CN108545777A - A kind of molybdenum disulfide/indium oxide quaternary gas sensitive and preparation method thereof of antimony-cerium modification - Google Patents
A kind of molybdenum disulfide/indium oxide quaternary gas sensitive and preparation method thereof of antimony-cerium modification Download PDFInfo
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- CN108545777A CN108545777A CN201810480682.9A CN201810480682A CN108545777A CN 108545777 A CN108545777 A CN 108545777A CN 201810480682 A CN201810480682 A CN 201810480682A CN 108545777 A CN108545777 A CN 108545777A
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Abstract
The present invention relates to a kind of antimony ceriums to modify molybdenum disulfide/indium oxide gas sensitive and preparation method thereof, belongs to sensor gas sensitive preparation field.The gas sensitive is made of antimony element, Ce elements, molybdenum disulfide, indium oxide, and indium oxide particles are attached to molybdenum disulfide sheet surfaces and constitute MoS2/In2O3Nano complex, antimony and cerium atom are located at MoS2/In2O3In the lattice of nano complex；Include described in the preparation（1）Hydro-thermal method synthesizes MoS2/In2O3Nanocomposite；（2）Under protective atmosphere, by antimony source, cerium source and MoS2/In2O3Nanocomposite hydro-thermal reaction, centrifugation, drying, calcining to get.The present invention effectively reduces the activation energy of the chemisorption of tested gas by the introducing of antimony, cerium, substantially increase the specific surface area and electric conductivity of indium oxide Semiconductor gas sensors material, the electric charge transfer for enhancing gas molecule and storeroom has obtained having excellent gas sensitive.
Description
Technical field
The invention belongs to the preparing technical fields of sensor gas sensitive, and in particular to a kind of curing of antimony-cerium modification
Molybdenum/indium oxide quaternary gas sensitive and preparation method thereof.
Background technology
With the rapid development of economy, urbanization trend is constantly reinforced, some poisonous and harmful, inflammable and explosive gases are direct
It is discharged into air, not only pollutes ecological environment and living environment, but also great damage can be brought to the physical and mental health of people
Evil.Find the research that a kind of monitoring of high sensitivity, analysis and the gas sensor of alarm material are air-sensitive monitoring fields
Hot spot.Long ago, people find that with Metal Oxide Semiconductor Gas Sensing sensor made of the materials such as zinc oxide, tin oxide
It is with a wide range of applications and researching value.
However, there is also the drawbacks such as operating temperature height, poor selectivity for the air-sensitive technology based on these semiconductors, influence
With constrain their applications in the industry.Then, people begin look for the air-sensitive prison that new method improves conductor oxidate
Performance is surveyed, preferable second phase of electric conductivity is for example introduced in the material, can not only increase the specific surface area of semi-conducting material, together
When can enhance the electric charge transfer of gas molecule and storeroom, improve material electric conductivity (see reference document J.Li, K.Yu,
Y.Tan,et al.Dalton Transactions,2014,43(34):13136.)。
Two-dimension nano materials, such as graphene, MoS2(molybdenum disulfide) nano material etc. is with excellent physics and chemically
Can, it is wide in energy storage, Laser Modulation, fluorescence, catalysis, machinery etc. application, in the research heat as material circle interior in recent years
Point.But graphene is oxidized easily under air atmosphere high temperature, limits the performance and application of its performance to a certain extent
(see reference document Z.Min, L.X.Wen, X.Yi, Nano Today, 2013,8 (6):598.).And class graphene-structured curing
Molybdenum (MoS2) nano material not only has good electric conductivity, but also has in air atmosphere at high temperature and stablize well
Property.Therefore, it is extremely urgent to find a kind of high performance class graphene molybdenum disulfide/metal oxide nano composite material.
Invention content
For the above-mentioned prior art the problem of, the present invention is intended to provide a kind of molybdenum disulfide/oxygen of antimony-cerium modification
Change indium quaternary gas sensitive (Sb/Ce-MoS2/In2O3) and preparation method thereof.The present invention by with Sb and Ce elements to MoS2/
In2O3The modification of nano complex makes Sb and Ce enter MoS2/In2O3In lattice inside nano complex, the air-sensitive prepared
Material high sensitivity, stability are good, and air-sensitive performance is good.
An object of the present invention is to provide a kind of molybdenum disulfide/indium oxide quaternary gas sensitive of antimony-cerium modification.
The second object of the present invention is to provide a kind of system of molybdenum disulfide/indium oxide quaternary gas sensitive of antimony-cerium modification
Preparation Method.
The third object of the present invention is to provide a kind of biography of molybdenum disulfide/indium oxide quaternary gas sensitive of antimony-cerium modification
Sensor.
The fourth object of the present invention is to provide molybdenum disulfide/indium oxide quaternary gas sensitive and its preparation of antimony-cerium modification
The application of the sensor of molybdenum disulfide/indium oxide quaternary gas sensitive of method, antimony-cerium modification.
For achieving the above object, specifically, the invention discloses following technical proposals：
First, the invention discloses a kind of molybdenum disulfide/indium oxide quaternary gas sensitive of antimony-cerium modification, the air-sensitives
Material is made of antimony element, Ce elements, molybdenum disulfide, indium oxide, wherein indium oxide particles are attached to molybdenum disulfide sheet surfaces
Constitute MoS2/In2O3Nano complex, antimony and cerium atom are located at MoS2/In2O3In the lattice of nano complex, the MoS2：
In2O3Molar ratio be 1:The molar content of 2-4, antimony and cerium is In2O30.1%-5%.
Secondly, the invention discloses a kind of preparation sides of molybdenum disulfide/indium oxide quaternary gas sensitive of antimony-cerium modification
Method includes the following steps：
(1) hydro-thermal method synthesizes MoS2/In2O3Nano complex；
(2) under protective atmosphere, by antimony source, cerium source and the MoS in step (1)2/In2O3It is carried out after nano complex mixing
Hydro-thermal reaction dries product after centrifugation, spare；
(3) will it is dry in step (2) after product calcine to get.
In step (1), the hydrothermal synthesis MoS2/In2O3Nano complex be specially：1) hydro-thermal method prepares MoS2, make
For In2O3Carrier；2) by MoS2Carrier and In2O3Mixing, by hydro-thermal method by In2O3Nano particle is distributed to MoS2Lamella table
Face to get；The MoS2：In2O3Molar ratio be 1:2-4, preferably 1:3.
In step (2), the protective atmosphere includes argon gas, nitrogen.
In step (2), the antimony source includes that either the Antimony pentachloride cerium source includes cerous nitrate or hydrogen-oxygen to antimony trichloride
Change cerium.
In step (2), the antimony source, cerium source addition are：Sb:Ce:In2O3Molar ratio is (0.01-0.05):(0.01-
0.05):(1-10), wherein Sb:The content of Ce is identical always, i.e. the molar content of Sb and Ce are In2O30.1%-5%.
In step (2), the temperature that the hydro-thermal closes reaction is 180-240 DEG C, time 16-24h.
In step (3), the temperature of the calcining is 300-600 DEG C, reaction time 1-8h.
Again, the invention discloses a kind of sensors, and the gas sensitive of the sensor is that antimony-cerium prepared by the present invention is repaiied
The molybdenum disulfide of decorations/indium oxide quaternary gas sensitive.
Molybdenum disulfide/indium oxide quaternary gas sensitive finally, modified the invention discloses antimony-cerium and preparation method thereof,
Sensor the answering in environmental monitoring monitoring, analysis and alarm of molybdenum disulfide/indium oxide quaternary gas sensitive of antimony-cerium modification
With.
Compared with prior art, the advantageous effect that the present invention obtains is：The In of three-dimensional structure2O3With high-specific surface area and
The characteristics of macroporosity, can greatly improve the contact area with detection gas, ensure that sensor has good sensitivity, height
Stability, highly selective, the present invention is using molybdenum disulfide as carrier, In2O3Nano particle is distributed to MoS2Sheet surfaces are formed
MoS2/In2O3Nano complex increases substantially the specific surface area and electric conductivity of indium oxide Semiconductor gas sensors material, then uses Sb
With Ce elements to MoS2/In2O3Nano complex is modified, and Sb and Ce is made to enter MoS2/In2O3Crystalline substance inside nano complex
In lattice, Sb and Ce elements enter in lattice the activation energy for the chemisorption that can effectively reduce tested gas, greatly improve gas
The electric charge transfer of molecule and storeroom promotes sensitivity and the stability of material, to acquisition with excellent sensitivity and surely
Qualitative Sb/Ce-MoS2/In2O3Gas sensitive.
Description of the drawings
The accompanying drawings which form a part of this application are used for providing further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation do not constitute the improper restriction to the application for explaining the application.
Fig. 1 is Sb/Ce-MoS prepared by embodiment 12/In2O3The SEM figures (figure a) and TEM figures (figure b) of quick material.
Fig. 2 is Sb/Ce-MoS prepared by embodiment 12/In2O3Alcohol gas sensitivity response of the gas sensitive to 50ppm
With the relational graph of temperature.
Fig. 3 is Sb/Ce-MoS prepared by embodiment 12/In2O3Gas sensitive is in 260 DEG C of optimum temperature to gas with various
Air-sensitive detection performance figure.
Specific implementation mode
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, there is all technical and scientific terms used herein the logical technical staff with the application technical field usually to manage
The identical meanings of solution.
It should be noted that term used herein above is merely to describe specific implementation mode, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or combination thereof.
As background technology is introduced, existing sensor still has that operating temperature is high, sensitivity is low, stability
The problems such as low, poor selectivity, therefore, the present invention, propose a kind of molybdenum disulfide/indium oxide quaternary gas sensitive of antimony-cerium modification
(Sb/Ce-MoS2/In2O3) and preparation method thereof, the present invention will be further described with reference to the accompanying drawings and detailed description.
It should be noted that：Hydro-thermal method prepares MoS2For ordinary skill in the art means, to make help technology of the present invention
Personnel clearly understand the present invention, now provide a kind of specific hydro-thermal preparation MoS2Method.
The hydro-thermal method prepares MoS2For：By sodium molybdate, thiocarbamide, citric acid formation mixed liquor soluble in water, then will mix
Close liquid carry out hydro-thermal reaction to get.
Preferably, the hydro-thermal method prepares MoS2For：Sodium molybdate, thiocarbamide, citric acid, water are pressed into 1mmol：4mmol：
1mmol：30-50ml is dissolved in a milliliter water, and hydro-thermal reaction 18-24h is to get MoS at 180-200 DEG C2。
Embodiment 1
A kind of preparation method of antimony-cerium modification molybdenum disulfide/indium oxide gas sensitive, includes the following steps：
(1) hydro-thermal method synthesizes MoS2/In2O3Nanocomposite：1) by 1mmol sodium molybdates, 4mmol thiocarbamides, 1mmol lemons
Lemon acid is dissolved in 50 milliliters of water, and hydro-thermal reaction 21h is to get MoS at 200 DEG C2, as In2O3Carrier；2) by 1mmolMoS2It carries
Body and 3mmol In2O3Mixing, by In under 180 DEG C, 18 hours hydrothermal conditions2O3Nano particle is distributed to MoS2Lamella table
Face to get；
(2) under argon atmosphere, using 0.06mmol antimony trichlorides, 0.06mmol cerous nitrates as antimony source, cerium
MoS in source, with step (1)2/In2O3(antimony source and cerium source addition are for nanocomposite mixing：Sb：Ce：In2O3Mole
Than being 0.01:0.01：1), the hydro-thermal reaction 16h at 180 DEG C is then centrifuged for, is dried to product, spare；
(3) product after will be dry in step (2) calcined in 300 DEG C of argon gas atmosphere 3h to get.
Embodiment 2
A kind of preparation method of antimony-cerium modification molybdenum disulfide/indium oxide gas sensitive, includes the following steps：
(1) hydro-thermal method synthesizes MoS2/In2O3Nanocomposite：1) by 2mmol sodium molybdates, 8mmol thiocarbamides, 2mmol lemons
Lemon acid is dissolved in 50 milliliters of water, and hydro-thermal reaction 18h is to get MoS at 200 DEG C2, as In2O3Carrier；2) by 2mmolMoS2It carries
Body and 4mmol In2O3Mixing, by hydro-thermal method by In2O3Nano particle is distributed to MoS2Sheet surfaces to get；
(2) under argon atmosphere, using 0.02mmol antimony trichlorides, 0.02mmol cerous nitrates as antimony source, cerium
MoS in source, with step (1)2/In2O3(antimony source and cerium source addition are for nanocomposite mixing：Sb：Ce：In2O3Mole
Than being 0.01:0.01：10), hydro-thermal reaction for 24 hours, is then centrifuged for, is dried to product at 240 DEG C, spare；
(3) product after will be dry in step (2) calcined in 600 DEG C of argon gas atmosphere 8h to get.
Embodiment 3
A kind of preparation method of antimony-cerium modification molybdenum disulfide/indium oxide gas sensitive, includes the following steps：
(1) hydro-thermal method synthesizes MoS2/In2O3Nanocomposite：1) by 1mmol sodium molybdates, 4mmol thiocarbamides, 1mmol lemons
Lemon acid is dissolved in 30 milliliters of water, and hydro-thermal reaction is for 24 hours to get MoS at 180 DEG C2, as In2O3Carrier；2) by 2mmolMoS2It carries
Body and 8mmol In2O3Mixing, by hydro-thermal method by In2O3Nano particle is distributed to MoS2Sheet surfaces to get；
(2) under argon atmosphere, using 0.05mmol antimony trichlorides, 0.05mmol cerous nitrates as antimony source, cerium
MoS in source, with step (1)2/In2O3(antimony source and cerium source addition are for nanocomposite mixing：Sb：Ce：In2O3Mole
Than being 0.05:0.05：1), the hydro-thermal reaction 20h at 200 DEG C is then centrifuged for, is dried to product, spare；
(3) product after will be dry in step (2) calcined in 500 DEG C of argon gas atmosphere 5h to get.
Embodiment 4
A kind of preparation method of antimony-cerium modification molybdenum disulfide/indium oxide gas sensitive, includes the following steps：
(1) hydro-thermal method synthesizes MoS2/In2O3Nanocomposite：1) by 1mmol sodium molybdates, 4mmol thiocarbamides, 1mmol lemons
Lemon acid is dissolved in 40 milliliters of water, and hydro-thermal reaction 20h is to get MoS at 180 DEG C2, as In2O3Carrier；2) by 5mmolMoS2It carries
Body and 15mmol In2O3Mixing, by hydro-thermal method by In2O3Nano particle is distributed to MoS2Sheet surfaces to get；
(2) under argon atmosphere, using 0.05mmol antimony trichlorides, 0.05mmol cerous nitrates as antimony source, cerium
MoS in source, with step (1)2/In2O3(antimony source and cerium source addition are for nanocomposite mixing：Sb：Ce：In2O3Mole
Than being 0.05:0.05：10), the hydro-thermal reaction 18h at 200 DEG C is then centrifuged for, is dried to product, spare；
(3) product after will be dry in step (2) calcined in 400 DEG C of argon gas atmosphere 6h to get.
Embodiment 5
A kind of preparation method of antimony-cerium modification molybdenum disulfide/indium oxide gas sensitive, includes the following steps：
(1) hydro-thermal method synthesizes MoS2/In2O3Nanocomposite：1) by 1mmol sodium molybdates, 4mmol thiocarbamides, 1mmol lemons
Lemon acid is dissolved in 50 milliliters of water, and hydro-thermal reaction 21h is to get MoS at 180 DEG C2, as In2O3Carrier；2) by 6mmolMoS2It carries
Body and 18mmol In2O3Mixing, by hydro-thermal method by In2O3Nano particle is distributed to MoS2Sheet surfaces to get；
(2) under argon atmosphere, using 0.08mmol antimony trichlorides, 0.08mmol cerous nitrates as antimony source, cerium
MoS in source, with step (1)2/In2O3(antimony source and cerium source addition are for nanocomposite mixing：Sb：Ce：In2O3Mole
Than being 0.04:0.04：5), the hydro-thermal reaction 16h at 220 DEG C is then centrifuged for, is dried to product, spare；
(3) product after will be dry in step (2) calcined in 550 DEG C of argon gas atmosphere 1h to get.
Performance test：
Fig. 2 is Sb/Ce-MoS prepared by embodiment 12/In2O3Gas sensitive is to alcohol gas sensitivity response and temperature
Relational graph.It can be seen from the figure that within the temperature range of 180 DEG C -320 DEG C, Sb/Ce-MoS prepared by the present invention2/In2O3Gas
Quick material maintains good air-sensitive performance to alcohol gas, it can be seen that the detection temperature of gas sensitive prepared by the present invention
Window is wide, low temperature performance well.
Fig. 3 is Sb/Ce-MoS prepared by embodiment 12/In2O3Gas sensitive is in 260 DEG C of optimum temperature to gas with various
Air-sensitive detection performance figure.It can be seen from the figure that ethyl alcohol, ammonium hydroxide, acetone, four kinds of gas of benzene detection in, the present invention
The Sb/Ce-MoS of preparation2/In2O3Gas sensitive has highest responsiveness (64.2) to alcohol gas, illustrates material to ethyl alcohol
Gas has excellent selectivity and sensitivity.
The foregoing is merely the preferred embodiments of the application, are not intended to limit this application, for those skilled in the art
For member, the application can have various modifications and variations.Any modification made by within the spirit and principles of this application,
Equivalent replacement, improvement etc., should be included within the protection domain of the application.
Claims (10)
1. a kind of antimony-cerium modifies molybdenum disulfide/indium oxide gas sensitive, it is characterised in that：The gas sensitive is by antimony element, cerium
Element, molybdenum disulfide, indium oxide are constituted, wherein indium oxide particles are attached to molybdenum disulfide sheet surfaces and constitute MoS2/In2O3
Nano complex, antimony and cerium atom are located at MoS2/In2O3In the lattice of nano complex, the MoS2：In2O3Molar ratio be
1:The molar content of 2-4, antimony and cerium is In2O30.1%-5%.
2. a kind of preparation method of antimony-cerium modification molybdenum disulfide/indium oxide gas sensitive, it is characterised in that：Include the following steps：
(1) hydro-thermal method synthesizes MoS2/In2O3Nanocomposite；
(2) under protective atmosphere, by the MoS in antimony-cerium source and step (1)2/In2O3Hydro-thermal is carried out after nanocomposite mixing
Reaction so dries product after centrifugation, spare；
(3) will it is dry in step (2) after product calcine to get.
3. the preparation method of antimony as claimed in claim 2-cerium modification molybdenum disulfide/indium oxide gas sensitive, it is characterised in that：
In step (1), the hydrothermal synthesis MoS2/In2O3Nanocomposite be specially：1) hydro-thermal method prepares MoS2, as In2O3
Carrier；2) by MoS2Carrier and In2O3In molar ratio 1：2-4 is mixed, by hydro-thermal method by In2O3Nano particle is distributed to MoS2
Sheet surfaces to get；Preferably, MoS2Carrier and In2O3Molar ratio be 1：3.
4. the preparation method of antimony as claimed in claim 2-cerium modification molybdenum disulfide/indium oxide gas sensitive, it is characterised in that：
The hydro-thermal method prepares MoS2For：By sodium molybdate, thiocarbamide, then citric acid formation mixed liquor soluble in water carries out mixed liquor
Hydro-thermal reaction to get；
It is further preferred that the hydro-thermal method prepares MoS2For：Sodium molybdate, thiocarbamide, citric acid, water are pressed into 1mmol：4mmol：
1mmol：30-50ml is dissolved in a milliliter water, and hydro-thermal reaction 18-24h is to get MoS at 180-200 DEG C2。
5. the preparation method of antimony as claimed in claim 2-cerium modification molybdenum disulfide/indium oxide gas sensitive, it is characterised in that：
In step (2), the protective atmosphere includes argon gas, nitrogen or ammonia；Preferably, the antimony source includes antimony trichloride, the cerium
Source includes cerous nitrate.
6. the preparation method of antimony as claimed in claim 2-cerium modification molybdenum disulfide/indium oxide gas sensitive, it is characterised in that：
In step (2), the antimony cerium, cerium source addition be：Sb:Ce:In2O3Molar ratio be (0.01-0.05):(0.01-
0.05):(1-10), and Sb:The content of Ce is identical always.
7. the preparation method of antimony as claimed in claim 2-cerium modification molybdenum disulfide/indium oxide gas sensitive, it is characterised in that：
In step (2), the temperature that the hydro-thermal closes reaction is 180-240 DEG C, is 16-24h.
8. the preparation method of antimony as claimed in claim 2-cerium modification molybdenum disulfide/indium oxide gas sensitive, it is characterised in that：
In step (3), the temperature of the calcining is 300-600 DEG C, reaction time 1-8h.
9. a kind of sensor, it is characterised in that：The gas sensitive of the sensor is antimony as described in claim 1-cerium modification
Molybdenum disulfide/indium oxide quaternary gas sensitive or the gas sensitive of the sensor be any one of such as claim 2-8 institutes
Molybdenum disulfide/indium oxide quaternary gas sensitive of antimony prepared by the method stated-cerium modification.
10. molybdenum disulfide/indium oxide quaternary the gas sensitive and/or such as claim of antimony as described in claim 1-cerium modification
2-8 any one of them preparation method and/or sensor as claimed in claim 9 monitor, in environmental monitoring in analysis and alarm
Application.
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| CN113125521B (en) * | 2021-04-26 | 2022-05-27 | 中国石油大学(华东) | Preparation method of molybdenum disulfide/cerium oxide composite gas-sensitive structure and application of molybdenum disulfide/cerium oxide composite gas-sensitive structure in gas-sensitive coating, element and sensor |
| CN114768530A (en) * | 2022-04-29 | 2022-07-22 | 中国工程物理研究院材料研究所 | Application of molybdenum disulfide in hydrogen isotope electrolytic separation |
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