CN103183503A - Rodlike nano barium ferrite, and preparation method and application thereof - Google Patents
Rodlike nano barium ferrite, and preparation method and application thereof Download PDFInfo
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- CN103183503A CN103183503A CN 201110451405 CN201110451405A CN103183503A CN 103183503 A CN103183503 A CN 103183503A CN 201110451405 CN201110451405 CN 201110451405 CN 201110451405 A CN201110451405 A CN 201110451405A CN 103183503 A CN103183503 A CN 103183503A
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Abstract
The invention discloses a preparation method of a rodlike nano barium ferrite. The preparation method comprises the following steps of (1) mixing a Ba<2+>-containing aqueous solution and a Fe<3+>-containing aqueous solution uniformly to obtain a mixed liquid, mixing the mixed solution with citric acid, adjusting a pH value of the solution to 6.5-7.5, mixing the obtained solution with polymethyl methacrylate spheres with a D50 average particle size of 13-18 [mu]m, dispersing the spheres uniformly, and volatilizing the solvent to obtain a wet gel, wherein the usage amount of the polymethyl methacrylate spheres is 82.3-213.7 gin each mol of the Ba<2+>; and (2) drying the wet gel, performing heat treatment on the dried wet gel, and cooling to obtain the rodlike nano barium ferrite. The invention also provides the rodlike nano barium ferrite prepared by the above preparation method and an application in the field of magnetic records. The preparation method is simple in process, low in cost and low in synthetic temperature, and is easy for industrialized production. The prepared rodlike nano barium ferrite has relatively high coercive force.
Description
Technical field
The present invention relates to field of magnetic material, relate in particular to a kind of rod-like nano barium ferrite and its preparation method and application.
Background technology
Magneticsubstance has been penetrated into human being's production, various fields in life as the base mateiral of electronic devices and components.Wherein, had the brilliant barium ferrite of M type hexagonal of Magnetoplumbate-type structure since 1938 are synthesized by Adelskold first, owing to possess higher saturation magnetization and coercive force, and excellent chemical stability and corrosion resistance, and the prices of raw and semifnished materials are cheap, are widely used in fields such as permanent magnet material, microwave absorbing material and high-density perpendicular recording material.
Research to the brilliant barium ferrite of M type hexagonal concentrates on two aspects: the one, and adopt different synthetic methods to prepare homodisperse superfine powder, the preparation method comprises coprecipitation method, salt-melting method, microemulsion method, hydrothermal synthesis method, sol-gel method etc.; The 2nd, Fe
3+Substitution studies, refer to substitute Fe in the ferrite with single ionic or different kinds of ions
3+Five kinds of brilliant positions, thereby improve ferritic magnetic property.
In recent years, the 1-dimention nano magnetic particle is owing to the potential application in high-density magnetic recording media and magnetic carrier field is subject to people's attention.One-dimensional rod-like spinel type vectolite (F.Dumestre et al., Angew.Chem.115 (2003) 5371-74) and Ni ferrite (N.Cordente et al, Nano Lett.1 (2001) 565-68) successfully prepared, its synthetic method is the organometallic precursor reduction method, technological process is comparatively complicated, and the preparation of the brilliant barium ferrite of the M type hexagonal of one-dimensional rod-like then rarely has report.
Summary of the invention
Technical problem to be solved by this invention is to overcome the defective of 1-dimention nano magneticsubstance preparation process complexity in the prior art, and a kind of rod-like nano barium ferrite and its preparation method and application is provided.Preparation method's technology of the present invention is simple, and cost is low, and synthesis temperature is low, is easy to suitability for industrialized production, and the rod-like nano barium ferrite that makes has higher coercive force.
The present invention addresses the above problem by the following technical programs.
The invention provides a kind of preparation method of rod-like nano barium ferrite, it comprises the steps:
(1) will contain Ba
2+The aqueous solution and contain Fe
3+Aqueous solution even mixed solution, mixes with citric acid, adjusting pH value is to 6.5-7.5, with median size D
50Polymethylmethacrylate (being called for short PMMA) ball mixing for 13-18 μ m is uniformly dispersed, and solvent flashing gets wet gel; Wherein, the consumption of described polymethylmethacrylate ball is the Ba of 82.3-213.7g/mol
2+
(2) will heat-treat after the described wet gel drying, after the cooling namely.
In the step (1), the median size D of described PMMA ball
50Preferably be 15 μ m.
In the step (1), the consumption of described polymethylmethacrylate ball preferably is the Ba of 90.8-181.7g/mol
2+
In the step (1), the described Ba that contains
2+The aqueous solution in Ba
2+Concentration be the conventional concentration of this area, preferably be 0.03-0.1mol/L.Described Ba
2+Form with the soluble barium salt adds water solution, and described soluble barium salt can be the conventional various soluble barium salts that use in this area, preferably is nitrate of baryta and/or bariumchloride.
In the step (1), the described Fe that contains
3+The aqueous solution in Fe
3+Concentration be the conventional concentration of this area, preferably be 0.03-0.1mol/L.Described Fe
3+Form with soluble ferric iron salt adds water solution, and described soluble ferric iron salt can be the conventional various soluble ferric iron salt of using in this area, preferably is in iron nitrate, iron(ic) chloride and the ferric sulfate one or more.
In the step (1), Ba in the described mixed solution
2+And Fe
3+Mol ratio be the mol ratio of the conventional preparation in this area barium ferrite, preferably be 1: 11.4-1: 12.0.
In the step (1), the consumption of described citric acid is this area conventional amount used.Described citric acid and described Ba
2+Mol ratio preferably be more than 13, more preferably be 13-14.
In the step (1), the method for described adjusting pH value is this area ordinary method, generally uses alkaline agent to regulate.Described alkaline agent preferably is ammoniacal liquor and/or urea.Described pH value preferably is 7.0.
In the step (1), described dispersion is preferably carried out under ultrasonic condition.Condition and method that described ultrasonic condition and method are this area routine, described ultrasonic so that the PMMA ball evenly disperses to be as the criterion, the described ultrasonic time preferably is 8-15 minute.
In the step (1), the condition of described solvent flashing and method are condition and the method for this area routine.Described solvent flashing preferably under agitation carries out.The temperature of described stirring preferably is 65-75 ℃.
In the step (1), the condition of described drying and method are condition and the method for this area routine.Described drying preferably is vacuum-drying.The temperature of described drying preferably is 105-120 ℃.
In the step (2), described heat treated condition and method are condition and the method for this area routine.Formed barium ferrite in this heat treatment process, the PMMA ball also decomposes in this heat treatment process.Described heat treated temperature preferably is 800-1000 ℃, more preferably is 800-850 ℃.Described heat treatment period preferably is 1-2.5 hour, more preferably is 1-1.5 hour.
Preparation principle of the present invention is not only applicable to prepare the one-dimensional rod-like nano barium ferrite, also be applicable to other one-dimensional rod-like magneticsubstance of preparation, mainly including, but not limited to the brilliant strontium ferrites of M type hexagonal, spinel type soft magnetic ferrite, W type, Z type and U-shaped ferrite.
The present invention also provides the rod-like nano that is made by above-mentioned preparation method barium ferrite, and it is the brilliant barium ferrite of pure M type hexagonal.The average aspect ratio of rod-like nano barium ferrite of the present invention is generally more than 4.5.
The present invention also provides described rod-like nano barium ferrite in the magnetic recording Application for Field.
On the basis that meets this area general knowledge, above-mentioned each optimum condition, but arbitrary combination namely get the preferred embodiments of the invention.
Agents useful for same of the present invention and raw material be commercially available getting all.
Positive progressive effect of the present invention is:
(1) preparation technology of the present invention is simple, and cost is low, and synthesis temperature is low, is easy to suitability for industrialized production.
(2) the present invention's rod-like nano barium ferrite that makes and comparing that prior art makes has higher coercive force, has wide practical use in the magnetic recording field.
Description of drawings
Fig. 1 is the XRD figure spectrum of the barium ferrite of embodiment 1, comparative example 1 and pdf standard card #27-1029.
Fig. 2 is the electromicroscopic photograph of embodiment 1 and comparative example's 1 barium ferrite.
Fig. 3 is embodiment 1 and comparative example's 1 magnetic hysteresis loop.
Embodiment
Mode below by embodiment further specifies the present invention, but does not therefore limit the present invention among the described scope of embodiments.The experimental technique of unreceipted actual conditions in the following example according to ordinary method and condition, or is selected according to catalogue.
The PMMA ball that adopts among the following embodiment is available from grinding chemistry (Suzhou) company limited in combining, and the ultrasonic device that uses must believe that as Shanghai the model of ultrasonic company limited production is the ultrasonic cleaner of SB-2200.
Embodiment 1:
The preparation process of rod-like nano barium ferrite:
(1) with 4.89gBa (NO
3)
2Fe (NO with 88.53g
3)
39H
2O is made into the aqueous solution of 0.05mol/L respectively, mix mixed solution (mol ratio Ba
2+: Fe
3+=1: 11.7), add 49.39g citric acid (mol ratio citric acid: Ba
2+=13.7) mix, progressively dropping ammonia is regulated pH to 7, and adding the 2.0g median size is the PMMA ball of 15 μ m, and ultrasonic 10 minutes, in 70 ℃ of stirring in water bath, volatilization moisture got wet gel;
(2) with wet gel after 110 ℃ of vacuum-drying, place retort furnace in 850 ℃ of thermal treatments 1.5 hours, namely get black powder shape barium ferrite after the cooling.
Fig. 1 and Fig. 2 show that the barium ferrite that makes is the brilliant barium ferrite of pure M type hexagonal, and particle shape is that bar-shaped, bar-shaped length is about 300nm, and diameter is about 60nm, and average aspect ratio is 5.VSM analyzes and shows (see figure 3): the specific saturation magnetization σ of the rod-like nano barium ferrite that makes
sBe 57.5emu/g, than residual magnetization σ
rBe 31.8emu/g, σ
s/ σ
rBe 0.55, coercivity H then is 5350Oe.
Embodiment 2:
The preparation process of rod-like nano barium ferrite:
(1) with 4.89gBa (NO
3)
2Fe (NO with 88.53g
3)
39H
2O is made into the aqueous solution of 0.05mol/L respectively, mix mixed solution (mol ratio Ba
2+: Fe
3+=1: 11.7), add 49.39g citric acid (mol ratio citric acid: Ba
2+=13.7) mix, progressively dropping ammonia is regulated pH to 6.5, and adding the 3.4g median size is the PMMA ball of 15 μ m, and ultrasonic 10 minutes, in 70 ℃ of stirring in water bath, volatilization moisture got wet gel;
(2) with wet gel after 110 ℃ of vacuum-drying, place retort furnace in 850 ℃ of thermal treatments 1.5 hours, namely get black powder shape barium ferrite after the cooling.
The barium ferrite that makes is the brilliant barium ferrite of pure M type hexagonal, is shaped as rod-shpaed particle (SEM figure is with embodiment 1), and its average aspect ratio is 4.8.VSM analyzes demonstration: its specific saturation magnetization σ
sBe 57.3emu/g, than residual magnetization σ
rBe 31.1emu/g, σ
s/ σ
rBe 0.56, coercivity H then is 5300Oe.
Embodiment 3:
The preparation process of rod-like nano barium ferrite:
(1) with 4.89gBa (NO
3)
2Fe (NO with 88.53g
3)
39H
2O is made into the aqueous solution of 0.05mol/L respectively, mix mixed solution (mol ratio Ba
2+: Fe
3+=1: 11.7), add 49.39g citric acid (mol ratio citric acid: Ba
2+=13.7: 1) mix, progressively dropping ammonia is regulated pH to 7.5, and adding the 1.7g median size is the PMMA ball of 15 μ m, and ultrasonic 10 minutes, in 70 ℃ of stirring in water bath, volatilization moisture got wet gel;
(2) with wet gel after 110 ℃ of vacuum-drying, place retort furnace in 850 ℃ of thermal treatments 1.5 hours, namely get black powder shape barium ferrite after the cooling.
The barium ferrite that makes is the brilliant barium ferrite of pure M type hexagonal, is shaped as rod-shpaed particle (SEM figure is with embodiment 1), and its average aspect ratio is 4.5.VSM analyzes demonstration: its specific saturation magnetization σ
sBe 57.4emu/g, than residual magnetization σ
rBe 31.6emu/g, σ
s/ σ
rBe 0.55, coercivity H then is 5280Oe.
The comparative example 1:
The nano barium ferrite preparation process:
(1) with 4.89gBa (NO
3)
2Fe (NO with 88.53g
3)
39H
2O is made into the aqueous solution of 0.05mol/L respectively, mix mixed solution, add the 49.39g citric acid and mix, progressively dropping ammonia is regulated pH to 7, in 70 ℃ of stirring in water bath, volatilization moisture gets wet gel;
(2) with wet gel after 110 ℃ of vacuum-drying, place retort furnace in 850 ℃ of thermal treatments 1.5 hours, namely get black powder shape barium ferrite after the cooling.
Fig. 1 and Fig. 2 show that when not adding PMMA, making barium ferrite is the brilliant barium ferrite of pure M type hexagonal, is shaped as random particulate state, and average particle size particle size is 120nm, less than the critical single domain particle size of barium ferrite 460nm.VSM analyzes and shows (see figure 3): its specific saturation magnetization σ
sBe 57.2emu/g, than residual magnetization σ
rBe 32.2emu/g, σ
s/ σ
rBe 0.56, coercivity H is 4800Oe, and its coercive force is starkly lower than the prepared barium ferrite of embodiment 1-3.
The comparative example 2:
The nano barium ferrite preparation process:
(1) with 4.89gBa (NO
3)
2Fe (NO with 88.53g
3)
39H
2O is made into the aqueous solution of 0.05mol/L respectively, mix mixed solution, add the 49.39g citric acid and mix, progressively dropping ammonia is regulated pH to 7, and adding the 2.0g median size is the PMMA ball of 10 μ m, ultrasonic 10 minutes, in 70 ℃ of stirring in water bath, volatilization moisture gets wet gel;
(2) with wet gel after 110 ℃ of vacuum-drying, place retort furnace in 850 ℃ of thermal treatments 1.5 hours, namely get black powder shape barium ferrite after the cooling.
When adding the PMMA of 10 μ m, making barium ferrite is the brilliant barium ferrite of pure M type hexagonal, is shaped as random particulate state.
Claims (10)
1. the preparation method of a rod-like nano barium ferrite, it comprises the steps:
(1) will contain Ba
2+The aqueous solution and contain Fe
3+Aqueous solution even mixed solution, mixes with citric acid, adjusting pH value is to 6.5-7.5, with median size D
50Polymethylmethacrylate ball mixing for 13-18 μ m is uniformly dispersed, and solvent flashing gets wet gel; The consumption of described polymethylmethacrylate ball is the Ba of 82.3-213.7g/mol
2+
(2) will heat-treat after the described wet gel drying, after the cooling namely.
2. preparation method as claimed in claim 1 is characterized in that, contains Ba described in the step (1)
2+The aqueous solution in Ba
2+Concentration be 0.03-0.1mol/L, described Ba
2+Form with the soluble barium salt adds water solution, and described soluble barium salt preferably is nitrate of baryta and/or bariumchloride; And/or, contain Fe described in the step (1)
3+The aqueous solution in Fe
3+Concentration be 0.03-0.1mol/L, described Fe
3+Form with soluble ferric iron salt adds water solution, and described soluble ferric iron salt preferably is one or more in iron nitrate, iron(ic) chloride and the ferric sulfate; And/or, the median size D of described polymethylmethacrylate ball
50Be 15 μ m.
3. preparation method as claimed in claim 1 or 2 is characterized in that, Ba in the mixed solution described in the step (1)
2+And Fe
3+Mol ratio be 1: 11.4-1: 12.0; And/or, described citric acid and described Ba
2+Mol ratio be more than 13, preferably be 13-14; And/or the consumption of described polymethylmethacrylate ball is the Ba of 90.8-181.7g/mol
2+
4. preparation method as claimed in claim 1 or 2 is characterized in that, uses ammoniacal liquor and/or urea to regulate the pH value in the step (1); Described pH value preferably is 7.0.
5. preparation method as claimed in claim 1 or 2 is characterized in that, being dispersed under the ultrasonic condition described in the step (1) carried out; The described ultrasonic time preferably is 8-15 minute.
6. preparation method as claimed in claim 1 or 2 is characterized in that, solvent flashing under agitation carries out described in the step (1); The temperature of described stirring preferably is 65-75 ℃.
7. preparation method as claimed in claim 1 or 2 is characterized in that, dry described in the step (1) is vacuum-drying; The temperature of described drying is 105-120 ℃.
8. preparation method as claimed in claim 1 or 2 is characterized in that, heat treated temperature is 800-1000 ℃ described in the step (2), preferably is 800-850 ℃; Described heat treatment period is 1-2.5 hour, preferably is 1-1.5 hour.
9. rod-like nano barium ferrite that is made by each described preparation method of claim 1-8.
10. rod-like nano barium ferrite as claimed in claim 9 is in the magnetic recording Application for Field.
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| CN105110379A (en) * | 2015-08-21 | 2015-12-02 | 重庆科技学院 | Ferroelectric nanochain preparation method |
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| CN114656269A (en) * | 2022-04-06 | 2022-06-24 | 中国科学院电工研究所 | Homogeneous fiber reinforced manganese-zinc ferrite material and preparation method thereof |
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2011
- 2011-12-27 CN CN 201110451405 patent/CN103183503A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105070790A (en) * | 2015-08-21 | 2015-11-18 | 重庆科技学院 | Nanochain solar cell preparation method |
| CN105110379A (en) * | 2015-08-21 | 2015-12-02 | 重庆科技学院 | Ferroelectric nanochain preparation method |
| CN105140041A (en) * | 2015-08-21 | 2015-12-09 | 重庆科技学院 | Liquid solar cell and preparation method thereof |
| CN105185867A (en) * | 2015-08-21 | 2015-12-23 | 重庆科技学院 | Preparation method for nano-chain solar cell |
| CN105070790B (en) * | 2015-08-21 | 2017-04-19 | 重庆科技学院 | Nanochain solar cell preparation method |
| CN105140041B (en) * | 2015-08-21 | 2017-11-07 | 重庆科技学院 | Liquid solar energy battery and preparation method thereof |
| CN114656269A (en) * | 2022-04-06 | 2022-06-24 | 中国科学院电工研究所 | Homogeneous fiber reinforced manganese-zinc ferrite material and preparation method thereof |
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Application publication date: 20130703 |