CN102285690A - Chemical coprecipitation method for synthesizing Bi2Fe4O9 submicron rods - Google Patents

Chemical coprecipitation method for synthesizing Bi2Fe4O9 submicron rods Download PDF

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CN102285690A
CN102285690A CN2011101031516A CN201110103151A CN102285690A CN 102285690 A CN102285690 A CN 102285690A CN 2011101031516 A CN2011101031516 A CN 2011101031516A CN 201110103151 A CN201110103151 A CN 201110103151A CN 102285690 A CN102285690 A CN 102285690A
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coprecipitation method
chemical coprecipitation
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CN102285690B (en
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卢朝靖
李永平
张永成
叶万能
刘东奇
夏临华
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Qingdao University
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Abstract

The invention belongs to the technical field of chemical preparation of physical materials and discloses a chemical coprecipitation method for synthesizing Bi2Fe4O9 submicron rods, which comprises three steps, i.e. precursor precipitation, drying and heat treatment. The chemical coprecipitation method comprises the steps of preparing precursors first, weighing Bi(NO3)3.5H2O and Fe(NO3)3.9H2O according to molar ratio, dissolving the Bi(NO3)3.5H2O and Fe(NO3)3.9H2O in dilute nitric acid, dropping NaOH water solution into the mixed solution till sediment is fully precipitated; then naturally air-drying the obtained sediment, grinding the sediment, directly putting the sediment into a 600 DEG C tubular furnace for calcination, keeping temperature to be constant for 2 hours and taking out and putting the obtained product at room temperature; and finally grinding, acid-cleaning and water-washing the obtained block to be neutral, putting the obtained product into a drying oven for drying and obtaining yellow powder which is the Bi2Fe4O9 submicron rods. The chemical coprecipitation method for synthesizing the Bi2Fe4O9 submicron rods has the advantages of simple, convenient and feasible process steps, low cost and good repeatability.

Description

A kind of synthetic Bi＜sub〉2＜/sub〉Fe＜sub〉4＜/sub〉O＜sub〉9＜/sub〉chemical coprecipitation method of sub-micrometer rod
Technical field
The invention belongs to physical material chemical preparation technical field, relate to pure phase Bi 2Fe 4O 9The preparation method of powder particularly is the synthetic Bi of precipitating reagent with NaOH 2Fe 4O 9The chemical coprecipitation method of sub-micrometer rod.
Background technology
BiFeO 3Be at present knownly uniquely to have ferroelectricity and ferromagnetic single-phase multi-ferroic material simultaneously in room temperature.Utilize its magnetoelectric effect, can realize with electric field no write de-lay information, again with the quick sense information in magnetic field, the memory of development high density, high access speed.Pure phase BiFeO 3Preparation relatively the difficulty, often follow Bi to occur 2Fe 4O 9, Bi 25FeO 40Deng the thing phase.Bibliographical information is arranged recently, Bi 2Fe 4O 9Also has many iron property (A.K.Singh, S.D.Kaushik, et al., Appl.Phys.Lett.92,132910 (2008)).
Bi 2Fe 4O 9Or a kind of functional material with characteristics such as air-sensitive, photocatalysis and opto-electronic conversion.Bi 2Fe 4O 9Ethanol and acetone gas there are stronger sensitiveness, can make semiconductor gas sensor with it; It can also replace the precious metals such as platinum, rhodium, palladium, is industrial ammoxidation NO, using value very huge (A.S.Poghossian, H.V.Abovian, et al.Sens.Actuators B 4,545 (1991); N.I.Zakharchenko, Russ.J.Appl.Chem.73,2047 (2000)).Recent research is found, Bi 2Fe 4O 9Band gap 2eV about, at visible region, thereby Bi 2Fe 4O 9Can effectively absorb sunshine, can be used as conductor photocatalysis material (Q.J.Ruan and W.D.Zhang, J.Phys.Chem.C, 113,4168 (2009)).The conductor photocatalysis oxidation is a kind of environmental purification new technology, has except that cleanliness height, non-secondary pollution, rate of decomposition advantages such as fast and easy handling, is used widely in wastewater treatment.What is interesting is that more we find Bi recently 2Fe 4O 9Have light transfer characteristic, have tempting application prospect in area of solar cell, may substitute the wider titanium dioxide of present application, become one of important selection that solves lack of energy and environmental pollution.
The performance of functional materials and its particulate pattern, size, microtexture have closely gets in touch.The control of microscopic appearance is not only significant to the fundamental research of material, and directly influences the practical application (X.Wang, J.Zhuang, Q.Peng, et al., Nature, 437,121 (2005)) of material.For example, concerning the ferrite that electronic industry is used always, the specific surface area of spherical ferrite particle is bigger, and magnetic strengthens but coercive force weakens; And the sheet ferrite can be used as the solid raw material of perpendicular magnetic recording, and saturation magnetization and coercive force are higher; Bar-shaped ferrite particle is owing to the anisotropy of its particle shape, and its coercive force can reach the highest (Zheng Shufang, Xiong Guoxuan etc., material Leader, 23,26, (2009)).As seen, granule-morphology is very big to the performance impact of functional material.Therefore, necessary synthetic pattern and the controlled Bi of size 2Fe 4O 9Material is to strengthen it in the application of semiconductor gas sensor, photocatalysis and area of solar cell.Reported Bi 2Fe 4O 9Synthetic pattern comprises ball shaped nano particle, petal-shaped particle, nanometer sheet, nano wire and submicron square (Yu Zhiwei, seedling swan goose, what is said or talked about Guoqiang, Chinese Journal of Inorganic Chemistry, 24,483 (2008); S.M.Sun, W.Z.Wang, et al., J.Phys.Chem.C 113,12826 (2009); J.T.Han, Y.H.Huang, X.J.Wu, et al., Adv.Mater.18,2145 (2006); Z.Yang, Y.Huang, et al, J.Solid State Chem., 179,3324 (2006); T.J.Park, G.C.Papaefthymiou, et al., J.Mater.Chem.15,2099 (2005)).Existing studies show that, petal-shaped Bi 2Fe 4O 9Nano particle and Bi 2Fe 4O 9Nanometer sheet have the visible light catalytic characteristic (S.M.Sun, W.Z.Wang, et al., J.Phys.Chem.C 113,12826 (2009); Q.J.Ruan and W.D.Zhang, J.Phys.Chem.C 113,4168 (2009)).
The synthetic technology of material and concrete technology directly affect its microstructure, and then affect its performance.The technologies such as existing human hydro-thermal method, solid phase method, sol-gel process synthesize the pure phase Bi of different-shape 2Fe 4O 9The Bi of the usefulness such as Han hydro-thermal legal system is standby petal-shaped and sheet 2Fe 4O 9(J.T.Han, Y.H.Huang, X.J.Wu, et al., Adv.Mater.18,2145 (2006)), but its experimental situation is relatively harsher, stoichiometric proportion is strict, and pH value in reaction needs accurately control, very easily produces dephasign.The people such as Yang use sol gel process to prepare Bi in the AAO template 2Fe 4O 9Nano wire (Z.Yang, Y.Huang, et al., J.Solid State Chem.179,3324 (2006)), but the reaction time is long, the temperature height, energy consumption is big.The human molten-salt growth methods such as Park have prepared Bi 2Fe 4O 9Sub-micron square (T.J.Park, G.C.Papaefthymiou, et al., J.Mater.Chem.15,2099 (2005)), but its calcining heat height, energy consumption is big.
At present, synthetic pure phase Bi 2Fe 4O 9Still relatively more difficult, this is that bismuth ion is volatile, has the oxygen room, and the change of iron ion valence state, makes BiFeO because its synthetic warm area is narrower 3, Bi 2Fe 4O 9, Bi 25FeO 40Deng the dephasign each other that coexists.From application point, be necessary very much to consider economy and the controllability of its synthetic method.Therefore, it is simple to be badly in need of groping a kind of technology, the synthetic high-quality of method with low cost and the controlled pure phase Bi of pattern 2Fe 4O 9, to promote it at the application and development in the fields such as photocatalysis and solar cell.
Summary of the invention
The object of the present invention is to provide a kind of synthetic Bi 2Fe 4O 9The chemical coprecipitation method of sub-micrometer rod.This method technology is simple, high, easy to operate, cheap, the non-environmental-pollution of stability, can synthesize the Bi of pure phase 2Fe 4O 9Sub-micrometer rod is expected to be used widely in fields such as photocatalysis and solar cells.
To achieve these goals, the technical scheme that the present invention realizes comprises precursor solution preparation and precipitation, drying and three steps of thermal treatment, and the specific implementation process is as follows:
One, precursor solution preparation and precipitation
By stoichiometric proportion weighing Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2Two kinds of components of O, mixing is dissolved in rare nitric acid, is placed on the magnetic stirring apparatus and stirs, and treats Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O dissolves namely obtain brown solution fully.Then, take by weighing an amount of NaOH, be mixed with the NaOH aqueous solution of finite concentration (2～10 mol), NaOH solution is dropwise splashed into Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2Promptly produce precipitation in the O blended brown solution; To pH＞10, guarantee Bi 3+And Fe 3+Precipitation and solution are alkalescence fully.At last, continuing to be stirred to the precipitation body mixes.
Two, powder drying and grinding
With the presoma sediment that obtains, leave standstill certain hour after, with the clear water sucking-off of dropper with the upper strata, be placed in the air natural air drying to bone dry, gained is precipitated body grinds and obtain pink powder.
Three, thermal treatment and washing and drying
The alumina crucible that pink powder is housed is directly put into 600 ℃ quartz tube furnace, behind the heat preservation sintering 2h, its direct taking-up is placed the cooling of air at room temperature naturally, the powder in the crucible becomes red block.After treating that it drops to room temperature, red block grind into powder.Then with the rare HNO of 2 mol 3Clean, be washed with distilled water to neutrality again.At last, will precipitate body and put into 80 ℃ of drying boxes, the yellow powder that oven dry obtains namely is Bi 2Fe 4O 9Sub-micrometer rod.
Method provided by the invention is less demanding to experimental installation, and technology is simple, good reproducibility, and cheap, non-environmental-pollution, the sub-micrometer rod that obtains are about 0.1～1.5 μ m, wide about 100～200nm.X ray research finds that the mol ratio of Bi: Fe all can obtain pure phase Bi at 1: 2～1: 1 o'clock in addition 2Fe 4O 9Sub-micrometer rod, illustrate that this method is subjected to the impact of initial feed stoichiometric proportion fluctuation little.
Description of drawings
Fig. 1 is in molar ratio Bi of embodiments of the invention: Fe=1: 2, NaOH concentration is 2 mol/L, the Bi of preparation 2Fe 4O 9The XRD collection of illustrative plates of sub-micrometer rod.
Fig. 2 is in molar ratio Bi of embodiments of the invention: Fe=1: 2, NaOH concentration is 2 mol/L, the Bi of preparation 2Fe 4O 9The FESEM figure of sub-micrometer rod.
Embodiment
Also the present invention is described further in conjunction with the accompanying drawings below by specific embodiment.
Embodiment 1
One, precursor solution preparation and precipitation
Bi: Fe=1 in molar ratio: 2,14.697g Bi (NO 3) 35H 2O and 24.609g Fe (NO 3) 39H 2The O mixing is dissolved in the rare nitric acid of 28m1 (2 mol/L), is placed on stir about 1h on the magnetic stirring apparatus, treats Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O dissolves namely obtain brown solution fully.Then, take by weighing 20g NaOH, be mixed with the NaOH aqueous solution of 2 mol, NaOH solution is dropwise splashed into Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2Promptly produce precipitation in the O blended brown solution; To pH=12, guarantee Bi 3+And Fe 3+Precipitation and solution are alkalescence fully.At last, continuing stir about 2h mixes to precipitating body.
Two, powder drying and grinding
With the presoma sediment that obtains, leave standstill 1h after,, be placed in the air natural air drying and need 5～10 days approximately unnecessary water sucking-off with dropper, treat its bone dry after, gained is precipitated body grinds and obtain pink powder.
Three, thermal treatment and washing and drying
The alumina crucible that pink powder is housed is directly put into 600 ℃ quartz tube furnace, behind the heat preservation sintering 2h, its direct taking-up is placed the cooling of air at room temperature naturally, the powder in the crucible becomes red block.After treating that it drops to room temperature, red block grind into powder.Then with the rare HNO of 2 mol 3Clean, be washed with distilled water to neutrality again.At last, will precipitate body and put into 80 ℃ of drying boxes, behind the dry 10h, the yellow powder that obtains namely is Bi 2Fe 4O 9Sub-micrometer rod.
Embodiment 2
One, precursor solution preparation and precipitation
Bi: Fe=1 in molar ratio: 1,14.697g Bi (NO 3) 35H 2O and 12.305g Fe (NO 3) 39H 2The O mixing is dissolved in the rare nitric acid of 28ml (2 mol/L), is placed on stir about 1h on the magnetic stirring apparatus, treats Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O dissolves namely obtain brown solution fully.Then, take by weighing 20g NaOH, be mixed with the NaOH aqueous solution of 2 mol, NaOH solution is dropwise splashed into Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2Promptly produce precipitation in the O blended brown solution; To pH=12, guarantee Bi 3+And Fe 3+Precipitation and solution are alkalescence fully.At last, continuing stir about 2h mixes to precipitating body.
Two, powder drying and grinding
With the presoma sediment that obtains, leave standstill 1h after,, be placed in the air natural air drying and need 5～10 days approximately unnecessary water sucking-off with dropper, treat its bone dry after, gained is precipitated body grinds and obtain pink powder.
Three, thermal treatment and washing and drying
The alumina crucible that pink powder is housed is directly put into 600 ℃ quartz tube furnace, behind the heat preservation sintering 2h, its direct taking-up is placed the cooling of air at room temperature naturally, the powder in the crucible becomes red block.After treating that it drops to room temperature, red block grind into powder.Follow rare HNO with 2 mol 3Clean, be washed with distilled water to neutrality again.At last, will precipitate body and put into 80 ℃ of drying boxes, behind the dry 10h, the yellow powder that obtains namely is Bi 2Fe 4O 9Sub-micrometer rod.

Claims (2)

1. synthetic Bi 2Fe 4O 9The chemical coprecipitation method of sub-micrometer rod is characterized in that the (NO with Bi 3) 35H 2O and Fe (NO 3) 39H 2O is raw material, take NaOH as precipitating reagent, with the synthetic Bi of chemical coprecipitation 2Fe 4O 9Sub-micrometer rod.
2. a kind of synthetic Bi as claimed in claim 1 2Fe 4O 9The chemical coprecipitation method of sub-micrometer rod is characterized in that following steps:
One, precursor solution preparation and precipitation
By stoichiometric proportion weighing Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2Two kinds of components of O, mixing is dissolved in rare nitric acid, is placed on the magnetic stirring apparatus and stirs, and treats Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O dissolves namely obtain brown solution fully, then, takes by weighing an amount of NaOH, is mixed with the NaOH aqueous solution of finite concentration (2～10 mol/L), and NaOH solution is dropwise splashed into Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2Namely produce precipitation in the brown solution that O mixes, to pH＞10, guarantee Bi 3+And Fe 3+Precipitation and solution are alkalescence fully, and is last, continues to be stirred to the precipitation body and mix;
Two, powder drying and grinding
After the presoma throw out that obtains left standstill certain hour,, be placed in the air natural air drying, gained precipitated body grind and obtain pink powder to complete drying with the clear water sucking-off of dropper with the upper strata;
Three, thermal treatment and washing and drying
The alumina crucible that pink powder is housed is directly put into 600 ℃ quartz tube furnace, behind the heat preservation sintering 2h, its direct taking-up is placed the cooling of air at room temperature naturally, powder in the crucible becomes red block, after treating that it drops to room temperature, red block grind into powder, then with the rare HNO of 2 mol/L 3Clean, be washed with distilled water to again neutrality, last, will precipitate body and put into 80 ℃ of drying boxes, the yellow powder that oven dry obtains namely is Bi 2Fe 4O 9Sub-micrometer rod.
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CN102583571A (en) * 2012-02-29 2012-07-18 南京信息工程大学 Wet chemical method for preparing Bi2Fe4O9 nanometer powder
CN103193471A (en) * 2013-04-18 2013-07-10 华中科技大学 Bi2Fe4O9 multiferroic ceramic material and preparation method thereof
CN103265281A (en) * 2013-06-19 2013-08-28 华中科技大学 Cr-doped Bi2Fe4O9 multiferroic ceramic material and preparation method thereof
CN106379944A (en) * 2016-08-29 2017-02-08 上海应用技术学院 Preparation method of pure-phase bismuth ferrite
CN106654401A (en) * 2016-11-30 2017-05-10 湘潭大学 Bismuth ferrite/nickel hydroxide secondary alkali battery and preparation method therefor
CN109126809A (en) * 2018-10-09 2019-01-04 沈阳工业大学 A kind of catalyst and the preparation method and application thereof of efficient catalytic reduction nitrophenol
CN111410237A (en) * 2020-05-09 2020-07-14 中南林业科技大学 Resource utilization method for waste polluted biomass
CN113336271A (en) * 2021-06-11 2021-09-03 浙江理工大学 Micron-sized regular square strip Bi2Fe4O9Preparation method, product and application of multiferroic material

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102583571A (en) * 2012-02-29 2012-07-18 南京信息工程大学 Wet chemical method for preparing Bi2Fe4O9 nanometer powder
CN103193471A (en) * 2013-04-18 2013-07-10 华中科技大学 Bi2Fe4O9 multiferroic ceramic material and preparation method thereof
CN103193471B (en) * 2013-04-18 2014-10-08 华中科技大学 Bi2Fe4O9 multiferroic ceramic material and preparation method thereof
CN103265281A (en) * 2013-06-19 2013-08-28 华中科技大学 Cr-doped Bi2Fe4O9 multiferroic ceramic material and preparation method thereof
CN106379944A (en) * 2016-08-29 2017-02-08 上海应用技术学院 Preparation method of pure-phase bismuth ferrite
CN106654401A (en) * 2016-11-30 2017-05-10 湘潭大学 Bismuth ferrite/nickel hydroxide secondary alkali battery and preparation method therefor
CN109126809A (en) * 2018-10-09 2019-01-04 沈阳工业大学 A kind of catalyst and the preparation method and application thereof of efficient catalytic reduction nitrophenol
CN111410237A (en) * 2020-05-09 2020-07-14 中南林业科技大学 Resource utilization method for waste polluted biomass
CN113336271A (en) * 2021-06-11 2021-09-03 浙江理工大学 Micron-sized regular square strip Bi2Fe4O9Preparation method, product and application of multiferroic material
CN113336271B (en) * 2021-06-11 2022-06-28 浙江理工大学 Micron-sized regular square strip Bi2Fe4O9Preparation method, product and application of multiferroic material

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