CN107500359B - A kind of Ag2S-MoS2The simple synthesis of sheet self assembly composite spherical powder - Google Patents
A kind of Ag2S-MoS2The simple synthesis of sheet self assembly composite spherical powder Download PDFInfo
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- CN107500359B CN107500359B CN201710894850.4A CN201710894850A CN107500359B CN 107500359 B CN107500359 B CN 107500359B CN 201710894850 A CN201710894850 A CN 201710894850A CN 107500359 B CN107500359 B CN 107500359B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G5/00—Compounds of silver
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
Abstract
A kind of Ag2S‑MoS2The simple synthesis of sheet self assembly composite spherical powder, is related to catalysis material preparation technical field.Amino acid, Ammonium Molybdate Tetrahydrate, thiocarbamide, silver nitrate and ammonium metavanadate are dissolved in the water, are uniformly mixed；Then liquid will be stirred to be transferred in reaction kettle, reaction kettle is covered and is put into constant temperature convection oven and is reacted, obtain the Ag of black through post-processing after fully reacting2S‑MoS2Sheet self assembly composite spherical powder.The present invention successfully obtains a kind of Ag by amino acid assisting alcohol-hydrothermal method2S‑MoS2Sheet self assembly composite spherical powder.By serial experiment the result shows that can successfully prepare sheet self assembly Ag as template and raw material by different aminoacids2S‑MoS2The spherical composite granule of micron has the characteristics that narrower particle size distribution, topographic profile be uniform and size tunable.
Description
Technical field
The present invention relates to catalysis material preparation technical fields, are specifically related to a kind of Ag2S-MoS2Sheet self assembly is compound
The simple synthesis of spherical powder.
Background technique
MoS2It is mainly used for photocatalysis hydrogen production and photocatalytic degradation.The main purpose of photocatalytic degradation is reduced by water pollution
Bring environmental problem, and photocatalysis hydrogen production can alleviate energy crisis caused by the increasingly reduction of fossil fuel, and can be with
It is obviously improved environmental pollution.MoS2It is a kind of conductor material that band system is narrow, has higher response in visible light wave range, be before applying
The very wide catalyst of scape.Hu et al. has studied different-shape nano grade and micron-sized MoS2Particle is right under visible light
SO4 2-Degradation rate, over time, MoS2The catalytic degradation efficiency of nanometer sheet is higher, followed by micron-sized MoS2, finally
It is nanoscale MoS2Nanosphere.And the specific surface area of three is descending is successively: MoS2Nano flake, MoS2Nanosphere
With micron-sized MoS2。
At present about one pot process Ag2S-MoS2The report of flake-assembly mode composite spherical powder is less.
Summary of the invention
For presently, there are above-mentioned technical problem, the present invention provides a kind of simple process, it is at low cost, be suitble to industrialization
The Ag of large-scale production2S-MoS2The simple synthesis of sheet self assembly composite spherical powder.
To achieve the goals above, the technical scheme adopted by the invention is as follows: a kind of Ag2S-MoS2Sheet self assembly is compound
Amino acid, Ammonium Molybdate Tetrahydrate, thiocarbamide, silver nitrate and ammonium metavanadate are dissolved in the water by the simple synthesis of spherical powder,
It is uniformly mixed；Then liquid will be stirred to be transferred in reaction kettle, reaction kettle is covered and be put into constant temperature convection oven into
Row reaction, obtains the Ag of black through post-processing after fully reacting2S-MoS2Sheet self assembly composite spherical powder.
As the preferred technical solution of the present invention, amino acid is selected from glycine or L-Aspartic acid, amino acid, four hydration molybdenums
Molar ratio between sour ammonium, thiocarbamide, silver nitrate and ammonium metavanadate is 2~15:1:4~16:0.1~0.2:0.1~0.2, mixing
The molarity of Molybdenum in Solution acid ammonium is 0.05~0.15mol/L.
As present invention further optimization technical solution, reaction temperature is 140~180 DEG C, the reaction time is 10~
36h.Post-processing is alternately washed using dehydrated alcohol and deionized water respectively after being separated by solid-liquid separation reaction product, and perseverance is subsequently placed in
It is dried in warm drying box, drying temperature is 20~60 DEG C in thermostatic drying chamber, and drying time is 3~10h.
The present invention successfully obtains a kind of Ag by amino acid assisting alcohol-hydrothermal method2S-MoS2Sheet self assembly composite spherical
Powder.By serial experiment the result shows that can successfully prepare sheet self assembly as template and raw material by different aminoacids
Ag2S-MoS2The spherical composite granule of micron has the characteristics that narrower particle size distribution, topographic profile be uniform and size tunable.With it is existing
There is technology to compare, the invention has the following advantages that
1), present invention process is simple, and the easy building of entire preparation system, easy to operate, condition is easily-controllable, low in cost, production
Object composition it is easily-controllable, product is evenly distributed, it is not easy to reunite, be suitable for large-scale industrial production.
2), the present invention is to use conventional soluble ammonium molybdate as reactant, is not added during the preparation process other auxiliary
Substance is helped, the by-product of generation is few, and environmental pollution is smaller, is a kind of environment-friendly type synthesis technology.
3), product prepared by the present invention has good catalytic activity, can be used in environmental pollution reparation and battery electrode material
Material etc..
Detailed description of the invention
With reference to embodiments with attached drawing to Ag of the invention2S-MoS2The simple conjunction of sheet self assembly composite spherical powder
It makes and being discussed further at method.
Fig. 1 is Ag prepared by embodiment 12S-MoS2Composite spherical powder field emission scanning electron microscope (FE-SEM) figure (figure a,
B respectively corresponds low, high magnification image)；
Fig. 2 is Ag prepared by embodiment 12S-MoS2The elemental analysis figure (EDS) of composite spherical powder；
Fig. 3 is Ag prepared by embodiment 12S-MoS2XRD diagram (a Ag of composite spherical powder2S-MoS2Composite spherical powder
The XRD diagram of body and its and Ag2Standard card JCPDS (14-0072) comparison diagram of S, b Ag2S-MoS2Composite spherical powder with it is pure
MoS2XRD comparison diagram)；
Fig. 4 is Ag prepared by embodiment 12S-MoS2The TG of composite spherical powder schemes；
Fig. 5 is Ag prepared by embodiment 22S-MoS2Composite spherical powder field emission scanning electron microscope (FE-SEM) figure (figure a,
B respectively corresponds low, high magnification image)；
Fig. 6 is Ag prepared by embodiment 32S-MoS2Composite spherical powder field emission scanning electron microscope (FE-SEM) figure (figure a,
B respectively corresponds low, high magnification image).
Specific embodiment
Embodiment 1
(1) 1.8538g Ammonium Molybdate Tetrahydrate, 0.4567g thiocarbamide, 1.1260g glycine, 0.0255g nitric acid are weighed respectively
Silver and 0.0263g ammonium metavanadate pour into beaker, and 15mL deionized water dissolving is added.Then it is placed on magnetic stirring apparatus and stirs
30min。
(2) liquid will be stirred to be transferred in advance washed 25mL reaction kettle, then after being rinsed beaker with 5mL deionized water
It pours into reaction kettle；Reaction kettle is covered and is put into constant temperature convection oven, setting temperature is 180 DEG C, reacts 10h；Wait react knot
Shu Hou takes out reaction kettle, the powder generated after reaction is centrifuged with centrifuge, and is replaced respectively with dehydrated alcohol and deionized water
For several times, powder after washing is put into thermostatic drying chamber for washing, and setting temperature is 30 DEG C, and dry 5h obtains dry black powder
End.
Fig. 1 is Ag prepared by embodiment 12S-MoS2Field emission scanning electron microscope (FE-SEM) figure (figure of composite spherical powder
A, b respectively corresponds low, high magnification image).The obtained composite spherical morphology microstructure known to Fig. 1 a is more uniform, and average particle size is
1μm；The spherical particle as known to Fig. 1 b is the (MoS as made of sheet self assembly2), the thickness of piece is nanoscale.Above insert
Piece is the product Ag of load2S.EDS analysis in part is carried out to Fig. 1 b, as shown in Fig. 2, showing wherein to contain elements A g and S really.
Fig. 3 is Ag prepared by embodiment 12S-MoS2The XRD diagram of composite spherical powder.It can be seen from Fig. 3 a and Ag2S
Standard card JCPDS (14-0072) comparison it is found that in products therefrom silver sulfide be monocline body phase Ag2S；In Fig. 3 a
Ag2For S in 20.433 ° of appearance, one diffraction maximum (- 101), this is Ag2The diffraction maximum of S.2 θ are respectively at 26.322 ° later,
28.966 °, 31.52 °, 34.385 °, 34.7 °, 37.104 °, 37.718 °, 40.739 °, 43.406 °, 46.208 °,
47.754 °, 48.761 °, 53.277 °, 58.073 °, 62.585 °, 63.202 °, 63.734 °, 67.915 ° occur respectively
Ag2(012) of S, (111), (- 112), (- 121), (013), (- 103), (031), (200), (- 123), (- 212),
(014), (- 141), (- 134), (232) crystal face.In Fig. 3 b, diffraction maximum above is Ag2S-MoS2X-ray diffraction curve,
Following diffraction curve is MoS2X-ray diffraction curve, there is the phenomenon that widthization in the characteristic peak of molybdenum disulfide, this should be with
The size of molybdenum disulfide is related.It can be seen that MoS from Fig. 3 b2Certain characteristic peaks and silver sulfide characteristic peak be overlapped, such as exist
(004) diffraction maximum occurred at 29.355 °.
Fig. 4 is Ag prepared by embodiment 12S-MoS2The TG of composite spherical powder schemes.As shown in Figure 4, prepared by embodiment 1
Ag2S-MoS2Composite spherical powder produces lesser mass loss during high temperature sintering.It is attached to 70 DEG C by start temperature
The curve of product is in apparent downward trend when close, this is the decomposition of dehydrated alcohol in product, and the loss of this stage quality is
0.22%, residual mass 99.78%.This shows the dehydrated alcohol for having 0.22% in sample.Until being increased to 160 DEG C when temperature
Curve starts again in apparent downward trend when left and right, and decrease speed is 0.04%/10 DEG C.When temperature drops to 790 DEG C, matter
Amount loss is 2.44%, residual mass 97.56%.In conclusion removing 0.22% dehydrated alcohol of sample loss, also damage
Lose 2.22%.This indicates that Ag2S-MoS2Mass ratio shared by silver sulfide is about 2.22% in composite spherical powder.
Embodiment 2
(1) 0.9269g Ammonium Molybdate Tetrahydrate, 0.5709g thiocarbamide, 0.1996g L-Aspartic acid, 0.1911g are weighed respectively
Silver nitrate and 0.0175g ammonium metavanadate pour into beaker, and 15mL deionized water dissolving is added.Then it is placed on magnetic stirring apparatus and stirs
Mix 30min.
(2) liquid will be stirred to be transferred in advance washed 25mL reaction kettle, then after being rinsed beaker with 5mL deionized water
It pours into reaction kettle；Reaction kettle is covered and is put into constant temperature convection oven, setting temperature is 160 DEG C, and reaction is for 24 hours；Wait react knot
Shu Hou takes out reaction kettle, the powder generated after reaction is centrifuged with centrifuge, and is replaced respectively with dehydrated alcohol and deionized water
For several times, powder after washing is put into thermostatic drying chamber for washing, and setting temperature is 40 DEG C, and dry 10h obtains dry black powder
End.
Fig. 5 is Ag prepared by embodiment 22S-MoS2Field emission scanning electron microscope (FE-SEM) figure (figure of composite spherical powder
A, b respectively corresponds low, high magnification image).By Fig. 5 a it is found that obtained Ag2S-MoS2Composite spherical morphology microstructure is uniform, puts down
Equal partial size is 1.5 μm, and good crystallinity；Meanwhile the rough surface of spherical particle, be by more tiny nano-sheet assembling and
At.Fig. 5 b is observed that Ag2S nanometer sheet is evenly distributed in spherical MoS2The surface of powder is to form Ag2S-MoS2It is multiple
Close spherical powder.
Embodiment 3
(1) 2.7807g Ammonium Molybdate Tetrahydrate, 2.7403g thiocarbamide, 2.5336g glycine, 0.0764g nitric acid are weighed respectively
Silver and 0.0263g ammonium metavanadate pour into beaker, and 15mL deionized water dissolving is added.Then it is placed on magnetic stirring apparatus and stirs
30min。
(2) liquid will be stirred to be transferred in advance washed 25mL reaction kettle, then after being rinsed beaker with 5mL deionized water
It pours into reaction kettle；Reaction kettle is covered and is put into constant temperature convection oven, setting temperature is 140 DEG C, reacts 36h；Wait react knot
Shu Hou takes out reaction kettle, the powder generated after reaction is centrifuged with centrifuge, and is replaced respectively with dehydrated alcohol and deionized water
For several times, powder after washing is put into thermostatic drying chamber for washing, and setting temperature is 60 DEG C, and dry 3h obtains dry black powder
End.
Fig. 6 is Ag prepared by embodiment 32S-MoS2Field emission scanning electron microscope (FE-SEM) figure (figure of composite spherical powder
A, b respectively corresponds low, high magnification image).By Fig. 6 a it is found that obtained Ag2S-MoS2Composite spherical morphology microstructure is uniform, puts down
Equal partial size is 0.5 μm, and good crystallinity；Meanwhile the rough surface of spherical particle, be by more tiny nano-sheet assembling and
At.Fig. 6 b is observed that Ag2S nanometer sheet is evenly distributed in spherical MoS2The surface of powder is to form Ag2S-MoS2It is multiple
Close spherical powder.
The above content is just an example and description of the concept of the present invention, affiliated those skilled in the art
It makes various modifications or additions to the described embodiments or is substituted in a similar manner, without departing from invention
Design or beyond the scope defined by this claim, be within the scope of protection of the invention.
Claims (3)
1. a kind of Ag2S-MoS2The simple synthesis of sheet self assembly composite spherical powder, which is characterized in that by amino acid, four
Ammonium paramolybdate tetrahydrate, thiocarbamide, silver nitrate and ammonium metavanadate are dissolved in the water, and are uniformly mixed；Then liquid will be stirred to be transferred to
In reaction kettle, reaction kettle is covered and is put into constant temperature convection oven and is reacted, obtains black through post-processing after fully reacting
Ag2S-MoS2Sheet self assembly composite spherical powder；
Amino acid is selected from glycine or L-Aspartic acid；
Molar ratio between amino acid, Ammonium Molybdate Tetrahydrate, thiocarbamide, silver nitrate and ammonium metavanadate is 2~15:1:4~16:0.1
~0.2:0.1~0.2；
The molarity of ammonium molybdate is 0.05~0.15mol/L in mixed solution；
Reaction temperature is 140~180 DEG C, and the reaction time is 10~36h.
2. simple synthesis as described in claim 1, which is characterized in that post-processing is divided after being separated by solid-liquid separation reaction product
Not Shi Yong dehydrated alcohol and deionized water alternately wash, be subsequently placed in thermostatic drying chamber and be dried.
3. simple synthesis as claimed in claim 2, which is characterized in that drying temperature is 20~60 in thermostatic drying chamber
DEG C, drying time is 3~10h.
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| CN109126829B (en) * | 2018-09-18 | 2021-12-14 | 合肥学院 | Preparation method of CdS-MoS2 composite powder with three-dimensional heterostructure |
| CN109364950A (en) * | 2018-10-16 | 2019-02-22 | 湖南文理学院 | A kind of graphene/metal sulfide multi-stage nano material and its green synthesis method |
| CN110357143B (en) * | 2019-03-01 | 2021-11-26 | 东北电力大学 | Sensitive material MoS for Hg (0) sensor2-Ag2S |
| CN110975887A (en) * | 2019-12-28 | 2020-04-10 | 合肥学院 | SiO (silicon dioxide)2/Ag2Preparation method of S composite powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104307537A (en) * | 2014-09-22 | 2015-01-28 | 江苏大学 | Preparation method of MoS2 / Ag2S nano-composite photocatalytic material |
| CN107098390A (en) * | 2017-04-20 | 2017-08-29 | 合肥学院 | One kind simply prepares the adjustable sheet self assembly MoS of particle diameter2The method of bobbles shape powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104307537A (en) * | 2014-09-22 | 2015-01-28 | 江苏大学 | Preparation method of MoS2 / Ag2S nano-composite photocatalytic material |
| CN107098390A (en) * | 2017-04-20 | 2017-08-29 | 合肥学院 | One kind simply prepares the adjustable sheet self assembly MoS of particle diameter2The method of bobbles shape powder |
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