CN103898589A - Preparation method of nanometer bismuth oxide film - Google Patents
Preparation method of nanometer bismuth oxide film Download PDFInfo
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- CN103898589A CN103898589A CN201410149155.1A CN201410149155A CN103898589A CN 103898589 A CN103898589 A CN 103898589A CN 201410149155 A CN201410149155 A CN 201410149155A CN 103898589 A CN103898589 A CN 103898589A
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- sull
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Abstract
The invention provides a preparation method of a nanometer bismuth oxide film. The preparation method is characterized by comprising the following steps: by taking bismuth nitrate as a bismuth source, dissolving the bismuth nitrate in an aqueous solution of acetic acid to form a bismuth-containing electro-deposition solution; taking conductive glass as a film deposition substrate, depositing for 30-7200s by use of an electrochemical method in the electro-deposition solution within a potential range of minus 0.04V to minus 0.64V and at a sweep speed of 10-100mV/s, and thus preparing the nanometer bismuth oxide film by use of deposition; putting the film in a muffle furnace and oxidizing for 1-4 hours in an air atmosphere at a temperature ranging from 200 to 600 DEG C, thereby obtaining the nanometer bismuth oxide film. The method is simple in equipment, and simple and convenient to operate, large-scale production can be realized, and the obtained film is even, and controllable in thickness.
Description
Technical field
The present invention is the preparation method of nanometer bismuth sull.Relate to a kind of method that galvanic deposit and high temperature oxidation process process are prepared bismuth sull that comprises, the nanometer bismuth sull that adopts the present invention to make has potential purposes in photoelectrocatalysis field.
Background technology
Nano thin-film photocatalyst material is because have good photocatalytic activity and opto-electronic conversion performance, thereby enjoys the attention of field of photovoltaic materials.The oxide compound of bismuth, as the important functional materials of a class, has been widely used in the fields such as semiconductive ceramic, high-temperature superconductor, ferroelectric material, photoelectrocatalysis agent.The production of bismuth nano-oxide at present mostly concentrates in the preparation of oxide powder.Along with the continuous growth of human society to energy demand, the demand particularly clean energy being used, preparation has the nanometer bismuth sull of high efficiency photocatalysis and opto-electronic conversion performance and thickness homogeneous, starts to be constantly subject to people's concern.
The crystalline structure more complicated of bismuth oxide compound, common are the crystalline structure such as α, β, δ, γ, and the bismuth sull that therefore preparation has a single crystalline structure is a difficult point in current industrial production.The preparation method of current bismuth sull is mainly cladding process, magnetron sputtering method (Li Chui zhi, zhang Jun ying, Liu ke jia, A new method of Enhancing photoelectrochemical Characteristics of Bi/Bi
2o
3electrode for Hydrogen Generation via water splitting, Int.J.Electrochem.SCI., 7 (2012) 5028-5034; Chuan Fei Guo, Sihai Cao, Jianming Zhang, Topotactic Transformations of Superstructures:From Thin Films to Two-Dimensional Networks to Nested Two-Dimensional Networks, J.Am.Chem.Soc., 133 (2011) 8211 – 8215).Bismuth oxide film electrode prepared by cladding process is because existing the defect photoelectric properties such as lack of homogeneity, film and substrate Contact resistance are large bad.Magnetron sputtering method can be prepared the bismuth sull with good homogeneity, and can realize the accurate control of film thickness, and its shortcoming is to be difficult for scale operation, and equipment is relatively costly, and cost is higher.Therefore, research and develop new bismuth sull technology of preparing, realize the controlled scale operation of film thickness and homogeneity, significant in the application of new energy field to exploitation bismuth sull.
Summary of the invention
Object of the present invention is intended to overcome the deficiencies in the prior art, based on galvanic deposit and high-temperature oxidation process, provides a kind of preparation method of nanometer bismuth sull.
Content of the present invention is: a kind of preparation method of nanometer bismuth sull, is characterized in that comprising the following steps: a) configuration of electrodeposit liquid: electrodeposit liquid is for containing Bismuth trinitrate and second aqueous acid.Wherein Bismuth trinitrate concentration is 1-10mmol/L, and the volumn concentration of acetic acid is 2-5%.Solution preparation process is: first Bismuth trinitrate is dissolved in to acetic acid, then adds deionized water and be diluted to finite concentration, can make electrodeposit liquid.B) galvanic deposit of bismuth thin film: electrodeposit liquid is injected to electrolyzer, depositing temperature is controlled between 15～35 ℃, take platinum guaze as to electrode, saturated calomel electrode is reference electrode, conductive glass is working electrode, at-0.04～-0.64V(with respect to saturated calomel electrode) potential window in, in sweeping under speed of 10～100mV/s, deposition 30～7200s, can obtain nanometer bismuth thin film.C) preparation of nanometer bismuth sull: the nanometer bismuth thin film that deposition is obtained is placed in retort furnace, under 200～600 ℃ of air atmospheres, is oxidized 1～4 hour, can make nanometer bismuth sull.
In content of the present invention: described platinum guaze and conductive glass are just right, spacing 2-5cm.
In content of the present invention: when described galvanic deposit, the current potential of conductive glass electrode changes in-0.04～-0.64V, and Changing Pattern is for from-be decreased to gradually-0.64V of 0.04V, then not only-0.64V but also fade to gradually-0.04V, and constantly circulation is until deposited.
In content of the present invention: the Trichlorobismuthine of the replaceable 1-10mmol concentration of described Bismuth trinitrate.
In content of the present invention: described bismuth thin film oxidation is replaceable with retort furnace is tube furnace.
In content of the present invention: described bismuth thin film oxidizing atmosphere air is replaceable is oxygen.
In content of the present invention: the described bismuth thin film bismuth oxide compound that roasting oxidation makes in differing temps interval has different crystal formations.The bismuth sull making within the scope of 265～350 ℃ is beta crystal Bi
2o
3film is oxygen-starved Bi in 450 ℃～520 ℃ temperature ranges
2o
2.33film is alpha-crystal form Bi within the scope of 550～650 ℃
2o
3film.
With respect to prior art, bismuth sull preparation method's involved in the present invention feature is: processing unit is simple, and preparation condition requires lower, simple to operate, can realize scale operation, and film is even, thickness is controlled.
Accompanying drawing explanation
Fig. 1 is the XRD figure that preparation method of the present invention produces three kinds of different crystal forms bismuth oxide compounds.
Fig. 2 is the nanometer bismuth thin film SEM figure that preparation method of the present invention produces
Fig. 3 is the β type Bi that preparation method of the present invention produces
2o
3film SEM figure
Fig. 4 is the oxygen-starved Bi that preparation method of the present invention produces
2o
2.33film SEM figure
Fig. 5 is the α type Bi that preparation method of the present invention produces
2o
3film SEM figure
Embodiment
Following specific embodiment be only three kinds of embodiments of the present invention, but the present invention is confined to following examples incessantly.
Embodiment 1: take 1mmol Bismuth trinitrate, be dissolved in containing 20%(V%) in the 100ml aqueous solution of acetic acid, be then diluted to 1000ml.In above-mentioned deposit fluid, in-0.04～-0.64V(with respect to saturated calomel electrode) within the scope of potential region, 10mV/s sweeps under speed, scan round 3600s, can deposit and obtain nanometer bismuth deposit film.The film having deposited with deionized water clean, in baking oven at 50 ℃ dry for standby.Above-mentioned nano thin-film is placed in to retort furnace in 300 ℃, and roasting 2h in air atmosphere, can obtain corresponding bismuth sull.Film is analyzed through X-ray powder diffraction, is defined as β type Bi
2o
3(Fig. 1).
Embodiment 2: take 1mmol Bismuth trinitrate, be dissolved in containing 20%(V%) in the 100ml aqueous solution of acetic acid, be then diluted to 1000ml.In above-mentioned deposit fluid, in-0.04～-0.64V(with respect to saturated calomel electrode) within the scope of potential region, 10mV/s sweeps under speed, scan round 3600s, can deposit and obtain nanometer bismuth deposit film.The film having deposited with deionized water clean, in baking oven at 50 ℃ dry for standby.Above-mentioned nano thin-film is placed in to retort furnace in 500 ℃, and roasting 2h in air atmosphere, can obtain corresponding bismuth sull.Film is analyzed through X-ray powder diffraction, is defined as oxygen-starved Bi
2o
2.33(Fig. 1).
Embodiment 3: take 1mmol Bismuth trinitrate, be dissolved in containing 20%(V%) in the 100ml aqueous solution of acetic acid, be then diluted to 1000ml.In above-mentioned deposit fluid, in-0.04～-0.64V(with respect to saturated calomel electrode) within the scope of potential region, 10mV/s sweeps under speed, scan round 3600s, can deposit and obtain nanometer bismuth deposit film.The film having deposited with deionized water clean, in baking oven at 50 ℃ dry for standby.Above-mentioned nano thin-film is placed in to retort furnace in 600 ℃, and roasting 2h in air atmosphere, can obtain corresponding bismuth sull.Film is analyzed through X-ray powder diffraction, is defined as α type Bi
2o
3(Fig. 1).
Claims (7)
1. a preparation method for nanometer bismuth sull, is characterized in that comprising the following steps: a) configuration of electrodeposit liquid: electrodeposit liquid is for containing Bismuth trinitrate and second aqueous acid.Wherein Bismuth trinitrate concentration is 1-10mmol/L, and the volumn concentration of acetic acid is 2-5%.Solution preparation process is: first Bismuth trinitrate is dissolved in to acetic acid, then adds deionized water and be diluted to finite concentration, can make electrodeposit liquid.B) galvanic deposit of bismuth thin film: electrodeposit liquid is injected to electrolyzer, depositing temperature is controlled between 15～35 ℃, take platinum guaze as to electrode, saturated calomel electrode is reference electrode, conductive glass is working electrode, at-0.04～-0.64V(with respect to saturated calomel electrode) potential window in, in sweeping under speed of 10～100mV/s, deposition 30～7200s, can obtain nanometer bismuth thin film.The preparation of c nanometer bismuth sull: the nanometer bismuth thin film that deposition is obtained is placed in retort furnace, under 200～600 ℃ of air atmospheres, is oxidized 1～4 hour, can make nanometer bismuth sull.
2. by the preparation method of nanometer bismuth sull claimed in claim 1, it is characterized in that: described platinum guaze and conductive glass are just right, spacing 2-5cm.
3. by claim 1,2, the preparation method of the nanometer bismuth sull described in 3, it is characterized in that: when described galvanic deposit, the current potential of conductive glass electrode changes in-0.04～-0.64V, and Changing Pattern is for from-be decreased to gradually-0.64V of 0.04V, then not only-0.64V but also fade to gradually-0.04V, constantly circulation is until deposited.
4. by the preparation method of nanometer bismuth sull claimed in claim 1, it is characterized in that: the Trichlorobismuthine of the replaceable 1-10mmo concentration of Bismuth trinitrate.
5. press claim 1,2,3, the preparation method of the nanometer bismuth sull described in 4, is characterized in that: described bismuth thin film oxidation is replaceable with retort furnace is tube furnace.
6. press claim 1,2,3, the preparation method of the nanometer bismuth sull described in 4,5, is characterized in that: described bismuth thin film oxidizing atmosphere air is replaceable is oxygen.
7. press claim 1,2,3,4,5, the preparation method of the nanometer bismuth sull described in 6, is characterized in that: the described bismuth thin film bismuth oxide compound that roasting oxidation makes in differing temps interval has different crystal formations.The bismuth sull making within the scope of 265～275 ℃ is beta crystal Bi
2o
3film is oxygen-starved Bi in 480 ℃～520 ℃ temperature ranges
2o
2.33film is alpha-crystal form Bi within the scope of 550～600 ℃
2o
3film.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106955699A (en) * | 2016-01-11 | 2017-07-18 | 中国科学院上海硅酸盐研究所 | A kind of high-efficiency solar fixed nitrogen catalysis material and preparation method thereof |
| CN107815701A (en) * | 2017-10-26 | 2018-03-20 | 太原理工大学 | A kind of electrochemical preparation method of nano-sheet fluorination bismuth thin film and its application |
| CN108190952A (en) * | 2018-01-19 | 2018-06-22 | 中南大学 | Bi2O2.33The preparation method of nanometer sheet |
| CN117181254A (en) * | 2022-08-30 | 2023-12-08 | 海南华盛水泥投资有限公司 | Preparation method of bismuth-based catalyst, bismuth-based catalyst and application |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103285891A (en) * | 2013-06-05 | 2013-09-11 | 河北工业大学 | Preparation method of bismuth oxide halide-titanium oxide nanotube array composite photo-catalytic membrane |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103285891A (en) * | 2013-06-05 | 2013-09-11 | 河北工业大学 | Preparation method of bismuth oxide halide-titanium oxide nanotube array composite photo-catalytic membrane |
Non-Patent Citations (1)
| Title |
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| 张红强等: "铋电镀液的配方研究", 《精细化工》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106955699A (en) * | 2016-01-11 | 2017-07-18 | 中国科学院上海硅酸盐研究所 | A kind of high-efficiency solar fixed nitrogen catalysis material and preparation method thereof |
| CN106955699B (en) * | 2016-01-11 | 2019-07-16 | 中国科学院上海硅酸盐研究所 | A kind of high-efficiency solar fixed nitrogen catalysis material and preparation method thereof |
| CN107815701A (en) * | 2017-10-26 | 2018-03-20 | 太原理工大学 | A kind of electrochemical preparation method of nano-sheet fluorination bismuth thin film and its application |
| CN108190952A (en) * | 2018-01-19 | 2018-06-22 | 中南大学 | Bi2O2.33The preparation method of nanometer sheet |
| CN108190952B (en) * | 2018-01-19 | 2020-03-24 | 中南大学 | Bi2O2.33Preparation method of nanosheet |
| CN117181254A (en) * | 2022-08-30 | 2023-12-08 | 海南华盛水泥投资有限公司 | Preparation method of bismuth-based catalyst, bismuth-based catalyst and application |
| CN117181254B (en) * | 2022-08-30 | 2024-04-12 | 海南华盛水泥投资有限公司 | Preparation method of bismuth-based catalyst, bismuth-based catalyst and application |
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Application publication date: 20140702 |