CN105800687A - Method for preparing bismuth sulfide nanorod - Google Patents
Method for preparing bismuth sulfide nanorod Download PDFInfo
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- CN105800687A CN105800687A CN201610272787.6A CN201610272787A CN105800687A CN 105800687 A CN105800687 A CN 105800687A CN 201610272787 A CN201610272787 A CN 201610272787A CN 105800687 A CN105800687 A CN 105800687A
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- C01G29/00—Compounds of bismuth
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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Abstract
The invention relates to bismuth sulfide, in particular to a method for preparing a bismuth sulfide nanorod. Bismuth tungstate flower balls are weighed, dissolved in distilled water and stirred to be uniformly dispersed; thioacetamide is dissolved in the solution, and continuous stirring is performed to realize uniform mixing; after stirring is stopped, the obtained solution is transferred into a reaction kettle lined with polytetrafluoroethylene to perform hydrothermal reaction, natural cooling is performed to room temperature, centrifugal separation is performed to obtain black solid, the black solid is alternately washed twice by using distilled water and ethanol, and centrifugal separation, drying and grinding are performed to obtain powder; the temperature and reaction of hydrothermal reaction and the amount of the added thioacetamide are controlled to obtain nanorod bismuth sulfide.
Description
Technical field
The present invention relates to bismuth sulfide (Bi2S3), refering in particular to a kind of method preparing bismuth sulfide nano-rod being raw material with bismuth nitrate, sodium tungstate and thioacetamide, especially a kind of preparation technology is simple, the preparation method of uniform product appearance.
Background technology
The small-size effect of nanoparticle, skin effect, quantum size effect and macro quanta tunnel effect etc. make its magnetic, optical, electrical, sensitive etc. in present the characteristic that conventional material does not possess, have broad application prospects in the materials such as electronics, optics, catalysis, magnetic, biomedicine and coating.Particularly one-dimensional nano structure (such as nanometer rods, line, band etc.), because its structure is unique, great potential in basic research and commercial Application.
Bismuth sulfide (Bi2S3) it is subordinate to tetragonal crystal system, it is generally burgundy pulverulent solids, wherein Bi atom is constituted the polyhedral structure of approximate tetragonal pyramid in the way of pentacoordinate, is attracted each other by electrostatic interaction between Bi-S.In nature, bismuth sulfide is widely present in bismuthine, has significantly high application prospect in fields such as sensor, optoelectronic semiconductor, thermoelectric semiconductor, electrochemical hydrogen storages.Block bismuth sulfide at room temperature band gap is 1.3eV, belongs to direct band-gap semicondictor material, has good photoelectric effect and pyroelectric effect, has good application prospect in photodiode and solaode.And owing to the photoelectric conversion effect of bismuth sulfide nano material obtains improvement corresponding to block bismuth sulfide material so that bismuth sulfide one-dimensional nano structure is widely used in photoelectric sensor and catalysis.
But, the method for the bismuth sulfide nano-rod of current reported preparation has certain limitation, and character and pattern to product all have a certain impact.Bismuth sulfide nano-rod pattern prepared by the present invention is homogeneous, specific surface area big, therefore can provide more avtive spot in the application aspect of photocatalysis and solaode, it is possible to become a more potential photocatalysis and solar cell material.
Summary of the invention
It is an object of the present invention to provide a kind of with bismuth nitrate, sodium tungstate and thioacetamide for raw material, utilize the hydro-thermal method method to synthesize the bismuth sulfide nano-rod of pattern stable homogeneous.
The present invention is realized by following steps:
(1) bismuth tungstate bouquet is prepared: weigh sodium tungstate according to stoichiometric proportion and be dissolved in distilled water, stirring is to being completely dissolved, weigh bismuth nitrate according still further to stoichiometric proportion to add wherein, stirring does not have the particle precipitation of white to bottom, make sodium tungstate and bismuth nitrate complete reaction, regulate solution ph to 1, be further continued for stirring and make solution mix homogeneously；After stopping stirring, being transferred in the reactor that liner is politef by gained solution, hydro-thermal reaction, after room temperature, it is centrifuged out white solid, with distilled water and ethanol alternately washing three times, centrifugal, dry, be ground to Powdered, obtain bismuth tungstate bouquet.
Described hydrothermal temperature is 160-180 DEG C, and the response time is 16-24h.
The described distilled water that is dissolved in, the addition of distilled water is the 60% of reactor volume
(2) preparing bismuth sulfide nano-rod: weigh bismuth tungstate bouquet, be dissolved in distilled water, stirring makes it be uniformly dispersed.Thioacetamide is dissolved in wherein, continues stirring and make mix homogeneously；Gained solution is transferred in the reactor that liner is politef, hydro-thermal reaction, after room temperature, is centrifuged out black solid after stopping by stirring, with distilled water and ethanol alternately washing three times, centrifugal, dries, is ground to Powdered.
Described hot water temperature is 160-180 DEG C, and the response time is 16h-24h.
The addition of thioacetamide makes S element quality account for the 10% of bismuth tungstate.
This patent has invented bismuth sulfide nano-rod by a kind of new mode, and its specific surface area is bigger, and activity is higher, and nanometer sheet is become nanometer rods by the Bi atomic reaction on S atom and Bismuth tungstate nano-sheet.
Accompanying drawing explanation
Fig. 1 be add various sulphur sources quality corresponding to product SEM figure.What figure a to f was corresponding is the quality respectively 1%, 2%, 4%, 6%, 8%, 10% of element sulphur respectively.It can be seen that along with the increasing of amount adding sulfur, product is changed into the bismuth sulfide (10%) of nano bar-shape gradually from the bismuth tungstate of nano-sheet.
Fig. 2 is different SEM figure corresponding to the hydro-thermal reaction time after adding sulfur source；Response time corresponding for figure a to f is 4h, 6h, 8h, 12h, 16h, 24h respectively.It can be seen that along with the increase in response time, the pattern of product is also changed into nanorod structure (more than 16h) from the flower ball-shaped being made up of nanometer sheet gradually.
Fig. 3 is the XRD figure of bismuth tungstate and bismuth sulfide.Figure a is the XRD and corresponding standard card PDF#39-0256 of bismuth tungstate, it can be seen that the peak of synthesized bismuth tungstate and standard card is identical；Figure b is the XRD and corresponding standard card PDF#65-3884 of bismuth sulfide, it can be seen that be pure bismuth sulfide by the material synthesized by this method, and crystallinity is also very good.
Detailed description of the invention
The impact on product morphology of the mass ratio in the different S source of example 1
The sodium tungstate weighing 1mmol is dissolved in 30ml distilled water, and stirring is to being completely dissolved, then the bismuth nitrate weighing 2mmol adds wherein, stirs 2h, and bottom does not have the particle precipitation of white, makes sodium tungstate and bismuth nitrate complete reaction, regulates pH value of solution to 1, is further continued for stirring 30min；After stopping stirring, gained solution is transferred in the reactor that 50ml liner is politef, hydro-thermal reaction, 160 DEG C of reaction 24h, after room temperature, it is centrifuged out white solid, with distilled water and ethanol alternately washing three times, centrifugal, dry, be ground to Powdered.
Weighing the bismuth tungstate of 0.1g, be dissolved in 30ml distilled water, stirring makes it be uniformly dispersed, and is dissolved in by thioacetamide wherein, continues stirring, and the addition in added sulfur source makes the quality of S element respectively the 1% of bismuth tungstate quality, 2%, 4%, 6%, 8%, 10%.After stopping stirring, gained solution is transferred in the reactor that 50ml liner is politef, hydro-thermal reaction, 160-180 DEG C, reaction 16h, after room temperature, is centrifuged out black solid, with distilled water and ethanol alternately washing three times, centrifugal, dry, be ground to Powdered.
The impact on product morphology of the example 2 differential responses time
The sodium tungstate weighing 1mmol is dissolved in 30ml distilled water, stirring is to being completely dissolved, the bismuth nitrate weighing 2mmol again adds wherein, stirring 2h, bottom does not have the particle precipitation of white, makes sodium tungstate and bismuth nitrate complete reaction, regulate and dissolve pH to 1, it is further continued for stirring 30min, after stopping stirring, gained solution is transferred in the reactor that 50ml liner is politef, hydro-thermal reaction, 180 DEG C of reaction 16h, after room temperature, are centrifuged out white solid, with distilled water and ethanol alternately washing three times, centrifugal, dry, be ground to Powdered.
Weighing the bismuth tungstate of 0.1g, be dissolved in 30ml distilled water, stirring makes it be uniformly dispersed, and is dissolved in wherein by 0.0234g thioacetamide, continues stirring.After stopping stirring, gained solution is transferred in the reactor that 50ml liner is politef, the addition in added sulfur source make S element be bismuth tungstate 10%, hydro-thermal reaction, 170 DEG C of reactions, hydro-thermal reaction time respectively 4h, 6h, 8h, 12h, 16h, 24h, after room temperature, be centrifuged out black solid, with distilled water and ethanol alternately washing three times, centrifugal, dry, be ground to Powdered.
Claims (6)
1. the preparation method of a bismuth sulfide nano-rod, it is characterised in that: weighing bismuth tungstate bouquet, be dissolved in distilled water, stirring makes it be uniformly dispersed；Thioacetamide is dissolved in wherein, continues stirring and make mix homogeneously；Gained solution is transferred in the reactor that liner is politef, hydro-thermal reaction, after room temperature, is centrifuged out black solid after stopping by stirring, with distilled water and ethanol alternately washing three times, centrifugal, dries, is ground to Powdered；The bismuth sulfide of nano bar-shape is obtained by control hydrothermal temperature and the addition of time, thioacetamide.
2. the preparation method of a kind of bismuth sulfide nano-rod as claimed in claim 1, it is characterised in that: described hot water temperature is 160-180 DEG C, and the response time is 16h-24h.
3. the preparation method of a kind of bismuth sulfide nano-rod as claimed in claim 1, it is characterised in that: the addition of thioacetamide makes S element quality account for the 10% of bismuth tungstate.
4. the preparation method of a kind of bismuth sulfide nano-rod as claimed in claim 1, it is characterized in that, the preparation method of described bismuth tungstate bouquet carries out in accordance with the following steps: weighs sodium tungstate according to stoichiometric proportion and is dissolved in distilled water, stirring is to being completely dissolved, weighing bismuth nitrate according still further to stoichiometric proportion to add wherein, stirring does not have the particle precipitation of white to bottom, makes sodium tungstate and bismuth nitrate complete reaction, regulate solution ph to 1, be further continued for stirring and make solution mix homogeneously；After stopping stirring, being transferred in the reactor that liner is politef by gained solution, hydro-thermal reaction, after room temperature, it is centrifuged out white solid, with distilled water and ethanol alternately washing three times, centrifugal, dry, be ground to Powdered, obtain bismuth tungstate bouquet.
5. the preparation method of a kind of bismuth sulfide nano-rod as claimed in claim 5, it is characterised in that: described hydrothermal temperature is 160-180 DEG C, and the response time is 16-24h.
6. the preparation method of a kind of bismuth sulfide nano-rod as claimed in claim 5, it is characterised in that: described in be dissolved in distilled water, the addition of distilled water is the 60% of reactor volume.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106299357A (en) * | 2016-10-14 | 2017-01-04 | 成都理工大学 | There is bismuth sulfide electrode material and the application thereof of specific morphology structure |
| CN106477629A (en) * | 2016-10-08 | 2017-03-08 | 江苏大学 | A kind of bismuth sulfide classifying nano flower electrode material for super capacitor and preparation method |
| CN107098387A (en) * | 2017-02-24 | 2017-08-29 | 河南师范大学 | A kind of aqueous phase preparation method of near-infrared photo-thermal nano material bismuth sulfide |
| CN107308957A (en) * | 2017-06-27 | 2017-11-03 | 河南师范大学 | A kind of spherical Bi2S3/Bi2WO6The preparation method of heterojunction photocatalysis material |
| CN107376942A (en) * | 2017-06-27 | 2017-11-24 | 河南师范大学 | A kind of spherical Bi2S3The preparation method of catalysis material |
| CN107658425A (en) * | 2017-09-28 | 2018-02-02 | 成都理工大学 | A kind of needle-like bismuth sulfide carbon cloth electrode and preparation method thereof |
| CN112647132A (en) * | 2020-10-28 | 2021-04-13 | 新疆大学 | Single crystal (Bi)19S27I3）0.6667Nano-rod and preparation method and application thereof |
| CN115814818A (en) * | 2022-11-17 | 2023-03-21 | 中南大学 | Composite semiconductor photocatalytic material and preparation method and application thereof |
| CN115893487A (en) * | 2022-10-27 | 2023-04-04 | 南方科技大学 | Morphology-controllable bismuth sulfide nano material and preparation method and application thereof |
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| SU850591A1 (en) * | 1979-11-13 | 1981-07-30 | За витель ---3;i., ,,. .. t . - :..;,. Jl;;,,I f ..-,.. 5:; - -,1 - «;X.jt..;g Р. | Method of qualitative determination of bismuth |
| CN101638803A (en) * | 2009-08-04 | 2010-02-03 | 陕西科技大学 | Method for preparing Bi2S3 optical thin film of nanorod structure |
| CN102689926A (en) * | 2012-06-21 | 2012-09-26 | 湖南金旺铋业股份有限公司 | Process for preparing high-purity bismuth sulfide |
| CN102965735A (en) * | 2012-11-16 | 2013-03-13 | 杭州师范大学 | Synthesis method of bismuth sulfide nanorod arrays with length-diameter ratios regulated and controlled by solvent hydrothermal method |
| CN103086429A (en) * | 2013-01-28 | 2013-05-08 | 中南林业科技大学 | Preparation method of novel bismuth sulfide nanorods |
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2016
- 2016-04-28 CN CN201610272787.6A patent/CN105800687B/en not_active Expired - Fee Related
Patent Citations (5)
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| SU850591A1 (en) * | 1979-11-13 | 1981-07-30 | За витель ---3;i., ,,. .. t . - :..;,. Jl;;,,I f ..-,.. 5:; - -,1 - «;X.jt..;g Р. | Method of qualitative determination of bismuth |
| CN101638803A (en) * | 2009-08-04 | 2010-02-03 | 陕西科技大学 | Method for preparing Bi2S3 optical thin film of nanorod structure |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106477629A (en) * | 2016-10-08 | 2017-03-08 | 江苏大学 | A kind of bismuth sulfide classifying nano flower electrode material for super capacitor and preparation method |
| CN106299357A (en) * | 2016-10-14 | 2017-01-04 | 成都理工大学 | There is bismuth sulfide electrode material and the application thereof of specific morphology structure |
| CN107098387B (en) * | 2017-02-24 | 2019-06-25 | 河南师范大学 | A kind of aqueous phase preparation method of near-infrared photo-thermal nano material bismuth sulfide |
| CN107098387A (en) * | 2017-02-24 | 2017-08-29 | 河南师范大学 | A kind of aqueous phase preparation method of near-infrared photo-thermal nano material bismuth sulfide |
| CN107376942B (en) * | 2017-06-27 | 2020-03-31 | 河南师范大学 | Spherical Bi2S3Preparation method of photocatalytic material |
| CN107376942A (en) * | 2017-06-27 | 2017-11-24 | 河南师范大学 | A kind of spherical Bi2S3The preparation method of catalysis material |
| CN107308957B (en) * | 2017-06-27 | 2020-03-31 | 河南师范大学 | Spherical Bi2S3/Bi2WO6Preparation method of heterojunction photocatalytic material |
| CN107308957A (en) * | 2017-06-27 | 2017-11-03 | 河南师范大学 | A kind of spherical Bi2S3/Bi2WO6The preparation method of heterojunction photocatalysis material |
| CN107658425A (en) * | 2017-09-28 | 2018-02-02 | 成都理工大学 | A kind of needle-like bismuth sulfide carbon cloth electrode and preparation method thereof |
| CN107658425B (en) * | 2017-09-28 | 2020-10-30 | 成都理工大学 | Needle-shaped bismuth sulfide carbon cloth electrode and preparation method thereof |
| CN112647132A (en) * | 2020-10-28 | 2021-04-13 | 新疆大学 | Single crystal (Bi)19S27I3）0.6667Nano-rod and preparation method and application thereof |
| CN112647132B (en) * | 2020-10-28 | 2022-08-09 | 新疆大学 | Single crystal (Bi) 19 S 27 I 3 ) 0.6667 Nano-rod and preparation method and application thereof |
| CN115893487A (en) * | 2022-10-27 | 2023-04-04 | 南方科技大学 | Morphology-controllable bismuth sulfide nano material and preparation method and application thereof |
| CN115893487B (en) * | 2022-10-27 | 2024-02-13 | 南方科技大学 | Bismuth sulfide nano material with controllable morphology and preparation method and application thereof |
| CN115814818A (en) * | 2022-11-17 | 2023-03-21 | 中南大学 | Composite semiconductor photocatalytic material and preparation method and application thereof |
| CN115814818B (en) * | 2022-11-17 | 2024-04-05 | 中南大学 | Composite semiconductor photocatalytic material and preparation method and application thereof |
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