CN102091632A - Microwave hydrothermal method for preparing Bi25FeO40-BiFeO3 powder - Google Patents

Microwave hydrothermal method for preparing Bi25FeO40-BiFeO3 powder Download PDF

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CN102091632A
CN102091632A CN 201010615880 CN201010615880A CN102091632A CN 102091632 A CN102091632 A CN 102091632A CN 201010615880 CN201010615880 CN 201010615880 CN 201010615880 A CN201010615880 A CN 201010615880A CN 102091632 A CN102091632 A CN 102091632A
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powder
microwave
feo
bifeo
hydrothermal
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谈国强
郑玉芹
宋丽花
程蒙
博海洋
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a microwave hydrothermal method for preparing a novel photocatalytic material Bi25FeO40-BiFeO3 powder, which comprises the following steps of: (1) dissolving FeCl3.6H2O and Bi(NO3)3.5H2O in a proper amount of glycol to prepare mother salt solution; (2) dripping the mother salt solution into ammonium aqueous solution with the concentration of 0.1-0.5mol/L at a titrate speed of less than 2mL/min, and after the titration is finished, continuously stirring for 0.4 to 1 hour to obtain a precipitate; (3) repeatedly cleaning the precipitate by using deionized water, and ageing to prepare a hydrothermal reaction precursor; and (4) adding precursor solution into a microwave hydrothermal kettle, ensuring the packing ratio is 40-75 percent, adding a mineralizer into the reaction kettle, putting the reaction kettle into a microwave-assisted hydrothermal synthesizer, reacting for a period of time, taking a product out of the reaction kettle, washing with deionized water to obtain a neutral product, cleaning the neutral product by using absolute ethanol, and drying at room temperature to obtain the Bi25FeO40-BiFeO3 powder. The invention has the advantage that: the Bi25FeO40-BiFeO3 powder has excellent photocatalytic performance and good magnetic performance, and is a novel photocatalytic material which is convenient to recycle.

Description

A kind of microwave-hydrothermal method prepares Bi＜sub〉25＜/sub〉FeO＜sub〉40＜/sub 〉-BiFeO＜sub〉3＜/sub〉method of powder
Technical field
The present invention relates to a kind of preparation method of bismuth ferrite powder, particularly a kind of microwave-hydrothermal method prepares Bi 25FeO 40-BiFeO 3The method of powder.
Background technology
In recent years, catalysis material has caused the very big interest of people.Sillenite Bi 25FeO 40Crystal structure is the body-centered cubic phase structure, and the space point group is I23, and a large amount of defectives that exist in its crystal structure cause it to have nonlinear optical effect and piezo-electric effect, has a good application prospect in light conduction and visible light catalytic field.Ferrous acid bismuth (BiFeO 3) have typical perovskite structure, photocatalysis performance is preferably arranged, it has ferromagnetism simultaneously, is convenient to reclaim, and also is one to have the catalysis material of applications well prospect.
Heating using microwave has the incomparable advantage of the especially traditional synthetic technology of additive method, as: the rate of heat addition is fast, reaction condition is gentle, and the preparation powder granularity is even, and heat energy utilization rate height is convenient to control automatically and advantage such as continued operation.So far do not see about microwave hydrothermal both at home and abroad and prepare Bi 25FeO 40-BiFeO 3The report of powder prepares Bi with the microwave-hydrothermal method method 25FeO 40-BiFeO 3Powder only needs 30min, obtains 10 μ m left and right sides porous cubic powders, and particle diameter is evenly distributed, and photocatalysis performance is superior.
The present invention has summed up microwave-hydrothermal method and has prepared Bi 25FeO 40-BiFeO 3The condition and range of powder is for further investigation and production application later on provides reliable basis.
Summary of the invention
The object of the present invention is to provide a kind of novel catalysis material Bi 25FeO 40-BiFeO 3Powder, this material have magnetic simultaneously and are convenient to recycle.The Bi that makes by microwave-hydrothermal method preparation method of the present invention 25FeO 40-BiFeO 3Powder, even particle size distribution and preparation process have good repeatability.
For achieving the above object, the technical solution used in the present invention is (it is pure that raw material is analysis):
A kind of microwave-hydrothermal method prepares ferrous acid bismuth Bi 25FeO 40-BiFeO 3The method of powder is characterized in that:
(1) with FeCl 36H 2O and Bi (NO 3) 35H 2O is dissolved in and is made into female salting liquid in the 10-30ml ethylene glycol; Press atomic molar in female salting liquid than Fe: Bi=1: 1;
(2) according to female salting liquid and ammonia spirit be 1: 25 ratio, female salting liquid be added drop-wise in the ammonia spirit that concentration is 0.1-0.5mol/L that rate of titration, continues to stir 0.4-1h and obtains sediment after titration finishes less than 2mL/min;
(3) sediment is cleaned repeatedly with deionized water, be neutral up to supernatant, ageing 1-10 days, remove supernatant, make the hydro-thermal reaction precursor solution, precursor solution concentration is 0.01-0.05mol/L;
(4) precursor solution is added in the reactor, packing ratio is 60%-75%, and in reactor, add mineralizer, to reflect that still places microwave auxiliary water thermal synthesis instrument, in 160 ℃-230 ℃, pressure is 0.6-2.7Mpa, behind the reaction 20-120min, take out product and spend deionised water to neutral, clean 2-4 time with absolute ethyl alcohol, drying obtains Bi under the room temperature 25FeO 40-BiFeO 3Powder.
Further, the present invention also comprises following characteristics:
In the described step (1), with FeCl 36H 2O and Bi (NO 3) 35H 2O is dissolved in 10ml, 20ml or the 30ml ethylene glycol and is made into female salting liquid.
Described step (2) is that female salting liquid is added drop-wise in the ammonia spirit that concentration is 0.1mol/L, 0.2mol/L, 0.3mol/L, 0.4mol/L or 0.5mol/L, rate of titration is less than 2mL/min, after titration finishes, continue stirring 0.4h, 0.8h or 1h and obtain sediment.
Described step (3) is that sediment is cleaned repeatedly with deionized water, be neutral up to supernatant, ageing 1 day, 5 days or 10 days, remove supernatant, make the hydro-thermal reaction precursor solution, precursor solution concentration is 0.01mol/L, 0.02mol/L, 0.03mol/L, 0.04mol/L or 0.05mol/L.
Described step (4) adds precursor solution in the reactor, packing ratio is 60%, 70% or 75%, and in reactor, add mineralizer, reactor is placed microwave auxiliary water thermal synthesis instrument, utilize the microwave hydrothermal synthesizer that temperature is controlled at 160 ℃, 180 ℃, 200 ℃, 220 ℃ or 230 ℃, pressure is 0.6Mpa, 1.0Mpa, 1.5Mpa, 2.3Mpa or 2.7Mpa, reaction 20min, 40min, 60min, 80min, behind 100min or the 120min, product in the taking-up microwave hydrothermal still spends deionised water and obtains neutral products, again neutral products is cleaned 2 with absolute ethyl alcohol, 3 or 4 times, drying obtains Bi under the room temperature 25FeO 40-BiFeO 3Powder.
In the described step (4), mineralizer is for analyzing pure KOH solid or NaOH solid or urea solid; The addition of mineralizer is 0.03mol/, 0.05mol/ or 1mol/L.
The invention has the beneficial effects as follows and prepare the superior Bi of photochemical catalyst magnetic property 25FeO 40-BiFeO 3Powder, and summed up preparation Bi 25FeO 40-BiFeO 3The condition and range of powder.The powder granularity that obtains evenly adopts temperature control to select suitable compactedness, so that course of reaction is reduced by ectocine, makes preparation process have good repeatability.Technology controlling and process is simple, and process cycle is short, saves the energy.
Description of drawings
Fig. 1 is predecessor concentration 0.03mol/L of the present invention, 200 ℃, and the Bi of KOH 0.15mol/L preparation 25FeO 40-BiFeO 3The XRD figure of powder;
Fig. 2 is predecessor concentration 0.03mol/L of the present invention, 200 ℃, and the Bi of KOH 0.15mol/L preparation 25FeO 40-BiFeO 3The SEM figure of powder;
Fig. 3 is Bi of the present invention 25FeO 40-BiFeO 3Powder, pure phase Bi 25FeO 40And pure phase BiFeO 3Ultraviolet-visible light catalysis degradation modulus-the time graph of powder;
Fig. 4 is Bi of the present invention 25FeO 40-BiFeO 3Powder, pure phase Bi 25FeO 40And pure phase BiFeO 3Powder hysteresis curve;
Bi when Fig. 5 is predecessor concentration 0.05mol/L of the present invention 25FeO 40-BiFeO 3The formation range figure of powder.
Fig. 6 is for summing up preparation Bi 25FeO 40-BiFeO 3The formation range of powder.
The specific embodiment
The present invention will be further described below in conjunction with specific embodiment.
Embodiment 1
Select FeCl for use 36H 2O, Bi (NO 3) 35H 2O is that raw material is dissolved in and is made into female salting liquid (0.5mol/L) in the 20ml ethylene glycol, wherein, presses atomic molar in female salting liquid than Fe: Bi=1: 1; It is splashed into the concentration of diluting under stirring condition be in the 0.3mol/L ammonia spirit, rate of titration is less than 2mL/min, after titration finishes, continue to stir 0.5h, the sediment that reaction obtains cleans repeatedly with deionized water, is neutral up to supernatant, ageing 5d, remove supernatant, promptly make the hydro-thermal reaction predecessor, precursor solution concentration is 0.03mol/L;
Predecessor is moved to the microwave hydrothermal still, filling rate 70%, and in reactor, add 0.03mol/L KOH as mineralizer, in the microwave hydrothermal instrument, temperature is controlled to be 200 ℃, pressure is 1.5Mpa, reaction 60min takes out product and spends deionised water to neutral, cleans 3 times with absolute ethyl alcohol at last, dry under the room temperature, preservation obtain Bi 25FeO 40-BiFeO 3Powder.
As can be seen from Figure 1 KOH concentration 0.15mol/L, 200 ℃ of temperature about pressure 1.5Mpa, can be prepared Bi 25FeO 40-BiFeO 3Powder, wherein n (Bi 25FeO 40: BiFeO 3) be about 1: 2.
Bi as can be seen from Figure 2 25FeO 40-BiFeO 3Powder is the cubic structure of the porous about 10nm.
As can be seen from Figure 3 Bi 25FeO 40-BiFeO 3The powder photocatalysis performance is than pure phase Bi 25FeO 40And pure phase BiFeO 3Powder is superior a lot.
As can be seen from Figure 4 Bi 25FeO 40-BiFeO 3Powder magnetic can be than pure phase Bi 25FeO 40And BiFeO 3Powder is superior.
Embodiment 2
Select FeCl for use 36H 2O, Bi (NO 3) 35H 2O is that raw material is dissolved in and is made into female salting liquid (0.5mol/L) in the 10ml ethylene glycol, wherein, presses atomic molar in female salting liquid than Fe: Bi=1: 1; It is splashed into the concentration of diluting under stirring condition be in the 0.1mol/L ammonia spirit, rate of titration is less than 2mL/min, after titration finishes, continue to stir 0.8h, the sediment that reaction obtains cleans repeatedly with deionized water, is neutral up to supernatant, ageing 1d, remove supernatant, promptly make the hydro-thermal reaction predecessor, precursor solution concentration is 0.05mol/L;
Predecessor is moved to the microwave hydrothermal still, filling rate 60%, and in reactor, add 0.05mol/L KOH as mineralizer, in the microwave hydrothermal instrument, temperature is controlled to be 180 ℃, and pressure is 1.0Mpa, take out product behind the reaction 40min and spend deionised water to neutral, clean 4 times with absolute ethyl alcohol at last, dry under the room temperature, preservation obtain Bi 25FeO 40-BiFeO 3Powder.
Embodiment 3
Select FeCl for use 36H 2O, Bi (NO 3) 35H 2O is that raw material is dissolved in and is made into female salting liquid (0.5mol/L) in the 30ml ethylene glycol, wherein, presses atomic molar in female salting liquid than Fe: Bi=1: 1; It is splashed into the concentration of diluting under stirring condition be in the 0.5mol/L ammonia spirit, rate of titration is less than 2mL/min, after titration finishes, continue to stir 1h, the sediment that reaction obtains cleans repeatedly with deionized water, is neutral up to supernatant, ageing 10d, remove supernatant, promptly make the hydro-thermal reaction predecessor, precursor solution concentration is 0.04mol/L;
Predecessor is moved to the microwave hydrothermal still, filling rate 75%, and in reactor, add 0.05mol/L KOH as mineralizer, in the microwave hydrothermal instrument, temperature is controlled to be 160 ℃, and pressure is 0.6Mpa, take out product behind the reaction 20min and spend deionised water to neutral, clean 2 times with absolute ethyl alcohol at last, dry under the room temperature, preservation obtain Bi 25FeO 40-BiFeO 3Powder.
Embodiment 4
Select FeCl for use 36H 2O, Bi (NO 3) 35H 2O is that raw material is dissolved in and is made into female salting liquid (0.5mol/L) in the 20ml ethylene glycol, wherein, presses atomic molar in female salting liquid than Fe: Bi=1: 1; It is splashed into the concentration of diluting under stirring condition be in the 0.2mol/L ammonia spirit, rate of titration is less than 2mL/min, after titration finishes, continue to stir 0.8h, the sediment that reaction obtains cleans repeatedly with deionized water, is neutral up to supernatant, ageing 5d, remove supernatant, promptly make the hydro-thermal reaction predecessor, precursor solution concentration is 0.02mol/L;
Predecessor is moved to the microwave hydrothermal still, filling rate 70%, and in reactor, add 0.05mol/L KOH as mineralizer, in the microwave hydrothermal instrument, temperature is controlled to be 220 ℃, and pressure is 2.3Mpa, take out product behind the reaction 80min and spend deionised water to neutral, clean 3 times with absolute ethyl alcohol at last, dry under the room temperature, preservation obtain Bi 25FeO 40-BiFeO 3Powder.
Embodiment 5
Select FeCl for use 36H 2O, Bi (NO 3) 35H 2O is that raw material is dissolved in and is made into female salting liquid (0.5mol/L) in the 30ml ethylene glycol, wherein, presses atomic molar in female salting liquid than Fe: Bi=1: 1; It is splashed into the concentration of diluting under stirring condition be in the 0.4mol/L ammonia spirit, rate of titration is less than 2mL/min, after titration finishes, continue to stir 0.4h, the sediment that reaction obtains cleans repeatedly with deionized water, is neutral up to supernatant, ageing 5d, remove supernatant, promptly make the hydro-thermal reaction predecessor, precursor solution concentration is 0.01mol/L;
Predecessor is moved to the microwave hydrothermal still, filling rate 60%, and in reactor, add 1mol/L KOH as mineralizer, in the microwave hydrothermal instrument, temperature is controlled to be 230 ℃, and pressure is 2.7Mpa, take out product behind reaction 100min or the 120min and spend deionised water to neutral, clean 3 times with absolute ethyl alcohol at last, dry under the room temperature, preservation obtain Bi 25FeO 40-BiFeO 3Powder.
Fig. 5 is 170 ℃, and KOH 0.25mol/L is the Bi of reaction 60min generation down 25FeO 40-BiFeO 3The powder XRD figure.Powder n (the Bi for preparing as can be seen among the figure 25FeO 40: BiFeO 3) be about 1: 1.
Fig. 6 is for summing up preparation Bi 25FeO 40-BiFeO 3The formation range of powder (B district between two curves).
The invention has the beneficial effects as follows the Bi that obtains having superior photocatalysis performance and magnetic property 25FeO 40-BiFeO 3Powder sums up the Bi that uses microwave-hydrothermal method to prepare 25FeO 40-BiFeO 3The suitable synthetic scope of powder.And it is even to prepare powder granularity with microwave-hydrothermal method, adopts pressure control to select suitable compactedness, and reaction temperature and pressure so that course of reaction is reduced by ectocine, make preparation process have good repeatability.And technology controlling and process is simple, and process cycle is short, saves the energy.
Above content is to further describing that the present invention did in conjunction with concrete preferred implementation; can not assert that the specific embodiment of the present invention only limits to this; for the general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; can also make some simple deduction or replace, all should be considered as belonging to the protection domain that the present invention is determined by claims of being submitted to.

Claims (6)

1. a microwave-hydrothermal method prepares ferrous acid bismuth Bi 25FeO 40-BiFeO 3The method of powder is characterized in that:
(1) with FeCl 36H 2O and Bi (NO 3) 35H 2O is dissolved in and is made into female salting liquid in the 10-30ml ethylene glycol; Press atomic molar in female salting liquid than Fe: Bi=1: 1;
(2) according to female salting liquid and ammonia spirit be 1: 25 ratio, female salting liquid be added drop-wise in the ammonia spirit that concentration is 0.1-0.5mol/L that rate of titration, continues to stir 0.4-1h and obtains sediment after titration finishes less than 2mL/min;
(3) sediment is cleaned repeatedly with deionized water, be neutral up to supernatant, ageing 1-10 days, remove supernatant, make the hydro-thermal reaction precursor solution, precursor solution concentration is 0.01-0.05mol/L;
(4) precursor solution is added in the reactor, packing ratio is 60%-75%, and in reactor, add mineralizer, to reflect that still places microwave auxiliary water thermal synthesis instrument, in 160 ℃-230 ℃, pressure is 0.6-2.7Mpa, behind the reaction 20-120min, take out product and spend deionised water to neutral, clean 2-4 time with absolute ethyl alcohol, drying obtains Bi under the room temperature 25FeO 40-BiFeO 3Powder.
2. prepare Bi according to the described a kind of microwave-hydrothermal method of claim 1 25FeO 40-BiFeO 3The method of powder is characterized in that: in the described step (1), with FeCl 36H 2O and Bi (NO 3) 35H 2O is dissolved in 10ml, 20ml or the 30ml ethylene glycol and is made into female salting liquid.
3. prepare Bi according to the described a kind of microwave-hydrothermal method of claim 1 25FeO 40-BiFeO 3The method of powder, it is characterized in that: described step (2) is that female salting liquid is added drop-wise in the ammonia spirit that concentration is 0.1mol/L, 0.2mol/L, 0.3mol/L, 0.4mol/L or 0.5mol/L, rate of titration is less than 2mL/min, after titration finishes, continue stirring 0.4h, 0.8h or 1h and obtain sediment.
4. prepare Bi according to the described a kind of microwave-hydrothermal method of claim 1 25FeO 40-BiFeO 3The method of powder, it is characterized in that: described step (3) is that sediment is cleaned repeatedly with deionized water, be neutral up to supernatant, ageing 1 day, 5 days or 10 days, remove supernatant, make the hydro-thermal reaction precursor solution, precursor solution concentration is 0.01mol/L, 0.02mol/L, 0.03mol/L, 0.04mol/L or 0.05mol/L.
5. prepare Bi according to the described a kind of microwave-hydrothermal method of claim 1 25FeO 40-BiFeO 3The method of powder powder, it is characterized in that: described step (4) adds precursor solution in the reactor, packing ratio is 60%, 70% or 75%, and in reactor, add mineralizer, reactor is placed microwave auxiliary water thermal synthesis instrument, utilize the microwave hydrothermal synthesizer that temperature is controlled at 160 ℃, 180 ℃, 200 ℃, 220 ℃ or 230 ℃, pressure is 0.6Mpa, 1.5Mpa, 1.8Mpa, 2.1Mpa or 2.7Mpa, reaction 20min, 40min, 60min, 80min, behind 100min or the 120min, product in the taking-up microwave hydrothermal still spends deionised water and obtains neutral products, again neutral products is cleaned 2 with absolute ethyl alcohol, 3 or 4 times, drying obtains Bi under the room temperature 25FeO 40-BiFeO 3Powder.
6. prepare Bi according to the described a kind of microwave-hydrothermal method of claim 1 25FeO 40-BiFeO 3The method of powder is characterized in that: in the described step (4), mineralizer is for analyzing pure KOH solid or NaOH solid or urea solid; The addition of mineralizer is 0.03mol/, 0.05mol/ or 1mol/L.
CN 201010615880 2010-12-31 2010-12-31 Microwave hydrothermal method for preparing Bi25FeO40-BiFeO3 powder Pending CN102091632A (en)

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Cited By (4)

* 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
CN108479777A (en) * 2018-03-28 2018-09-04 常州大学 A kind of preparation method and applications of attapulgite composite photo-catalyst
CN110227476A (en) * 2019-06-25 2019-09-13 长春工程学院 A kind of BiFeO3/Bi25FeO40The preparation method and applications of heterojunction structure catalyst
CN115007164A (en) * 2022-06-27 2022-09-06 中山大学 Preparation of rod-shaped bismuth ferrite piezoelectric catalyst and application of rod-shaped bismuth ferrite piezoelectric catalyst in preparation of hydrogen peroxide and hydrogen by catalytic cracking of water

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101654283A (en) * 2009-09-17 2010-02-24 陕西科技大学 Method for preparing bismuth ferrite powder by microwave hydrothermal method

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101654283A (en) * 2009-09-17 2010-02-24 陕西科技大学 Method for preparing bismuth ferrite powder by microwave hydrothermal method

Cited By (5)

* 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
CN108479777A (en) * 2018-03-28 2018-09-04 常州大学 A kind of preparation method and applications of attapulgite composite photo-catalyst
CN110227476A (en) * 2019-06-25 2019-09-13 长春工程学院 A kind of BiFeO3/Bi25FeO40The preparation method and applications of heterojunction structure catalyst
CN110227476B (en) * 2019-06-25 2023-01-20 长春工程学院 BiFeO 3 /Bi 25 FeO 40 Preparation method and application of heterostructure catalyst
CN115007164A (en) * 2022-06-27 2022-09-06 中山大学 Preparation of rod-shaped bismuth ferrite piezoelectric catalyst and application of rod-shaped bismuth ferrite piezoelectric catalyst in preparation of hydrogen peroxide and hydrogen by catalytic cracking of water

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Application publication date: 20110615