CN104817111A - Room-temperature water phase preparation method of bismuth sulfide nanospheres - Google Patents
Room-temperature water phase preparation method of bismuth sulfide nanospheres Download PDFInfo
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Abstract
The invention discloses a room-temperature water phase preparation method of bismuth sulfide nanospheres. A surfactant is dissolved in de-ionized water, then a chelating agent is added, next bismuth nitrate pentahydrate is added, the materials are stirred at room temperature, sulfur-containing solution is slowly dropwise added into bismuth iron solution, and the materials are uniformly mixed and then react for 2 h at room temperature to obtain the bismuth sulfide nanospheres. The bismuth sulfide nanometer material prepared by the method has good shape and uniform size, and has a potential application value in the fields such as thermoelectricity, electronics and photo-electronic devices; the method has the advantages of simple equipment, mild condition, low energy consumption, short preparation period and easiness in implementation and is an ideal method for preparing the bismuth sulfide nanometer material.
Description
Technical field
The present invention relates to the preparation field of sulfide nano-material, particularly relate to a kind of room temperature aqueous phase preparation method of bismuth sulfide nano ball.
Background technology
Bismuth sulfide is a kind of important semiconductor material, and thermoelectricity, electronics and opto-electronic device and Infrared spectroscopy have potential using value.Its energy gap is 1.2 ~ 1.7eV, can be used to make photoelectric conversion material, is widely used in multiple field.Nano level bismuth sulfide can not only make ultravioletvisible absorption wavelength and fluorescence emission wavelengths generation blue shift, nonlinear optical response can also be produced, strengthen the redox ability of nanoparticle, also there is excellent PhotoelectrocatalytiPerformance Performance simultaneously, have a wide range of applications in luminescent material, nonlinear optical material, photocatalyst material etc.People also find that nanometer bismuth sulfide is a kind of contrast medium of excellent x-ray tomography (CT) in recent years, and relative to traditional iodine contrast agent, it has unique superiority.As bismuth element has very strong absorption to X-ray, the more important thing is that bismuth sulfide toxicity is lower, less on the impact of organism.
The main method of conventional synthesis bismuth sulfide nano material is solvent thermal process, and the method needs to react in airtight autoclave, and the granular size heterogeneity obtained, easily reunites.Subsequently, occurred that the method for a kind of " heat injection " is to obtain the homogeneous bismuth sulfide particle of size distribution, namely uses oleyl amine as part and solvent.But in this process, bismuth ion is inevitably reduced to bismuth metal by oleylamide, and bismuth metal has very strong chemically reactive, and is not suitable for application in body.In addition, in the washing process of phase after the test, because interaction force is more weak, oleyl amine is easy to split away off from bismuth sulfide nano particle surface, and this just causes nano particle to be easy to reunite.Further improvement oleic acid replaces oleyl amine to synthesize bismuth sulfide nano particle afterwards, although uniform bismuth sulfide nano particle finally can be obtained, and reaction system or organic phase and need heat.In addition, Zhang Qi etc. (Chinese Journal of Inorganic Chemistry, 2008,24,547-552.) synthesize bismuth sulfide nano particle in an aqueous medium, but reaction still needs heat, and the product morphology obtained is not fixed, and is easily agglomerated into bulk, is unfavorable for that the later stage is applied.
By adding tensio-active agent, the present invention increases that it is water-soluble, the hydrolysis of bismuth is avoided by adding sequestrant, at ambient temperature, Bismuth trinitrate and sulphur source direct reaction obtain bismuth sulfide nano ball in aqueous, also microwave can be used, the method synthesis such as ultrasonic, the bismuth sulfide nano spherolite footpath of gained is less, good dispersity.
Summary of the invention
The present invention mainly proposes a kind of room temperature aqueous phase preparation method of bismuth sulfide nano ball, gained bismuth sulfide nano ball, and size is homogeneous, and preparation technology is simple, number of devices is few, and preparation cycle is short, and energy consumption is low, environmental friendliness, be convenient to promote, solving of the prior artly needs heat, and the product morphology obtained is not fixed, easily be agglomerated into bulk, be unfavorable for that the later stage such as to apply at the technical problem.
The present invention is by the following technical solutions: a kind of room temperature aqueous phase preparation method of bismuth sulfide nano ball, comprises the steps:
The first step: 20 ~ 100 mmol/L sequestrants are dissolved into 1 ~ 30 mg/mL and contain in the aqueous solution of tensio-active agent, adds five nitric hydrate bismuths subsequently, and stirred at ambient temperature dissolves;
Second step: be added drop-wise in the mixed solution of the first step by 50 ~ 1800 mmol/L sulfur-bearing regent solution, stirred at ambient temperature is even;
3rd step: by the product of second step through water-bath temperature control, ultrasonic reaction or microwave reaction 10 min ~ 24 h, then carry out centrifugal treating and drying treatment, obtain bismuth sulfide nano ball.
As a preferred technical solution of the present invention: described sequestrant refers to N.F,USP MANNITOL or nitrilotriacetic acid(NTA).
As a preferred technical solution of the present invention: in described five nitric hydrate bismuths, the substance withdrawl syndrome of Bismuth trinitrate is 20 ~ 100 mmol/L.
As a preferred technical solution of the present invention: described tensio-active agent refers to one or more mixtures in polyvinyl alcohol, polyvinylpyrrolidone, polyoxyethylene glycol or polyethylene oxide-poly(propylene oxide)-polyethylene oxide.
As a preferred technical solution of the present invention: described sulfur-bearing regent refers to sodium sulphite, thioacetamide or Sulfothiorine, the concentration of described sulfur-bearing regent is 50 ~ 1800 mmol/L, stirs 5 min at room temperature 25 DEG C.
As a preferred technical solution of the present invention: described centrifugal treating is the velocity process 10 minutes with 8000 ~ 10000 revs/min, and described drying treatment refers to 30 DEG C of vacuum-drying 12h.
beneficial effect: the room temperature aqueous phase preparation method of a kind of bismuth sulfide nano ball of the present invention adopts above technical scheme compared with prior art, has following technique effect: 1, in aqueous phase, directly synthesize bismuth sulfide nano material under room temperature.The solid bead of the bismuth sulfide nano material of gained to be particle diameter be 200 ~ 300nm, pattern is good, size is homogeneous; 2, product is not easily reunited good dispersity in water.Reaction can be carried out at normal temperatures and pressures, and Preparation equipment is simple, mild condition, and energy consumption is low; 3, preparation cycle is short, easily realizes, and is convenient to promote.
accompanying drawing illustrates:
The scanning electron microscope (SEM) photograph (SEM) of the bismuth sulfide nano ball that Fig. 1 obtains for the embodiment of the present invention 1 and transmission electron microscope picture (TEM);
The X ray diffracting spectrum of the bismuth sulfide nano ball that Fig. 2 obtains for the embodiment of the present invention 1;
The SEM scanning electron microscope (SEM) photograph of the bismuth sulfide nano ball that Fig. 3 obtains for the embodiment of the present invention 3;
The SEM scanning electron microscope (SEM) photograph of the bismuth sulfide nano ball that Fig. 4 obtains for the embodiment of the present invention 5;
The SEM scanning electron microscope (SEM) photograph of the bismuth sulfide nano ball that Fig. 5 obtains for the embodiment of the present invention 6;
The SEM scanning electron microscope (SEM) photograph of the bismuth sulfide nano ball that Fig. 6 obtains for the embodiment of the present invention 8;
The SEM scanning electron microscope (SEM) photograph of the bismuth sulfide nano ball that Fig. 7 obtains for the embodiment of the present invention 9;
The TEM transmission electron microscope picture of the bismuth sulfide nano material that Fig. 8 obtains for comparative example 2 of the present invention.
Embodiment
Below in conjunction with Figure of description, the specific embodiment of the present invention is described in further detail:
Embodiment 1:
The first step: the N.F,USP MANNITOL adding 4.5 mmol in 45mL (20 mg/mL) polyvinyl alcohol (PVA) aqueous solution, after stirred at ambient temperature dissolves, add the five nitric hydrate bismuth particles of 0.5 mmol, stirred at ambient temperature dissolves 10 min, forms the solution containing bismuth ion;
Second step: be slowly added drop-wise in bismuth ion solution by 10 mL (75 mmol/L) thioacetyl amine aqueous solution, stirred at ambient temperature 5min, forms bismuth-sulphur mixed solution;
3rd step: bismuth-sulphur mixed solution is put into 25 DEG C of water-baths and heats 2 h, then carry out centrifugal treating, black solid deionized water centrifugal treating obtained and ethanol wash 3 times successively respectively, and 20 DEG C of vacuum drying treatment 12 h, make bismuth sulfide nano ball.
Embodiment 2:
The first step: to 45 mL(20 mg/mL) add the five nitric hydrate bismuth particles of 0.5 mmol in polyvinyl alcohol water solution, stirred at ambient temperature dissolves 10 min;
Second step: be slowly added drop-wise in above-mentioned solution by 10 mL (75 mmol/L) thioacetyl amine aqueous solution, stirred at ambient temperature 5min, forms bismuth-sulphur mixed solution.
Experimental result shows, when not having sequestrant, bismuth ion is very easily hydrolyzed and forms white insoluble precipitation, cannot carry out subsequent reactions.
Embodiment 3:
The first step: to 45mL(20 mg/mL) add the nitrilotriacetic acid(NTA) of 2 mmol in polyvinyl alcohol water solution, with sodium hydroxide solution regulator solution pH to solution clear, after dissolving completely, add the five nitric hydrate bismuth particles of 0.5 mmol, stirred at ambient temperature dissolves 10 min, forms the solution containing bismuth ion;
Second step: be slowly added drop-wise in bismuth ion solution by 10 mL (75 mmol/L) thioacetyl amine aqueous solution, stirred at ambient temperature 5min, forms bismuth-sulphur mixed solution;
3rd step: bismuth-sulphur mixed solution is put into 25 DEG C of water-baths and heats 8 h, then carry out centrifugal treating, black solid deionized water centrifugal treating obtained and ethanol wash 3 times successively respectively, and 20 DEG C of vacuum drying treatment 12 h, make bismuth sulfide nano material.
Embodiment 4:
The first step: the N.F,USP MANNITOL adding 4.5 mmol in 45 mL deionized waters, after stirred at ambient temperature dissolves, add the five nitric hydrate bismuth particles of 0.5 mmol, stirred at ambient temperature dissolves 10 min, forms the solution containing bismuth ion;
Second step: be slowly added drop-wise in bismuth ion solution by 10 mL (75 mmol/L) thioacetyl amine aqueous solution, stirred at ambient temperature 5min, forms bismuth-sulphur mixed solution;
3rd step: bismuth-sulphur mixed solution is put into 25 DEG C of water-baths and heats 2 h, then carry out centrifugal treating, black solid deionized water centrifugal treating obtained and ethanol wash 3 times successively respectively, and 20 DEG C of vacuum drying treatment 12 h, make bismuth sulfide nano ball.
Embodiment 5:
The first step: to 45mL(20 mg/mL) add the N.F,USP MANNITOL of 4.5 mmol in polyvinylpyrrolidone (PVP) aqueous solution, after stirred at ambient temperature dissolves, add the five nitric hydrate bismuth particles of 0.5 mmol, stirred at ambient temperature dissolves 10 min, forms the solution containing bismuth ion;
Second step: be slowly added drop-wise in bismuth ion solution by 10 mL (75 mmol/L) thioacetyl amine aqueous solution, stirred at ambient temperature 5min, forms bismuth-sulphur mixed solution;
3rd step: bismuth-sulphur mixed solution is put into 25 DEG C of water-baths and heats 2 h, then carry out centrifugal treating, black solid deionized water centrifugal treating obtained and ethanol wash 3 times successively respectively, and 20 DEG C of vacuum drying treatment 12 h, make bismuth sulfide nano ball.
Embodiment 6:
The first step: to 45mL(20 mg/mL) polyethylene oxide-poly(propylene oxide)-polyethylene oxide (P
123) adding the N.F,USP MANNITOL of 4.5 mmol in the aqueous solution, after stirred at ambient temperature dissolves, add the five nitric hydrate bismuth particles of 0.5 mmol, stirred at ambient temperature dissolves 10 min, forms the solution containing bismuth ion;
Second step: be slowly added drop-wise in bismuth ion solution by 10 mL (75 mmol/L) thioacetyl amine aqueous solution, stirred at ambient temperature 5min, forms bismuth-sulphur mixed solution;
3rd step: bismuth-sulphur mixed solution is put into 25 DEG C of water-baths and heats 2 h, then carry out centrifugal treating, black solid deionized water centrifugal treating obtained and ethanol wash 3 times successively respectively, and 20 DEG C of vacuum drying treatment 12 h, make bismuth sulfide nano ball.
Embodiment 7:
The first step: to 45 mL(20 mg/mL) add the N.F,USP MANNITOL of 4.5 mmol in Aqueous Solutions of Polyethylene Glycol,
After stirred at ambient temperature dissolves, add the five nitric hydrate bismuth particles of 0.5 mmol, stirred at ambient temperature dissolves 10 min, forms the solution containing bismuth ion;
Second step: be slowly added drop-wise in bismuth ion solution by 10 mL (75 mmol/L) thioacetyl amine aqueous solution, stirred at ambient temperature 5min, forms bismuth-sulphur mixed solution;
3rd step: bismuth-sulphur mixed solution is put into 25 DEG C of water-baths and heats 2 h, then carry out centrifugal treating, black solid deionized water centrifugal treating obtained and ethanol wash 3 times successively respectively, and 20 DEG C of vacuum drying treatment 12 h, make bismuth sulfide nano material.
Experimental result shows, after replacing polyvinyl alcohol with polyoxyethylene glycol, reaction generates large stretch of bismuth sulfide flocks, and synthetic effect is undesirable.
Embodiment 8:
The first step: to 45 mL(20 mg/mL) add the N.F,USP MANNITOL of 4.5 mmol in polyvinyl alcohol water solution, after stirred at ambient temperature dissolves, add the five nitric hydrate bismuth particles of 0.5 mmol, stirred at ambient temperature dissolves 10 min, forms the solution containing bismuth ion;
Second step: be slowly added drop-wise in bismuth ion solution by 10 mL (75 mmol/L) thioacetyl amine aqueous solution, stirred at ambient temperature 5min, forms bismuth-sulphur mixed solution;
3rd step: bismuth-sulphur mixed solution is put into Microwave synthesize instrument temperature control 40 DEG C reaction 40min, then centrifugal treating is carried out, black solid deionized water centrifugal treating obtained and ethanol wash 3 times successively respectively, and 20 DEG C of vacuum drying treatment 12 h, make bismuth sulfide nano ball.
Embodiment 9:
The first step: to 45mL(20 mg/mL) add the N.F,USP MANNITOL of 4.5 mmol in polyvinyl alcohol water solution, after stirred at ambient temperature dissolves, add the five nitric hydrate bismuth particles of 0.5 mmol, stirred at ambient temperature dissolves 10 min, forms the solution containing bismuth ion;
Second step: be slowly added drop-wise in bismuth ion solution by 10 mL (75 mmol/L) thioacetyl amine aqueous solution, stirred at ambient temperature 5min, forms bismuth-sulphur mixed solution;
3rd step: bismuth-sulphur mixed solution is put into ultrasonic cell disruptor ultrasonic reaction 40 min, then carries out centrifugal treating, black solid deionized water centrifugal treating obtained and ethanol wash 3 times successively respectively,
20 DEG C of vacuum drying treatment 12 h, make bismuth sulfide nano ball.
Comparative example 1:
Join in 20 mL deionized waters by 0.53 g five nitric hydrate bismuth and 0.85 g thiocarbamide, vigorous stirring, until form homogeneous orange solution, continues stirring reaction 2 h under normal temperature condition.
Experimental result shows, reacting reaction system after 2 h under room temperature is still homogeneous orange solution, and without considerable change, namely this reaction can not be carried out at ambient temperature.
Comparative example 2:
The first step: join in 20 mL deionized waters by 0.53 g five nitric hydrate bismuth and 0.85 g thiocarbamide, vigorous stirring is until form homogeneous orange solution;
Second step: back flow reaction 2h under 80 DEG C of conditions, obtains brownish black precipitation.After reaction terminates, naturally cool to room temperature, centrifugation, wash 3 times respectively successively with deionized water and ethanol, 30 DEG C of vacuum drying treatment 12 h, make bismuth sulfide nano material.
Experimental result shows, this reaction only just occurs under 80 DEG C of conditions, and the bismuth sulfide particle diameter of gained is comparatively large, without fixing pattern.
By reference to the accompanying drawings embodiments of the present invention are explained in detail above, but the present invention is not limited to above-mentioned embodiment, in the ken that those of ordinary skill in the art possess, can also makes a variety of changes under the prerequisite not departing from present inventive concept.
Claims (6)
1. a room temperature aqueous phase preparation method for bismuth sulfide nano ball, is characterized in that, comprise the steps:
The first step: 20 ~ 100 mmol/L sequestrants are dissolved into 1 ~ 30 mg/mL and contain in the aqueous solution of tensio-active agent, adds five nitric hydrate bismuths subsequently, and stirred at ambient temperature dissolves;
Second step: be added drop-wise in the mixed solution of the first step by 50 ~ 1800 mmol/L sulfur-bearing regent solution, stirred at ambient temperature is even;
3rd step: by the product of second step through water-bath temperature control, ultrasonic reaction or microwave reaction 10 min ~ 24 h, then carry out centrifugal treating and drying treatment, obtain bismuth sulfide nano ball.
2. the room temperature aqueous phase preparation method of bismuth sulfide nano ball according to claim 1, is characterized in that: described sequestrant refers to N.F,USP MANNITOL or nitrilotriacetic acid(NTA).
3. the room temperature aqueous phase preparation method of bismuth sulfide nano ball according to claim 1, is characterized in that: in described five nitric hydrate bismuths, the substance withdrawl syndrome of Bismuth trinitrate is 20 ~ 100 mmol/L.
4. the room temperature aqueous phase preparation method of bismuth sulfide nano ball according to claim 1, is characterized in that: described tensio-active agent refers to one or more mixtures in polyvinyl alcohol, polyvinylpyrrolidone, polyoxyethylene glycol or polyethylene oxide-poly(propylene oxide)-polyethylene oxide.
5. the room temperature aqueous phase preparation method of bismuth sulfide nano ball according to claim 1, it is characterized in that: in described second step, sulfur-bearing regent refers to sodium sulphite, thioacetamide or Sulfothiorine, the concentration of described sulfur-bearing regent is 50 ~ 1800 mmol/L, stirs 5 min at room temperature 25 DEG C.
6. the room temperature aqueous phase preparation method of bismuth sulfide nano ball according to claim 1, is characterized in that: described centrifugal treating is the velocity process 10 minutes with 8000 ~ 10000 revs/min, and described drying treatment refers to 30 DEG C of vacuum-drying 12h.
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| CN111777098A (en) * | 2020-06-05 | 2020-10-16 | 中国科学院大学温州研究院(温州生物材料与工程研究所) | Method for preparing two-dimensional bismuth oxide nanosheet |
| CN112299459A (en) * | 2020-10-14 | 2021-02-02 | 沈阳工业大学 | Method for preventing hydrolysis in separation process of bauxite dissolution experiment |
| CN112591794A (en) * | 2020-12-22 | 2021-04-02 | 武汉工程大学 | Preparation method of bismuth oxide fluorescent quantum dots |
| WO2022210032A1 (en) * | 2021-04-01 | 2022-10-06 | 石原産業株式会社 | Bismuth sulfide particles, method for producing same, and application of same |
| CN115536063A (en) * | 2022-09-23 | 2022-12-30 | 电子科技大学长三角研究院(湖州) | Nanometer flower-like bismuth sulfide, preparation method and application |
| CN116251566A (en) * | 2023-03-01 | 2023-06-13 | 西华师范大学 | Preparation method and application of bismuth-doped polyvinylpyrrolidone porous carbon material |
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| CN110282658A (en) * | 2019-08-02 | 2019-09-27 | 湖南柿竹园有色金属有限责任公司 | A kind of high-purity bismuth sulfide preparation method |
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| CN111777098A (en) * | 2020-06-05 | 2020-10-16 | 中国科学院大学温州研究院(温州生物材料与工程研究所) | Method for preparing two-dimensional bismuth oxide nanosheet |
| CN112299459A (en) * | 2020-10-14 | 2021-02-02 | 沈阳工业大学 | Method for preventing hydrolysis in separation process of bauxite dissolution experiment |
| CN112591794A (en) * | 2020-12-22 | 2021-04-02 | 武汉工程大学 | Preparation method of bismuth oxide fluorescent quantum dots |
| WO2022210032A1 (en) * | 2021-04-01 | 2022-10-06 | 石原産業株式会社 | Bismuth sulfide particles, method for producing same, and application of same |
| CN115536063A (en) * | 2022-09-23 | 2022-12-30 | 电子科技大学长三角研究院(湖州) | Nanometer flower-like bismuth sulfide, preparation method and application |
| CN115536063B (en) * | 2022-09-23 | 2023-09-26 | 电子科技大学长三角研究院(湖州) | Nanometer flower-shaped bismuth sulfide, preparation method and application |
| CN116251566A (en) * | 2023-03-01 | 2023-06-13 | 西华师范大学 | Preparation method and application of bismuth-doped polyvinylpyrrolidone porous carbon material |
| CN116251566B (en) * | 2023-03-01 | 2024-04-30 | 西华师范大学 | Preparation method and application of bismuth-doped polyvinylpyrrolidone porous carbon material |
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