CN107500359A - 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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- CN107500359A CN107500359A CN201710894850.4A CN201710894850A CN107500359A CN 107500359 A CN107500359 A CN 107500359A CN 201710894850 A CN201710894850 A CN 201710894850A CN 107500359 A CN107500359 A CN 107500359A
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- self assembly
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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 preparing 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 reactor, reactor is covered and is put into constant temperature convection oven and is reacted, the Ag of black is obtained through post processing after reaction completely2S‑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.Show that sheet self assembly Ag can successfully be prepared by being used as template and raw material by different aminoacids by serial experiment result2S‑MoS2The spherical composite granule of micron, it has the characteristics that narrower particle size distribution, topographic profile be homogeneous and size tunable.
Description
Technical field
The present invention relates to catalysis material preparing technical field, is specifically related to a kind of Ag2S-MoS2Sheet self assembly is compound
The simple synthesis of spherical powder.
Background technology
MoS2It is mainly used in photocatalysis hydrogen production and photocatalytic degradation.The main purpose of photocatalytic degradation is reduced by water pollution
The environmental problem brought, 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 narrow conductor material of band system, there is higher response in visible light wave range, is before applying
The very wide catalyst of scape.Hu et al. have studied different-shape nano level and micron-sized MoS2Particle is right under visible light
SO4 2-Degradation rate, with the growth of time, MoS2The catalytic degradation efficiency of nanometer sheet is higher, next to that micron-sized MoS2, finally
It is nano level MoS2Nanosphere.And the specific surface area of three is descending is successively:MoS2Nano flake, MoS2Nanoparticle
With micron-sized MoS2。
At present on one pot process Ag2S-MoS2The report of flake-assembly mode composite spherical powder is less.
The content of the invention
For the above-mentioned technical problem that presently, there are, the invention provides a kind of technique is simple, cost is low, is adapted to industrialization
The Ag of large-scale production2S-MoS2The simple synthesis of sheet self assembly composite spherical powder.
To achieve these goals, the technical solution adopted in the present invention is:A kind of Ag2S-MoS2Sheet self assembly is compound
The simple synthesis of spherical powder, amino acid, Ammonium Molybdate Tetrahydrate, thiocarbamide, silver nitrate and ammonium metavanadate are dissolved in the water,
It is uniformly mixed;Then liquid will be stirred to be transferred in reactor, reactor is covered and is put into constant temperature convection oven
Row reaction, the Ag of black is obtained after reaction completely through post processing2S-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
Mol 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 scheme, reaction temperature is 140~180 DEG C, the reaction time is 10~
36h.Post processing is will alternately to be washed using absolute ethyl alcohol and deionized water respectively after reaction product separation of solid and liquid, be subsequently placed in perseverance
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.Show that sheet self assembly can successfully be prepared by being used as template and raw material by different aminoacids by serial experiment result
Ag2S-MoS2The spherical composite granule of micron, it has the characteristics that narrower particle size distribution, topographic profile be homogeneous and size tunable.With showing
There is technology to compare, the present invention has advantages below:
1), present invention process is simple, and whole preparation system easily builds, be easy to operate, condition is easily-controllable, cost is cheap, production
Thing composition is easily-controllable, product is evenly distributed, is not easy to reunite, is suitable for large-scale industrial production.
2), the present invention is not added in preparation process other auxiliary as reactant using conventional soluble ammonium molybdate
Material is helped, caused accessory substance is few, and environmental pollution is smaller, is a kind of environment-friendly type synthesis technique.
3), product prepared by the present invention has good catalytic activity, can be used in environmental pollution reparation and battery electrode material
Material etc..
Brief description of the drawings
Ag with accompanying drawing to the present invention with reference to embodiments2S-MoS2The simple conjunction of sheet self assembly composite spherical powder
Make and being discussed further into method.
Fig. 1 is Ag prepared by embodiment 12S-MoS2Composite spherical powder field emission scanning electron microscope (FE-SEM) figure (figure a,
B corresponds to low, high magnification image respectively);
Fig. 2 is Ag prepared by embodiment 12S-MoS2The elementary analysis figure (EDS) of composite spherical powder;
Fig. 3 is Ag prepared by embodiment 12S-MoS2XRD (a Ag of composite spherical powder2S-MoS2Composite spherical powder
The XRD of body and its and Ag2S standard card JCPDS (14-0072) comparison diagram, b Ag2S-MoS2Composite spherical powder with it is pure
MoS2XRD comparison diagrams);
Fig. 4 is Ag prepared by embodiment 12S-MoS2The TG figures of composite spherical powder;
Fig. 5 is Ag prepared by embodiment 22S-MoS2Composite spherical powder field emission scanning electron microscope (FE-SEM) figure (figure a,
B corresponds to low, high magnification image respectively);
Fig. 6 is Ag prepared by embodiment 32S-MoS2Composite spherical powder field emission scanning electron microscope (FE-SEM) figure (figure a,
B corresponds to low, high magnification image respectively).
Embodiment
Embodiment 1
(1) 1.8538g Ammonium Molybdate Tetrahydrates, 0.4567g thiocarbamides, 1.1260g glycine, 0.0255g nitric acid are weighed respectively
Silver and 0.0263g ammonium metavanadates are poured into beaker, add 15mL deionized water dissolvings.Then it is placed on magnetic stirring apparatus and stirs
30min。
(2) liquid will be stirred to be transferred in advance washed 25mL reactors, then after with 5mL deionized waters, beaker is rinsed
Pour into reactor;Reactor is covered and is put into constant temperature convection oven, it is 180 DEG C to set temperature, reacts 10h;Question response knot
Shu Hou, reactor, the powder centrifuge that will be generated after reaction are taken out, and replaced respectively with absolute ethyl alcohol and deionized water
For several times, powder after washing is put into thermostatic drying chamber for washing, and it is 30 DEG C to set temperature, is dried 5h and is obtained dry black powder
End.
Fig. 1 is Ag prepared by embodiment 12S-MoS2Composite spherical powder field emission scanning electron microscope (FE-SEM) figure (figure a,
B corresponds to low, high magnification image respectively).Composite spherical morphology microstructure obtained by being understood by Fig. 1 a is more uniform, and particle mean size is 1 μ
m;The spherical particle knowable to Fig. 1 b is the (MoS formed by sheet self assembly2), the thickness of piece is nanoscale.Inserted sheet above
For the product Ag of load2S.Local EDS analyses are 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 of composite spherical powder.It can be seen from Fig. 3 a and Ag2S's
Standard card JCPDS (14-0072) contrasts understand that silver sulfide is the body phase Ag of monocline in products therefrom2S;Ag in Fig. 3 a2S
There is a diffraction maximum (- 101) at 20.433 °, this is Ag2S diffraction maximum.2 θ are respectively at 26.322 °, 28.966 ° afterwards,
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 ° there is Ag respectively2S (012), (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, diffraction curve below is MoS2X- penetrate
There is the phenomenon of widthization in line diffraction curve, the characteristic peak of molybdenum disulfide, and this should be relevant with the size of molybdenum disulfide.From Fig. 3 b
It can be seen that MoS2Some characteristic peaks and silver sulfide characteristic peak overlap, (004) diffraction maximum such as occurred at 29.355 °.
Fig. 4 is Ag prepared by embodiment 12S-MoS2The TG figures of composite spherical powder.As shown in Figure 4, prepared by embodiment 1
Ag2S-MoS2Composite spherical powder generates less mass loss during high temperature sintering.It is attached to 70 DEG C by start temperature
The curve of product is in obvious downward trend when near, and this is the decomposition of absolute ethyl alcohol in product, and the loss of this stage quality is
0.22%, residual mass 99.78%.This shows the absolute ethyl alcohol for having 0.22% in sample.Until being increased to 160 DEG C when temperature
Curve starts to be in obvious downward trend again during 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 summary, 0.22% absolute ethyl alcohol of sample loss is removed, is also damaged
Lose 2.22%.This indicates that Ag2S-MoS2Mass ratio in composite spherical powder shared by silver sulfide is about 2.22%.
Embodiment 2
(1) 0.9269g Ammonium Molybdate Tetrahydrates, 0.5709g thiocarbamides, 0.1996g L-Aspartic acids, 0.1911g are weighed respectively
Silver nitrate and 0.0175g ammonium metavanadates are poured into beaker, add 15mL deionized water dissolvings.Then it is placed on magnetic stirring apparatus and stirs
Mix 30min.
(2) liquid will be stirred to be transferred in advance washed 25mL reactors, then after with 5mL deionized waters, beaker is rinsed
Pour into reactor;Reactor is covered and is put into constant temperature convection oven, it is 160 DEG C to set temperature, reacts 24h;Question response knot
Shu Hou, reactor, the powder centrifuge that will be generated after reaction are taken out, and replaced respectively with absolute ethyl alcohol and deionized water
For several times, powder after washing is put into thermostatic drying chamber for washing, and it is 40 DEG C to set temperature, is dried 10h and is obtained dry black powder
End.
Fig. 5 is Ag prepared by embodiment 22S-MoS2Composite spherical powder field emission scanning electron microscope (FE-SEM) figure (figure a,
B corresponds to low, high magnification image respectively).From Fig. 5 a, resulting Ag2S-MoS2Composite spherical morphology microstructure is homogeneous, average
Particle diameter is 1.5 μm, and good crystallinity;Meanwhile the rough surface of spherical particle, it is to be assembled by more tiny nano-sheet.
Fig. 5 b are observed that Ag2S nanometer sheets are evenly distributed in spherical MoS2The surface of powder is so as to forming Ag2S-MoS2Composite balls
Shape powder.
Embodiment 3
(1) 2.7807g Ammonium Molybdate Tetrahydrates, 2.7403g thiocarbamides, 2.5336g glycine, 0.0764g nitric acid are weighed respectively
Silver and 0.0263g ammonium metavanadates are poured into beaker, add 15mL deionized water dissolvings.Then it is placed on magnetic stirring apparatus and stirs
30min。
(2) liquid will be stirred to be transferred in advance washed 25mL reactors, then after with 5mL deionized waters, beaker is rinsed
Pour into reactor;Reactor is covered and is put into constant temperature convection oven, it is 140 DEG C to set temperature, reacts 36h;Question response knot
Shu Hou, reactor, the powder centrifuge that will be generated after reaction are taken out, and replaced respectively with absolute ethyl alcohol and deionized water
For several times, powder after washing is put into thermostatic drying chamber for washing, and it is 60 DEG C to set temperature, is dried 3h and is obtained dry black powder
End.
Fig. 6 is Ag prepared by embodiment 32S-MoS2Composite spherical powder field emission scanning electron microscope (FE-SEM) figure (figure a,
B corresponds to low, high magnification image respectively).From Fig. 6 a, resulting Ag2S-MoS2Composite spherical morphology microstructure is homogeneous, average
Particle diameter is 0.5 μm, and good crystallinity;Meanwhile the rough surface of spherical particle, it is to be assembled by more tiny nano-sheet.
Fig. 6 b are observed that Ag2S nanometer sheets are evenly distributed in spherical MoS2The surface of powder is so as to forming Ag2S-MoS2Composite balls
Shape powder.
Above content is only to design example and explanation of the invention, affiliated those skilled in the art
Various modifications or supplement are made to described specific embodiment or is substituted using similar mode, without departing from invention
Design or surmount scope defined in the claims, protection scope of the present invention all should be belonged to.
Claims (7)
- A kind of 1. Ag2S-MoS2The simple synthesis of sheet self assembly composite spherical powder, it is characterised 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 reactor, reactor is covered and is put into constant temperature convection oven and is reacted, black is obtained through post processing after reaction completely Ag2S-MoS2Sheet self assembly composite spherical powder.
- 2. simple synthesis as claimed in claim 1, it is characterised in that amino acid is selected from glycine or L-Aspartic acid.
- 3. simple synthesis as claimed in claim 1, it is characterised in that amino acid, Ammonium Molybdate Tetrahydrate, thiocarbamide, nitric acid Mol ratio between silver and ammonium metavanadate is 2~15:1:4~16:0.1~0.2:0.1~0.2.
- 4. simple synthesis as claimed in claim 3, it is characterised in that the molarity of ammonium molybdate in mixed solution For 0.05~0.15mol/L.
- 5. simple synthesis as claimed in claim 1, it is characterised in that reaction temperature is 140~180 DEG C, the reaction time For 10~36h.
- 6. the simple synthesis as described in any one of Claims 1 to 5, it is characterised in that post processing is to consolidate reaction product Alternately washed using absolute ethyl alcohol and deionized water respectively after liquid separation, be subsequently placed in thermostatic drying chamber and be dried.
- 7. simple synthesis as claimed in claim 6, it is characterised in that drying temperature is 20~60 in thermostatic drying chamber DEG C, drying time is 3~10h.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109126829A (en) * | 2018-09-18 | 2019-01-04 | 合肥学院 | A kind of 3-D heterojunction structure CdS-MoS2The preparation method of composite granule |
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 |
CN110357143A (en) * | 2019-03-01 | 2019-10-22 | 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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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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2017
- 2017-09-28 CN CN201710894850.4A patent/CN107500359B/en active Active
Patent Citations (2)
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 |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109126829A (en) * | 2018-09-18 | 2019-01-04 | 合肥学院 | A kind of 3-D heterojunction structure CdS-MoS2The preparation method of composite granule |
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 |
CN110357143A (en) * | 2019-03-01 | 2019-10-22 | 东北电力大学 | Sensitive material MoS for Hg (0) sensor2-Ag2S |
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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