CN108373141A - A kind of preparation method of hollow sulphur selenizing molybdenum nanosphere - Google Patents
A kind of preparation method of hollow sulphur selenizing molybdenum nanosphere Download PDFInfo
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- CN108373141A CN108373141A CN201810528627.2A CN201810528627A CN108373141A CN 108373141 A CN108373141 A CN 108373141A CN 201810528627 A CN201810528627 A CN 201810528627A CN 108373141 A CN108373141 A CN 108373141A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/002—Compounds containing, besides selenium or tellurium, more than one other element, with -O- and -OH not being considered as anions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
The present invention discloses a kind of simple and feasible preparation method, and for a kind of uniform preparation method of hollow sulphur selenizing molybdenum nanosphere of hydro-thermal preparation scale, flow is as follows：A. selenium powder and sulphur powder are dissolved in hydrazine hydrate, heating water bath stirring；B. Ammonium Molybdate Tetrahydrate is added in dimethyl formamide solution, is transferred in polytetrafluoroethyllining lining after stirring；Hydrazine hydrate solution is injected in liner by C, is heated after sealing；D. reaction kettle cooled to room temperature collects black product, is washed using absolute ethyl alcohol and deionized water, in 60 DEG C of vacuum drying.The raw materials technology is easy to get, and preparation method is easy to operate, and reaction condition is easily achieved, and product has hollow-core construction, and size uniformity, form is regular, is evenly distributed, and constituent content is continuously adjustable, has wide in range visible absorption range and photothermal conversion ability.
Description
Technical field
The present invention relates to field of nanometer material technology more particularly to a kind of preparation methods of hollow sulphur selenizing molybdenum nanosphere.
Background technology
Transition Metal Sulfur, selenides have unique similar to graphene because of its unique crystal structure and electronic structure
Physics, chemical property and non-carbon atoms and be known as " inorganic graphite alkene ".This kind of compound often has X-M-X（M：Mo, W
Equal transition metal elements；X：The VI A races element such as S, Se）The sandwich sandwich structure of class is traditionally applied to kollag, shines
Diode, field-effect transmitting tube etc., in recent years its application range constantly expand, in optics, electricity, the energy, sensing, biology
Etc. research obtain huge progress, therefore cause the extensive concern of educational circles.
MoS2, MoSe2Belong to Transition Metal Sulfur, selenides, there is the layer structure of similar graphene, in layer Mo-S or
Mo-Se is combined in the form of covalent bond, and interlayer is combined with Van der Waals force, therefore such material is mostly with nano lamellar, laminated structure at present
See report.Other special shapes are for example rodlike, tubulose, linear, and the nanostructures such as flower-shaped are mostly with Template synthesis, complex steps,
Cost is higher.And nanometer is spherical, especially one step of non-template method is prepared, the hollow ball-shape sulphur that two kinds of elements of S and Se coexist
Selenizing molybdenum (MoS2xSe2(1-x)) fewer and fewer.
Invention content
The object of the present invention is to provide a kind of simple and feasible one step hydro thermal methods, and being used to prepare scale uniformly has
The sulphur selenizing molybdenum nanosphere of hollow-core construction.
Above-mentioned purpose is achieved by the following technical solution：With hydrazine hydrate（N2H4·H2O）, selenium powder, sulphur powder, four hydrations
Ammonium molybdate is raw material, and hollow sulphur selenizing molybdenum nanosphere is directly prepared by hydro-thermal method, is as follows：
(1) selenium powder and sulphur powder are dissolved in hydrazine hydrate, persistently stir 1h at 80 DEG C, make to be completely dissolved, makes certain S/Se
The hydrazine hydrate mixed solution of element ratio；
(2) Ammonium Molybdate Tetrahydrate is added in dimethyl formamide solution, and 100ml capacity polytetrafluoroethylene (PTFE) is transferred to after stirring
In liner；
(3) hydrazine hydrate mixed solution is injected in polytetrafluoroethyllining lining, hydrothermal reaction kettle is transferred to drying box after sealing
It is interior, keep the temperature 4-12h in 180-200 DEG C；
(4) it waits for hydrothermal reaction kettle cooled to room temperature, collects black product, and repeatedly using absolute ethyl alcohol and deionized water
Washing, in 60 DEG C of vacuum drying chambers dry 4h after both hollow sulphur selenizing molybdenum nanosphere.
The molar ratio of two kinds of elements of S, Se of described addition in step (1) is set as 1:0, 3:1, 1:1, 1:3, 0:
1。
The mole of described Mo elements should be the 1/2 of the sum of two kinds of element moles of S, Se in step (2).
The volume ratio of described absolute ethyl alcohol and deionized water should be 1 in step (4):3.
Raw material of the present invention is easy to get, and preparation method is easy to operate, and reaction condition is easily achieved, the hollow sulphur selenizing molybdenum nanometer of gained
Ball size uniformity, diameter are about 230nm or so, are evenly distributed.
Description of the drawings
Scanning electron microscope (SEM) figure of a product for Fig. 1；
Transmission electron microscope (TEM) figure of a product for Fig. 2；
X-ray diffraction (XRD) figure of a product for Fig. 3；
The X-ray photoelectron spectroscopic analysis of a product for Fig. 4（XPS）Collection of illustrative plates；
The ultraviolet-visible absorption spectroscopy of a product for Fig. 5（uv-vis）Figure；
Fig. 6 is the photothermal conversion ability of hollow sulphur selenizing molybdenum nanosphere prepared by the present invention.
Specific implementation mode
In order to better understand the present invention, in conjunction with example, invention is further explained, but claimed
Range be not limited to embodiment indicate within the scope of.
Embodiment 1
0.19mmol sulphur powders are taken to be dissolved in 10ml hydrazine hydrates with 0.19mmol selenium powders, magnetic agitation simultaneously heats 1h in 80 DEG C.It will
0.027mmol Ammonium Molybdate Tetrahydrates are added in 30ml dimethylformamides, are transferred to after being stirred in 100ml polytetrafluoroethylene (PTFE)
In lining, then hydrazine hydrate mixed solution is injected into above-mentioned solution.It is sealed using stainless steel cauldron and in 180 DEG C of heating
12h.It waits for reaction kettle cooled to room temperature, collects black product, washed repeatedly using absolute ethyl alcohol and with deionized water, in 60
In DEG C vacuum drying chamber after drying 4h both hollow sulphur selenizing molybdenum nanosphere.
Embodiment 2
0.19mmol sulphur powders are taken to be dissolved in 10ml hydrazine hydrates with 0.19mmol selenium powders, magnetic agitation simultaneously heats 1h in 80 DEG C.It will
0.027mmol Ammonium Molybdate Tetrahydrates are added in 30ml dimethylformamides, are transferred to after being stirred in 100ml polytetrafluoroethylene (PTFE)
In lining, then hydrazine hydrate mixed solution is injected into above-mentioned solution.It is sealed using stainless steel cauldron and in 180 DEG C of heating
4h.It waits for reaction kettle cooled to room temperature, collects black product, washed repeatedly using absolute ethyl alcohol and with deionized water, in 60
In DEG C vacuum drying chamber after drying 4h both hollow sulphur selenizing molybdenum nanosphere.Scanning electron microscope (SEM) photograph is similar to embodiment 1.
Embodiment 3
0.29mmol sulphur powders are taken to be dissolved in 10ml hydrazine hydrates with 0.10mmol selenium powders, magnetic agitation simultaneously heats 1h in 80 DEG C.It will
0.027mmol Ammonium Molybdate Tetrahydrates are added in 30ml dimethylformamides, are transferred to after being stirred in 100ml polytetrafluoroethylene (PTFE)
In lining, then hydrazine hydrate mixed solution is injected into above-mentioned solution.It is sealed using stainless steel cauldron and in 180 DEG C of heating
4h.It waits for reaction kettle cooled to room temperature, collects black product, washed repeatedly using absolute ethyl alcohol and with deionized water, in 60
In DEG C vacuum drying chamber after drying 4h both hollow sulphur selenizing molybdenum nanosphere, scanning electron microscope (SEM) photograph is similar to embodiment 1.
Embodiment 4
0.10mmol sulphur powders are taken to be dissolved in 10ml hydrazine hydrates with 0.29mmol selenium powders, magnetic agitation simultaneously heats 1h in 80 DEG C.It will
0.027mmol Ammonium Molybdate Tetrahydrates are added in 30ml dimethylformamides, are transferred to after being stirred in 100ml polytetrafluoroethylene (PTFE)
In lining, then hydrazine hydrate mixed solution is injected into above-mentioned solution.It is sealed using stainless steel cauldron and in 180 DEG C of heating
4h.It waits for reaction kettle cooled to room temperature, collects black product, washed repeatedly using absolute ethyl alcohol and with deionized water, in 60
In DEG C vacuum drying chamber after drying 4h both hollow sulphur selenizing molybdenum nanosphere, scanning electron microscope (SEM) photograph is similar to embodiment 1.
Embodiment 5
0.38mmol sulphur powders are taken to be dissolved in 10ml hydrazine hydrates, magnetic agitation simultaneously heats 1h in 80 DEG C.0.027mmol tetra- is hydrated molybdenum
Sour ammonium is added in 30ml dimethylformamides, is transferred to after being stirred in 100ml polytetrafluoroethyllining linings, then by hydrazine hydrate
Mixed solution is injected into above-mentioned solution.It is sealed using stainless steel cauldron and heats 12h in 180 DEG C.Wait for that reaction kettle is naturally cold
But to room temperature, black product is collected, and wash repeatedly using absolute ethyl alcohol and with deionized water, is dried in 60 DEG C of vacuum drying chambers
After dry 4h both MoS coexists in spherical and sheet2。
Embodiment 6
0.38mmol selenium powders are taken to be dissolved in 10ml hydrazine hydrates, magnetic agitation simultaneously heats 1h in 80 DEG C.0.027mmol tetra- is hydrated molybdenum
Sour ammonium is added in 30ml dimethylformamides, is transferred to after being stirred in 100ml polytetrafluoroethyllining linings, then by hydrazine hydrate
Mixed solution is injected into above-mentioned solution.It is sealed using stainless steel cauldron and heats 4h in 180 DEG C.Wait for reaction kettle natural cooling
To room temperature, black product is collected, is washed repeatedly using absolute ethyl alcohol and with deionized water, in drying 4h in 60 DEG C of vacuum drying chambers
Afterwards both hollow ball-shape is spherical that MoSe coexists with sheet2。
Such as Figure 1A, Figure 1B, shown in Fig. 2, for sulphur selenizing molybdenum nanosphere grain size prepared by the present invention in 230nm or so, size is equal
One, good dispersion and have hollow-core construction.
As shown in figure 3,1 sample of embodiment does not have apparent characteristic peak to occur, illustrate that crystallographic disorder degree is higher.
As shown in Figure 4 A, the peak occurred at 234.8,232.1,229.3 and 225.7ev represents a small amount of MoVI, MoIV
3d3/2, MoIV 3d5/2And S2-The track signal of 2s；In Fig. 4 B, occur on 166.5,162.6,161.3 and 160.1 positions ev
Peak respectively represents Se 3P1/2, S 3p1/2, S 3p3/2, Se 3P3/2Track；In Fig. 4 C, two peaks 55 and 54.2 ev represent Se
The 3d of element3/2And 3d5/2Two tracks.The above XPS statistics indicate that, sample is by Mo, and tri- kinds of elements of S, Se are constituted, by peak area
Calculating, Mo:S:Se = 1:0.83:1.17, i.e. 1 sample composition of embodiment is MoS0.83Se1.17。
As shown in figure 5, embodiment a sample has wide in range spectral absorption in 200-800nm wave-length coverages.
As shown in fig. 6, the hollow sulphur selenizing molybdenum nanosphere prepared by the present invention has good photothermal conversion ability.It takes each
Embodiment sample 4mg, ultrasonic disperse is in 20mL ultra-pure waters.Using the xenon lamp of installation 1.5 filter plates of A.M as simulation nature
Sample dispersion liquid is placed in 100 μ W/cm of energy density by light source2It is irradiated under light, real time temperature is recorded per 2min.Various kinds when 10min
Product dispersion liquid is warming up to close to 65 DEG C for 26 DEG C or so from room temperature, and highest increasing extent of temperature is up to 38.3 DEG C, while blank sample only heats up
15.7 DEG C, illustrate that hollow sulphur selenizing molybdenum nanosphere has good photothermal conversion ability.
Claims (4)
1. a kind of hollow sulphur selenizing molybdenum nanosphere and preparation method thereof, feature includes being following steps：
(1) selenium powder and sulphur powder are dissolved in hydrazine hydrate, persistently stir 1h at 80 DEG C, make to be completely dissolved, makes certain S/Se
The hydrazine hydrate mixed solution of element ratio；
(2) Ammonium Molybdate Tetrahydrate is added in dimethyl formamide solution, and 100ml capacity polytetrafluoroethylene (PTFE) is transferred to after stirring
In liner；
(3) hydrazine hydrate mixed solution is injected in polytetrafluoroethyllining lining, hydrothermal reaction kettle is transferred to drying box after sealing
It is interior, keep the temperature 4-12h in 180-200 DEG C；
(4) it waits for hydrothermal reaction kettle cooled to room temperature, collects black product, and repeatedly using absolute ethyl alcohol and deionized water
Washing, in 60 DEG C of vacuum drying chambers dry 4h after both hollow sulphur selenizing molybdenum nanosphere.
2. a kind of hollow sulphur selenizing molybdenum nanosphere as described in right one and preparation method thereof, it is characterised in that：Institute in step (1)
Say that the molar ratio for the two kinds of elements of S, Se being added is continuously adjustable.
3. a kind of hollow sulphur selenizing molybdenum nanosphere as described in right one and preparation method thereof, it is characterised in that：Institute in step (2)
Say that the mole of Mo elements should be the 1/2 of the sum of two kinds of element moles of S, Se.
4. a kind of hollow sulphur selenizing molybdenum nanosphere preparation method as described in right one, it is characterised in that：It is described in step (4)
The volume ratio of absolute ethyl alcohol and deionized water should be 1:3.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112002884A (en) * | 2020-08-27 | 2020-11-27 | 扬州大学 | Flower ball shaped MoSe1.48S0.52@ C positive electrode composite material and aluminum ion battery |
| CN114105107A (en) * | 2021-12-31 | 2022-03-01 | 西安工业大学 | Highly monodisperse MoSe with different morphologies2Preparation method of nano material |
| CN114351181A (en) * | 2021-12-23 | 2022-04-15 | 台州学院 | Fiber bundle-shaped nickel-iron-sulfur-selenium compound and preparation method thereof |
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| CN105271136A (en) * | 2015-10-28 | 2016-01-27 | 常州轻工职业技术学院 | Preparation method of ultra-thin nanometer hollow sphere MoSe2 |
| CN105836715A (en) * | 2016-03-25 | 2016-08-10 | 合肥工业大学 | Self-assembly ternary sulfur molybdenum selenide nanotube with controllable composition and preparation method thereof |
| CN106207125A (en) * | 2016-08-23 | 2016-12-07 | 东华大学 | Sulfur doping selenizing molybdenum/Graphene graphene nanobelt aeroge and preparation thereof |
| CN107275600A (en) * | 2017-05-31 | 2017-10-20 | 浙江大学 | The preparation method of molybdenum disulfide/carbon composite of hollow sphere |
| US20180346337A1 (en) * | 2015-11-25 | 2018-12-06 | William Marsh Rice University | Formation of three-dimensional materials by combining catalytic and precursor materials |
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2018
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271136A (en) * | 2015-10-28 | 2016-01-27 | 常州轻工职业技术学院 | Preparation method of ultra-thin nanometer hollow sphere MoSe2 |
| US20180346337A1 (en) * | 2015-11-25 | 2018-12-06 | William Marsh Rice University | Formation of three-dimensional materials by combining catalytic and precursor materials |
| CN105836715A (en) * | 2016-03-25 | 2016-08-10 | 合肥工业大学 | Self-assembly ternary sulfur molybdenum selenide nanotube with controllable composition and preparation method thereof |
| CN106207125A (en) * | 2016-08-23 | 2016-12-07 | 东华大学 | Sulfur doping selenizing molybdenum/Graphene graphene nanobelt aeroge and preparation thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112002884A (en) * | 2020-08-27 | 2020-11-27 | 扬州大学 | Flower ball shaped MoSe1.48S0.52@ C positive electrode composite material and aluminum ion battery |
| CN114351181A (en) * | 2021-12-23 | 2022-04-15 | 台州学院 | Fiber bundle-shaped nickel-iron-sulfur-selenium compound and preparation method thereof |
| CN114105107A (en) * | 2021-12-31 | 2022-03-01 | 西安工业大学 | Highly monodisperse MoSe with different morphologies2Preparation method of nano material |
| CN114105107B (en) * | 2021-12-31 | 2023-11-07 | 西安工业大学 | Highly monodisperse MoSe with different morphologies 2 Method for preparing nano material |
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