CN102701287A - Preparation method of one-dimensional nano Bi25FeO40 material capable of generating photocurrent - Google Patents

Preparation method of one-dimensional nano Bi25FeO40 material capable of generating photocurrent Download PDF

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CN102701287A
CN102701287A CN2012101941446A CN201210194144A CN102701287A CN 102701287 A CN102701287 A CN 102701287A CN 2012101941446 A CN2012101941446 A CN 2012101941446A CN 201210194144 A CN201210194144 A CN 201210194144A CN 102701287 A CN102701287 A CN 102701287A
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feo
titanium sheet
preparation
koh
reaction
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孙华君
张小娜
陈文�
周静
朱泉峣
沈杰
郭姗姗
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Wuhan University of Technology WUT
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Abstract

The invention discloses a preparation method of a one-dimensional nano Bi25FeO40 material capable of generating photocurrent. A hydrothermal process is used for synthesizing one-dimensional nano Bi25FeO40 crystals. The preparation method mainly adopts the hydrothermal process and comprises the steps of: dissolving Bi(NO3)3.5H2O and Fe(NO3)3.9H2O in dilute nitric acid, wherein the weight ratio of the Bi(NO3)3.5H2O to the Fe(NO3)3.9H2O is 6:1 to 16:1, then titrating with 10mol/L KOH water solution till sediment is fully precipitated, filtering the sediment and washing with water till the solution is neutral; dissolving the obtained sediment in 0.5-2mol/L KOH solution, pouring the obtained solution into a reaction kettle in which a metal titanium sheet with thickness of 0.1mm and size of 1cm*1cm is placed and keeping reaction for 12-72 hours at 150-190DEG C; and taking the titanium sheet, repetitively washing the titanium sheet with deionized water and ethanol for 2-3 times and placing the titanium sheet in a drying oven for drying to obtain final products, i.e. the one-dimensional nano Bi25FeO40 crystals.

Description

Produce the 1-dimention nano Bi of photoelectric current 25FeO 40Material preparation method
Technical field
The present invention relates to a kind of synthetic 1-dimention nano Bi that can produce photoelectric current of hydrothermal method that utilizes 25FeO 40The preparation method.Belong to nano photoelectric technology category.
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 meaningful to the fundamental research of material, and the utilization of material is also had very big value.Bi 25FeO 40Have a large amount of oxygen room and ion room in the crystalline structure, have photorefractive property, pl-and photoconductive property, using value is very huge, can be applicable to photocatalytic degradation water or atmospheric pollution, fields such as photoswitch.
Now about Bi 25FeO 40The report of one-dimensional material preparation is still rarely found, does not also see Bi 25FeO 40The report of photogenerated current.Seal can ring and use sol-gel method to prepare Bi 25FeO 40The product thing that powdered material, sol-gel method obtain is mutually impure, has Bi 2O 3Assorted peak, this possibly be because the solid phase method reaction product is mixed inhomogeneous causing [1].Wang Yonggang has synthesized a cube phase Bi with hydrothermal method 12(Bi 0.5Fe 0.5) O 19.5Powder presents spherical pattern [2].Han Jiantao has adopted Hydrothermal Preparation Bi 12Fe 0.63O 20-δPowdered material, product are multiple pattern [3].Old literary grace uses NaOH to be mineralizer, Hydrothermal Preparation Bi 2Fe 4O 9One-dimensional nano-array, the material of this structure are not reported and can be produced photogenerated current [4].
[1] seal can ring. the preparation of bismuth-based oxide material and Photocatalytic Performance Study thereof [D]. and Shandong: Shandong University, 2007.
[2]?Wang?Y?G,?Xu?G,?Yang?L?L,?Ren?Z?H,?Wei?X.?Alkali?metal?ions-assisted?controllable?synthesis?of?bismuth?ferrites?by?a?hydrothermal?method.Journal?of?the?American?Ceramic?Society,?90(2007)?3673。
[3] Han Jiantao. the preparation of novel magnetoelectricity functional compounds and sign [D]. Shanghai: Shanghai Communications University, 2007.
[4] Chen Wen. template-free hydrothermal synthesis of one-dimensional nano Bi 2Fe 4O 9[P]. Chinese patent: 101830514A, 2010-09-15.
Summary of the invention
The object of the present invention is to provide a kind of hydrothermal method synthesizing one-dimensional nanometer Bi that utilizes 25FeO 40The method of material.
The technical scheme that realizes the object of the invention is:
A kind of no template hydrothermal method synthesizing one-dimensional nanometer Bi 25FeO 40The crystalline method is characterized in that, with Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O as the hydro-thermal reaction mineralizer, is a substrate with the metal titanium sheet with KOH as reaction raw materials, under 150-190 ℃ of condition, and hydrothermal method synthesizing one-dimensional nanometer Bi 25FeO 40Crystal.
No template hydrothermal method synthesizing one-dimensional nanometer Bi of the present invention 25FeO 40The crystalline method steps comprises:
1) with reaction raw materials Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O is dissolved in 0.1 centinormal 1 rare nitric acid, and then with 10 mol KOH aqueous solution titration to deposition fully, suction filtration also is neutral with deionized water washing sediment to wash solution;
2) the washing postprecipitation thing that step 1) is obtained is dissolved in the KOH aqueous solution that concentration is the 0.5-2 mol, and pouring into then and being placed with thickness is 0.1mm, and size is in the reaction kettle of metal titanium sheet of 1cm * 1cm, and reaction is 12-72 hour under 150-190 ℃ of condition;
3) with step 2) growth that obtains after the titanium sheet of product washes 2-3 time repeatedly with deionized water and ethanol, put into baking oven and dry, the final product that obtains on the titanium sheet is 1-dimention nano Bi 25FeO 40Crystal.
Among the preparation method of the present invention, reaction raw materials Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O the hydro-thermal reaction concentration range be the 6-150 mmole/liter.
Among the preparation method of the present invention, reaction raw materials Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O adds according to the proportioning of 6:1-16:1 amount of substance.
Among the preparation method of the present invention, putting into the baking oven bake out temperature in the step 3) is 60-100 ℃.
Description of drawings
Fig. 1 is embodiment 1 180 ℃ of hydro-thermal reactions 36 hours, R (Bi/Fe)=16:1, the Bi for preparing when KOH concentration is 0.5 mol 25FeO 40XRD figure spectrum, (01-078-1543) is corresponding with the JCPDF card;
Fig. 2 is embodiment 3 160 ℃ of hydro-thermal reactions 48 hours, R (Bi/Fe)=12:1, the Bi that KOH concentration prepares when being 1.5 mol 25FeO 40SEM photo (20000 times);
Fig. 3 is embodiment 5 180 ℃ of hydro-thermal reactions 48 hours, R (Bi/Fe)=12:1, the Bi that KOH concentration prepares when being 1 mol 25FeO 40SEM photo (10000 times);
Fig. 4 is embodiment 5 180 ℃ of hydro-thermal reactions 48 hours, R (Bi/Fe)=12:1, the Bi that KOH concentration prepares when being 1 mol 25FeO 40SEM photo (50000 times);
Fig. 5 is embodiment 5 180 ℃ of hydro-thermal reactions 48 hours, R (Bi/Fe)=12:1, the Bi that KOH concentration prepares when being 1 mol 25FeO 40Transient state photoelectricity flow graph.
Embodiment
No template hydrothermal method synthesizing one-dimensional nanometer Bi of the present invention 25FeO 40Crystal Concrete preparation process is:
1), with reaction raw materials Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O is dissolved in 0.1 centinormal 1 rare nitric acid with the proportioning of 6:1-16:1 amount of substance, with 10 mol KOH aqueous solution titration to deposition fully, gained is precipitated suction filtration then, and is neutral with deionized water washing sediment to wash solution;
2), washing postprecipitation thing that step 1 is obtained is dissolved in the KOH aqueous solution that concentration is the 0.5-2.0 mol, pours in the reaction kettle that is placed with metal titanium sheet, reaction is 12-72 hour under 150-190 ℃ of condition;
3), product that step 2 is obtained with deionized water and alcohol washing after, put into oven dry in 60-100 ℃ of baking oven 2-4 hour, the final product that obtains is 1-dimention nano Bi 25FeO 40Crystal.
From FESEM figure, can obviously find the bar-shaped Bi of 1-dimention nano to product 25FeO 40Key of the present invention is to control concentration and the Bi (NO of mineralizer KOH 3) 35H 2O and Fe (NO 3) 39H 2The proportioning of the amount of substance of O.The concentration of KOH between the 0.5-2.0 mol, Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O adds according to the proportioning of 6:1-16:1 amount of substance.
Used Bi (NO among the present invention 3) 35H 2O, Fe (NO 3) 39H 2O, nitric acid, KOH are commercial AR.
The testing transient photoelectric current is with Bi among the present invention 25FeO 40Sample electrode is a working electrode, and SCE (SCE) is as reference electrode, and platinum electrode is formed the standard three-electrode system as counter electrode, on Autolab PGATAT30 type electrochemical workstation, tests.Light source uses be 125w from the ballast high pressure mercury fluorescent lamp.Test whenever changed the switch of light source at a distance from 250 seconds.
Embodiment 1
Press amount of substance 16:1 proportioning raw material, get 1.94 gram Bi (NO 3) 35H 2O and 0.101 gram Fe (NO 3) 39H 2O is dissolved in 0.1 centinormal 1 rare nitric acid, and is complete to deposition with the KOH titration of 10 mol then, and suction filtration is washed to solution and is neutral, also washes K wherein off +And NO 3 -The deposition that obtains is dissolved in the KOH solution that concentration is 0.5 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 6.25 mmoles/liter; Pour 50 milliliters reaction kettle rapidly into and add the titanium sheet, in 180 ℃ of baking ovens, placed 36 hours, after taking-up titanium sheet washes 3 times repeatedly with deionized water and ethanol; Put into 100 ℃ of baking ovens and placed 3 hours, obtain the 1-dimention nano Bi that final product is oriented growth 25FeO 40Crystal.The XRD figure spectrum of product is like Fig. 1.
Embodiment 2
Press amount of substance 12:1 proportioning raw material, promptly get 2.91 gram Bi (NO 3) 35H 2O and 0.202 gram Fe (NO 3) 39H 2O is dissolved in 0.1 centinormal 1 rare nitric acid, and is complete to deposition with the KOH titration of 10 mol then, and suction filtration is washed to solution and is neutral, also washes K wherein off +And NO 3 -The deposition that obtains is dissolved in the KOH solution that concentration is 0.5 mol, is made into 40 ml solns, Bi (NO 3) 35H 2The concentration of O be 150 mmoles/liter, Fe (NO 3) 39H 2The concentration of O be 12.5 mmoles/liter; Pour 50 milliliters reaction kettle rapidly into and add the titanium sheet, in 180 ℃ of baking ovens, placed 48 hours, after taking-up titanium sheet washes 3 times repeatedly with deionized water and ethanol; Put into 100 ℃ of baking ovens and placed 2 hours, obtain final product and be 1-dimention nano Bi 25FeO 40Crystal.
Embodiment 3
Press amount of substance 12:1 proportioning raw material, i.e. 2.91 gram Bi (NO 3) 35H 2O and 0.202 gram Fe (NO 3) 39H 2O is dissolved in 0.1 centinormal 1 rare nitric acid, and is complete to deposition with the KOH titration of 10 mol then, and suction filtration is washed to solution and is neutral, also washes K wherein off +And NO 3 -The deposition that obtains is dissolved in the KOH solution that concentration is 1.5 mol, is made into 40 ml solns, Bi (NO 3) 35H 2The concentration of O be 150 mmoles/liter, Fe (NO 3) 39H 2The concentration of O be 12.5 mmoles/liter; Pour 50 milliliters reaction kettle rapidly into and add the titanium sheet, in 160 ℃ of baking ovens, placed 48 hours, after taking-up titanium sheet washes 3 times repeatedly with deionized water and ethanol; Put into 80 ℃ of baking ovens and placed 4 hours, obtain final product and be 1-dimention nano Bi 25FeO 40Crystal.The SEM photo of product is seen Fig. 2 (20000 times).
Embodiment 4
Press amount of substance 6:1 proportioning raw material, i.e. 2.91 gram Bi (NO 3) 35H 2O and 0.404 gram Fe (NO 3) 39H 2O is dissolved in 0.1 centinormal 1 rare nitric acid, and the KOH titration of 10 mol is complete to deposition then, and suction filtration is washed to solution and is neutral, also washes K wherein off +And NO 3 -The deposition that obtains is dissolved in the KOH solution that concentration is 2 mol, is made into 40 ml solns, Bi (NO 3) 35H 2The concentration of O be 150 mmoles/liter, Fe (NO 3) 39H 2The concentration of O is 40 milliliters of solution of 25 mmoles/rise; Pour 50 milliliters reaction kettle rapidly into and add the titanium sheet, in 190 ℃ of baking ovens, placed 24 hours, after taking-up titanium sheet washes 3 times repeatedly with deionized water and ethanol; Put into 100 ℃ of baking ovens and placed 2 hours, obtain final product and be 1-dimention nano Bi 25FeO 40Crystal.
Embodiment 5
Press amount of substance 12:1 proportioning raw material, get 2.91 gram Bi (NO 3) 35H 2O and 0.202 gram Fe (NO 3) 39H 2O is dissolved in 0.1 centinormal 1 rare nitric acid, and is complete to deposition with the KOH titration of 10 mol then, and suction filtration is washed to solution and is neutral, also washes K wherein off +And NO 3 -The deposition that obtains is dissolved in the KOH solution that concentration is 1 mol, is made into 40 ml solns, Bi (NO 3) 35H 2The concentration of O be 150 mmoles/liter, Fe (NO 3) 39H 2The concentration of O be 12.5 mmoles/liter; Pour 50 milliliters reaction kettle rapidly into and add the titanium sheet, in 180 ℃ of baking ovens, placed 48 hours, after taking-up titanium sheet washes 3 times repeatedly with deionized water and ethanol; Put into 100 ℃ of baking ovens and placed 3 hours, obtain the one-dimensional rod-like Bi that final product is oriented growth 25FeO 40Crystal.The SEM photo of product is seen Fig. 3 (10000 times), Fig. 4 (50000 times).Transient state photoelectricity flow graph is seen Fig. 5.
Embodiment 6
Amount of substance 6:1 proportioning raw material, i.e. 2.91 gram Bi (NO 3) 35H 2O and 0.404 gram Fe (NO 3) 39H 2O is dissolved in 0.1 centinormal 1 rare nitric acid, and is complete to deposition with the KOH solution titration of 10 mol then, and suction filtration is washed to solution and is neutral, also washes K wherein off +And NO 3 -The deposition that obtains is dissolved in the KOH solution that concentration is 1 mol, is made into 40 ml solns, Bi (NO 3) 35H 2The concentration of O be 150 mmoles/liter, Fe (NO 3) 39H 2The concentration of O be 25 mmoles/liter; Pour 50 milliliters reaction kettle rapidly into and add the titanium sheet, in 150 ℃ of baking ovens, placed 48 hours, after taking-up titanium sheet washes 3 times repeatedly with deionized water and ethanol; Put into 60 ℃ of baking ovens and placed 4 hours, obtain final product and be 1-dimention nano Bi 25FeO 40Crystal.
Embodiment 7
Press amount of substance 16:1 proportioning raw material, get 1.94 gram Bi (NO 3) 35H 2O and 0.101 gram Fe (NO 3) 39H 2O is dissolved in 0.1 centinormal 1 rare nitric acid, and is complete to deposition with the KOH titration of 10 mol then, and suction filtration is washed to solution and is neutral, also washes K wherein off +And NO 3 -The deposition that obtains is dissolved in the KOH solution that concentration is 1 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 6.25 mmoles/liter; Pour 50 milliliters reaction kettle rapidly into and add the titanium sheet, in 190 ℃ of baking ovens, placed 48 hours, after taking-up titanium sheet washes 3 times repeatedly with deionized water and ethanol; Put into 100 ℃ of baking ovens and placed 2 hours, obtain the one-dimensional rod-like Bi that final product is oriented growth 25FeO 40Crystal.

Claims (5)

1. there is not template hydrothermal method synthesizing one-dimensional nanometer Bi 25FeO 40The crystalline method is characterized in that, with Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O as the hydro-thermal reaction mineralizer, is a substrate with the metal titanium sheet with KOH as reaction raw materials, under 150-190 ℃ of condition, and hydrothermal method synthesizing one-dimensional nanometer Bi 25FeO 40Crystal.
2. no template hydrothermal method synthesizing one-dimensional nanometer Bi as claimed in claim 1 25FeO 40The crystalline method is characterized in that preparation process comprises:
1) with reaction raw materials Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O is dissolved in 0.1 centinormal 1 rare nitric acid, and then with 10 mol KOH aqueous solution titration to deposition fully, suction filtration also is neutral with deionized water washing sediment to wash solution;
2) the washing postprecipitation thing that step 1) is obtained is dissolved in the KOH aqueous solution that concentration is the 0.5-2 mol, pours into then to be placed with in the reaction kettle of metal titanium sheet that size is 0.1mm for 1cm * 1cm, thickness, and reaction is 12-72 hour under 150-190 ℃ of condition;
3) with step 2) growth that obtains after the titanium sheet of product washes 2-3 time repeatedly with deionized water and ethanol, put into baking oven and dry, the final product that obtains on the titanium sheet is 1-dimention nano Bi 25FeO 40Crystal.
3. no template hydrothermal method synthesizing one-dimensional nanometer Bi as claimed in claim 2 25FeO 40The crystalline preparation method is characterized in that, reaction raw materials Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O the hydro-thermal reaction concentration range be the 6-150 mmole/liter.
4. no template hydrothermal method synthesizing one-dimensional nanometer Bi as claimed in claim 2 25FeO 40The crystalline preparation method is characterized in that, reaction raw materials Bi (NO 3) 35H 2O and Fe (NO 3) 39H 2O adds according to the proportioning of 6:1-16:1 amount of substance.
5. no template hydrothermal method synthesizing one-dimensional nanometer Bi as claimed in claim 2 25FeO 40The crystalline preparation method is characterized in that, putting into the baking oven bake out temperature in the step 3) is 60-100 ℃.
CN2012101941446A 2012-06-13 2012-06-13 Preparation method of one-dimensional nano Bi25FeO40 material capable of generating photocurrent Pending CN102701287A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106587162A (en) * 2016-10-31 2017-04-26 宝鸡文理学院 Method for preparing sillenite Bi25FeO40 nano powder through normal pressure water phase method

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CN101830514A (en) * 2010-03-23 2010-09-15 武汉理工大学 Method for template-free hydrothermal synthesis of one-dimensional nano-Bi2Fe4O9
CN102101700A (en) * 2010-12-31 2011-06-22 陕西科技大学 Method for preparing sillenite powder by microwave-hydrothermal method

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Publication number Priority date Publication date Assignee Title
CN106587162A (en) * 2016-10-31 2017-04-26 宝鸡文理学院 Method for preparing sillenite Bi25FeO40 nano powder through normal pressure water phase method

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Application publication date: 20121003