CN106379944B - A kind of pure phase bismuth ferric raw powder's production technology - Google Patents
A kind of pure phase bismuth ferric raw powder's production technology Download PDFInfo
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- CN106379944B CN106379944B CN201610755790.3A CN201610755790A CN106379944B CN 106379944 B CN106379944 B CN 106379944B CN 201610755790 A CN201610755790 A CN 201610755790A CN 106379944 B CN106379944 B CN 106379944B
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- precursor liquid
- phase bismuth
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- C—CHEMISTRY; METALLURGY
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention provides a kind of pure phase bismuth ferric raw powder's production technology, including the step of preparation precursor liquid, by Fe (NO3)3·9H2O and Bi (NO3)3·5H2O is dissolved in solution, obtains the precursor liquid that concentration of metal ions is 0.2 mol/L；Ammoniacal liquor is mixed with ammonium bicarbonate soln and obtains precipitating reagent；Under magnetic stirring, precursor liquid is equably added dropwise in precipitant solution, titration end-point pH value is controlled in 9 ~ 10, after titration terminates, continue stirring and obtain sediment, sediment is still aging, filtering, is washed with deionized water and absolute ethyl alcohol, is dried to obtain presoma powder；Presoma powder is placed in Muffle furnace, heating calcining, cooling obtains pure phase bismuth ferric powder.Preparation technology and equipment of the present invention are simple, can a property time is a large amount of prepares, it is green without using organic solvent, and bismuth ferrite complete crystallization, powder granularity are uniform.
Description
Technical field
The invention belongs to chemical field, is related to a kind of bismuth ferrite powder, specifically a kind of pure phase bismuth ferric powder
Preparation method.
Background technology
Pure phase bismuth ferric is only a few at room temperature while has one of ferroelectricity and anti-ferromagnetic multi-ferroic material, this
Kind magnetic makes it before information storage, spin electric device and sensor etc. have wide application with the control of comparing of electricity
Scape, and the focus of Recent study.However, preparing, pure phase bismuth ferric is relatively difficult, and the presence of dephasign causes leakage current larger,
Hamper the development and application of bismuth ferrite material.In recent years, many scholars prepare pure phase bismuth ferric powder by various methods, main
There are solid sintering technology, hydrothermal synthesis method, sol-gel process and chemical coprecipitation.Solid phase method reaction temperature is high, reappearance
Difference, dephasign are more, it is difficult to obtain pure phase bismuth ferric；Although hydrothermal synthesis method can be prepared, particle diameter is small, the complete powder of grain development,
The method need to be reacted under high temperature and high pressure environment, and reaction is whard to control, and high to equipment requirement, certain risk be present；It is molten
Glue-gel method accurately controls the chemical composition of powder, 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 nonhazardous of raw material, and in addition, the method is easy to
Operation, is especially beneficial industrialized production.
The 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
Method, described this pure phase bismuth ferric raw powder's production technology will solve the technique for preparing pure phase bismuth ferric powder in the prior art
Complexity, the pure phase bismuth ferric of acquisition hamper the technology of bismuth ferrite materials application because the presence of dephasign causes leakage current larger
Problem.
The invention provides a kind of pure phase bismuth ferric raw powder's production technology, comprise the following steps：
（1）The step of one preparation precursor liquid, by Fe (NO3)3·9H2O and Bi (NO3)3·5H2O is dissolved in 1mol/L HNO3
In solution, Fe3+：Bi3+Mol ratio be 1：1, obtain the precursor liquid that concentration of metal ions is 0.2 mol/L；
（2）One the step of preparing precipitating reagent, by ammoniacal liquor and 0.1mol/L ammonium bicarbonate soln by volume 1：2 are made into
NH3·H2O/NH4HCO3Mixed solution, as precipitating reagent；
（3）One the step of preparing presoma, under magnetic stirring, precursor liquid is equably added dropwise in precipitant solution
In, titration end-point pH value is controlled in 9 ~ 10, after titration terminates, is continued 20 ~ 30min of stirring and is obtained sediment, and sediment is quiet
Ageing is put, filters, is washed repeatedly to neutrality with deionized water, then is washed 2 ~ 3 times with absolute ethyl alcohol, is dried to obtain presoma powder；
（4）Presoma powder is placed in Muffle furnace, is warming up to 600 DEG C of calcinings, cooling obtains pure phase bismuth ferric powder.
Further, in step 3）In, digestion time is 16 ~ 24h, and drying 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 uses chemical coprecipitation process method, by controlling pH value of reaction system to obtain bismuth ferrite presoma, then
The pure phase bismuth ferric powder with perovskite structure is obtained by the calcining of suitable temperature and time, preparation technology of the present invention and is set
It is standby simple, can a property time is a large amount of prepares, it is green without using organic solvent, and bismuth ferrite complete crystallization, powder granularity are equal
It is 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 for preparing pure phase bismuth ferric powder, the bismuth ferrite prepared in the present inventive method
Powder is pure phase BiFeO3, complete crystallization, epigranular, and single reacting dose is unrestricted, beneficial to industrialized production.
Brief description of the drawings：
Fig. 1 is pure phase bismuth ferric powder XRD prepared by embodiment 1.
Fig. 2 is pure phase bismuth ferric powder XRD prepared by embodiment 2.
Fig. 3 is pure phase bismuth ferric powder XRD prepared by embodiment 3.
Fig. 4 is pure phase bismuth ferric powder SEM figures prepared by embodiment 1.
Fig. 5 is pure phase bismuth ferric powder SEM figures prepared by embodiment 2.
Fig. 6 is pure phase bismuth ferric powder SEM figures prepared by embodiment 3.
Embodiment
With reference to embodiment and relevant chart, the present invention will be described in detail, but real the invention is not restricted to give
Example：
Embodiment 1
40.4024g Fe (NO are weighed respectively3)3·9H2O and 48.5102g Bi (NO3)3·5H2O
It is dissolved in the HNO that 1L concentration is 1mol/L3The precursor liquid that concentration of metal ions is 0.2 mol/L is made into solution,
Under magnetic stirring, it is 1 precursor aqueous solution to be slowly equably added dropwise in 200mL volume ratios：2 NH3·H2O/NH4HCO3Mixing
Precipitating reagent（NH4HCO3Concentration is 0.1mol/L）In, terminate when titrating system pH and being 9.5, continue to stir 20min, stand old
Change 16h, the sediment for reacting to obtain is filtered, and deionized water is washed to neutrality, then is washed 3 times with absolute ethyl alcohol, in drying box
50 DEG C are dried to obtain presoma powder, then presoma powder are placed in Muffle furnace, and being warming up to 600 DEG C with 10 DEG C/min speed forges
1h is burnt, cooling obtains pure phase bismuth ferric powder.
The XRD phenograms of the preparation-obtained pure phase bismuth ferric powder of the present embodiment are as shown in figure 1, from XRD diffracting spectrums
Analysis learns, diffraction maximum and PDF#（86-1518）It is corresponding good, and peak shape is sharp, and peak is stronger, no dephasign peak, is pure phase iron
Sour bismuth meal body.
The SEM figures of the preparation-obtained pure phase bismuth ferric powder of the present embodiment are as shown in Figure 4, it can be seen that powder granule compared with
Uniformly, nm of granularity 100 or so.
Embodiment 2
40.4024g Fe (NO are weighed respectively3)3·9H2O and 48.5102g Bi (NO3)3·5H2O
It is dissolved in the HNO that 1L concentration is 1mol/L3The precursor liquid that concentration of metal ions is 0.2 mol/L is made into solution,
Under magnetic stirring, it is 1 precursor aqueous solution to be slowly equably added dropwise in 200mL volume ratios：2 NH3·H2O/NH4HCO3Mixing
Precipitating reagent（NH4HCO3Concentration is 0.1mol/L）In, terminate when titrating system pH and being 10, continue to stir 20min, stand old
Change 20h, the sediment for reacting to obtain is filtered, and deionized water is washed to neutrality, then is washed 3 times with absolute ethyl alcohol, in drying box
50 DEG C are dried to obtain presoma powder, then presoma powder are placed in Muffle furnace, and being warming up to 600 DEG C with 10 DEG C/min speed forges
2h is burnt, cooling obtains pure phase bismuth ferric powder.
The XRD phenograms of the preparation-obtained pure phase bismuth ferric powder of the present embodiment are as shown in Fig. 2 from XRD diffracting spectrums
Analysis learns, diffraction maximum and PDF#（86-1518）It is corresponding good, and peak shape is sharp, and peak is stronger, no dephasign peak, is pure phase iron
Sour bismuth meal body.
The SEM figures of the preparation-obtained pure phase bismuth ferric powder of the present embodiment are as shown in Figure 5, it can be seen that powder granule compared with
Uniformly, nm of granularity 100 or so.
Embodiment 3
40.4024g Fe (NO are weighed respectively3)3·9H2O and 48.5102g Bi (NO3)3·5H2O
It is dissolved in the HNO that 1L concentration is 1mol/L3The precursor liquid that concentration of metal ions is 0.2 mol/L is made into solution,
Under magnetic stirring, it is 1 precursor aqueous solution to be slowly equably added dropwise in 200mL volume ratios：2 NH3·H2O/NH4HCO3Mixing
Precipitating reagent（NH4HCO3Concentration is 0.1mol/L）In, terminate when titrating system pH and being 9, continue to stir 20min, it is still aging
24h, the sediment for reacting to obtain is filtered, and deionized water is washed to neutrality, then is washed 2 times with absolute ethyl alcohol, 60 in drying box
DEG C presoma powder is dried to obtain, then presoma powder is placed in Muffle furnace, 600 DEG C of calcinings are warming up to 10 DEG C/min speed
3h, cooling obtain pure phase bismuth ferric powder.
The XRD phenograms of the preparation-obtained pure phase bismuth ferric powder of the present embodiment are as shown in figure 3, from XRD diffracting spectrums
Analysis learns, diffraction maximum and PDF#（86-1518）It is corresponding good, and peak shape is sharp, and peak is stronger, no dephasign peak, is pure phase iron
Sour bismuth meal body.
The SEM figures of the preparation-obtained pure phase bismuth ferric powder of the present embodiment are as shown in Figure 6, it can be seen that powder granule compared with
Uniformly, nm of granularity 100 or so.
Claims (1)
1. a kind of pure phase bismuth ferric raw powder's production technology, it is characterised in that comprise the following 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）One the step of preparing precipitating reagent, by ammoniacal liquor and 0.1mol/L ammonium bicarbonate soln by volume 1：2 are made into NH3·
H2O/NH4HCO3Mixed solution, as precipitating reagent；
（3）One the step of preparing presoma, under magnetic stirring, precursor liquid is equably added dropwise in precipitant solution, dripped
Endpoint pH control is determined in 9 ~ 10, after titration terminates, is continued 20 ~ 30min of stirring and is obtained sediment, sediment is stood old
Change, digestion time is 16 ~ 24h, filtering, is washed repeatedly to neutrality with deionized water, then is washed 2 ~ 3 times with absolute ethyl alcohol, 50 ~ 60
Presoma powder is dried to obtain at a temperature of DEG C；
（4）Presoma powder is placed in Muffle furnace, is warming up to 600 DEG C of calcinings, heating rate is 10 DEG C/min, after calcining 1 ~ 3h
Cooling obtains pure phase bismuth ferric powder.
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