CN106006752A - Preparation method of pure-phase BiFeO3 powder - Google Patents
Preparation method of pure-phase BiFeO3 powder Download PDFInfo
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- CN106006752A CN106006752A CN201610325853.1A CN201610325853A CN106006752A CN 106006752 A CN106006752 A CN 106006752A CN 201610325853 A CN201610325853 A CN 201610325853A CN 106006752 A CN106006752 A CN 106006752A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
- C01G49/0081—Mixed oxides or hydroxides containing iron in unusual valence state [IV, V, VI]
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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
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention relates to a preparation method of pure-phase BiFeO3 powder. The preparation method comprises the following steps: Bi2O3 powder and Fe2O3 powder taken as raw materials are subjected to ball milling mixing, and a blank is prepared through pressing; the blank is placed in a sintering furnace heated to 800-850 DEG C for heat preservation for 0.5-2 h and then placed on a metal plate for rapid cooling, and BiFeO3 ceramic is obtained; the BiFeO3 ceramic is ground into powder, the powder is soaked in a dilute nitric acid solution and filtered, a filtrate is cleaned and dried, and the pure-phase BiFeO3 powder is obtained. The method is simple to operate, practical and effective, and the purity of the BiFeO3 powder obtained with a dilute nitric acid cleaning method is quite high.
Description
Technical field
The invention belongs to multi-ferroic material research field, especially relate to the technology of preparing of a kind of single pure phase bismuth ferric powder
And technique.
Background technology
BiFeO3It is the unique material showing ferroelectricity and magnetic more than room temperature found up to now, higher owing to having
Curie temperature (about 1103K) and Ne&1&el temperature (about 643K), and there is the characteristic of magnetoelectric effect, thus conduct
Typical single-phase multi-ferroic material receives much concern, and has potential using value in terms of magnetic storage medium.But due to
BiFeO3Pure compare difficult preparation, be frequently accompanied by Bi2Fe4O9、Bi25FeO40Deng dephasign, and the existence of dephasign makes in sample
Leakage current is the highest, and the ferroelectricity directly resulting in sample is deteriorated.And due to BiFeO3Middle magnetic and ferroelectric coupling ratio itself
More weak, the increase of sample leakage current is the most extremely unfavorable for studying the magneto-electric coupled mechanism of this material and regulation and control, therefore synthesizes pure phase
To promoting BiFeO3The development of sill and apply particularly important, but current pure phase BiFeO3Preparation remain in research
An individual difficult problem.Therefore simple and effective pure phase BiFeO is developed3Preparation method and technique for the study on the modification of this material and application
The most necessary.
Summary of the invention
For the problems referred to above, it is an object of the invention to provide the preparation of a kind of easy and simple to handle, effective pure phase bismuth ferric
Method.
The invention provides the preparation method of a kind of pure phase bismuth ferric powder, it is characterised in that including:
With Bi2O3Powder and Fe2O3Powder is raw material, is pressed into base substrate after ball milling mixing；
Gained base substrate is put into and rises to insulation in the sintering furnace of 800～850 DEG C and within 0.5～2 hour, be placed on metallic plate and quickly cool down,
Obtain bismuth ferrite pottery；
Filter after becoming powder to soak in dilute nitric acid solution gained bismuth ferrite ceramic grinding and clean and dry, obtain described pure phase bismuth ferric powder
End.
The present invention, first by body preparation flakiness shape, coordinates moment to heat up and (puts into the sintering rising to 800～850 DEG C
Stove) and moment quenching (being placed on metallic plate quenching) technology, it is suppressed that Bi2Fe4O9The generation of dephasign, has prepared containing single
One Bi25FeO40The bismuth ferrite sintered product of dephasign.Utilize the way that dust technology cleans after pulverizing, decompose bismuth ferrite sintering
Bi in product25FeO40Dephasign, it is possible to obtain the bismuth ferrite powder of pure phase.
It is preferred that described Bi2O3The mean diameter of powder is 0.5～5 μm, and purity is more than 99.99%.
It is preferred that described Fe2O3The mean diameter of powder is 0.5～5 μm, and purity is more than 99.999%.
It is preferred that described Bi2O3Powder and Fe2O3The mol ratio of powder is (1～1.07): 1, preferably 1.02:1.
It is preferred that described base substrate be shaped as flake.Also, the thickness of base substrate is less than 3mm, preferably 2mm.
It is preferred that described metallic plate is corrosion resistant plate or the good metallic plate of other heat conductivity.
It is preferred that the concentration of described dilute nitric acid solution is 5～20%, soak time is 0.5～2 hour.
The beneficial effects of the present invention is: the method is simple to operate, effective, the way utilizing dust technology to clean obtains
Bismuth ferrite powder purity high.
Accompanying drawing explanation
Fig. 1 is that the sample of embodiment 1 preparation XRD before and after dust technology cleans contrasts collection of illustrative plates；
Fig. 2 is that the sample of embodiment 2 preparation XRD before and after dust technology cleans contrasts collection of illustrative plates；
Fig. 3 is that the sample of embodiment 3 preparation XRD before and after dust technology cleans contrasts collection of illustrative plates；
Fig. 4 is that the sample utilizing embodiment 2 to prepare of embodiment 4 is before and after different hydrogen nitrate concentrations, different soak time are cleaned
XRD contrasts collection of illustrative plates.
Detailed description of the invention
The present invention is further illustrated, it should be appreciated that accompanying drawing and following embodiment are only below in conjunction with accompanying drawing and following embodiment
For the present invention is described, and the unrestricted present invention.
The preparation method that the present invention provides is easy and simple to handle, effective.The method set moment rises gentle quenching technology,
Preparing containing single Bi25FeO40On the basis of the bismuth ferrite ceramic material of dephasign, dust technology after pulverizing, is utilized to clean
Way, it is possible to obtain the bismuth ferrite powder of pure phase.
The preparation method of the pure phase bismuth ferric that the explanation present invention in following exemplary ground provides.
The present invention is not less than the micron order Bi of 99.99% with purity2O3Powder and purity are not less than the micron order of 99.999%
Fe2O3Powder is raw material, is pressed into base substrate after ball milling mixing.When raw material is chosen, typically choose mean diameter be preferably 0.5～
Material powder (such as, the Bi of 5 μm2O3The mean diameter of powder can be 0.5～5 μm, Fe2O3Powder average particle size can be
0.5～5 μm).Due to Bi2O3Powder is easily decomposed when high temperature volatilization, notes also and should choose little over amount when raw material is chosen
Bi2O3Powder, such as Bi2O3Powder and Fe2O3The mol ratio of powder can be (1～1.07): 1, preferably 1.02:1.Its
Described in time of ball milling can be 0.5-3 hour.Flake can be pressed into powder compressing machine after raw material ball milling mix homogeneously
(such as, disc-shaped), thickness is usually no more than 3mm, preferably 2mm.THICKNESS CONTROL, at below 3mm, can make base
Internal portion effectively rises gentleness cooling during moment rises gentleness quenching, it is to avoid internal-external temperature difference is excessive and the surface that causes with internal
Reactions vary causes.
Base substrate is put in the sintering furnace having risen to 800～850 DEG C (such as, temperature reaches 800-850 DEG C tube furnace or horse
Not stove) sinter 0.5～2 hour, then quickly base substrate (such as, certain thickness, the disc-shaped base substrate of diameter) is taken out,
It is placed on a block plate or quickly transfers heat to quickly cool down on steel plate on metallic plate that other heat conductivity are good.
Base substrate after cooling is pulverized again by reacting, with dilute nitric acid solution, the Bi removed in sintered product25FeO40Miscellaneous
Phase, thus obtain single pure phase BiFeO3Powder.Specifically, the fine powder after grinding is 5%～20% in concentration
Soaking 2～0.5h hour in dust technology, concentration of nitric acid can be inversely proportional to soak time, say, that when using slightly lower dilute of concentration
During nitric acid, can proper extension soak time.With deionized water to remaining after dilute nitric acid solution being filtered out with filter paper again
Solids cleans for several times, is finally put by remaining solids and dries in an oven, obtains the bismuth ferrite powder of pure phase.
As a detailed example, choose the Bi of mean diameter 0.5-5 μm, mol ratio 1.02:12O3And Fe2O3Powder
As raw material, by its ball milling 1.5h repeatedly in ball mill, then will be sufficiently mixed uniform powder with tablet machine and be pressed into
Type, the wafer sample pressed is optimal with 2mm thickness, is quickly put into by wafer sample in the tube furnace of temperature 850 DEG C, protects
Take out after temperature 1h, then sample is quickly placed on a sheet of steel plate or other metallic plates, after cooling sample is ground to form
Powder, is then immersed in this powder in the diluted nitric acid aqueous solution of concentration 5%, after crossing 1.5h, salpeter solution filter paper is carried out
Filter, cleans the brown material that stays on filter paper afterwards 2-3 time, is finally dried in an oven by this material, make with deionized water
Obtain the BiFeO of single pure phase3Powder.
Enumerate embodiment further below to describe the present invention in detail.It will similarly be understood that following example are served only for this
Bright it is further described, it is impossible to being interpreted as limiting the scope of the invention, those skilled in the art is according to the present invention's
Some nonessential improvement and adjustment that foregoing is made belong to protection scope of the present invention.The technique ginseng that following example is concrete
Number etc. is the most only an example in OK range, in the range of i.e. those skilled in the art can be done suitably by explanation herein
Select, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
Choose the Bi of mol ratio 1.01:12O3And Fe2O3Powder is as raw material, by its ball milling 1.5h repeatedly in ball mill, then
To be sufficiently mixed uniform powder pressing forming with tablet machine, the wafer sample thickness pressed is 1.95mm, and wafer sample is fast
Speed is put in the tube furnace of temperature 850 DEG C, takes out after insulation 1h, then sample is quickly placed on a sheet of steel plate or other gold
Belong on plate, after cooling sample is pulverized, this powder is immersed in the diluted nitric acid aqueous solution of concentration 5%, after crossing 1.5h
Salpeter solution filter paper is filtered, cleans the brown material that stays on filter paper afterwards with deionized water 2-3 time, finally general
This material is dried in an oven, prepares the BiFeO of single pure phase3Powder.In Fig. 1, upper and lower collection of illustrative plates is before dust technology cleans respectively
After XRD figure spectrum.
Embodiment 2
Choose the Bi of mol ratio 1.02:12O3And Fe2O3Powder is as raw material, by its ball milling 1.5h repeatedly in ball mill, then
To be sufficiently mixed uniform powder pressing forming with tablet machine, the wafer sample thickness pressed is 2.0mm, and wafer sample is quick
Put in the tube furnace of temperature 850 DEG C, take out after insulation 1h, then sample is quickly placed on a sheet of steel plate or other metals
On plate, after cooling sample is pulverized, this powder is immersed in the diluted nitric acid aqueous solution of concentration 5%, cross handle after 1.5h
Salpeter solution filter paper filters, and cleans the brown material that stays on filter paper afterwards with deionized water 2-3 time, finally should
Material is dried in an oven, prepares the BiFeO of single pure phase3Powder.In Fig. 2, upper and lower collection of illustrative plates is before and after dust technology cleans respectively
XRD figure spectrum.
Embodiment 3
Choose the Bi of mol ratio 1.05:12O3And Fe2O3Powder is as raw material, by its ball milling 1.5h repeatedly in ball mill, then
To be sufficiently mixed uniform powder pressing forming with tablet machine, the wafer sample thickness pressed is 1.99mm, and wafer sample is fast
Speed is put in the tube furnace of temperature 850 DEG C, takes out after insulation 1h, then sample is quickly placed on a sheet of steel plate or other gold
Belong on plate, after cooling sample is pulverized, this powder is immersed in the diluted nitric acid aqueous solution of concentration 5%, after crossing 1.5h
Salpeter solution filter paper is filtered, cleans the brown material that stays on filter paper afterwards with deionized water 2-3 time, finally general
This material is dried in an oven, prepares the BiFeO of single pure phase3Powder.In Fig. 3, upper and lower collection of illustrative plates is before dust technology cleans respectively
After XRD figure spectrum.
Embodiment 4
The sample that embodiment 2 prepares is pulverized, this powder is separately immersed in the diluted nitric acid aqueous solution of concentration 5% and 10%,
After crossing 1.5h and 50min, salpeter solution filter paper is filtered, clean the brown stayed on filter paper afterwards with deionized water
Material 2-3 time, finally dries in an oven by this material, prepares the BiFeO of single pure phase3Powder.Upper and lower collection of illustrative plates in Fig. 4
It is that the XRD figure that variable concentrations dust technology cleaning different time obtains is composed respectively.
Fig. 1 is that the sample of embodiment 1 preparation XRD before and after dust technology cleans contrasts collection of illustrative plates.Fig. 2 is that embodiment 2 is made
Standby sample XRD before and after dust technology cleans contrasts collection of illustrative plates.Fig. 3 is that the sample of embodiment 3 preparation is before dust technology cleans
After XRD contrast collection of illustrative plates.Understanding from Fig. 1,2,3, the sample before cleaning is except containing BiFeO3Diffraction maximum outside, also all
Containing dephasign Bi25FeO40Diffraction maximum, and clean after sample contain only BiFeO3Diffraction maximum, this shows to utilize dust technology
The method that solution cleans can effectively remove dephasign Bi25FeO40。
Fig. 4 is the sample of embodiment 2 preparation XRD comparison diagram before and after different hydrogen nitrate concentrations, soak time are cleaned
Spectrum.The most visible, use 5% dust technology to soak 1.5 hours, and use 10% dust technology immersion all can effectively go for 50 minutes
Remove impurity phase.
Claims (8)
1. the preparation method of a pure phase bismuth ferric powder, it is characterised in that including:
With Bi2O3Powder and Fe2O3Powder is raw material, is pressed into base substrate after ball milling mixing；
Gained base substrate is put into and rises to insulation in the sintering furnace of 800～850 DEG C and within 0.5～2 hour, be placed on metallic plate and quickly cool down, obtain bismuth ferrite pottery；
Filter after becoming powder to soak in dilute nitric acid solution gained bismuth ferrite ceramic grinding and clean and dry, obtain described pure phase bismuth ferric powder.
Described preparation method the most according to claim 1, it is characterised in that described Bi2O3The mean diameter of powder is 0.5～5 μm, and purity is more than 99.99%.
3. according to the described preparation method of claim 1 or 2, it is characterised in that described Fe2O3The mean diameter of powder is 0.5～5 μm, and purity is more than 99.999%.
4. according to the preparation method according to any one of claim 1-3, it is characterised in that described Bi2O3Powder and Fe2O3The mol ratio of powder is (1～1.07): 1.
5. according to the preparation method according to any one of claim 1-4, it is characterised in that described base substrate be shaped as flake.
Preparation method the most according to claim 5, it is characterised in that the thickness of described base substrate is less than 3mm.
7. according to the preparation method according to any one of claim 1-6, it is characterised in that described metallic plate is corrosion resistant plate.
8., according to the preparation method according to any one of claim 1-7, it is characterised in that the concentration of described dilute nitric acid solution is 5～20%, soak time is 0.5～2 hour.
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| CN201610325853.1A CN106006752A (en) | 2016-05-16 | 2016-05-16 | Preparation method of pure-phase BiFeO3 powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110002506A (en) * | 2019-05-08 | 2019-07-12 | 东北大学秦皇岛分校 | A kind of preparation method of pure phase nanometer crystalline substance bismuth ferrite |
| CN116283339A (en) * | 2023-04-11 | 2023-06-23 | 昆明理工大学 | Preparation method of pure-phase bismuth ferrite ceramic |
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| CN1686932A (en) * | 2005-04-08 | 2005-10-26 | 南京大学 | Method for preparing single-phase BiFeO3 ceramics through hardening process |
| CN101671173A (en) * | 2009-09-27 | 2010-03-17 | 哈尔滨工业大学 | Method for improving multi-ferrum property of BiFeO3 ceramic block material |
| CN101734724A (en) * | 2009-12-31 | 2010-06-16 | 厦门大学 | Ferromagnetic bismuth ferrite and the synthesis method thereof |
| CN104556238A (en) * | 2014-12-19 | 2015-04-29 | 上海师范大学 | Method for preparing pure-phase bismuth ferrite powder and block |
| CN104843796A (en) * | 2015-01-20 | 2015-08-19 | 吉林师范大学 | Preparation method of bismuth ferrite |
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2016
- 2016-05-16 CN CN201610325853.1A patent/CN106006752A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1686932A (en) * | 2005-04-08 | 2005-10-26 | 南京大学 | Method for preparing single-phase BiFeO3 ceramics through hardening process |
| CN101671173A (en) * | 2009-09-27 | 2010-03-17 | 哈尔滨工业大学 | Method for improving multi-ferrum property of BiFeO3 ceramic block material |
| CN101734724A (en) * | 2009-12-31 | 2010-06-16 | 厦门大学 | Ferromagnetic bismuth ferrite and the synthesis method thereof |
| CN104556238A (en) * | 2014-12-19 | 2015-04-29 | 上海师范大学 | Method for preparing pure-phase bismuth ferrite powder and block |
| CN104843796A (en) * | 2015-01-20 | 2015-08-19 | 吉林师范大学 | Preparation method of bismuth ferrite |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110002506A (en) * | 2019-05-08 | 2019-07-12 | 东北大学秦皇岛分校 | A kind of preparation method of pure phase nanometer crystalline substance bismuth ferrite |
| CN116283339A (en) * | 2023-04-11 | 2023-06-23 | 昆明理工大学 | Preparation method of pure-phase bismuth ferrite ceramic |
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Application publication date: 20161012 |