-on drips by Calculation of chemical equilibrium excessive 50%, under 25 ℃ of conditions, stirs in the time of ultrasonic then, reacts constant to the pH value, the precursor solution that obtains reacting completely;
Above-mentioned solution is poured in the centrifuge tube centrifugal, the throw out after centrifugal is carried out vacuum-drying under-0.08MPa, 80 ℃ condition, obtain reddish brown presoma after 24 hours;
The gained presoma ground be placed in the retort furnace calcining 2 hours, temperature is 800 ℃, namely obtains the barium ferrite of single thing phase after the calcining, its XRD spectrum as shown in Figure 4, Fig. 5 is its SEM photo, Fig. 6 is its barium ferrite powder magnetic hysteresis loop.
By analyzing as can be known, the barium ferrite pattern of the single thing phase of present embodiment is bordering on sphere, and median size is 50～90nm, and grain diameter is even.
The present invention introduces ultrasonic auxiliary in coprecipitation process; make subsphaeroidal pattern; the uniform barium ferrite superfine powder of grain diameter; the product powder that obtains; can be applicable to use as the efficient microwave absorbing medium; simultaneously; this kind method also has good reference function for synthetic high quality complex oxide nano-powder; above-described embodiment only is the detailed description that embodiments of the present invention are carried out; be not limited to design of the present invention and protection domain; under the prerequisite that does not break away from design concept of the present invention; various distortion and improvement that the common engineering technical personnel in this area make technical scheme of the present invention all fall into protection scope of the present invention.
Claims (4)
1. the method for the synthetic subsphaeroidal barium ferrite superfine powder of ultrasonic auxiliary coprecipitation method is characterized in that: comprise the steps:
Step 1: be raw material with solubility barium, molysite, with barium ion and iron ion mol ratio preparation barium, the ferrous metal salts solution according to 1:10～12, in the solution concentration of barium ion at 0.01～0.05mol/L, iron concentration 0.10～0.60mol/L;
Step 2: selective precipitation agent, according to excessive 0%～100% preparation precipitant solution of the total amount of metal ion, and under ultrasonic auxiliary condition, drip precipitant solution, simultaneously, the water-bath magnetic agitation, keep reaction system to be in room temperature, wait to dropwise, continue to stir 1～5 hour, it is fully reacted, guarantee that barium, ferrous metal ion precipitate fully;
Step 3: gained precipitated product, through centrifugation, centrifugal rotational speed is 2500～10000 rev/mins, centrifugation time is 5～20 minutes, with the washing of gained precipitated product and centrifugation, clean 2～3 times, products therefrom carries out vacuum-drying to constant weight at 60 ℃～80 ℃, 12～24 hours time of drying, obtain presoma;
Step 4: the grinding of gained presoma is placed in the crucible, puts into retort furnace and heat-treat, thermal treatment temp 700～1000
oC, generated time 1～8 hour obtains the subsphaeroidal barium ferrite superfine powder of product.
2. a kind of ultrasonic auxiliary coprecipitation method according to claim 1 is synthesized the method for subsphaeroidal barium ferrite superfine powder, and it is characterized in that: the solubility barium in the described step 1, molysite are bariumchloride, iron(ic) chloride, nitrate of baryta, iron nitrate.
3. a kind of ultrasonic auxiliary coprecipitation method according to claim 1 is synthesized the method for subsphaeroidal barium ferrite superfine powder, it is characterized in that: the method that adopts ultrasonic auxiliary coprecipitation reaction in the described step 2, ultrasonic output rating is between 9.5W～104.5W, ultrasonic amplitude transformer diameter 6mm, 10mm, ultrasonic power adopts intermittent type, ultrasonic time 1～5 second, 2～10 seconds pitch times, be aided with stirring in water bath in the ultrasonic procedure, system temperature is constant in the maintenance ultrasonic procedure.
4. a kind of ultrasonic auxiliary coprecipitation method according to claim 1 is synthesized the method for subsphaeroidal barium ferrite superfine powder, it is characterized in that: in ultrasonic, add precipitation agent in the described step in two, precipitation agent is one or more the combination in sodium hydroxide, ammoniacal liquor, volatile salt and the yellow soda ash, and contained precipitation agent amount of substance is according to the additional excessive value of precipitating ion theoretical consumption in its solution.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058736A (en) * | 2014-06-09 | 2014-09-24 | 青岛东方循环能源有限公司 | Preparation method of nickel-iron-zirconium compound ferrite |
| CN105253918A (en) * | 2015-09-24 | 2016-01-20 | 南京工业大学 | Preparation method of easy-dispersible hexagonal-plate shaped W-type ferrite BaZn2Fe16O27 |
| CN105344366A (en) * | 2015-12-11 | 2016-02-24 | 湘潭大学 | Preparation method for sunlight responding BiPO4 photocatalyst |
| CN106498497A (en) * | 2016-12-09 | 2017-03-15 | 扬州大学 | A kind of method for preparing granule single crystallization Co2Z hexad ferrite powder body |
| CN110136907A (en) * | 2019-04-26 | 2019-08-16 | 南京睿磐内尔环保复合新材料有限公司 | A kind of method of ultrasonic wave added Co deposited synthesis complex ferrite |
| CN114735754A (en) * | 2022-05-24 | 2022-07-12 | 沈阳理工大学 | Barium ferrite and preparation method thereof |
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| CN102260071A (en) * | 2011-05-23 | 2011-11-30 | 哈尔滨工业大学 | Method for preparing high-dispersion quasi-spherical M type barium ferrite |
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2013
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Patent Citations (1)
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| CN102260071A (en) * | 2011-05-23 | 2011-11-30 | 哈尔滨工业大学 | Method for preparing high-dispersion quasi-spherical M type barium ferrite |
Non-Patent Citations (1)
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| 刘萍等: "超声辅助共沉淀制备近球形钡铁氧体单畴粉体", 《2012中国功能新材料学术论坛暨第三届全国电磁材料及器件学术会议论文摘要集》, 19 October 2012 (2012-10-19) * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058736A (en) * | 2014-06-09 | 2014-09-24 | 青岛东方循环能源有限公司 | Preparation method of nickel-iron-zirconium compound ferrite |
| CN104058736B (en) * | 2014-06-09 | 2015-10-28 | 青岛东方循环能源有限公司 | A kind of preparation method of ferronickel zirconium complex ferrite |
| CN105253918A (en) * | 2015-09-24 | 2016-01-20 | 南京工业大学 | Preparation method of easy-dispersible hexagonal-plate shaped W-type ferrite BaZn2Fe16O27 |
| CN105344366A (en) * | 2015-12-11 | 2016-02-24 | 湘潭大学 | Preparation method for sunlight responding BiPO4 photocatalyst |
| CN106498497A (en) * | 2016-12-09 | 2017-03-15 | 扬州大学 | A kind of method for preparing granule single crystallization Co2Z hexad ferrite powder body |
| CN110136907A (en) * | 2019-04-26 | 2019-08-16 | 南京睿磐内尔环保复合新材料有限公司 | A kind of method of ultrasonic wave added Co deposited synthesis complex ferrite |
| CN114735754A (en) * | 2022-05-24 | 2022-07-12 | 沈阳理工大学 | Barium ferrite and preparation method thereof |
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Application publication date: 20130710 |