CN108448091A - A kind of MoO2/SnS2Nanocomposite and preparation method thereof - Google Patents
A kind of MoO2/SnS2Nanocomposite and preparation method thereof Download PDFInfo
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- CN108448091A CN108448091A CN201810227164.6A CN201810227164A CN108448091A CN 108448091 A CN108448091 A CN 108448091A CN 201810227164 A CN201810227164 A CN 201810227164A CN 108448091 A CN108448091 A CN 108448091A
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Abstract
The invention discloses a kind of MoO2/SnS2Nanocomposite and preparation method thereof, method are：It takes sulphur source, tin source, water to be mixed evenly, obtains precursor solution, precursor solution is subjected to hydro-thermal reaction, obtains SnS2Six square pieces；By SnS2Six square pieces are distributed in the mixed aqueous solution of ammonium heptamolybdate and EDTA 2Na, are adjusted secondary hydro-thermal after pH, are obtained product.Preparation process of the present invention is simple, and preparation method is reproducible, and controllability is good, at low cost, has very strong operability and practicability, is suitble to industrialized production.Product form of the present invention has not been reported, it is product novel in shape, single, microscopic appearance is reproducible, good dispersion, stability is preferable, and size and component ratio are adjustable, particle size distribution narrow range, MoO2 can significantly improve the electric conductivity of SnS2 as metallicity semiconductor, have great importance to the capacity and cyclical stability that improve negative electrode of lithium ion battery.
Description
Technical field
The present invention relates to one kind by MoO2And SnS2The MoO being combined2/SnS2Nanocomposite and preparation method thereof,
More particularly to a kind of area load MoO2The SnS of nano particle2Six square pieces and preparation method thereof.
Background technology
With the high speed development of social economy and society, human lives and industrial development are to naturally asking for and destroying constantly
Aggravation, global energy shortage and problem of environmental pollution are increasingly serious.In order to substitute the fossil energy of increasingly depleted, slowing down the energy needs
It asks the destruction to environment, the mankind to constantly look for all kinds of regenerative resources, expands the use ratio of new energy.Lithium ion battery is recognized
To be the heavy-duty battery that can most meet future society sustainable development requirement, the application of lithium ion battery at present has covered me
The every field lived, status it is more and more important.In order to pursue higher battery performance, researcher constantly designs,
It finds, develop new electrode material, improve the capacity and cycle performance of lithium ion battery.
SnS2It is a kind of semi-conducting material that band gap is about 2.35eV, there is more excellent optical property and electrical property
Can, it is had a wide range of applications in photocatalysis field.In cathode material for lithium ion battery field, SnS2Theoretical specific capacity be
645mAh g-1 are far longer than carbon negative pole material, however in practical applications, SnS2It is swollen that volume is easy to happen in cyclic process
Swollen, dusting and influence its cycle performance；It is used as semi-conducting material, SnS simultaneously2Electronic conductivity is poor.Therefore researcher is logical
Various modifications are crossed to improve SnS2Chemical property.For its volume dusting expansion issues, generally pass through the nanosizing of material
Multipolarization is realized, such as document " Liu S A, Yin X M, Chen L B, et al.Synthesis of self-
assembled 3D flowerlike SnS2 nanostructures with enhanced lithium ion storage
Property [J] .Solid State Sci., 2010,12 (5)：The nanometer sheet of 712-718. " reports assembles three-dimensional flower-shaped
SnS2Capacity is maintained at 502mAh g after recycling 50 weeks-.Document " Zhai C X, Du N, Zhang H, et al.Multiwalled
Carbon Nanotubes Anchored with SnS2 Nanosheets as High—Performance Anode
Materials of Lithium-Ion Batteries [J] .Appl.Mater.Interfaces, 2011,3 (10)：4067-
4074. " report SnS2It loading in carbon nanotube, improves the conductivity of system, carbon material electric conductivity is although good,
Due to lower theoretical capacity, the whole volume of system is improved and is helped less, therefore a kind of good conductivity of searching, theoretical capacity
The same SnS of high material2It is compound to improve SnS2Chemical property have great importance.
Nanometer MoO2Theoretical specific capacity be up to 838mAhg-1, while MoO2With lower resistance（Good electronics passes
The property led）, height electrochemical reversibility, be the research hotspot in electrochemical energy storage field.Prepare MoO2And SnS2Nano combined material
Material has great importance to the capacity and cyclical stability that improve negative electrode of lithium ion battery, but yet there are no and have been reported that.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of MoO2/SnS2Nanocomposite, the nano combined material
Material is compound with artificial gold by molybdenum oxide, has special pattern, MoO2Load improve the chemical property of artificial gold, have
Important application value.
The present invention also provides above-mentioned MoO2/SnS2The preparation method of nanocomposite, this method operating process is simple,
Tin molybdenum ratio is adjustable, and product morphology controllability is strong, and yield is high.
Specific technical solution of the present invention is as follows：
Present invention firstly provides molybdenum oxide is compound with artificial gold, and MoO is successfully obtained2/SnS2Nanocomposite, this is received
Nano composite material is by MoO2Nano particle and SnS2Six square pieces are combined, the MoO2Nano particle is supported on SnS2Six square pieces
Surface.
Further, MoO2Nano particle is in SnS2The surface of six square pieces is evenly dispersed, soilless sticking phenomenon.MoO2Nanometer
Grain is in irregular shape.SnS2Six square pieces are hexagon.
Further, the MoO2The size of nano particle is 20-80nm.The SnS2The thickness of six square pieces is 40-
60nm, size are 500nm~1 μm.Because of SnS2Six square piece thickness are nanoscale, therefore can also claim SnS2Six square pieces are SnS2Six
Square nanometer sheet.
The present invention also provides above-mentioned MoO2/SnS2The preparation method of nanocomposite, this approach includes the following steps：
（1）It takes sulphur source, tin source, water to be mixed evenly, obtains precursor solution；
（2）Above-mentioned precursor solution is heated up and carries out hydro-thermal reaction, obtains SnS2Six square pieces；
（3）By SnS2Six square pieces are distributed in the aqueous solution of ammonium heptamolybdate and EDTA-2Na, adjust solution ph to 2-3, then
Hydro-thermal reaction is carried out, MoO is obtained2/SnS2Nanocomposite.
In above-mentioned preparation method, the sulphur source is thiocarbamide or thioacetamide.
In above-mentioned preparation method, the tin source is butter of tin.
Above-mentioned steps（1）In, sulphur source and water are first uniformly mixed, then mixed again with tin source or tin source aqueous solution, before obtaining
Drive liquid solution.
The SnS2 six of size uniform, good dispersion is made using water as solvent in sulphur source and tin source by the present invention by hydro-thermal method
SnS2 hexagonal nano-flakes are dispersed in ammonium heptamolybdate aqueous solution then using EDTA-2Na as complexing agent, pass through two by square nanometer sheet
Secondary hydro-thermal forms MoO2 nano particles on SnSO2 hexagonal nano-flakes surface.EDTA-2Na has the function of complex ion, in SnS2
Ammonium heptamolybdate can be complexed in six square piece surfaces, EDTA-2Na, can play the role of connecting molybdenum and sulphur, be controlled by pH value
The complexing power of EDTA-2Na makes molybdenum dioxide smoothly load to SnSO2 hexagonal nano-flakes surface, is otherwise difficult to realize MoO2's
Load.
In above-mentioned preparation method, by adjusting hydrothermal reaction condition, tin source, sulphur source concentration, EDTA-2Na dosages, acid and pH
Etc. the good product of size adjustable, pattern can be obtained.By controlling the concentration of ammonium heptamolybdate, the load of molybdenum oxide can be adjusted
Amount.
Preferably, in precursor solution, the molar ratio of sulphur source and tin source is 6:1.
Preferably, in precursor solution, a concentration of 0.05-0.15mol/L of tin source.
Preferably, step（2）In, the temperature of hydro-thermal reaction is 120-160 DEG C.The time of hydro-thermal reaction is 6-24h.
Preferably, step（2）In, hydro-thermal reaction carries out under closed environment.
Preferably, step（3）In, ammonium heptamolybdate a concentration of 0.005-0.02mol/L in aqueous solution, EDTA-2Na and
The molar ratio of Mo is 1:The molar ratio of 0.8-1.5, Mo and Sn are 0.05-0.3：1.
Preferably, step（3）In, hydrothermal temperature is 180-200 DEG C, and the hydro-thermal time is generally 12-24h.
Preferably, step（3）In, hydro-thermal reaction carries out under closed environment.
Further, step（3）In, pH is adjusted using citric acid and tartaric acid, citric acid and tartaric acid are both used as pH
Conditioning agent, and as auxiliary complex-former, improve the load capacity of molybdenum dioxide.Preferably, the mass ratio of citric acid and tartaric acid
For 2-5:1.
Preparation process of the present invention is simple, and synthesis condition is easily controllable, and raw materials used price is low, and preparation method is reproducible,
Controllability is good, at low cost, has very strong operability and practicability, is suitble to industrialized production.Product MoO of the present invention2/SnS2It receives
Nano composite material material is by MoO2Nano particle and SnS2Six square pieces are combined, which has not been reported.The product novel in shape,
Single, microscopic appearance is reproducible, and good dispersion, stability is preferable, and size and component ratio are adjustable, particle size distribution range
It is narrow, MoO2Good electronic conductivity, the electrochemical reversibility of height, high theoretical specific capacity improve SnS well2Electricity
Chemical property has great importance to the capacity and cyclical stability that improve negative electrode of lithium ion battery.
Description of the drawings
The X-ray diffraction for six square pieces of SnS2 that Fig. 1 embodiment of the present invention 1 synthesizes（XRD）Collection of illustrative plates.
The scanning electron microscope for six square pieces of SnS2 that Fig. 2 embodiment of the present invention 1 synthesizes（SEM）Photo.
The X-ray diffraction of the hexagonal flake SnS2 of load MoO2 nano particles prepared by Fig. 3 embodiment of the present invention 1（XRD）
Collection of illustrative plates.
The scanning electron microscope of the hexagonal flake SnS2 for the load MoO2 nano particles that Fig. 4 embodiment of the present invention 1 synthesizes（SEM）According to
Piece.
The transmission electron microscope of the hexagonal flake SnS2 for the load MoO2 nano particles that Fig. 5 embodiment of the present invention 1 synthesizes（TEM）According to
Piece.
Fig. 6 is the scanning electron microscope of the hexagonal flake SnS2 for the load MoO2 nano particles that the embodiment of the present invention 2 synthesizes（SEM）
Photo.
Fig. 7 is the scanning electron microscope of the hexagonal flake SnS2 for the load MoO2 nano particles that the embodiment of the present invention 3 synthesizes（SEM）
Photo.
The scanning electron microscope of the hexagonal flake SnS2 for the load MoO2 nano particles that Fig. 8 embodiment of the present invention 4 synthesizes（SEM）According to
Piece.
The scanning electron microscope of the hexagonal flake SnS2 for the load MoO2 nano particles that Fig. 9 comparative examples 1 of the present invention synthesize（SEM）According to
Piece.
The scanning electron microscope of the hexagonal flake SnS2 for the load MoO2 nano particles that Figure 10 comparative examples 3 of the present invention synthesize（SEM）
Photo.
Specific implementation method
Below by embodiment, the present invention will be further elaborated, it should be appreciated that, following the description is merely to explain
The present invention is not defined its content.
Embodiment 1
1.1 are dissolved in 0.912 g thiocarbamides in 30 mL deionized waters, and 30min is stirred at room temperature.
1.2 0.7 g SnCl are added into 1.1 solution4·5H2O stirs to get homogeneous solution, i.e. precursor solution.
1.3 are transferred to 1.2 precursor solutions in 50 mL reaction kettles, are heated to 160 DEG C in an oven, closed anti-
Answer 12 h.
Sample after cooling is carried out centrifuge washing by 1.4, obtains red SnS2Nanometer sheet, nanometer sheet are hexagonal structure,
As hexagon, SnS2The size of hexagonal nano-flake is between 500 nm-1000nm, and thickness is in 50nm or so, and XRD diagram is as schemed
Shown in 1, scanning electron microscope (SEM) photograph is as shown in Figure 2.
1.5 by SnS2Hexagonal nano-flake is scattered in 30ml ammonium heptamolybdates containing 0.1g and the mixed aqueous solution of 0.2gEDTA-2Na
In, it is 3 to adjust pH value of solution with citric acid and tartaric acid, and the mass ratio of citric acid and tartaric acid is 2:1.
1.6 are transferred to the solution in 1.5 in 50 mL reaction kettles, are heated to 200 DEG C in an oven, confined reaction 12
H obtains MoO2/SnS2Nanocomposite, the XRD diagram of the nanocomposite is as shown in figure 3, scanning electron microscope (SEM) photograph such as Fig. 4 institutes
Show, transmission electron microscope picture is as shown in Figure 5.It can be seen from the figure that the nanocomposite is by six side of MoO2 nano particles and SnS2
Nanometer sheet forms, and MoO2 nano particles are uniformly dispersed in SnS2 hexagonal nano on pieces, and soilless sticking, wherein MoO2 nano particles is big
It is small between 50-80nm, the sizes of SnS2 hexagonal nano-flakes is 800 nm or so, and thickness 50nm is analyzed through EDS, and nanometer is multiple
The molar ratio of MoO2 and SnS2 is about 0.27 in condensation material：1.
Embodiment 2
2.1 are dissolved in 0.1824 g thiocarbamides in 30 mL deionized waters, and 30min is stirred at room temperature.
2.2 1.4g SnCl45H2O are added into 2.1 solution, stir to get homogeneous solution, i.e. precursor solution.
2.3 are transferred to 2.2 precursor solutions in 50 mL reaction kettles, are heated to 120 DEG C in an oven, closed anti-
Answer 24 h.
Sample after cooling is carried out centrifuge washing by 2.4, obtains red SnS2 nanometer sheets, nanometer sheet is hexagonal structure.
2.5 by SnS2Hexagonal nano-flake is scattered in 30ml ammonium heptamolybdates containing 0.14g and 0.3g EDTA-2Na solution, is used
It is 2.5 that citric acid and tartaric acid, which adjust pH value of solution, and the mass ratio of citric acid and tartaric acid is 3:1.
2.6 are transferred to the solution in 2.5 in 50 mL reaction kettles, are heated to 200 DEG C in an oven, confined reaction 12
H obtains MoO2/SnS2The scanning electron microscope (SEM) photograph of nanocomposite, the nanocomposite is as shown in Figure 6.It can from figure
Go out, which is made of MoO2 nano particles and SnS2 hexagonal nano-flakes, and MoO2 nano particles are received in six sides of SnS2
Rice on piece is uniformly dispersed, and soilless sticking, the wherein size of MoO2 nano particles are in 50nm or so, the size of SnS2 hexagonal nano-flakes
300-500 nm, thickness are about 50 nm.It is analyzed through EDS, the molar ratio of MnO2 and SnS2 is about 0.19 in nanocomposite：
1。
Embodiment 3
3.1 are dissolved in 0.912 g thiocarbamides in 30 mL deionized waters, and 30min is stirred at room temperature.
3.2 0.7 g SnCl45H2O are added into 3.1 solution, stir to get homogeneous solution, i.e. presoma is molten
Liquid.
3.3 are transferred to 3.2 precursor solutions in 50 mL reaction kettles, are heated to 140 DEG C in an oven, closed anti-
Answer 20 h.
Sample after cooling is carried out centrifuge washing by 3.4, obtains red SnS2 nanometer sheets, nanometer sheet is hexagonal structure.
3.5 by SnS2Hexagonal nano-flake is scattered in the solution of 30ml ammonium heptamolybdates containing 0.03g and 0.06g EDT-2Na,
It is 2 to adjust pH value of solution with citric acid and tartaric acid, and the mass ratio of citric acid and tartaric acid is 2:1.
3.6 are transferred to the solution in 3.5 in 50 mL reaction kettles, are heated to 200 DEG C in an oven, confined reaction 20
H obtains MoO2/SnS2The scanning electron microscope (SEM) photograph of nanocomposite, the nanocomposite is as shown in Figure 7.It can from figure
Go out, which is made of MoO2 nano particles and SnS2 hexagonal nano-flakes, and MoO2 nano particles are received in six sides of SnS2
Rice on piece is uniformly dispersed, and soilless sticking, the wherein size of MoO2 nano particles are between 20-50nm, the ruler of SnS2 hexagonal nano-flakes
Very little is 500 nm, and thickness is about 40 nm.It is analyzed through EDS, the molar ratio of MnO2 and SnS2 is about 0.08 in nanocomposite：
1。
Embodiment 4
4.1 are dissolved in 0.9g thioacetamides in 30 mL deionized waters, and 30min is stirred at room temperature.
4.2 0.7 g SnCl45H2O are added into 4.1 solution, stir to get homogeneous solution, i.e. presoma is molten
Liquid.
4.3 are transferred to 4.2 precursor solutions in 50 mL reaction kettles, are heated to 150 DEG C in an oven, closed anti-
Answer 16 h.
Sample after cooling is carried out centrifuge washing by 4.4, obtains red SnS2 nanometer sheets, nanometer sheet is hexagonal structure.
4.5 by SnS2Hexagonal nano-flake is scattered in the solution of 30 ml ammonium heptamolybdates containing 0.07g and 0.15g EDTA-2Na
In, it is 2.7 to adjust pH value of solution with citric acid and tartaric acid, and the mass ratio of citric acid and tartaric acid is 5:1.
4.6 are transferred to the solution in 4.5 in 50 mL reaction kettles, are heated to 180 DEG C in an oven, confined reaction 24
H obtains MoO2/SnS2The scanning electron microscope (SEM) photograph of nanocomposite, the nanocomposite is as shown in Figure 8.It can from figure
Go out, which is made of MoO2 nano particles and SnS2 hexagonal nano-flakes, and MoO2 nano particles are received in six sides of SnS2
Rice on piece is uniformly dispersed, and soilless sticking, the wherein size of MoO2 nano particles are between 50-80nm, the ruler of SnS2 hexagonal nano-flakes
It is very little be 500-600nm between, thickness is about 40 nm.It is analyzed through EDS, the molar ratio of MnO2 and SnS2 is about in nanocomposite
It is 0.2：1.
Embodiment 5
5.1 are dissolved in 0.9g thioacetamides in 30 mL deionized waters, and 30min is stirred at room temperature.
5.2 0.7 g SnCl45H2O are added into 5.1 solution, stir to get homogeneous solution, i.e. presoma is molten
Liquid.
5.3 are transferred to 5.2 precursor solutions in 50 mL reaction kettles, are heated to 120 DEG C in an oven, closed anti-
Answer 24 h.
Sample after cooling is carried out centrifuge washing by 5.4, obtains red SnS2 nanometer sheets, nanometer sheet is hexagonal structure.
5.5 by SnS2Hexagonal nano-flake is scattered in the solution of 30 ml ammonium heptamolybdates containing 0.06g and 0.13g EDTA-2Na
In, it is 2.1 to adjust pH value of solution with citric acid and tartaric acid, and the mass ratio of citric acid and tartaric acid is 4:1.
5.6 are transferred to the solution in 5.5 in 50 mL reaction kettles, are heated to 190 DEG C in an oven, confined reaction 20
H obtains MoO2/SnS2Nanocomposite obtains MoO2/SnS2Nanocomposite, the nanocomposite is by MoO2 nanometers
Particle and SnS2 hexagonal nano-flakes composition, MoO2 nano particles are uniformly dispersed in SnS2 hexagonal nano on pieces, soilless sticking, wherein
The size of MoO2 nano particles is in 60-80nm, and the size of SnS2 hexagonal nano-flakes is 500 nm, and thickness is about 40 nm.Through EDS
It analyzes, the molar ratio of MnO2 and SnS2 is about 0.17 in nanocomposite：1.
Embodiment 6
6.1 are dissolved in 1.8g thioacetamides in 30 mL deionized waters, and 30min is stirred at room temperature.
6.2 1.4g SnCl45H2O are added into 6.1 solution, stir to get homogeneous solution, i.e. precursor solution.
6.3 are transferred to 6.2 precursor solutions in 50 mL reaction kettles, are heated to 160 DEG C in an oven, closed anti-
Answer 10 h.
Sample after cooling is carried out centrifuge washing by 6.4, obtains red SnS2 nanometer sheets, nanometer sheet is hexagonal structure.
6.5 by SnS2Hexagonal nano-flake is scattered in the solution of 30 ml ammonium heptamolybdates containing 0.08g and 0.16g EDTA-2Na
In, it is 2.3 to adjust pH value of solution with citric acid and tartaric acid, and the mass ratio of citric acid and tartaric acid is 2:1.
6.6 are transferred to the solution in 6.5 in 50 mL reaction kettles, are heated to 200 DEG C in an oven, confined reaction 20
H obtains MoO2/SnS2Nanocomposite, the nanocomposite are made of MoO2 nano particles and SnS2 hexagonal nano-flakes,
MoO2 nano particles are uniformly dispersed in SnS2 hexagonal nano on pieces, soilless sticking, and wherein the size of MoO2 nano particles is on the left sides 60nm
The size on the right side, SnS2 hexagonal nano-flakes is 900 nm, and thickness is about 60 nm.Analyzed through EDS, in nanocomposite MnO2 with
The molar ratio of SnS2 is about 0.11：1.
Embodiment 7
7.1 are dissolved in 0.9 g thioacetamides in 30 mL deionized waters, and 30min is stirred at room temperature.
7.2 0.7g SnCl45H2O are added into 7.1 solution, stir to get homogeneous solution, i.e. precursor solution.
7.3 are transferred to 7.2 precursor solutions in 50 mL reaction kettles, are heated to 120 DEG C in an oven, closed anti-
Answer 12 h.
Sample after cooling is carried out centrifuge washing by 7.4, obtains red SnS2 nanometer sheets, nanometer sheet is hexagonal structure.
7.5 by SnS2Hexagonal nano-flake is scattered in the solution of 30 ml ammonium heptamolybdates containing 0.05g and 0.11g EDTA-2Na
In, it is 2.8 to adjust pH value of solution with citric acid and tartaric acid, and the mass ratio of citric acid and tartaric acid is 2:1.
7.6 are transferred to the solution in 7.5 in 50 mL reaction kettles, are heated to 200 DEG C in an oven, confined reaction 20
H obtains MoO2/SnS2Nanocomposite, the nanocomposite are made of MoO2 nano particles and SnS2 hexagonal nano-flakes,
MoO2 nano particles are uniformly dispersed in SnS2 hexagonal nano on pieces, soilless sticking, and wherein the size of MoO2 nano particles is on the left sides 60nm
The size on the right side, SnS2 hexagonal nano-flakes is 900 nm, and thickness is about 60 nm.Analyzed through EDS, in nanocomposite MnO2 with
The molar ratio of SnS2 is about 0.15：1.
Embodiment 8
Product is prepared according to the method for embodiment 1, unlike：By SnS2Hexagonal nano-flake is scattered in 30ml seven molybdic acids containing 0.1g
It is 3 with hydrochloric acid conditioning solution pH in the mixed aqueous solution of ammonium and 0.2gEDTA-2Na.Products obtained therefrom by MoO2 nano particles and
SnS2 hexagonal nano-flakes form, and MoO2 nano particles are uniformly dispersed in SnS2 hexagonal nano on pieces, soilless sticking, wherein MoO2 nanometer
The size of particle is between 40-80nm, and the size of SnS2 hexagonal nano-flakes is 850nm or so, thickness 40-50nm, through EDS points
It analyses, the molar ratio of MoO2 and SnS2 is about 0.20 in product：1.
Comparative example 1
Product is prepared according to the method for embodiment 1, unlike：By SnS2Hexagonal nano-flake is scattered in 30ml seven molybdic acids containing 0.1g
In the mixed aqueous solution of ammonium and 0.2gEDTA-2Na, it is 5 to adjust pH value of solution with citric acid and tartaric acid, citric acid and tartaric acid
Mass ratio is 2:1.
Although products obtained therefrom scanning electron microscope (SEM) photograph is as shown in figure 9, it can be seen from the figure that form SnS2Hexagonal nano-flake, but
SnS2Hexagonal nano-flake surface is almost without MoO2.Illustrate that the adjusting of pH value is most important to the load of MoO2.
Comparative example 2
Product is prepared according to the method for embodiment 1, unlike：After adjusting pH, solution is transferred in 50 mL reaction kettles,
It is heated to 170 DEG C in an oven, 12 h of confined reaction.The scanning electron microscope (SEM) photograph of products obtained therefrom is similar with Fig. 9, although forming SnS2
Hexagonal nano-flake, but SnS2Hexagonal nano-flake surface is almost without MoO2.
Comparative example 3
Product is prepared according to the method for embodiment 1, unlike：After adjusting pH, solution is transferred in 50 mL reaction kettles,
It is heated to 210 DEG C in an oven, 12 h of confined reaction.The scanning electron microscope (SEM) photograph of products obtained therefrom is as shown in Figure 10, can from figure
Go out, SnS2 hexagonal flakes are destructurized, and what is obtained is the smooth irregular laminated structure in surface, and size is at 5 μm or more, and nothing
MoO2 particulate loads.
Comparative example 4
Product is prepared according to the method for embodiment 1, unlike：It is added without EDTA-2Na.The scanning electron microscope (SEM) photograph of products obtained therefrom with
Fig. 9 is similar, although forming SnS2Hexagonal nano-flake, but SnS2Hexagonal nano-flake surface is almost without MoO2.
Claims (10)
1. a kind of MoO2/SnS2Nanocomposite, it is characterized in that：It is combined by MoO2 nano particles and six square pieces of SnS2, institute
State MoO2Nano particle is supported on SnS2The surface of six square pieces.
2. MoO according to claim 12/SnS2Nanocomposite, it is characterized in that：The MoO2The grain size of nano particle
For 20-80nm, the SnS2The thickness of six square pieces is 40-60nm, and size is 500nm~1 μm.
3. a kind of MoO2/SnS2The preparation method of nanocomposite, it is characterized in that including the following steps：
（1）It takes sulphur source, tin source, water to be mixed evenly, obtains precursor solution；
（2）Above-mentioned precursor solution is heated up and carries out hydro-thermal reaction, obtains SnS2Six square pieces；
（3）By SnS2Six square pieces are distributed in the aqueous solution of ammonium heptamolybdate and EDTA-2Na, adjust solution ph to 2-3, then into
Row hydro-thermal reaction, obtains MoO2/SnS2Nanocomposite.
4. preparation method according to claim 3, it is characterized in that：Step（1）In, the molar ratio of sulphur source and tin source is 6:1,
A concentration of 0.05-0.15mol/L of tin source.
5. preparation method according to claim 3 or 4, it is characterized in that：Step（3）In, the molar ratio of Mo and EDTA-2Na
It is 1:The molar ratio of 0.8-1.5, Mo and Sn are 0.05-0.3:1.
6. preparation method according to claim 3, it is characterized in that：Step（3）In, ammonium heptamolybdate aqueous solution it is a concentration of
0.005-0.02mol/L。
7. according to the preparation method described in claim 3,5 or 6, it is characterized in that：Step（3）In, using citric acid and tartaric acid
Adjust pH, it is preferred that the mass ratio of citric acid and tartaric acid is 2-5:1.
8. preparation method according to claim 3, it is characterized in that：The sulphur source is thiocarbamide or thioacetamide；The tin
Source is butter of tin.
9. preparation method according to claim 3, it is characterized in that：Step（2）In, the temperature of hydro-thermal reaction is 120-160
DEG C, the time of hydro-thermal reaction is 6-24h；Step（3）In, the temperature of hydro-thermal reaction is 180-200 DEG C, and the time of hydro-thermal reaction is
12-24h。
10. preparation method according to claim 3, it is characterized in that：Step（2）And（3）In, hydro-thermal reaction is in closed environment
Lower progress.
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| CN115283668A (en) * | 2022-07-14 | 2022-11-04 | 中山大学 | Tin disulfide-gold composite material and preparation method and application thereof |
| CN115283668B (en) * | 2022-07-14 | 2023-11-21 | 中山大学 | Tin disulfide-gold composite material and preparation method and application thereof |
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