CN106379944A - Preparation method of pure-phase bismuth ferrite - Google Patents
Preparation method of pure-phase bismuth ferrite Download PDFInfo
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- CN106379944A CN106379944A CN201610755790.3A CN201610755790A CN106379944A CN 106379944 A CN106379944 A CN 106379944A CN 201610755790 A CN201610755790 A CN 201610755790A CN 106379944 A CN106379944 A CN 106379944A
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Abstract
The invention provides a preparation method of pure-phase bismuth ferrite. The method comprises a step of preparing a precursor liquid. Fe(NO3)3.9H2O and Bi(NO3)3.5H2O are dissolved in a solvent to obtain the precursor liquid with the metal ion concentration being 0.2 mol/L. Ammonia water is mixed with a ammonium bicarbonate solution to obtain a precipitating agent. In magnetic stirring, the precursor liquid is uniformly added to a precipitating agent solution dropwise till the pH value of a titration final point is controlled in 9-10. After titration is completed, stirring is continuously carried out to obtain a precipitate. The precipitate is allowed to stand and age, filtration is carried out, and the obtained product is washed with deionized water and absolute ethyl alcohol and is dried to obtain precursor powder. The precursor powder is put in a muffle furnace, the temperature is raised for calcination, and the obtained product is cooled to obtain pure-phase bismuth ferrite powder. The preparation method and the equipment are simple, and the pure-phase bismuth ferrite can be prepared in a large amount at one time. The preparation method is free of organic solvent and is green and eco-friendly, and the pure-phase bismuth ferrite is complete in crystallization and uniform in powder size.
Description
Technical field
The invention belongs to chemical field, it is related to a kind of bismuth ferrite powder, specifically a kind of pure phase bismuth ferric powder body
Preparation method.
Background technology
Pure phase bismuth ferric is that only a few has one of ferroelectricity and anti-ferromagnetic multi-ferroic material at room temperature simultaneously, this
Planting magnetic makes it before the aspects such as information Store, spin electric device and sensor have wide application with the control of comparing of electricity
Scape, is also the focus of Recent study.However, preparing, pure phase bismuth ferric is relatively difficult, the presence of dephasign leads to leakage current larger,
Hamper the development and application of bismuth ferrite material.In recent years, a lot of scholars prepare pure phase bismuth ferric powder body by various methods, main
Solid sintering technology to be had, hydrothermal synthesis method, sol-gel process and chemical coprecipitation.Solid phase method reaction temperature is high, repeatability
Difference, how dephasign is it is difficult to obtain pure phase bismuth ferric；The powder body that particle diameter is little although hydrothermal synthesis method can be prepared, grain development is complete,
This method need to be reacted under high temperature and high pressure environment, and reaction is wayward, and high to equipment requirements, there is certain risk；Molten
Glue-gel method is accurately controlled the chemical composition of powder body, but need to use organic solvent, and toxicity is larger.Relatively other chemical methods and
Speech, chemical coprecipitation technique and equipment are simple, reaction condition is gentle, the solvent-free nonhazardouss of raw material, and in addition, this method is easy to
Operation, is especially beneficial industrialized production.
Content of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of preparation side of pure phase bismuth ferric powder body
Method, the technique that described this pure phase bismuth ferric raw powder's production technology will solve to prepare pure phase bismuth ferric powder body in prior art
Complexity, the pure phase bismuth ferric of acquisition leads to leakage current larger due to the presence of dephasign, hampers the technology of bismuth ferrite materials application
Problem.
The invention provides a kind of pure phase bismuth ferric raw powder's production technology, comprise the steps：
（1）The step of one preparation precursor liquid, by Fe (NO3)3·9H2O and Bi (NO3)3·5H2O is dissolved in 1mol/LHNO3Solution
In, Fe3+：Bi3+Mol ratio be 1：1, obtain the precursor liquid that concentration of metal ions is 0.2 mol/L；
（2）The step of one preparation precipitant, by the ammonium bicarbonate soln of ammonia and 0.1mol/L by volume 1：2 are made into
NH3·H2O/NH4HCO3Mixed solution, as precipitant；
（3）One step preparing presoma, under magnetic stirring, by precursor liquid, equably Deca, in precipitant solution, is dripped
Determine endpoint pH and control in 9 ~ 10, after titration terminates, continue stirring 20 ~ 30min and be precipitated thing, precipitate is stood old
Change, filter, deionized water cyclic washing is to neutrality, then is washed 2 ~ 3 times with dehydrated alcohol, is dried to obtain presoma powder body；
（4）Presoma powder body is placed in Muffle furnace, is warming up to 600 DEG C of calcinings, cooling obtains pure phase bismuth ferric powder body.
Further, in step 3）In, digestion time is 16 ~ 24h, and baking temperature is 50 ~ 60 DEG C.
Further, in step 4）In, heating rate is 10 DEG C/min, and calcination time is 1 ~ 3h.
The present invention adopts chemical coprecipitation process method, obtains bismuth ferrite presoma by controlling pH value of reaction system, then
Calcining through suitable temperature and time obtains the pure phase bismuth ferric powder body with perovskite structure, preparation technology of the present invention and setting
Standby simple, can a property time prepare in a large number, without using organic solvent, environmental protection, and bismuth ferrite complete crystallization, powder granularity is equal
Even.
The present invention compares with prior art, and its technological progress is significant.The invention provides a kind of technological process is simple,
React easily controllable, the environment friendly and pollution-free method preparing pure phase bismuth ferric powder body, the bismuth ferrite prepared in the present inventive method
Powder body is pure phase BiFeO3, complete crystallization, epigranular, and single response magnitude is unrestricted, beneficial to industrialized production.
Brief description：
Fig. 1 is the pure phase bismuth ferric powder body XRD figure of embodiment 1 preparation.
Fig. 2 is the pure phase bismuth ferric powder body XRD figure of embodiment 2 preparation.
Fig. 3 is the pure phase bismuth ferric powder body XRD figure of embodiment 3 preparation.
Fig. 4 is the pure phase bismuth ferric powder body SEM figure of embodiment 1 preparation.
Fig. 5 is the pure phase bismuth ferric powder body SEM figure of embodiment 2 preparation.
Fig. 6 is the pure phase bismuth ferric powder body SEM figure of embodiment 3 preparation.
Specific embodiment
With reference to embodiment and relevant chart, the present invention will be described in detail, but the invention is not restricted to real
Example：
Embodiment 1
Weigh 40.4024g Fe (NO respectively3)3·9H2O and 48.5102g Bi (NO3)3·5H2O
It is dissolved in the HNO that 1L concentration is 1mol/L3It is made into the precursor liquid that concentration of metal ions is 0.2 mol/L, in magnetic in solution
Under power stirring, by slow for precursor aqueous solution equably Deca in 200mL volume ratio be 1：2 NH3·H2O/NH4HCO3Mixed precipitation
Agent（NH4HCO3Concentration is 0.1mol/L）In, terminate when titrating system pH and being 9.5, continue stirring 20min, still aging
16h, reacts the precipitate obtaining through filtering, deionized water wash is to neutrality, then is washed 3 times with dehydrated alcohol, 50 in drying baker
DEG C it is dried to obtain presoma powder body, then presoma powder body is placed in Muffle furnace, calcined to 600 DEG C with 10 DEG C/min ramp
1h, cooling obtains pure phase bismuth ferric powder body.
The XRD phenogram of the present embodiment preparation-obtained pure phase bismuth ferric powder body is as shown in figure 1, from XRD diffracting spectrum
Analysis is learnt, diffraction maximum and PDF#（86-1518）Corresponding good, and peak shape is sharp, and peak is stronger, no dephasign peak, is pure phase ferrum
Sour bismuth meal body.
The SEM figure of the present embodiment preparation-obtained pure phase bismuth ferric powder body as shown in Figure 4 it can be seen that powder granule relatively
Uniformly, granularity 100 nm.
Embodiment 2
Weigh 40.4024g Fe (NO respectively3)3·9H2O and 48.5102g Bi (NO3)3·5H2O
It is dissolved in the HNO that 1L concentration is 1mol/L3It is made into the precursor liquid that concentration of metal ions is 0.2 mol/L, in magnetic in solution
Under power stirring, by slow for precursor aqueous solution equably Deca in 200mL volume ratio be 1：2 NH3·H2O/NH4HCO3Mixed precipitation
Agent（NH4HCO3Concentration is 0.1mol/L）In, terminate when titrating system pH and being 10, continue stirring 20min, still aging
20h, reacts the precipitate obtaining through filtering, deionized water wash is to neutrality, then is washed 3 times with dehydrated alcohol, 50 in drying baker
DEG C it is dried to obtain presoma powder body, then presoma powder body is placed in Muffle furnace, calcined to 600 DEG C with 10 DEG C/min ramp
2h, cooling obtains pure phase bismuth ferric powder body.
The XRD phenogram of the present embodiment preparation-obtained pure phase bismuth ferric powder body is as shown in Fig. 2 from XRD diffracting spectrum
Analysis is learnt, diffraction maximum and PDF#（86-1518）Corresponding good, and peak shape is sharp, and peak is stronger, no dephasign peak, is pure phase ferrum
Sour bismuth meal body.
The SEM figure of the present embodiment preparation-obtained pure phase bismuth ferric powder body as shown in Figure 5 it can be seen that powder granule relatively
Uniformly, granularity 100 nm.
Embodiment 3
Weigh 40.4024g Fe (NO respectively3)3·9H2O and 48.5102g Bi (NO3)3·5H2O
It is dissolved in the HNO that 1L concentration is 1mol/L3It is made into the precursor liquid that concentration of metal ions is 0.2 mol/L, in magnetic in solution
Under power stirring, by slow for precursor aqueous solution equably Deca in 200mL volume ratio be 1：2 NH3·H2O/NH4HCO3Mixed precipitation
Agent（NH4HCO3Concentration is 0.1mol/L）In, terminate when titrating system pH and being 9, continue stirring 20min, still aging 24h,
React the precipitate obtaining through filtering, deionized water wash is to neutrality, then is washed 2 times with dehydrated alcohol, do for 60 DEG C in drying baker
Dry obtain presoma powder body, then presoma powder body is placed in Muffle furnace, with 10 DEG C/min ramp to 600 DEG C of calcining 3h,
Cooling obtains pure phase bismuth ferric powder body.
The XRD phenogram of the present embodiment preparation-obtained pure phase bismuth ferric powder body is as shown in figure 3, from XRD diffracting spectrum
Analysis is learnt, diffraction maximum and PDF#（86-1518）Corresponding good, and peak shape is sharp, and peak is stronger, no dephasign peak, is pure phase ferrum
Sour bismuth meal body.
The SEM figure of the present embodiment preparation-obtained pure phase bismuth ferric powder body as shown in Figure 6 it can be seen that powder granule relatively
Uniformly, granularity 100 nm.
Claims (3)
1. a kind of pure phase bismuth ferric raw powder's production technology is it is characterised in that comprise the steps：
（1）The step of one preparation precursor liquid, by Fe (NO3)3·9H2O and Bi (NO3)3·5H2O is dissolved in 1mol/L HNO3Solution
In, Fe3+：Bi3+Mol ratio be 1：1, obtain the precursor liquid that concentration of metal ions is 0.2 mol/L；
（2）The step of one preparation precipitant, by the ammonium bicarbonate soln of ammonia and 0.1mol/L by volume 1：2 are made into NH3·
H2O/NH4HCO3Mixed solution, as precipitant；
（3）One step preparing presoma, under magnetic stirring, by precursor liquid, equably Deca, in precipitant solution, is dripped
Determine endpoint pH and control in 9 ~ 10, after titration terminates, continue stirring 20 ~ 30min and be precipitated thing, precipitate is stood old
Change, filter, deionized water cyclic washing is to neutrality, then is washed 2 ~ 3 times with dehydrated alcohol, is dried to obtain presoma powder body；
（4）Presoma powder body is placed in Muffle furnace, is warming up to 600 DEG C of calcinings, cooling obtains pure phase bismuth ferric powder body.
2. a kind of pure phase bismuth ferric raw powder's production technology according to claim 1 is it is characterised in that in step 3）In,
Digestion time is 16 ~ 24h, and baking temperature is 50 ~ 60 DEG C.
3. a kind of pure phase bismuth ferric raw powder's production technology according to claim 1 is it is characterised in that in step 4）In,
Heating rate is 10 DEG C/min, and calcination time is 1 ~ 3h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101885868A (en) * | 2010-07-16 | 2010-11-17 | 扬州大学 | Method for preparing magnetic rubber from recovered rubber powder |
| CN102285690A (en) * | 2011-04-12 | 2011-12-21 | 青岛大学 | Chemical coprecipitation method for synthesizing Bi2Fe4O9 submicron rods |
| CN104495944A (en) * | 2014-12-05 | 2015-04-08 | 华南理工大学 | Method for preparing nitrogen-doped bismuth ferrite nano powder |
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- 2016-08-29 CN CN201610755790.3A patent/CN106379944B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101885868A (en) * | 2010-07-16 | 2010-11-17 | 扬州大学 | Method for preparing magnetic rubber from recovered rubber powder |
| CN102285690A (en) * | 2011-04-12 | 2011-12-21 | 青岛大学 | Chemical coprecipitation method for synthesizing Bi2Fe4O9 submicron rods |
| CN104495944A (en) * | 2014-12-05 | 2015-04-08 | 华南理工大学 | Method for preparing nitrogen-doped bismuth ferrite nano powder |
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