CN103420427A - Preparation method for bismuth ferrite Bi2Fe4O9 monocrystal nanosheets - Google Patents
Preparation method for bismuth ferrite Bi2Fe4O9 monocrystal nanosheets Download PDFInfo
- Publication number
- CN103420427A CN103420427A CN2012101615165A CN201210161516A CN103420427A CN 103420427 A CN103420427 A CN 103420427A CN 2012101615165 A CN2012101615165 A CN 2012101615165A CN 201210161516 A CN201210161516 A CN 201210161516A CN 103420427 A CN103420427 A CN 103420427A
- Authority
- CN
- China
- Prior art keywords
- bismuth
- reactor
- preparation
- single crystal
- bismuth ferrite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
The invention discloses a preparation method for bismuth ferrite Bi2Fe4O9 monocrystal nanosheets. Ferric nitrate and ammonium bismuth citrate are employed as raw materials. Deionized water and nitric acid are added. An appropriate amount of potassium hydroxide is added to promote crystallization. The above mixture is subjected to a hydrothermal reaction at the temperature of 160-230 DEG C to obtain bismuth ferrite Bi2Fe4O9 monocrystal nanosheets. The preparation method is advantaged by simple technological process, easy control, no pollution and low cost, and is easy for large-scale production. The prepared products have stable crystallization quality, and have wide application prospects in fields of semiconductor gas sensors, catalysts and the like.
Description
Technical field
The present invention relates to a kind of preparation method of bismuth ferrite single crystal nanoplate, belong to field of inorganic nonmetallic material.
Background technology
The performance of functional materials depends on their pattern, size and degree of crystallinity to a great extent, and the control of microscopic appearance has very large value to the utilization of material.Nano material has the physicochemical property more excellent than block materials, and the progress of science and technology and the miniaturization of electron device, and the nanometer of material has also been proposed to increasing requirement.Therefore, the preparation of control appearance of nano material becomes the focus that Materials science is paid close attention to and studied in recent years.
Bismuth ferrite (Bi
2Fe
4O
9) be a kind of important functional materials, the gases such as ethanol and acetone are had to good response, by extensively should be in the material of manufacturing semiconductor gas sensor.Bi
2Fe
4O
9Also can be used as industrial ammonia and be oxidized to nitric oxide production catalyzer, likely replace a large amount of expensive and expendable platinum, rhodium and palladium alloy catalysts of using at present.Due to its energy gap very narrow (~ 2.0eV), illustrate that it has good photoresponse in visible-range, its using value in photocatalysis field is very huge.
The method for preparing at present the bismuth iron series compound mainly adopts high temperature solid-state method and sol-gel method, and it reacts poor controllability, and product purity is low.Owing to there being the high-temperature calcination process, particle agglomeration is very serious, and the size of particle and pattern also are difficult to control.Hydrothermal method is a kind of evenly controlled material preparation method, has environmental protection, an advantage such as low, easy to control that consumes energy, and is commonly used to prepare the product of various multicomponent systems, also a kind of nano material preparation method commonly used, and this method is simple to operate, low for equipment requirements, with low cost.
Summary of the invention
The object of the present invention is to provide a kind of technique simply to prepare bismuth ferrite Bi
2Fe
4O
9The method of single crystal nanoplate.
Bismuth ferrite Bi of the present invention
2Fe
4O
9The preparation method of single crystal nanoplate comprises the following steps:
1) 1:1 metering in molar ratio takes iron nitrate and bismuth citrate amine, adds deionized water and nitric acid, and making the concentration of nitric acid in this system is 0.75mol/L ~ 1.125mol/L, fully stirs, and forms the settled solution that contains bismuth citrate amine and iron nitrate;
2) under whipped state, in the settled solution that contains bismuth citrate amine and iron nitrate made to step 1), add potassium hydroxide aqueous solution, the suspension of the oxyhydroxide precipitation that obtains containing bismuth and iron;
The suspension of the oxyhydroxide that contains bismuth and the iron precipitation that 3) will obtain is transferred in the reactor inner bag, reach the 70%-90% of reactor inner bag volume with the reaction mass volume in deionized water conditioned reaction still inner bag, stir at least 10 minutes, in reaction mass, the volumetric molar concentration of iron nitrate and bismuth citrate amine is 0.05mol/L, the volumetric molar concentration of potassium hydroxide is 1.5 ~ 2.5 mol/L, and the volume radix of volumetric molar concentration is the volume of material in all introducing reactor inner bags;
4) the reactor inner bag that step 3) is disposed to reaction mass is placed in reactor, sealing, under 160 ℃-230 ℃, hydrothermal treatment consists is carried out in insulation in 5-36 hour, then allow reactor naturally cool to room temperature, by deionized water and dehydrated alcohol repetitive scrubbing reaction product, filter, dry, obtain bismuth ferrite Bi
2Fe
4O
9Single crystal nanoplate.
In preparation process of the present invention, the reactor of use is polytetrafluoroethylliner liner, the reactor that the stainless steel external member is airtight.
In process of the present invention, the purity of said bismuth citrate amine, iron nitrate, potassium hydroxide and dehydrated alcohol all is not less than chemical pure.
The bismuth ferrite Bi that the inventive method makes
2Fe
4O
9The thickness of single crystal nanoplate is 5-150nm.
Beneficial effect of the present invention is:
Under the condition that the present invention is 1:1 at bismuth and iron molar concentration rate, use even controlled hydrothermal method to synthesize the bismuth ferrate nano sheet that bismuth and iron mol ratio are 1:2, prepared a kind of monocrystalline Bi of oriented growth by regulating some hydro-thermal reaction parameters
2Fe
4O
9Nanometer sheet.Technological process of the present invention is simple, is easy to control, and pollution-free, cost is low, is easy to produce.Synthetic monocrystalline Bi
2Fe
4O
9Nanometer sheet can be used for making well behaved Semiconductor gas sensors original paper, can be used as the catalyzer that the ammonia oxidation prepares NO, can also be as the photocatalyst of degradation of contaminant under visible ray.Its realization condition is all very good aspect feasibility and controllability.
The accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of the bismuth ferrite single crystal nanoplate for preparing of the present invention;
Fig. 2 is the stereoscan photograph of the bismuth ferrite single crystal nanoplate for preparing of the present invention.
Embodiment
Further illustrate the present invention below in conjunction with embodiment.
Example 1
1) 1:1 metering in molar ratio takes iron nitrate and bismuth citrate amine, adds deionized water and nitric acid, and making the concentration of nitric acid in this system is 1.125mol/L, fully stirs, and forms the settled solution that contains bismuth citrate amine and iron nitrate;
2) under whipped state, in the settled solution that contains bismuth citrate amine and iron nitrate made to step 1), add potassium hydroxide aqueous solution, the suspension of the oxyhydroxide precipitation that obtains containing bismuth and iron;
The suspension of the oxyhydroxide that contains bismuth and the iron precipitation that 3) will obtain is transferred in the reactor inner bag, reach 90% of reactor inner bag volume with the reaction mass volume in deionized water conditioned reaction still inner bag, stir 10 minutes, in reaction mass, the volumetric molar concentration of iron nitrate and bismuth citrate amine is 0.05mol/L, the volumetric molar concentration of potassium hydroxide is 1.5 mol/L, and the volume radix of volumetric molar concentration is the volume of material in all introducing reactor inner bags;
4) the reactor inner bag that step 3) is disposed to reaction mass is placed in reactor, sealing, and under 230 ℃, hydrothermal treatment consists is carried out in insulation in 5 hours, then allow reactor naturally cool to room temperature, by deionized water and dehydrated alcohol repetitive scrubbing reaction product, filter, dry, obtain bismuth ferrite Bi
2Fe
4O
9Single crystal nanoplate.
Example 2
1) 1:1 metering in molar ratio takes iron nitrate and bismuth citrate amine, adds deionized water and nitric acid, and making the concentration of nitric acid in this system is 0.75mol/L, fully stirs, and forms the settled solution that contains bismuth citrate amine and iron nitrate;
2) under whipped state, in the settled solution that contains bismuth citrate amine and iron nitrate made to step 1), add potassium hydroxide aqueous solution, the suspension of the oxyhydroxide precipitation that obtains containing bismuth and iron;
The suspension of the oxyhydroxide that contains bismuth and the iron precipitation that 3) will obtain is transferred in the reactor inner bag, reach 90% of reactor inner bag volume with the reaction mass volume in deionized water conditioned reaction still inner bag, stir 30 minutes, in reaction mass, the volumetric molar concentration of iron nitrate and bismuth citrate amine is 0.05mol/L, the volumetric molar concentration of potassium hydroxide is 1.5 mol/L, and the volume radix of volumetric molar concentration is the volume of material in all introducing reactor inner bags;
4) the reactor inner bag that step 3) is disposed to reaction mass is placed in reactor, sealing, under 200 ℃, hydrothermal treatment consists is carried out in insulation in 19 hours, then allow reactor naturally cool to room temperature, by deionized water and dehydrated alcohol repetitive scrubbing reaction product, filter, dry, the bismuth ferrite Bi that to obtain thickness be 10-30nm
2Fe
4O
9Single crystal nanoplate.Its XRD figure spectrum is shown in Fig. 1, and Fig. 2 is shown in by scanning electron microscope (SEM) photo.Monocrystalline Bi as seen from the figure
2Fe
4O
9The nanometer sheet oriented growth.
Example 3
1) 1:1 metering in molar ratio takes iron nitrate and bismuth citrate amine, adds deionized water and nitric acid, and making the concentration of nitric acid in this system is 1mol/L, fully stirs, and forms the settled solution that contains bismuth citrate amine and iron nitrate;
2) under whipped state, in the settled solution that contains bismuth citrate amine and iron nitrate made to step 1), add potassium hydroxide aqueous solution, the suspension of the oxyhydroxide precipitation that obtains containing bismuth and iron;
The suspension of the oxyhydroxide that contains bismuth and the iron precipitation that 3) will obtain is transferred in the reactor inner bag, reach 80% of reactor inner bag volume with the reaction mass volume in deionized water conditioned reaction still inner bag, stir 60 minutes, in reaction mass, the volumetric molar concentration of iron nitrate and bismuth citrate amine is 0.05mol/L, the volumetric molar concentration of potassium hydroxide is 2.5 mol/L, and the volume radix of volumetric molar concentration is the volume of material in all introducing reactor inner bags;
4) the reactor inner bag that step 3) is disposed to reaction mass is placed in reactor, sealing, and under 160 ℃, hydrothermal treatment consists is carried out in insulation in 36 hours, then allow reactor naturally cool to room temperature, by deionized water and dehydrated alcohol repetitive scrubbing reaction product, filter, dry, obtain bismuth ferrite Bi
2Fe
4O
9Single crystal nanoplate.
Claims (4)
1. a bismuth ferrite Bi
2Fe
4O
9The preparation method of single crystal nanoplate is characterized in that comprising the following steps:
1) 1:1 metering in molar ratio takes iron nitrate and bismuth citrate amine, adds deionized water and nitric acid, and making the concentration of nitric acid in this system is 0.75mol/L ~ 1.125mol/L, fully stirs, and forms the settled solution that contains bismuth citrate amine and iron nitrate;
2) under whipped state, in the settled solution that contains bismuth citrate amine and iron nitrate made to step 1), add potassium hydroxide aqueous solution, the suspension of the oxyhydroxide precipitation that obtains containing bismuth and iron;
The suspension of the oxyhydroxide that contains bismuth and the iron precipitation that 3) will obtain is transferred in the reactor inner bag, reach the 70%-90% of reactor inner bag volume with the reaction mass volume in deionized water conditioned reaction still inner bag, stir at least 10 minutes, in reaction mass, the volumetric molar concentration of iron nitrate and bismuth citrate amine is 0.05mol/L, the volumetric molar concentration of potassium hydroxide is 1.5 ~ 2.5 mol/L, and the volume radix of volumetric molar concentration is the volume of material in all introducing reactor inner bags;
4) the reactor inner bag that step 3) is disposed to reaction mass is placed in reactor, sealing, under 160 ℃-230 ℃, hydrothermal treatment consists is carried out in insulation in 5-36 hour, then allow reactor naturally cool to room temperature, by deionized water and dehydrated alcohol repetitive scrubbing reaction product, filter, dry, obtain bismuth ferrite Bi
2Fe
4O
9Single crystal nanoplate.
2. bismuth ferrite Bi according to claim 1
2Fe
4O
9The preparation method of single crystal nanoplate, is characterized in that reactor is polytetrafluoroethylliner liner, the reactor that the stainless steel external member is airtight.
3. bismuth ferrite Bi according to claim 1
2Fe
4O
9The preparation method of single crystal nanoplate, is characterized in that the purity of said bismuth citrate amine, iron nitrate, potassium hydroxide and dehydrated alcohol all is not less than chemical pure.
4. bismuth ferrite Bi according to claim 1
2Fe
4O
9The preparation method of single crystal nanoplate, is characterized in that resulting bismuth ferrite Bi
2Fe
4O
9Single crystal nanoplate thickness is 5-150nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101615165A CN103420427A (en) | 2012-05-23 | 2012-05-23 | Preparation method for bismuth ferrite Bi2Fe4O9 monocrystal nanosheets |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101615165A CN103420427A (en) | 2012-05-23 | 2012-05-23 | Preparation method for bismuth ferrite Bi2Fe4O9 monocrystal nanosheets |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103420427A true CN103420427A (en) | 2013-12-04 |
Family
ID=49645871
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012101615165A Pending CN103420427A (en) | 2012-05-23 | 2012-05-23 | Preparation method for bismuth ferrite Bi2Fe4O9 monocrystal nanosheets |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103420427A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105129861A (en) * | 2015-08-27 | 2015-12-09 | 华南理工大学 | Preparation method for bismuth ferrite BiFeO3 nanosheet |
| CN105668642A (en) * | 2016-01-12 | 2016-06-15 | 浙江大学 | Preparation method of bismuth ferrite monocrystalline nanometer sheet |
| CN111229240A (en) * | 2020-01-17 | 2020-06-05 | 力行氢能科技股份有限公司 | Bismuth ferrite catalyst and preparation method and application thereof |
| CN113244929A (en) * | 2021-05-28 | 2021-08-13 | 北京大学深圳研究生院 | Iron bismuth oxide Bi2Fe4O9Preparation method and application in organic wastewater treatment |
| CN114084911A (en) * | 2021-11-04 | 2022-02-25 | 江苏科技大学 | Bi2Fe4O9Preparation method and application of material |
| CN114956191A (en) * | 2022-04-20 | 2022-08-30 | 西安交通大学 | Flake Bi for catalysis of peroxymonosulfate 2 Fe 4 O 9 And preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101319381A (en) * | 2008-06-17 | 2008-12-10 | 武汉理工大学 | Low temperature condition preparation of orientated growth nanometer flaky Bi2Fe4O9 |
-
2012
- 2012-05-23 CN CN2012101615165A patent/CN103420427A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101319381A (en) * | 2008-06-17 | 2008-12-10 | 武汉理工大学 | Low temperature condition preparation of orientated growth nanometer flaky Bi2Fe4O9 |
Non-Patent Citations (2)
| Title |
|---|
| JIAN-TAO HAN,ET AL.: "Synthesis and magnetic property of submicron Bi2Fe4O9", 《JOURNAL OF CRYSTAL GROWTH》 * |
| YING XIONG, ET AL.: "Hydrothermal Synthesis and Characterization of Bi2Fe4O9 Nanoparticles", 《CHEMISTRY LETTERS》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105129861A (en) * | 2015-08-27 | 2015-12-09 | 华南理工大学 | Preparation method for bismuth ferrite BiFeO3 nanosheet |
| CN105668642A (en) * | 2016-01-12 | 2016-06-15 | 浙江大学 | Preparation method of bismuth ferrite monocrystalline nanometer sheet |
| CN111229240A (en) * | 2020-01-17 | 2020-06-05 | 力行氢能科技股份有限公司 | Bismuth ferrite catalyst and preparation method and application thereof |
| CN111229240B (en) * | 2020-01-17 | 2021-05-04 | 力行氢能科技股份有限公司 | Bismuth ferrite catalyst and preparation method and application thereof |
| CN113244929A (en) * | 2021-05-28 | 2021-08-13 | 北京大学深圳研究生院 | Iron bismuth oxide Bi2Fe4O9Preparation method and application in organic wastewater treatment |
| CN114084911A (en) * | 2021-11-04 | 2022-02-25 | 江苏科技大学 | Bi2Fe4O9Preparation method and application of material |
| CN114084911B (en) * | 2021-11-04 | 2023-12-22 | 江苏科技大学 | Bi (Bi) 2 Fe 4 O 9 Preparation method and application of material |
| CN114956191A (en) * | 2022-04-20 | 2022-08-30 | 西安交通大学 | Flake Bi for catalysis of peroxymonosulfate 2 Fe 4 O 9 And preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103420427A (en) | Preparation method for bismuth ferrite Bi2Fe4O9 monocrystal nanosheets | |
| CN101890354B (en) | Method for preparing bismuth ferrite photocatalyst | |
| CN100560504C (en) | The preparation method of the ZnO nano-powder of sheet porous structural | |
| CN103922425B (en) | A kind of preparation method of porous cobaltosic oxide nano band | |
| US10766787B1 (en) | Production of mixed metal oxide nanostructured compounds | |
| CN101549890B (en) | Solvothermal synthesis method of nickel cobaltate nano particles | |
| CN105562122A (en) | Perovskite type core-shell structured metal oxide and preparation method and application thereof | |
| CN103359773B (en) | A kind of preparation method of zinc oxide nano rod | |
| CN112875755B (en) | Preparation method of bismuth tungstate nano powder | |
| CN110104623B (en) | Preparation method of phosphorus-rich transition metal phosphide cobalt tetraphosphate with different morphologies | |
| CN102877130B (en) | Preparation method of bismuth ferrite BiFeO3 monocrystal micrometer sheet | |
| CN102139914A (en) | Method for preparing calcium titanate nanoparticles | |
| CN109019534A (en) | A kind of preparation method of ultrathin boron nitride nanosheet | |
| CN104192914A (en) | Preparation method of manganese tungsten single-crystalline nanowire | |
| CN102219263A (en) | Method for preparing Gamma-MnOOH nanometer rod | |
| CN102634842B (en) | Method for preparing {001} and {100} surface-exposed anatase TiO2 nano single crystals | |
| Yang et al. | Efficient visible light photocatalytic water oxidation on Zn3 (OH) 2V2O7· 2H2O nanoplates: Effects of exposed facet and local crystal structure distortion | |
| CN102139916A (en) | Method for preparing strontium titanate nanoparticles | |
| Wang et al. | Thermochemistry of nano-phased titanium dioxides relevant to energy application: A Review | |
| CN108163895B (en) | Preparation method of cation-modified molybdenum oxide or tungsten oxide nanowire with large specific surface area | |
| CN109317177B (en) | Method for synthesizing nitrogen-doped bismuth vanadate photocatalyst and application thereof | |
| CN105668642A (en) | Preparation method of bismuth ferrite monocrystalline nanometer sheet | |
| CN101302033B (en) | Method for preparing micro-nanostructure by heat evaporation of multiple reducers | |
| CN112846222B (en) | Flower-shaped Bi/Bi 2 WO 6 Preparation method of nano material | |
| CN106976914A (en) | A kind of preparation method of bismuth titanate nanowire |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20131204 |