CN104495944B - A kind of preparation method of N doping bismuth ferrite nano powder - Google Patents
A kind of preparation method of N doping bismuth ferrite nano powder Download PDFInfo
- Publication number
- CN104495944B CN104495944B CN201410740129.6A CN201410740129A CN104495944B CN 104495944 B CN104495944 B CN 104495944B CN 201410740129 A CN201410740129 A CN 201410740129A CN 104495944 B CN104495944 B CN 104495944B
- Authority
- CN
- China
- Prior art keywords
- bismuth ferrite
- preparation
- powder
- nano powder
- doping
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Hard Magnetic Materials (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention discloses the preparation method of a kind of N doping bismuth ferrite nano powder, comprise the following steps: five water bismuth nitrate and nine water ferric nitrates that (1) is weighed by molal quantity 1:1 are dissolved in dust technology respectively, add tartaric acid and carbamide, stirring and dissolving, obtain solution；(2) solution being preheated under 55～65 DEG C of oil bath stirrings 1～3h, at 105～115 DEG C, being then sufficiently stirred for reaction until being evaporated formation xerogel completely；(3) by xerogel grind into powder, at Muffle furnace in 300～500 DEG C of pre-burnings 1～3h, 0.5～2h is sintered at 600～800 DEG C, furnace cooling；(4) powder after sintering is put into stirring 1～3h in dilute nitric acid solution, repeatedly rinse with deionized water and sucking filtration, be vacuum dried at 60～100 DEG C.There is ferromagnetism while keeping bismuth ferrite structure constant on the whole in the product of the present invention.
Description
Technical field
The present invention relates to that there is ferromagnetic and two kinds of characteristics of ferroelectricity multi-ferroic material field, particularly to a kind of nitrogen
Doped bismuth ferrite nano raw powder's production technology.
Background technology
In recent years, multi-ferroic material cause as one of new material with application prospect most material and
The great interest of Condensed Matter Physics area research persons.Owing to multi-ferroic material is by magnetic material and ferroelectric material
Combine, had a new degree of freedom at device design aspect.Therefore, multi-ferroic material is at multiple necks
Territory shows the prospect of actual application.In numerous single-phase multi-ferroic materials, bismuth ferrite (BiFeO3) it is mesh
One of material that front research is the most popular.It is a kind of typical multi-ferroic material, has higher ferromagnetic transformation
Temperature TN～643K and ferroelectricity transition temperature Tc～1103K, it is that currently the only one has the most simultaneously
There are ferroelectricity and the single-phase multi-ferroic material of parasitic weak ferromagnetism.
At present, BiFeO3Leakage current that middle existence is bigger and the weak magnetic that spiral magnetic structure causes, become
BiFeO3Enter the major obstacle of reality application.Improve BiFeO3The Main Means of performance has growing film and change
Learn doping.Chemical doping is generally selected different size of ion pair BiFeO3A position and B position substitute,
Be equivalent to introduce a chemical pressure in original lattice, BiFeO can be made3Lattice be distorted, from
And improve ferroelectricity and the ferromagnetism of material.But the doping substitution studies for O position is the most few.
Summary of the invention
In order to overcome the disadvantages mentioned above of prior art with not enough, it is an object of the invention to provide a kind of N doping
The preparation method of bismuth ferrite nano powder, keeps BiFeO on the whole3While structure is constant, ferromagnetism occurs.
The purpose of the present invention is achieved through the following technical solutions:
The preparation method of a kind of N doping bismuth ferrite nano powder, comprises the following steps:
(1) weigh five appropriate water bismuth nitrate by molal quantity 1:1 and nine water ferric nitrates be dissolved in dust technology respectively,
Add tartaric acid and carbamide, stirring and dissolving, obtain solution；
Described carbamide and Fe in solution3+The mol ratio of ion is (0.5～1.2): 1；
(2) solution step (1) obtained preheats 1～3h under 55～65 DEG C of oil bath stirrings, rises the most again
Temperature is sufficiently stirred for reaction until being evaporated formation xerogel completely at 105～115 DEG C；
(3) by xerogel grind into powder, it is warming up to 300～500 DEG C of pre-burnings 1～3h at Muffle furnace, then rises
Temperature is to 600～800 DEG C of sintering 0.5～2h, then with stove natural cooling；
(4) powder after sintering is put into stirring and washing 1～3h in dilute nitric acid solution, then use deionized water
Repeatedly rinse and sucking filtration, at 60～100 DEG C, be finally vacuum dried the bismuth ferrate nano powder i.e. obtaining N doping.
Step (1) described tartaric acid and Fe in solution3+The mol ratio of ion is 1:1.
The concentration of step (1) described dust technology is 1M/L.
The concentration of step (4) described dust technology is 1M/L.
Step is warming up to 300～500 DEG C described in (3), particularly as follows:
It is warming up to 300～500 DEG C according to 5～10 DEG C per minute from room temperature.
Step is warming up to 600～800 DEG C described in (3), particularly as follows:
It is warming up to 600～800 DEG C according to the speed of 5～10 DEG C per minute.
The present invention makes metal ion and tartaric acid generation complex reaction form the basis of colloidal sol at sol-gal process
On, addition carbamide uniform dissolution, in wherein, eventually forms the uniform gelinite of rich Nitrogen element；Rationally control
The temperature and time of gelation processed prevents hydrolysis of urea, through being dried and conservative control calcining heat and time,
Make nitrogen source decompose and be fully dissolved in bismuth ferrite to crystallize into during mutually, obtain the bismuth ferrite powder of N doping.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) present invention achieves nitrogen part replacement in bismuth ferrite crystal lattices first on the basis of collosol and gel
Oxygen.
(2) present invention can avoid ferroelectricity-para-electric formula that generally doping replacement may cause on bismuth position or ferrum position
Phase transformation, is substituted by oxygen position and affects the original strong ferroelectric structures of bismuth ferrite as few as possible.
(3) present invention passes through N doping, makes bismuth ferrite while bulk crystal structure is constant because of doping induction
Local distortion produce ferromagnetism.
Accompanying drawing explanation
Fig. 1 is N doping bismuth ferrite and the X-ray diffractogram of pure bismuth ferrite nanometer powder of embodiment 1 gained.
Fig. 2 is the N doping bismuth ferrite of embodiment 2 gained and pure bismuth ferrite nanometer powder x-ray photoelectron energy
Spectrum (XPS).
Fig. 3 is N doping bismuth ferrite and the hysteresis curve of pure bismuth ferrite nanometer powder of embodiment 3 gained.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not
It is limited to this.
Embodiment 1
1:1 weighs 1.213g five water bismuth nitrate respectively and 1.01g nine water ferric nitrate is dissolved in 50ml in molar ratio
In dust technology；It is subsequently adding the dilution of 50ml deionized water, Fe in the mixed solution finally obtained3+Concentration
It is about 0.025mol/L, then presses and Fe3+Ion be 1:1 mol ratio add tartaric acid, finally by change with
Fe3+Ion is that the mol ratio of 1.2:1 adds carbamide in above-mentioned solution；Gained solution is stirred 55 DEG C of oil baths
Mixing lower preheating 1h, being warming up at 105 DEG C be sufficiently stirred for reaction the most again until being evaporated formation xerogel completely；
By xerogel grind into powder, pre-burning 2h at 300 DEG C in Muffle furnace, then it is warming up to 600 DEG C of sintering 1h,
Then with stove natural cooling；Powder after sintering is put into stirring in the dilute nitric acid solution that concentration is 1M/L clear
Wash 1h, then repeatedly rinse with deionized water and sucking filtration, be finally vacuum dried at 80 DEG C and i.e. obtain N doping
Bismuth ferrate nano powder.
The XPS spectrum of the product according to the present embodiment, can draw consisting of of sample by calculating
BiFeO1.8N1.2.Fig. 1 is the XRD spectra of the product of the present embodiment, it can be seen that compared with pure bismuth ferrite,
After N doping, the structure of sample does not change.The hysteresis curve after tested of the product of the present embodiment, it was demonstrated that
Present weak magnetic.
Embodiment 2
1:1 weighs 1.213g five water bismuth nitrate respectively and 1.01g nine water ferric nitrate is dissolved in 50ml in molar ratio
In dust technology；It is subsequently adding the dilution of 50ml deionized water, Fe in the mixed solution finally obtained3+Concentration
It is about 0.025mol/L, then presses and Fe3+Ion be 1:1 mol ratio add tartaric acid, finally by change with
Fe3+Ion is that the mol ratio of 0.9:1 adds carbamide in above-mentioned solution；Gained solution is stirred 60 DEG C of oil baths
Mixing lower preheating 1.5h, being warming up at 110 DEG C be sufficiently stirred for reaction the most again until being evaporated formation xerogel completely；
By xerogel grind into powder, pre-burning 2h at 350 DEG C in Muffle furnace, then it is warming up to 650 DEG C of sintering 1h,
Then with stove natural cooling；Powder after sintering is put into stirring in the dilute nitric acid solution that concentration is 1M/L clear
Wash 1h, then repeatedly rinse with deionized water and sucking filtration, be finally vacuum dried at 90 DEG C and i.e. obtain N doping
Bismuth ferrate nano powder.
Fig. 2 is the XPS spectrum of products therefrom, and doped products is found that the characteristic peak (figure of N as seen from Figure 2
In middle dotted line frame), by calculate can draw sample consist of BiFeO2.1N0.9.The product of the present embodiment
XRD spectra is similar to Example 1, it can be seen that compared with pure bismuth ferrite, and after N doping, the structure of sample does not has
Change.The hysteresis curve after tested of the product of the present embodiment, it was demonstrated that present weak magnetic.
Embodiment 3
1:1 weighs 1.213g five water bismuth nitrate respectively and 1.01g nine water ferric nitrate is dissolved in 50ml in molar ratio
In dust technology；It is subsequently adding the dilution of 50ml deionized water, Fe in the mixed solution finally obtained3+Concentration
It is about 0.025mol/L, then presses and Fe3+Ion be 1:1 mol ratio add tartaric acid, finally by change with
Fe3+Ion is that the mol ratio of 0.5:1 adds carbamide in above-mentioned solution；Gained solution is stirred 65 DEG C of oil baths
Mixing lower preheating 2h, being warming up at 110 DEG C be sufficiently stirred for reaction the most again until being evaporated formation xerogel completely；
By xerogel grind into powder, pre-burning 2h at 400 DEG C in Muffle furnace, then it is warming up to 750 DEG C of sintering 2h,
Then with stove natural cooling；Powder after sintering is put into stirring in the dilute nitric acid solution that concentration is 1M/L clear
Wash 1.5h, then repeatedly rinse with deionized water and sucking filtration, be finally vacuum dried at 110 DEG C and i.e. obtain nitrogen and mix
Miscellaneous bismuth ferrate nano powder.
The XPS spectrum of the product according to the present embodiment, can draw consisting of of sample by calculating
BiFeO2.5N0.5.The XRD spectra of the product of the present embodiment is similar to Example 1, it can be seen that with pure iron acid
Bismuth is compared, and after N doping, the structure of sample does not change.Fig. 3 is the hysteresis curve of product, can see
Go out with pure BiFeO3Comparing, the sample of N doping has obvious loop line, presents weak magnetic.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by described reality
Execute the restriction of example, the change made under other any spirit without departing from the present invention and principle, modification,
Substitute, combine, simplify, all should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (6)
1. the preparation method of a N doping bismuth ferrite nano powder, it is characterised in that comprise the following steps:
(1) five water bismuth nitrate and the nine water ferric nitrates weighed by molal quantity 1:1 are dissolved in dust technology respectively, add
Enter tartaric acid and carbamide, stirring and dissolving, obtain solution；
Described carbamide and Fe in solution3+The mol ratio of ion is (0.5～1.2): 1；
(2) solution step (1) obtained preheats 1～3h under 55～65 DEG C of oil bath stirrings, rises the most again
Temperature is sufficiently stirred for reaction until being evaporated formation xerogel completely at 105～115 DEG C；
(3) by xerogel grind into powder, it is warming up to 300～500 DEG C of pre-burnings 1～3h at Muffle furnace, then rises
Temperature is to 600～800 DEG C of sintering 0.5～2h, then with stove natural cooling；
(4) powder after sintering is put into stirring and washing 1～3h in dilute nitric acid solution, then use deionized water
Repeatedly rinse and sucking filtration, at 60～100 DEG C, be finally vacuum dried the bismuth ferrite nano powder i.e. obtaining N doping.
The preparation method of N doping bismuth ferrite nano powder the most according to claim 1, it is characterised in that
Step (1) described tartaric acid and Fe in solution3+The mol ratio of ion is 1:1.
The preparation method of N doping bismuth ferrite nano powder the most according to claim 1, it is characterised in that
The concentration of step (1) described dust technology is 1M.
The preparation method of N doping bismuth ferrite nano powder the most according to claim 1, it is characterised in that
The concentration of step (4) described dust technology is 1M.
The preparation method of N doping bismuth ferrite nano powder the most according to claim 1, it is characterised in that
Step is warming up to 300～500 DEG C described in (3), particularly as follows:
It is warming up to 300～500 DEG C according to 5～10 DEG C per minute from room temperature.
The preparation method of N doping bismuth ferrite nano powder the most according to claim 1, it is characterised in that
Step is warming up to 600～800 DEG C described in (3), particularly as follows:
It is warming up to 600～800 DEG C according to the speed of 5～10 DEG C per minute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410740129.6A CN104495944B (en) | 2014-12-05 | 2014-12-05 | A kind of preparation method of N doping bismuth ferrite nano powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410740129.6A CN104495944B (en) | 2014-12-05 | 2014-12-05 | A kind of preparation method of N doping bismuth ferrite nano powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104495944A CN104495944A (en) | 2015-04-08 |
| CN104495944B true CN104495944B (en) | 2016-08-24 |
Family
ID=52937424
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410740129.6A Active CN104495944B (en) | 2014-12-05 | 2014-12-05 | A kind of preparation method of N doping bismuth ferrite nano powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104495944B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2641203C2 (en) * | 2016-05-04 | 2018-01-16 | Федеральное государственное бюджетное образовательное учреждение высшего образования "ДАГЕСТАНСКИЙ ГОСУДАРСТВЕННЫЙ УНИВЕРСИТЕТ" | Method of producing bismuth ferrite nanopowder |
| CN106379944B (en) * | 2016-08-29 | 2018-03-13 | 上海应用技术学院 | A kind of pure phase bismuth ferric raw powder's production technology |
| CN110451575B (en) * | 2019-09-11 | 2022-04-05 | 哈尔滨工业大学 | Method for enhancing magnetic property of bismuth ferrite nanopowder based on size effect |
| CN113149080A (en) * | 2021-06-11 | 2021-07-23 | 中国科学技术大学 | Multiferroic bismuth ferrite nano-particle and preparation method thereof |
| CN114308097A (en) * | 2021-12-06 | 2022-04-12 | 哈尔滨学院 | Preparation method of nitrogen/bismuth ferrite-graphene composite material |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5267971B2 (en) * | 2008-03-21 | 2013-08-21 | 国立大学法人金沢大学 | Ferroelectric material and piezoelectric material |
| CN102320666B (en) * | 2011-06-21 | 2013-04-03 | 南京大学 | Preparation method for substituting fluorine for oxygen in bismuth ferrite crystal lattices |
| KR101394340B1 (en) * | 2012-06-21 | 2014-05-14 | 창원대학교 산학협력단 | Fabrication method of Zn and Ti-doped BiFeO3 Thin Film |
| CN104078564A (en) * | 2014-07-04 | 2014-10-01 | 南京邮电大学 | Resistive random access memory based on doped bismuth ferrite and preparing method of resistive random access memory |
-
2014
- 2014-12-05 CN CN201410740129.6A patent/CN104495944B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN104495944A (en) | 2015-04-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104495944B (en) | A kind of preparation method of N doping bismuth ferrite nano powder | |
| CN107322002B (en) | Rare earth oxide doped tungsten-based composite powder and preparation method thereof | |
| CN105384192B (en) | Method for preparing one-dimensional nanorod self-assembled flower type three-dimensional Nb2O5 | |
| Liu et al. | Cu-doping effect on structure and magnetic properties of Fe-doped ZnO powders | |
| CN108706637B (en) | A kind of preparation method of adjustable magnetic iron oxide mesomorphic material of uniform size | |
| CN101913854B (en) | Preparation method of nanometer strontium ferrite magnetic powder | |
| CN104071843A (en) | Preparation method of monodispersed M-phase vanadium dioxide nanoparticles | |
| CN101786668A (en) | Low-temperature preparation method of Co ferrite Nano powder | |
| CN102674825A (en) | Preparation method of M-type barium ferrite magnetic powder | |
| CN104925863A (en) | Preparation method of monoclinic structure vanadium dioxide powder | |
| CN105032397A (en) | Method for synthesizing bismuth vanadate photocatalyst through starch self-combustion | |
| CN102502821B (en) | Mixed organic solvent-thermal method for preparing spherical or hollow spherical BiVO4 | |
| CN103086706B (en) | Preparation method for Zr-Mn-Co multi-doped barium ferrite wave-absorbing material | |
| CN105731396B (en) | A kind of carbon containing item chain nano tellurium nickel and its preparation, application | |
| CN102285690A (en) | Chemical coprecipitation method for synthesizing Bi2Fe4O9 submicron rods | |
| CN106745303B (en) | A kind of three-dimensional flower ball-shaped cadmium ferrite bismuth meal body and preparation method thereof | |
| Banoth et al. | Structural, dielectric, magnetic, and ferroelectric properties of bismuth ferrite (BiFeO3) synthesized by a solvothermal process using hexamethylenetetramine (HMTA) as precipitating agent | |
| CN104973859A (en) | Preparation method for composite ferrite powder with exchange coupling effect | |
| CN106268844A (en) | Preparation method of photocatalyst bismuth ferrite | |
| CN103787420A (en) | Method for preparing SrFe12O19 magnetic nano powder by using microwave hydrothermal method | |
| CN108395542A (en) | A kind of MOFs nanocrystalline materials and preparation method thereof of porous membrane substrate regulation and control | |
| CN105948135B (en) | A kind of monodisperse porous magnetic sub-micro ball and preparation method thereof | |
| Jiang et al. | Synthesis of polycrystalline CoFe2O4 and NiFe2O4 powders by auto-combustion method using a novel amino-based gel | |
| CN104402050B (en) | D phase hypovanadic oxide nanometer star powder and preparation method thereof | |
| CN104495947B (en) | A kind of method preparing receiving bore croci |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |