CN104495944A - Method for preparing nitrogen-doped bismuth ferrite nano powder - Google Patents

Method for preparing nitrogen-doped bismuth ferrite nano powder Download PDF

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CN104495944A
CN104495944A CN201410740129.6A CN201410740129A CN104495944A CN 104495944 A CN104495944 A CN 104495944A CN 201410740129 A CN201410740129 A CN 201410740129A CN 104495944 A CN104495944 A CN 104495944A
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warming
bismuth ferrite
solution
nano powder
doping
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CN104495944B (en
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张弜
陈龙胜
张家敏
陈熹
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South China University of Technology SCUT
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Abstract

The invention discloses a method for preparing nitrogen-doped bismuth ferrite nano powder. The method comprises the following steps: (1) respectively dissolving bismuth nitrate pentahydrate and iron nitrate nonahydrate which are weighed according to a mole number of 1:1 in dilute nitric acid, adding tartaric acid and urea, dissolving by stirring to obtain a solution; (2) preheating the solution for 1 to 3h in a 55-65 DEG C oil bath by stirring, and then reacting by sufficiently stirring at a temperature of 105 to 115 DEG C until the solution is fully evaporated to dryness to form a dry gel; (3) grinding the dry gel into powder, presintering for 1 to 3h in a muffle furnace at a temperature of 300 to 500 DEG C, sintering for 0.5 to 2h at a temperature of 600 to 800 DEG C, and performing furnace cooling; and (4) putting the sintered powder into a dilute nitric acid solution to stir for 1 to 3h, repeatedly washing with deionized water and performing suction filtration, and drying in a vacuum at a temperature of 60 to 100 DEG C. The bismuth ferrite structure of the product provided by the invention keeps unchanged as a whole and the ferromagnetism appears.

Description

A kind of preparation method of N doping bismuth ferrite nano powder
Technical field
The present invention relates to the multi-ferroic material field with ferromagnetic and ferroelectric two kinds of characteristics, particularly a kind of preparation method of N doping bismuth ferrite nano powder.
Background technology
In recent years, multi-ferroic material causes the great interest of material and Condensed Matter Physics area research persons as one of type material with application prospect most.Because magneticsubstance and ferroelectric material combine by multi-ferroic material, in device layout, there is the degree of freedom that new.Therefore, multi-ferroic material shows the prospect of practical application in multiple field.In numerous single-phase multi-ferroic material, bismuth ferrite (BiFeO 3) be one of material that research is the most popular at present.It is a kind of typical multi-ferroic material, has higher ferromagnetic transformation temperature T n~ 643K and ferroelectric transition temperature Tc ~ 1103K is current uniquely a kind of single-phase multi-ferroic material simultaneously at normal temperatures with ferroelectricity and parasitic weak ferromagnetism.
At present, BiFeO 3the leakage current that middle existence is larger and the weak magnetic that spiral magnetic structure causes, become BiFeO 3enter the major obstacle of practical application.Improve BiFeO 3the Main Means of performance has growing film and chemical doping.Chemical doping selects the ion pair BiFeO of different size usually 3a position and B position substitute, be equivalent in original lattice introduce a chemical pressure, can BiFeO be made 3lattice distort, thus improve the ferroelectricity of material and ferromegnetism.But it is also few for the doping substitution studies of O position.
Summary of the invention
In order to overcome the above-mentioned shortcoming of prior art with not enough, the object of the present invention is to provide a kind of preparation method of N doping bismuth ferrite nano powder, keeping BiFeO on the whole 3ferromegnetism is there is while structure is constant.
Object of the present invention is achieved through the following technical solutions:
A preparation method for N doping bismuth ferrite nano powder, comprises the following steps:
(1) weigh five appropriate water Bismuth trinitrates by mole number 1:1 and nine water iron nitrates are dissolved in dust technology respectively, add tartrate and urea, stirring and dissolving, obtain solution;
Fe in described urea and solution 3+the mol ratio of ion is (0.5 ~ 1.2): 1;
(2) solution step (1) obtained is preheating 1 ~ 3h under 55 ~ 65 DEG C of oil baths are stirred, and then at being warming up to 105 ~ 115 DEG C abundant stirring reaction until evaporate to dryness formation xerogel completely;
(3) by xerogel grind into powder, be warming up to 300 ~ 500 DEG C of pre-burning 1 ~ 3h at retort furnace, then be warming up to 600 ~ 800 DEG C of sintering 0.5 ~ 2h, then with stove naturally cooling;
(4) powder after sintering is dropped into stirring and washing 1 ~ 3h in dilute nitric acid solution, then repeatedly rinse and suction filtration with deionized water, finally at 60 ~ 100 DEG C, namely vacuum-drying obtain the bismuth ferrate nano powder of N doping.
Fe in step (1) described tartrate and solution 3+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), is specially:
300 ~ 500 DEG C are warming up to according to per minute 5 ~ 10 DEG C from room temperature.
Step is warming up to 600 ~ 800 DEG C described in (3), is specially:
600 ~ 800 DEG C are warming up to according to the speed of per minute 5 ~ 10 DEG C.
The present invention makes metal ion and tartrate generation complex reaction be formed on the basis of colloidal sol at sol-gel method, adds urea uniform dissolution in wherein, finally forms the uniform gelinite of rich Nitrogen element; The temperature and time of conservative control gelation prevents hydrolysis of urea, through super-dry and conservative control calcining temperature and time, makes nitrogenous source decompose and fully be added to bismuth ferrite and crystallizes in the process of phase, obtain the bismuth ferrite powder of N doping.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) the present invention achieves nitrogen Some substitute oxygen in bismuth ferrite crystal lattices first on the basis of collosol and gel.
(2) the present invention can avoid usually on bismuth position or iron position doping substitute may cause ferroelectric-phase transformation of para-electric formula, substituted by oxygen position and affect the original strong ferroelectric structures of bismuth ferrite as few as possible.
(3) the present invention is by N doping, and the local distortion making bismuth ferrite while bulk crystal structure is constant to bring out because adulterating produces ferromegnetism.
Accompanying drawing explanation
Fig. 1 is the N doping bismuth ferrite of embodiment 1 gained and the X-ray diffractogram of pure bismuth ferrite nanometer powder.
Fig. 2 is the N doping bismuth ferrite of embodiment 2 gained and pure bismuth ferrite nanometer powder x-ray photoelectron power spectrum (XPS).
Fig. 3 is the N doping bismuth ferrite of embodiment 3 gained and the magnetic hysteresis loop of pure bismuth ferrite nanometer powder.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
1:1 weighs 1.213g five water Bismuth trinitrate and 1.01g nine water iron nitrate is dissolved in 50ml dust technology respectively in molar ratio; Then the dilution of 50ml deionized water is added, Fe in the mixing solutions finally obtained 3+concentration be about 0.025mol/L, then by and Fe 3+ion is that the mol ratio of 1:1 adds tartrate, finally by changing and Fe 3+ion is that the mol ratio of 1.2:1 adds urea in above-mentioned solution; By gained solution preheating 1h under 55 DEG C of oil baths are stirred, and then at being warming up to 105 DEG C abundant stirring reaction until evaporate to dryness formation xerogel completely; By xerogel grind into powder, pre-burning 2h at 300 DEG C in retort furnace, then be warming up to 600 DEG C of sintering 1h, then with stove naturally cooling; It is stirring and washing 1h in the dilute nitric acid solution of 1M/L that powder after sintering is dropped into concentration, and then repeatedly rinse and suction filtration with deionized water, finally at 80 DEG C, namely vacuum-drying obtain the bismuth ferrate nano powder of N doping.
According to the XPS spectrum of the product of the present embodiment, by calculate can draw sample consist of BiFeO 1.8n 1.2.Fig. 1 is the XRD spectra of the product of the present embodiment, can find out to compare with pure bismuth ferrite, and after N doping, the structure of sample does not change.The magnetic hysteresis loop after tested of the product of the present embodiment, confirms to present weak magnetic.
Embodiment 2
1:1 weighs 1.213g five water Bismuth trinitrate and 1.01g nine water iron nitrate is dissolved in 50ml dust technology respectively in molar ratio; Then the dilution of 50ml deionized water is added, Fe in the mixing solutions finally obtained 3+concentration be about 0.025mol/L, then by and Fe 3+ion is that the mol ratio of 1:1 adds tartrate, finally by changing and Fe 3+ion is that the mol ratio of 0.9:1 adds urea in above-mentioned solution; By gained solution preheating 1.5h under 60 DEG C of oil baths are stirred, and then at being warming up to 110 DEG C abundant stirring reaction until evaporate to dryness formation xerogel completely; By xerogel grind into powder, pre-burning 2h at 350 DEG C in retort furnace, then be warming up to 650 DEG C of sintering 1h, then with stove naturally cooling; It is stirring and washing 1h in the dilute nitric acid solution of 1M/L that powder after sintering is dropped into concentration, and then repeatedly rinse and suction filtration with deionized water, finally at 90 DEG C, namely vacuum-drying obtain the bismuth ferrate nano powder of N doping.
Fig. 2 is the XPS spectrum of products therefrom, and doped products has found the characteristic peak (in figure dotted line frame in) of N as seen from Figure 2, by calculate can draw sample consist of BiFeO 2.1n 0.9.The XRD spectra of the product of the present embodiment is similar to embodiment 1, can find out to compare with pure bismuth ferrite, and after N doping, the structure of sample does not change.The magnetic hysteresis loop after tested of the product of the present embodiment, confirms to present weak magnetic.
Embodiment 3
1:1 weighs 1.213g five water Bismuth trinitrate and 1.01g nine water iron nitrate is dissolved in 50ml dust technology respectively in molar ratio; Then the dilution of 50ml deionized water is added, Fe in the mixing solutions finally obtained 3+concentration be about 0.025mol/L, then by and Fe 3+ion is that the mol ratio of 1:1 adds tartrate, finally by changing and Fe 3+ion is that the mol ratio of 0.5:1 adds urea in above-mentioned solution; By gained solution preheating 2h under 65 DEG C of oil baths are stirred, and then at being warming up to 110 DEG C abundant stirring reaction until evaporate to dryness formation xerogel completely; By xerogel grind into powder, pre-burning 2h at 400 DEG C in retort furnace, then be warming up to 750 DEG C of sintering 2h, then with stove naturally cooling; It is stirring and washing 1.5h in the dilute nitric acid solution of 1M/L that powder after sintering is dropped into concentration, and then repeatedly rinse and suction filtration with deionized water, finally at 110 DEG C, namely vacuum-drying obtain the bismuth ferrate nano powder of N doping.
According to the XPS spectrum of the product of the present embodiment, by calculate can draw sample consist of BiFeO 2.5n 0.5.The XRD spectra of the product of the present embodiment is similar to embodiment 1, can find out to compare with pure bismuth ferrite, and after N doping, the structure of sample does not change.Fig. 3 is the magnetic hysteresis loop of product, can find out with pure BiFeO 3compare, the sample of N doping has obvious loop line, presents weak magnetic.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not limited by the examples; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.

Claims (6)

1. a preparation method for N doping bismuth ferrite nano powder, is characterized in that, comprises the following steps:
(1) by mole number 1:1 weigh five water Bismuth trinitrates and nine water iron nitrates be dissolved in respectively in dust technology, add tartrate and urea, stirring and dissolving, obtain solution;
Fe in described urea and solution 3+the mol ratio of ion is (0.5 ~ 1.2): 1;
(2) solution step (1) obtained is preheating 1 ~ 3h under 55 ~ 65 DEG C of oil baths are stirred, and then at being warming up to 105 ~ 115 DEG C abundant stirring reaction until evaporate to dryness formation xerogel completely;
(3) by xerogel grind into powder, be warming up to 300 ~ 500 DEG C of pre-burning 1 ~ 3h at retort furnace, then be warming up to 600 ~ 800 DEG C of sintering 0.5 ~ 2h, then with stove naturally cooling;
(4) powder after sintering is dropped into stirring and washing 1 ~ 3h in dilute nitric acid solution, then repeatedly rinse and suction filtration with deionized water, finally at 60 ~ 100 DEG C, namely vacuum-drying obtain the bismuth ferrate nano powder of N doping.
2. the preparation method of N doping bismuth ferrite nano powder according to claim 1, is characterized in that, Fe in step (1) described tartrate and solution 3+the mol ratio of ion is 1:1.
3. the preparation method of N doping bismuth ferrite nano powder according to claim 1, is characterized in that, the concentration of step (1) described dust technology is 1M/L.
4. the preparation method of N doping bismuth ferrite nano powder according to claim 1, is characterized in that, the concentration of step (4) described dust technology is 1M/L.
5. the preparation method of N doping bismuth ferrite nano powder according to claim 1, is characterized in that, step is warming up to 300 ~ 500 DEG C described in (3), is specially:
300 ~ 500 DEG C are warming up to according to per minute 5 ~ 10 DEG C from room temperature.
6. the preparation method of N doping bismuth ferrite nano powder according to claim 1, is characterized in that, step is warming up to 600 ~ 800 DEG C described in (3), is specially:
600 ~ 800 DEG C are warming up to according to the speed of per minute 5 ~ 10 DEG C.
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Cited By (6)

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CN106379944A (en) * 2016-08-29 2017-02-08 上海应用技术学院 Preparation method of pure-phase bismuth ferrite
RU2641203C2 (en) * 2016-05-04 2018-01-16 Федеральное государственное бюджетное образовательное учреждение высшего образования "ДАГЕСТАНСКИЙ ГОСУДАРСТВЕННЫЙ УНИВЕРСИТЕТ" Method of producing bismuth ferrite nanopowder
CN110451575A (en) * 2019-09-11 2019-11-15 哈尔滨工业大学 A method of bismuth ferrate nano powder magnetic is enhanced based on dimensional 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
RU2782944C1 (en) * 2022-07-13 2022-11-07 федеральное государственное бюджетное образовательное учреждение высшего образования "Южно-Российский государственный политехнический университет (НПИ) имени М.И. Платова" Method for obtaining composite coatings based on bismuth ferrites on the surface of steel

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Cited By (7)

* Cited by examiner, † Cited by third party
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
CN106379944A (en) * 2016-08-29 2017-02-08 上海应用技术学院 Preparation method of pure-phase bismuth ferrite
CN110451575A (en) * 2019-09-11 2019-11-15 哈尔滨工业大学 A method of bismuth ferrate nano powder magnetic is enhanced based on dimensional effect
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
RU2782944C1 (en) * 2022-07-13 2022-11-07 федеральное государственное бюджетное образовательное учреждение высшего образования "Южно-Российский государственный политехнический университет (НПИ) имени М.И. Платова" Method for obtaining composite coatings based on bismuth ferrites on the surface of steel

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