CN109569666A - A kind of rGO/MoS2/SnO2The preparation method of composite air-sensitive material - Google Patents
A kind of rGO/MoS2/SnO2The preparation method of composite air-sensitive material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 46
- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 31
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 21
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000008367 deionised water Substances 0.000 claims abstract description 35
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 35
- 238000005119 centrifugation Methods 0.000 claims abstract description 21
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 10
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 10
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 10
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 10
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 239000006185 dispersion Substances 0.000 claims abstract description 8
- 238000002604 ultrasonography Methods 0.000 claims abstract description 8
- 238000000137 annealing Methods 0.000 claims description 22
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 12
- 239000003054 catalyst Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000000047 product Substances 0.000 abstract 9
- 238000001816 cooling Methods 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 12
- 238000013507 mapping Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229910052718 tin Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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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
-
- B01J35/39—
-
- B01J35/61—
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
Abstract
The invention discloses a kind of rGO/MoS2/SnO2The preparation method of composite air-sensitive material, the specific steps of which are as follows: one, weigh a certain amount of graphene dispersion in deionized water, stir, ultrasound obtains first group of product；Two, ammonium molybdate is added in first group of product and thiocarbamide is stirred, obtain second group of product；Three, second group of product is put into reaction kettle, is put under baking oven set temperature and keeps, be cooled to room temperature and carry out eccentric cleaning, collected cooling and be dried to obtain third group product；Four, it disperses third group product in deionized water, certain density SnCl is added dropwise in high-speed stirred while4It is stood after solution and obtains the 4th group of product；Five, the 4th group of product is collected by centrifugation, is dried, in N2It is annealed to obtain final product in atmosphere.Preparation method of the invention is simple, and operability is stronger, and the structure and pattern of product have very strong novelty, and this special sandwich structure greatly improves the specific surface area of gas sensitive, significantly improves its air-sensitive performance.
Description
Technical field
The present invention relates to composite air-sensitive developing material technical field, in particular to a kind of rGO/MoS2/SnO2Composite air-sensitive material
The preparation method of material.
Background technique
In recent years, the exploitation and application of the development greatly pushing function material of nanosecond science and technology.Nanometer material structure system
With large specific surface area, the advantage of structure opening, so there is extremely important application value in gas sensitive field.Nanometer material
Size, pattern and the component of material all can greatly influence its property, to influence its application prospect.So far, researcher has been
Through by many physics and chemical method, by nano material from zero dimension, one-dimensional, starts to develop to multidimensional, be formed many abundant
Pattern, meanwhile, the modulation of nano-component also results in the great interest of researcher, becomes the new hot spot of nano materials research.It receives
Interaction between rice gas sensitive and gas molecule, causes the chemical property of sensitive material to change, and passes through these electricity
The variation of signal and reach to object gas detect.And nanometer hierarchical structure has due to the complexity and particularity of its structure
Higher specific surface area provides more activated adoption sites, can show gas more superior than some conventional gas sensitives
Quick performance.So preparing multicomponent, the gas sensitive of large specific surface area will study direction from now on.
Graphene GO has prominent large specific surface area, mechanical property, conductivity height, hot property excellent, as nanometer
Conductive filler carries out functionalization to gas sensitive, is expected to obtain high-performance or graphene-based nano combined with specific function
Material, thus its application range of further expansion.
Therefore, we need to find one kind can be by graphene, MoS2Composite air-sensitive material is prepared with INVENTIONConventional metal-oxide
Method.
Summary of the invention
It is an object of the invention to: in view of the above problems, providing one kind can be by rGO, MoS2With SnO2In conjunction with system
The preparation method of standby sandwich structure gas sensitive, and should preparation method is simple, operation possibility is strong.
In order to achieve the above-mentioned object of the invention, The technical solution adopted by the invention is as follows:
A kind of rGO/MoS2/SnO2The preparation method of composite air-sensitive material, comprising the following steps:
(1) it weighs graphene dispersion in deionized water, stirs, ultrasound obtains first group of product；
(2) first group of product in step (1) is continuously added into ammonium molybdate and thiocarbamide is stirred mixing, obtain second group
Product；
(3) second group of product in step (2) is put into reaction kettle, at a certain temperature hydro-thermal reaction certain time
Afterwards, it is cooled to after room temperature carries out eccentric cleaning, drying and obtains third group product；
(4) it disperses the third group product in step (3) in deionized water, is added dropwise after high-speed stirred a certain amount of
SnCl4It is stood after solution stirring and obtains the 4th group of product；
(5) the 4th group of product in step (4) is collected by centrifugation, dries, anneals in nitrogen atmosphere.
Further, in step (1), the amount of the graphene is 10~30mg, the amount of the deionized water is 20~
40ml, the mixing time are 20~40min, and ultrasonic time is 5~15min.
Further, in step (2), the content of the ammonium molybdate is 0.2~1mmol, the content of thiocarbamide is 10~
15mmol。
Further, in step (3), the hydro-thermal reaction is that second group of product is placed in reaction kettle, pressurization heating
And continuing stirring reacts second group of product inner material.
Further, the temperature of the hydro-thermal reaction be 150~200 DEG C, the drying time be 10~for 24 hours, it is described from
Heart rate is 8500~10000rpm, and centrifugation time is 5~15min.
Further, in step (4), the content of the deionized water is 20~40ml, the time of the high-speed stirred
For 15~30min, a certain amount of SnCl4Solution is 2mL, the SnCl of 0.01M4Solution.
Further, in step (5), the annealing is to be gradually heated in nitrogen atmosphere with certain heating rate
After annealing temperature, constant temperature 10h is kept.
Further, the annealing temperature is 180~220 DEG C, and the heating rate is 5 DEG C/min.
Further, the rGO/MoS2/SnO2Composite air-sensitive material can be used for sensor material, photochemical catalyst.
In conclusion by adopting the above-described technical solution, the beneficial effects of the present invention are:
(1) hydro-thermal method and annealing preparation rGO/MoS used2/SnO2Easy to operate, the environment of composite air-sensitive material
Friendly, repeatability is by force.
(2) rGO/MoS prepared by the present invention2/SnO2Composite air-sensitive material can be used for sensor material, photochemical catalyst etc.,
Compared with traditional gas sensitive, rGO and MoS are used2Combination can be based on of the two on crystal structure and microscopic appearance
With the complementarity on property and electric property, the composite material of formation can farthest show synergistic effect tool between the two
Have a superior air-sensitive performance, " the electronic reciprocal effect " that contact interface occurs will greatly enhance device stability,
Significantly improve air-sensitive performance.Using the method for efficiently constructing two dimensional heterostructures composite nano materials, by GO, MoS2With tradition
Metal oxide SnO2It is compounded to form hybrid material, it will help improve selectivity of such sensor to different VOC gas, spirit
Sensitivity and stability.
(3) the invention discloses a kind of rGO/MoS2/SnO2The preparation method of composite air-sensitive material, this method is simple and easy,
Operation possibility is strong, and product has nanometer hierarchical composite construction, will be with excellent gas compared to common nano-sensor
Quick performance.
Detailed description of the invention
Fig. 1 is the rGO/MoS prepared in embodiment 12The SEM of predecessor schemes；
Fig. 2 is the rGO/MoS prepared in embodiment 12/SnO2The SEM of composite material schemes；
Fig. 3 is the rGO/MoS prepared in embodiment 12/SnO2The SEM mapping of middle C schemes；
Fig. 4 is the rGO/MoS prepared in embodiment 12/SnO2The SEM mapping of middle S schemes；
Fig. 5 is the rGO/MoS prepared in embodiment 12/SnO2The SEM mapping of middle Mo schemes；
Fig. 6 is the rGO/MoS prepared in embodiment 12/SnO2The SEM mapping of middle Sn schemes；
Fig. 7 is the rGO/MoS prepared in embodiment 12/SnO2The SEM mapping of middle O schemes；
Fig. 8 is the rGO/MoS prepared in embodiment 12The XRD diagram of predecessor；
Fig. 9 is the rGO/MoS prepared in embodiment 12/SnO2The XRD diagram of composite material.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention more comprehensible, preferred embodiment is enumerated below, to this hair
Bright further description.However, it is necessary to illustrate, many details listed in specification are used for the purpose of making reader to this
The one or more aspects of invention have a thorough explanation, also may be implemented even without these specific details of the invention
These aspects.
Embodiment 1
A kind of rGO/MoS2/SnO2The preparation method of composite air-sensitive material, comprising the following steps:
(1) it weighs graphene dispersion in deionized water, stirs, ultrasound obtains first group of product, and the amount of graphene is
10mg, the amount of the deionized water are 20ml, and the mixing time is 20min, ultrasonic time 5min；
(2) first group of product in step (1) is continuously added into ammonium molybdate and thiocarbamide is stirred mixing, obtain second group
Product, the content of deionized water are 20ml, and the time of the high-speed stirred is 15min, a certain amount of SnCl4Solution is 2mL,
The SnCl of 0.01M4Solution；
(3) second group of product in step (2) is put into reaction kettle, one timing of pressurized thermal water reaction at a certain temperature
Between after, be cooled to room temperature and carry out eccentric cleaning, obtain third group product after drying, the temperature of the hydro-thermal reaction is 150 DEG C,
The drying time is 10h, and the centrifugation rate is 8500rpm, centrifugation time 5min；
(4) it disperses the third group product in step (3) in deionized water, is added dropwise after high-speed stirred a certain amount of
SnCl4It is stood after solution stirring and obtains the 4th group of product, the content of deionized water is 20ml, and the time of the high-speed stirred is
15min, a certain amount of SnCl4Solution is 2mL, the SnCl of 0.01M4Solution；
(5) the 4th group of product in step (4) is collected by centrifugation, dries, is annealed to obtain rGO/ in nitrogen atmosphere
MoS2/SnO2Composite air-sensitive material, annealing is after being gradually heated to annealing temperature in nitrogen atmosphere with certain heating rate,
Constant temperature 10h is kept, annealing temperature is 180 DEG C, and heating rate is 5 DEG C/min.
Embodiment 2
A kind of rGO/MoS2/SnO2The preparation method of composite air-sensitive material, comprising the following steps:
(1) it weighs graphene dispersion in deionized water, stirs, ultrasound obtains first group of product, and the amount of graphene is
30mg, the amount of the deionized water are 40ml, and the mixing time is 40min, ultrasonic time 15min；
(2) first group of product in step (1) is continuously added into ammonium molybdate and thiocarbamide is stirred mixing, obtain second group
Product, the content of deionized water are 40ml, and the time of the high-speed stirred is 30min, a certain amount of SnCl4Solution is 2mL,
The SnCl of 0.01M4Solution；
(3) second group of product in step (2) is put into reaction kettle, one timing of pressurized thermal water reaction at a certain temperature
Between after, be cooled to room temperature and carry out eccentric cleaning, obtain third group product after drying, the temperature of the hydro-thermal reaction is 200 DEG C,
The drying time is that for 24 hours, the centrifugation rate is 10000rpm, centrifugation time 15min；
(4) it disperses the third group product in step (3) in deionized water, is added dropwise after high-speed stirred a certain amount of
SnCl4It is stood after solution stirring and obtains the 4th group of product, the content of deionized water is 40ml, and the time of the high-speed stirred is
30min, a certain amount of SnCl4Solution is 2mL, the SnCl of 0.01M4Solution；
(5) the 4th group of product in step (4) is collected by centrifugation, dries, is annealed to obtain rGO/ in nitrogen atmosphere
MoS2/SnO2Composite air-sensitive material, annealing is after being gradually heated to annealing temperature in nitrogen atmosphere with certain heating rate,
Constant temperature 10h is kept, annealing temperature is 220 DEG C, and heating rate is 5 DEG C/min.
Embodiment 3
A kind of rGO/MoS2/SnO2The preparation method of composite air-sensitive material, comprising the following steps:
(1) it weighs graphene dispersion in deionized water, stirs, ultrasound obtains first group of product, and the amount of graphene is
20mg, the amount of the deionized water are 30ml, and the mixing time is 30min, ultrasonic time 10min；
(2) first group of product in step (1) is continuously added into ammonium molybdate and thiocarbamide is stirred mixing, obtain second group
Product, the content of deionized water are 30ml, and the time of the high-speed stirred is 20min, a certain amount of SnCl4Solution is 2mL,
The SnCl of 0.01M4Solution；
(3) second group of product in step (2) is put into reaction kettle, one timing of pressurized thermal water reaction at a certain temperature
Between after, be cooled to room temperature and carry out eccentric cleaning, obtain third group product after drying, the temperature of the hydro-thermal reaction is 180 DEG C,
The drying time is 15h, and the centrifugation rate is 8500rpm, centrifugation time 10min；
(4) it disperses the third group product in step (3) in deionized water, is added dropwise after high-speed stirred a certain amount of
SnCl4It is stood after solution stirring and obtains the 4th group of product, the content of deionized water is 30ml, and the time of the high-speed stirred is
20min, a certain amount of SnCl4Solution is 2mL, the SnCl of 0.01M4Solution；
(5) the 4th group of product in step (4) is collected by centrifugation, dries, is annealed to obtain rGO/ in nitrogen atmosphere
MoS2/SnO2Composite air-sensitive material, annealing is after being gradually heated to annealing temperature in nitrogen atmosphere with certain heating rate,
Constant temperature 10h is kept, annealing temperature is 200 DEG C, and heating rate is 5 DEG C/min.
Embodiment 4
A kind of rGO/MoS2/SnO2The preparation method of composite air-sensitive material, comprising the following steps:
(1) it weighs graphene dispersion in deionized water, stirs, ultrasound obtains first group of product, and the amount of graphene is
25mg, the amount of the deionized water are 30ml, and the mixing time is 35min, ultrasonic time 10min；
(2) first group of product in step (1) is continuously added into ammonium molybdate and thiocarbamide is stirred mixing, obtain second group
Product, the content of deionized water are 35ml, and the time of the high-speed stirred is 35min, a certain amount of SnCl4Solution is 2mL,
The SnCl of 0.01M4Solution；
(3) second group of product in step (2) is put into reaction kettle, one timing of pressurized thermal water reaction at a certain temperature
Between after, be cooled to room temperature and carry out eccentric cleaning, obtain third group product after drying, the temperature of the hydro-thermal reaction is 190 DEG C,
The drying time is 20h, and the centrifugation rate is 10000rpm, centrifugation time 10min；
(4) it disperses the third group product in step (3) in deionized water, is added dropwise after high-speed stirred a certain amount of
SnCl4It is stood after solution stirring and obtains the 4th group of product, the content of deionized water is 30ml, and the time of the high-speed stirred is
20min, a certain amount of SnCl4Solution is 2mL, the SnCl of 0.01M4Solution；
(5) the 4th group of product in step (4) is collected by centrifugation, dries, is annealed to obtain rGO/ in nitrogen atmosphere
MoS2/SnO2Composite air-sensitive material, annealing is after being gradually heated to annealing temperature in nitrogen atmosphere with certain heating rate,
Constant temperature 10h is kept, annealing temperature is 200 DEG C, and heating rate is 5 DEG C/min.
Embodiment 5
A kind of rGO/MoS2/SnO2The preparation method of composite air-sensitive material, comprising the following steps:
(1) it weighs graphene dispersion in deionized water, stirs, ultrasound obtains first group of product, and the amount of graphene is
15mg, the amount of the deionized water are 25ml, and the mixing time is 25min, and ultrasonic time is 5~15min；
(2) first group of product in step (1) is continuously added into ammonium molybdate and thiocarbamide is stirred mixing, obtain second group
Product, the content of deionized water are 22ml, and the time of the high-speed stirred is 18min, a certain amount of SnCl4Solution is 2mL,
The SnCl of 0.01M4Solution；
(3) second group of product in step (2) is put into reaction kettle, one timing of pressurized thermal water reaction at a certain temperature
Between after, be cooled to room temperature and carry out eccentric cleaning, obtain third group product after drying, the temperature of the hydro-thermal reaction is 170 DEG C,
The drying time is 15h, and the centrifugation rate is 9000rpm, centrifugation time 10min；
(4) it disperses the third group product in step (3) in deionized water, is added dropwise after high-speed stirred a certain amount of
SnCl4It is stood after solution stirring and obtains the 4th group of product, the content of deionized water is 25ml, and the time of the high-speed stirred is
20min, a certain amount of SnCl4Solution is 2mL, the SnCl of 0.01M4Solution；
(5) the 4th group of product in step (4) is collected by centrifugation, dries, is annealed to obtain rGO/ in nitrogen atmosphere
MoS2/SnO2Composite air-sensitive material, annealing is after being gradually heated to annealing temperature in nitrogen atmosphere with certain heating rate,
Constant temperature 10h is kept, annealing temperature is 185 DEG C, and heating rate is 5 DEG C/min.
The composite air-sensitive material prepared in embodiment 1 is scanned Electronic Speculum to take pictures, Fig. 1 rGO/MoS2Predecessor sample
Stereoscan photograph, can be seen that rGO/MoS from the photo2Predecessor MoS2Laminated structure is presented and is embedded in the surface rGO, this
Body structure surface product is very big, in order to enhance the stability of the structure, and improves its performance.Made by step (4) and step (5)
SnO2It is wrapped in MoS2Surface, Fig. 2 are rGO/MoS2/SnO2The SEM of composite air-sensitive material schemes, in Fig. 2 we have found that the structure
Surface topography is analyzed without too big variation, but by the mapping figure of SEM, and Fig. 3~Fig. 7 is respectively C, S, Mo, Sn, O member
The mapping figure of element, as can be seen from the figure contains C, S, Mo, Sn, O element, and Sn, O element are evenly distributed in rGO/
MoS2In nanometer film, it was demonstrated that SnO2Successfully it is wrapped on rGO/MoS.Fig. 8 is rGO/MoS2The XRD diagram of predecessor, on 10 ° of left sides
The right side has a parcel peak for rGO, and spectrogram and MoS2Standard card peak figure is compared, and corresponds, Fig. 9 rGO/MoS2/
SnO2It is rGO that the XRD diagram of composite material, which has a parcel peak at 10 ° or so, with SnO2With MoS2Standard card peak figure is compared
It is right, it corresponds, determines product.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the principle of the present invention, it can also make several improvements and retouch, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of rGO/MoS2/SnO2The preparation method of composite air-sensitive material, it is characterised in that: the following steps are included:
(1) it weighs graphene dispersion in deionized water, stirs, ultrasound obtains first group of product；
(2) first group of product in step (1) is continuously added into ammonium molybdate and thiocarbamide is stirred mixing, obtain second group of production
Object；
(3) second group of product in step (2) is put into reaction kettle, at a certain temperature hydro-thermal reaction after a certain period of time, to
It is cooled to room temperature after carrying out eccentric cleaning, drying and obtains third group product；
(4) it disperses the third group product in step (3) in deionized water, a certain amount of SnCl is added dropwise after high-speed stirred4
It is stood after solution stirring and obtains the 4th group of product；
(5) the 4th group of product in step (4) is collected by centrifugation, dries, anneals in nitrogen atmosphere.
2. a kind of rGO/MoS according to claim 12/SnO2The preparation method of composite air-sensitive material, it is characterised in that:
In step (1), the amount of the graphene is 10~30mg, and the amount of the deionized water is 20~40ml, and the mixing time is
20~40min, ultrasonic time are 5~15min.
3. a kind of rGO/MoS according to claim 12/SnO2The preparation method of composite air-sensitive material, it is characterised in that:
In step (2), the content of the ammonium molybdate is 0.2~1mmol, and the content of thiocarbamide is 10~15mmol.
4. a kind of rGO/MoS according to claim 12/SnO2The preparation method of composite air-sensitive material, it is characterised in that:
In step (3), the hydro-thermal reaction is that second group of product is placed in pressurization in reaction kettle and heats up and continues stirring to make second group of production
Object inner material is reacted.
5. a kind of rGO/MoS according to claim 42/SnO2The preparation method of composite air-sensitive material, it is characterised in that: institute
State hydro-thermal reaction temperature be 150~200 DEG C, the drying time be 10~for 24 hours, the centrifugation rate be 8500~
10000rpm, centrifugation time are 5~15min.
6. a kind of rGO/MoS according to claim 12/SnO2The preparation method of composite air-sensitive material, it is characterised in that:
In step (4), the content of the deionized water is 20~40ml, and the time of the high-speed stirred is 15~30min, described certain
Measure SnCl4Solution is 2mL, the SnCl of 0.01M4Solution.
7. a kind of rGO/MoS according to claim 12/SnO2The preparation method of composite air-sensitive material, it is characterised in that:
In step (5), the annealing is to keep constant temperature after being gradually heated to annealing temperature in nitrogen atmosphere with certain heating rate
10h。
8. a kind of rGO/MoS according to claim 72/SnO2The preparation method of composite air-sensitive material, it is characterised in that: institute
Stating annealing temperature is 180~220 DEG C, and the heating rate is 5 DEG C/min.
9. a kind of rGO/MoS according to claim 12/SnO2The preparation method of composite air-sensitive material, it is characterised in that: institute
State rGO/MoS2/SnO2Composite air-sensitive material is used for sensor material, photochemical catalyst.
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Cited By (4)
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| CN113354298A (en) * | 2021-06-02 | 2021-09-07 | 桂林电子科技大学 | SnO (stannic oxide)2/MoS2Two-dimensional macroporous composite material film, preparation method and application thereof |
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| CN113354298A (en) * | 2021-06-02 | 2021-09-07 | 桂林电子科技大学 | SnO (stannic oxide)2/MoS2Two-dimensional macroporous composite material film, preparation method and application thereof |
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| CN116124850A (en) * | 2023-04-17 | 2023-05-16 | 北京深谋科技有限公司 | Preparation method and application of electrode composite material |
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