CN101830514B - Method for template-free hydrothermal synthesis of one-dimensional nano-Bi2Fe4O9 - Google Patents

Method for template-free hydrothermal synthesis of one-dimensional nano-Bi2Fe4O9 Download PDF

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CN101830514B
CN101830514B CN2010101326255A CN201010132625A CN101830514B CN 101830514 B CN101830514 B CN 101830514B CN 2010101326255 A CN2010101326255 A CN 2010101326255A CN 201010132625 A CN201010132625 A CN 201010132625A CN 101830514 B CN101830514 B CN 101830514B
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titanium sheet
concentration
reaction
naoh
solution
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CN101830514A (en
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陈文�
孙华君
王一擘
周静
朱泉峣
徐庆
张成勇
王瑞兵
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Huang Duanping
Shandong Chanyan Ceramic Research Institute Co ltd
Wuhan Institute Of Technology Industry Group Co ltd
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Wuhan University of Technology WUT
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Abstract

The invention discloses a method for template-free hydrothermal synthesis of one-dimensional nano-Bi2Fe4O9. In the method, a hydrothermal preparation method is adopted and comprises the following steps of: dissolving Bi(NO3)3.5H2O and Fe(NO3)3.9H2O with the same amount in dilute nitric acid; and titrating by using the aqueous solution of NaOH for complete precipitation, and filtering and washing to obtain neutral solution; and the method is characterized by comprising the following steps of: dissolving the obtained precipitate into the solution of NaOH at the concentration of 8 to 20 Mol/L; putting the solution into a reaction kettle and adding a titanium plate, reacting for at the temperature of between 160 and 200 DEG C 12 to 72 hours, and growing the product on a titanium plate substrate; and after taking the titanium plate out, washing the titanium plate by using deionized water and alcohol, putting the titanium plate into a drying oven for drying, and obtaining the final product of the one-dimensional nano-Bi2Fe4O9 on the titanium plate.

Description

Template-free hydrothermal synthesis of one-dimensional nano Bi 2Fe 4O 9Method
Technical field
The present invention relates to a kind of titanium template hydrothermal method synthesizing one-dimensional nanometer Bi that utilizes 2Fe 4O 9Method, particularly under coldcondition, utilize the titanium sheet to be substrate hydrothermal method synthesizing one-dimensional nanometer Bi 2Fe 4O 9Method.Belong to the ferroelectric technological category of nanometer.
Background technology
The performance of functional materials and its pattern, size, microtexture and crystalline structure have very big relation.The control of microscopic appearance is not only useful to the fundamental research of material, and the utilization of material is also had very big value [1-4].Bi 2Fe 4O 9Being a kind of good gas sensitive, also is that industrial ammonia oxidation is a kind of important catalyst of NO, using value very huge [5-6].Now about Bi 2Fe 4O 9The report of preparation is still rarely found, the Bi of some utilization hydrothermal method preparations 2Fe 4O 9Experimental situation relatively harsh.Korea Spro of Fudan University in 2006 builds human hydrothermal methods such as great waves and has prepared Bi at 270 ℃ 2Fe 4O 9But reaction conditions is very harsh, and pH value in reaction needs accurately control [7].The same year, people such as Zhi Yang used sol-gel method on the AAO template, to prepare Bi 2Fe 4O 9Nano wire, but the desired reaction times is longer, temperature of reaction higher [8].
[1]A.P.Alivisatos，Science，271(1996)933.
[2]Y.Sun，Y.Xia，Science，298(2002)2176.
[3]C.J.Kiely，J.Fink，M.Brust，D.Bethel，D.J.Schiffrin，Nature，396(1998)444.
[4]X.Wang，J.Zhuang，Q.Peng，Y.D.Li，Nature，437(2005)121
[5]N.I.Zakharchenko，Russ.J.Appl.Chem.73(2000)2047.
[6]A.S.Poghossian，H.V.Abovian，P.B.Avakian，S.H.Mkrtchian，V.M.Haroutunian，Sens.Actuators?B.4(1991)545.
[7]J.T.Han，Y.H.Huang，R.J.Jia，G.C.Shan，R.Q.Guo，W.Huang，J.Cryst.Growth.294(2006)469.
[8]Z.Yang，Y.Huang，B.Dong，H.L.Li，S.Q.Shi，J.Solid?State?Chem.179(2006)3324.
Summary of the invention
The object of the present invention is to provide a kind of under lower temperature conditions template-free hydrothermal synthesis of one-dimensional nano Bi 2Fe 4O 9The material method.It can realize 1-dimention nano Bi 2Fe 4O 9The arrangement ordering.
The technical scheme that realizes the object of the invention is:
A kind of template-free hydrothermal synthesis of one-dimensional nano Bi 2Fe 4O 9Method, it is characterized in that, with Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O as the hydro-thermal reaction mineralizer, is that 99.9% titanium sheet be substrate with purity with NaOH as reaction raw materials, under 160-220 ℃ of coldcondition, and hydrothermal method synthesizing one-dimensional nanometer Bi 2Fe 4O 9
Wherein, the strength of solution scope of described hydro-thermal reaction mineralizer NaOH is the 8-20 mol.Reaction product did not reach high directed requirement when the strength of solution of NaOH was lower than 8 mol.Effect increases the not obvious and too high easy corrosion reaction equipment of alkali concn when being higher than 20 mol.
Temperature of reaction is lower than that 160 ℃ of reactions are slow, and the time is long, and reaction not exclusively, and is complete 200 ℃ of reactions 12 hours, and being higher than 220 ℃ of effects increases not obviously, and consumption heat energy is many.
The described hydro-thermal reaction time is 12-72 hour.Be less than reaction in 12 hours not exclusively, at 160 ℃, 220 ℃ were reacted 72 hours, and reacted all complete.
Described reaction raw materials Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O adds according to the amount of substance such as grade when reaction.Reaction raw materials Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O hydro-thermal reaction concentration be the 12-100 mmole/liter.Be lower than 12 mmoles/can not obtain unidimensional Bi when rising 2Fe 4O 9Crystal.Be higher than 100 mmoles/not obvious and waste reaction raw materials of effect variation when rising.
Concrete preparation process is:
1), with reaction raw materials Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O is dissolved in rare nitric acid (less than 1 centinormal 1 nitric acid) with the ratio that waits amount of substance, then fully with NaOH aqueous solution titration to deposition, and suction filtration, and be neutrality with deionized water washing sediment to wash solution;
2), washing postprecipitation thing that step 1) is obtained is dissolved in the NaOH aqueous solution that concentration is the 8-20 mol, and puts into the titanium sheet, puts into reaction kettle then and reaction 12-72 hour under 160-220 ℃ of condition, the product of on the titanium sheet, growing;
3), with step 2) product that obtains with deionized water and alcohol washing after, put into baking oven and dry, the final product that obtains on the titanium sheet is 1-dimention nano Bi 2Fe 4O 9
From FESEM figure, can obviously find 1-dimention nano Bi to product 2Fe 4O 9The vertical titanium sheet growth of crystal.The concentration that key of the present invention is to control mineralizer NaOH is between the 8-20 mol.
Used Bi (NO among the present invention 3) 35H 2O, Fe (NO 3) 39H 2O, nitric acid, NaOH are commercial AR.Beneficial effect of the present invention is:
The present invention utilizes the titanium sheet to be substrate template-free hydrothermal synthesis of one-dimensional nano Bi 2Fe 4O 9, make Bi through the reaction parameter of regulating some hydro-thermals 2Fe 4O 9Arrange ordering.Key of the present invention is to reach through regulating and controlling mineralizer concentration and makes material arrange ordering, has realized the regulation and control of material structure.The present invention be utilize the titanium sheet for substrate under 160-220 ℃ of low temperature environment, reaction mineralizer concentration controlled hydro-thermal reaction is prepared 1-dimention nano Bi 2Fe 4O 9Material, it can be used for making well behaved semiconductor gas sensor, can also prepare the catalyzer of NO as ammonia oxidation.Its realization condition is all very good aspect feasibility and controllability.
Description of drawings
Fig. 1 is at 200 ℃, the Bi for preparing when NaOH concentration is 12 mol 2Fe 4O 9XRD figure spectrum, (01-074-1098) is corresponding with the JCPDF card.
Fig. 2 is at 200 ℃, the Bi that NaOH concentration prepares when being 12 mol 2Fe 4O 9The SEM photo.(a is 10000 times, and b is 3000 times)
From the visible 1-dimention nano Bi of Fig. 2 2Fe 4O 9The vertical titanium sheet of crystal oriented growth, nano-sheet Bi 2Fe 4O 9By 1-dimention nano Bi 2Fe 4O 9Crystal constitutes.
Embodiment
Embodiment 1
With the Bi (NO that waits amount of substance 3) 35H 2O (1.94 gram) and Fe (NO 3) 39H 2O (1.616 gram) is dissolved in the 0.1 centinormal 1 nitric acid, and is complete to deposition with the NaOH solution titration of 12 mol then, and suction filtration is washed to solution and is neutral, also washes Na wherein off +And NO 3 -The deposition that obtains is dissolved in the NaOH solution that concentration is 8 mol, is made into 40 ml solns; Bi (NO 3) 35H 2The concentration of O be 100 mmoles/liter, Fe (NO 3) 39H 2The concentration of O be 100 mmoles/liter; Pour 50 milliliters reaction kettle rapidly into and add the titanium sheet; In 160 ℃ of baking ovens, placed 72 hours, take out and put into 60 ℃ of baking ovens placements 4 hours after the titanium sheet washes with deionized water and alcohol, the final product that obtains on the titanium sheet is 1-dimention nano Bi 2Fe 4O 9Crystal.
Embodiment 2
Bi (NO etc. amount 3) 35H 2O (970 milligrams) and Fe (NO 3) 39H 2O (808 milligrams) is dissolved in 0.1 centinormal 1 rare nitric acid, and is complete to deposition with the NaOH titration of 12 mol then, and suction filtration is washed to solution and is neutral, also washes Na wherein off +And NO 3 -The deposition that obtains is dissolved in the NaOH solution that concentration is 20 mol, is made into 40 ml solns, Bi (NO 3) 35H 2The concentration of O be 50 mmoles/liter, Fe (NO 3) 39H 2The concentration of O be 50 mmoles/liter; Pour 50 milliliters reaction kettle rapidly into and add the titanium sheet; In 180 ℃ of baking ovens, placed 50 hours; Take out and put into 100 ℃ of baking ovens placements 2 hours after the titanium sheet washes with deionized water and alcohol, the final product that obtains on the titanium sheet is the nano-sheet Bi of high orientation growth 2Fe 4O 9Sheet Bi 2Fe 4O 91-dimention nano Bi for vertical titanium sheet growth 2Fe 4O 9Crystal constitutes.
Embodiment 3
Bi (NO etc. amount 3) 35H 2O (232.8 milligrams) and Fe (NO 3) 39H 2O (193.9 milligrams) is dissolved in 0.1 centinormal 1 rare nitric acid, and is complete to deposition with the NaOH titration of 12 mol then, and suction filtration is washed to solution and is neutral, also washes Na wherein off +And NO 3 -The deposition that obtains is dissolved in the NaOH solution that concentration is 12 mol, is made into 40 ml solns, Bi (NO 3) 35H 2The concentration of O be 12 mmoles/liter, Fe (NO 3) 39H 2The concentration of O be 12 mmoles/liter; Pour 50 milliliters reaction kettle rapidly into and add the titanium sheet; In 220 ℃ of baking ovens, placed 50 hours; Take out and put into 80 ℃ of baking ovens placements 4 hours after the titanium sheet washes with deionized water and alcohol, the final product that obtains on the titanium sheet is the nano-sheet Bi of high orientation growth 2Fe 4O 9Sheet Bi 2Fe 4O 91-dimention nano Bi for vertical titanium sheet growth 2Fe 4O 9Crystal constitutes.
Embodiment 4
Bi (NO etc. amount 3) 35H 2O (1.552 gram) and Fe (NO 3) 39H 2O (1.293 gram) is dissolved in 0.1 centinormal 1 rare nitric acid, and the NaOH titration of 12 mol is complete to deposition then, and suction filtration is washed to solution and is neutral, also washes Na wherein off +And NO 3 -The deposition that obtains is dissolved in the NaOH solution that concentration is 12 mol, is made into 40 ml solns, Bi (NO 3) 35H 2The concentration of O be 80 mmoles/liter, Fe (NO 3) 39H 2The concentration of O is 40 milliliters of solution of 80 mmoles/rise; Pour 50 milliliters reaction kettle rapidly into and add the titanium sheet; In 200 ℃ of baking ovens, placed 24 hours; Take out and put into 100 ℃ of baking ovens placements 2 hours after the titanium sheet washes with deionized water and alcohol, the final product that obtains on the titanium sheet is the nano-sheet Bi of high orientation growth 2Fe 4O 9Sheet Bi 2Fe 4O 91-dimention nano Bi for vertical titanium sheet growth 2Fe 4O 9Crystal constitutes
Embodiment 5
Bi (NO etc. amount 3) 35H 2O (582 milligrams) and Fe (NO 3) 39H 2O (484.8 milligrams) is dissolved in 0.1 centinormal 1 rare nitric acid, and is complete to deposition with the NaOH titration of 12 mol then, and suction filtration is washed to solution and is neutral, also washes Na wherein off +And NO 3 -The deposition that obtains is dissolved in the NaOH solution that concentration is 12 mol, is made into 40 ml solns, Bi (NO 3) 35H 2The concentration of O be 30 mmoles/liter, Fe (NO 3) 39H 2The concentration of O be 30 mmoles/liter; Pour 50 milliliters reaction kettle rapidly into and add the titanium sheet; In 200 ℃ of baking ovens, placed 24 hours; Take out and put into 100 ℃ of baking ovens placements 3 hours after the titanium sheet washes with deionized water and alcohol, the final product that obtains on the titanium sheet is the nano-sheet Bi of high orientation growth 2Fe 4O 9Sheet Bi 2Fe 4O 91-dimention nano Bi for vertical titanium sheet growth 2Fe 4O 9Crystal constitutes.Bi 2Fe 4O 9XRD figure spectrum see Fig. 1, Bi 2Fe 4O 9FESEM photo Fig. 2.
Embodiment 6
Bi (NO etc. amount 3) 35H 2O (1.552 gram) and Fe (NO 3) 39H 2O (1.293 gram) is dissolved in 0.1 centinormal 1 rare nitric acid, and the NaOH titration of 12 mol is complete to deposition then, and suction filtration is washed to solution and is neutral, also washes Na wherein off +And NO 3 -The deposition that obtains is dissolved in the NaOH solution that concentration is 8 mol, is made into 40 ml solns, Bi (NO 3) 35H 2The concentration of O be 80 mmoles/liter, Fe (NO 3) 39H 2The concentration of O is 40 milliliters of solution of 80 mmoles/rise; Pour 50 milliliters reaction kettle rapidly into and add the titanium sheet; In 200 ℃ of baking ovens, placed 24 hours; Take out and put into 100 ℃ of baking ovens placements 2 hours after the titanium sheet washes with deionized water and alcohol, the final product that obtains on the titanium sheet is the nano-sheet Bi of high orientation growth 2Fe 4O 9Sheet Bi 2Fe 4O 91-dimention nano Bi for vertical titanium sheet growth 2Fe 4O 9Crystal constitutes.
Embodiment 7
Bi (NO etc. amount 3) 35H 2O (1.552 gram) and Fe (NO 3) 39H 2O (1.293 gram) is dissolved in 0.1 centinormal 1 rare nitric acid, and the NaOH titration of 12 mol is complete to deposition then, and suction filtration is washed to solution and is neutral, also washes Na wherein off +And NO 3 -The deposition that obtains is dissolved in the NaOH solution that concentration is 20 mol, is made into 40 ml solns, Bi (NO 3) 35H 2The concentration of O be 80 mmoles/liter, Fe (NO 3) 39H 2The concentration of O is 40 milliliters of solution of 80 mmoles/rise; Pour 50 milliliters reaction kettle rapidly into and add the titanium sheet; In 200 ℃ of baking ovens, placed 24 hours; Take out and put into 100 ℃ of baking ovens placements 2 hours after the titanium sheet washes with deionized water and alcohol, the final product that obtains on the titanium sheet is the nano-sheet Bi of high orientation growth 2Fe 4O 9Sheet Bi 2Fe 4O 91-dimention nano Bi for vertical titanium sheet growth 2Fe 4O 9Crystal constitutes.

Claims (1)

1. template-free hydrothermal synthesis of one-dimensional nano Bi 2Fe 4O 9Method, it is characterized in that, with Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O as the hydro-thermal reaction mineralizer, is that 99.9% titanium sheet be substrate with purity with NaOH as reaction raw materials, under 160-220 ℃ of coldcondition, and hydrothermal method synthesizing one-dimensional nanometer Bi 2Fe 4O 9, its preparation process comprises:
1), with reaction raw materials Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O with etc. the ratio of amount be dissolved in rare nitric acid Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O concentration be the 12-100 mmole/liter, then fully with NaOH aqueous solution titration to deposition, suction filtration, and be neutral with deionized water washing sediment to wash solution;
2), the throw out after the washing that step 1) is obtained is dissolved in the NaOH aqueous solution that concentration is the 8-20 mol, puts into reaction kettle then and puts into the titanium sheet, reaction is 12-72 hour under 160-220 ℃ of condition, the product of in the substrate of titanium sheet, growing;
3), with step 2) growth that obtains the titanium sheet of product with deionized water and alcohol flushing after, put into baking oven and dry, the final product that obtains on the titanium sheet is 1-dimention nano Bi 2Fe 4O 9
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