CN111994954A - MoO (MoO)3Gas-sensitive material and preparation method and application thereof - Google Patents

MoO (MoO)3Gas-sensitive material and preparation method and application thereof Download PDF

Info

Publication number
CN111994954A
CN111994954A CN202010843648.0A CN202010843648A CN111994954A CN 111994954 A CN111994954 A CN 111994954A CN 202010843648 A CN202010843648 A CN 202010843648A CN 111994954 A CN111994954 A CN 111994954A
Authority
CN
China
Prior art keywords
moo
solution
gas
ethanol
sensitive material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202010843648.0A
Other languages
Chinese (zh)
Inventor
梁士明
惠晓雨
宋学省
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Linyi University
Original Assignee
Linyi University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Linyi University filed Critical Linyi University
Priority to CN202010843648.0A priority Critical patent/CN111994954A/en
Publication of CN111994954A publication Critical patent/CN111994954A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/02—Oxides; Hydroxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
    • G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
    • G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer

Abstract

The invention discloses a MoO3A method of preparing a gas sensitive material, comprising: 1) adding a proper amount of Na2MoO4·2H2Dissolving O in deionized water to obtain a solution A; 2) adding a proper amount of EDTA powder into the solution A, and uniformly stirring and dissolving to obtain a solution B; 3) adding a hydrochloric acid solution into the solution B to obtain a solution C; 4) placing the solution C in a reaction kettle, sealing, reacting in an oven at 150 ℃ for 5.5h, and cooling at room temperature for 15h after the reaction is finished; 6) standing after complete cooling, removing supernatant, centrifuging the suspension and collecting precipitate; 7) and (4) putting the precipitate into an oven, and drying for 24h at 95 ℃ to obtain the product. The invention also provides MoO prepared by the method3Gas sensitive material and its application. MoO prepared by the invention3The (R) nano rod is an orthorhombic system, and the product has high purity and good crystallization propertyAt 310 ℃ ethanol was still detectable at low concentrations (5 ppm).

Description

MoO (MoO)3Gas-sensitive material and preparation method and application thereof
The technical field is as follows:
the invention relates to the technical field of nano materials, in particular to a MoO3A gas sensitive material, a preparation method and application thereof.
Background art:
molybdenum trioxide is an indispensable transition metal oxide because of its high thermal stability and abundanceThe rich valence state and the better chemical stability are closely concerned by people. The band gap of the molybdenum trioxide is wide, and the width of the molybdenum trioxide can reach 2.8-3.2 eV. The MoO has larger specific surface area, better gas-sensitive performance and electrical performance and the like3Gas sensitive materials are widely used in various industrial fields such as sensors, display devices, and battery electrodes.
MoO3The nano material is closely concerned by researchers due to the special superiority of the nano material. At present, a solid phase method, a hydrothermal method and the like can be used for preparing the nano MoO3However, these methods are still in the basic experimental exploration stage, and the preparation process is not yet mature. But with the continuously expanded application range, MoO3The preparation of the material is bound to develop towards the direction of low cost, high efficiency and simpler process[17]。
Arachchige et al in molybdenum trioxide (MoO)3) The powder is used as a raw material, molybdenum trioxide nanosheets with orthogonal structures are prepared by an evaporation-condensation method, and gas-sensitive detection is carried out on the molybdenum trioxide nanosheets. The results show that: MoO functionalized with gold3Nanoparticles to H at 400 deg.C2Gas sensitive response ratio of S pure MoO3Is 10 times higher. Yang et al prepare ultra-long MoO by hydrothermal method3Nanobelts and tested for Trimethylamine (TMA) response at an optimum sensitivity operating temperature of 240 c, while testing for selectivity to various reducing gases. The result shows that the sensor has better response to TMA compared with other gases, and the sensor has good application prospect in TMA detection.
In order to solve the problems of low sensitivity detection and the like caused by single structure of the gas sensitive material, scientists find that the gas sensitive property can be effectively improved by carrying out heterojunction structure with other gas sensitive materials. Such as Jiang, etc. by simple solvothermal method to prepare Ni doped with different concentrations2+Of MoO3The gas sensitive material and the microstructure and the appearance of the prepared sample are characterized, and the result shows that the gas sensitive material is prepared by adjusting Ni2+Can change its morphology. Meanwhile, the gas-sensitive performance detection is carried out on the composite material, and experiments show that: the response value of the sensor to the xylene is improved from 3.48 to 62.6The response time was about 1s and selectivity was best at 250 ℃, these breakthroughs were due to the increase of surface active sites and Ni2+Improvement of the micro-morphology caused by doping.
Li and the like adopt an in-situ diffusion method to realize CoMoO4Nanoparticles in MoO3In-situ diffusion growth of the surface of the nanobelt and characterization thereof confirmed that the CoMoO was present4The nano particles are uniformly distributed in the MoO3A nanoribbon surface. Original MoO was studied using a static test system3And CoMoO4/MoO3Trimethylamine sensing performance of the nanocomposite. The experimental result shows that CoMoO4/MoO3The nanocomposite responded 104.8 to 100ppm triethylamine at 220 ℃ and was pure MoO 34 times at 280 ℃. Indicating CoMoO4/MoO3The heterojunction structure of the nano composite material has great improvement effect on the gas-sensitive property of the nano composite material.
The invention content is as follows:
according to the invention, MoO with different morphologies is synthesized by a hydrothermal method, simultaneously controlling experiment conditions under mild conditions and using different surfactants3Powder; respectively carrying out appearance characterization on the nano microstructure by an X-ray and a transmission electron microscope, and analyzing the nano microstructure; and finally, detecting the gas-sensitive performance of the gas-sensitive material, and analyzing and exploring the gas-sensitive sensing material with higher performance.
In order to achieve the purpose, the invention provides the following technical scheme:
MoO (MoO)3A method of preparing a gas sensitive material, comprising:
1) adding a proper amount of Na2MoO4·2H2Dissolving O in deionized water to obtain a solution A;
2) adding a proper amount of EDTA powder into the solution A, and stirring and dissolving uniformly to obtain a solution B;
3) adding a hydrochloric acid solution into the solution B under a stirring state, and obtaining a solution C after the solution is transparent;
4) placing the solution C in a reaction kettle, sealing the reaction kettle, placing the reaction kettle in an oven, reacting for 5.5h at 150 ℃, and cooling for 15h at room temperature after the reaction is finished;
6) standing in a container after complete cooling, removing supernatant, centrifuging the suspension and collecting precipitate;
7) putting the precipitate in an oven, and drying at 95 ℃ for 24h to obtain MoO3And (3) nano powder.
In one embodiment according to the invention, in step 1) the
Na2MoO4·2H2O is in powder form, Na2MoO4·2H2The concentration of O dissolved in deionized water is 0.1-1 mmol/ml.
In one embodiment according to the invention, EDTA is mixed with Na2MoO4·2H2The mass ratio of O is 1-10: 40.
In one embodiment according to the invention, the hydrochloric acid is reacted with Na2MoO4·2H2The molar ratio of O is 2: 1.
the invention also provides MoO prepared according to the preparation method3A gas sensitive material.
The invention further provides the MoO3The application of the gas sensitive material in preparing a gas sensor.
The MoO provided by the invention3The gas sensitive material has the following beneficial effects:
1) MoO prepared by the invention3The (R) nano rod is an orthorhombic system, the lens appearance graph presents a nano rod shape, the appearance is complete, the dispersity is good, the product purity is high, and the crystallization performance is good.
2) MoO prepared by the invention3The optimum sensitive working temperature of the nano material for detecting the ethanol with the concentration of 100ppm is 310 ℃, the maximum sensitivity response value is 30, and the ethanol with low concentration (5ppm) can still be detected at 310 ℃.
Description of the drawings:
FIG. 1 is MoO3X-ray diffraction patterns of (a);
FIG. 2a is MoO3(R) transmission electron microscopy pictures;
FIG. 2b is MoO3(P) transmission electron microscopy pictures;
FIG. 3 is MoO3(R) at different temperatures for 100ppSensitivity histogram of mEtOH
FIG. 4 shows MoO3(R) and MoO3(P) sensitivity to different concentrations (10-1000ppm) of ethanol at 310 ℃;
FIG. 5 shows MoO3(R) and MoO3(P) sensitivity to low concentrations (5, 10, 50ppm) of ethanol at 310 ℃;
FIG. 6 shows MoO3(R) and MoO3(P) a sensitivity trend plot for different concentrations (10-1000ppm) of ethanol at 310 ℃;
FIG. 7 shows MoO3(R) and MoO3(P) sensitivity to different concentrations (10-1000ppm) of acetone at 310 ℃;
FIG. 8 shows MoO3(R) and MoO3(P) sensitivity trend plots for different concentrations (10-1000ppm) of acetone at 310 ℃;
FIG. 9 shows MoO3(R) and MoO3(P) sensitivity to 100ppm of different gases at 310 ℃.
The specific implementation mode is as follows:
the following detailed description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings, will make the advantages and features of the invention more readily understood by those skilled in the art, and thus will more clearly and distinctly define the scope of the invention.
Experimental reagent
The reagents used in this application are shown in table 1 unless otherwise stated.
TABLE 1 reagents required for the experiment
Figure BDA0002642311930000041
Main instrument
The main instruments used in this application are shown in table 2 unless otherwise stated.
TABLE 2 instruments required for the experiment
Figure BDA0002642311930000042
Example 1 MoO3Preparation of powder
A cylinder was used to measure 150mL of deionized water into a beaker, to which was added 3.63g (0.015mol) of Na under magnetic stirring2MoO4·2H2O powder, stirring for 5min to obtain solution A. 0.6g (about 0.002mol) of EDTA powder was weighed in and stirred to obtain solution B. 0.03mol (2.5mL) of concentrated hydrochloric acid is measured, and the solution is diluted by adding the solution into 20mL of deionized water and stirred to obtain solution C. And then adding the solution C into the solution B under a stirring state, and obtaining a solution D after the solution is transparent. Pouring the solution D into a liner of a reaction kettle, sealing the reaction kettle, placing the reaction kettle in an oven, and reacting for 5.5 hours at 150 ℃. After the reaction is finished, the reaction kettle is taken out and cooled for 15 hours at room temperature. After the mixture is completely cooled, the mixture is poured into a prepared beaker, the mixture is stood for a period of time, supernatant is poured out, and then the rest suspension is centrifuged to collect precipitate. Repeatedly washing with ultrapure water, washing with ethanol for 2-3 times, collecting the product, and drying in a 95 deg.C oven for 24 hr to obtain MoO3Nano powder with number marked as MoO3(R), and keeping for standby.
Comparative example 1
This comparative example uses Na2MoO4·2H2Preparing MoO with different morphologies under hydrothermal reaction at 150 ℃ by taking O as a molybdenum source, water as a solvent and water as a surfactant3The powder is prepared by the following specific operation process.
First, 150ml of deionized water was measured in a measuring cylinder into a beaker, to which 3.63g of Na was added under magnetic stirring2MoO4·2H2O powder, stirring for 15min, and adding 20ml deionized water to obtain solution A. 0.03mol (2.5mL) of concentrated hydrochloric acid is measured, and the solution is diluted by adding the solution into 20mL of deionized water and stirred to obtain solution B. Then adding the solution B into the solution A under the stirring state, and obtaining a transparent solution C. Pouring the solution C into a liner of a reaction kettle, sealing the reaction kettle, placing the reaction kettle in an oven, and reacting for 5.5 hours at 150 ℃. After the reaction is finished, the reaction kettle is taken out and cooled for 15 hours at room temperature. Pouring the mixture into a prepared beaker after the mixture is completely cooled, standing the mixture for a period of time, pouring out supernatant, and collecting the residual suspension by a centrifugal methodAnd (4) precipitating. Repeatedly washing with ultrapure water, washing with ethanol for 2-3 times, collecting the product, and drying in a 95 deg.C oven for 24 hr to obtain MoO3Nano powder with number marked as MoO3(P), and reserving for standby.
Example 2X-ray diffraction test
X-ray diffraction is a relatively common method of characterizing materials, and is commonly used to obtain the crystalline structure of a material. Different crystals have different internal structures and different X-ray scattering conditions, and different diffraction patterns can be obtained, so that diffraction results are analyzed, and the crystal structure of a product is obtained. The measured spectrum is shown in FIG. 1.
As can be seen from the XRD spectrum shown in figure 1, the powder prepared by the experiment is hexagonal phase molybdenum trioxide. Diffraction peaks in this spectrum occur at about 25.7, 29.1, 31.2, 33.8, 35.3, 41.5, 42.5, 45.0, 46.1, 49.2, 49.8, 52.0, 53.3, 56.2, 57.5, 58.0, 61.8, 66.4 and 68.5 ° 2 θ, respectively, corresponding to hexagonal phase MoO3The (210), (300), (204), (220), (310), (224), (320), (410), (404), (008), (500), (330), (420), (218), (334), (424), (430), (610) and (524) crystal planes of the standard card (JCPDS NO. 21-0569). The resulting (210) diffraction peak in FIG. 1 is stronger and sharper relative to the other peaks; by reaction with h-MoO3Comparing standard cards (JCPDS NO.21-0569), wherein all diffraction spectrum peaks measured by the experiment are completely consistent with the standard spectrum, and other miscellaneous peaks are not detected, which indicates that the prepared MoO3The powder is pure, other impurity elements are not introduced, and the crystallization performance of the product is good.
EXAMPLE 3 Transmission Electron microscopy Test (TEM)
The transmission electron microscope is mainly used for observing the fine morphology and the pore structure of a sample. The transmission electron microscope is used for accelerating and projecting a focused electron beam on a sample under high pressure, and after the focused electron beam penetrates through the sample, diffraction images with different light and shade can be formed on a complete crystal part and a defect part of the sample, so that the appearance information of the sample is reflected.
And (2) putting a small amount of powder to be detected into a sample tube, adding a little absolute ethyl alcohol into the sample tube by a dropper, performing ultrasonic treatment for more than 0.5h to disperse the sample to form a suspension state, then dropping a small amount of test solution on a copper mesh of a transmission electron microscope, adjusting the resolution of the transmission electron microscope, and observing and analyzing the appearance and the dispersion condition of the powder.
FIG. 2a is a MoO prepared with EDTA as surfactant and water as solvent3(R) the shape graph of the nano powder can show that the prepared molybdenum trioxide nano rod has complete shape, uniform size and good dispersibility through transmission electron microscope analysis of a sample, but the nano rod has a proper amount of bonding phenomenon. A large number of pore structures exist among the nanorods, and the specific surface area of a product is increased, so that the adsorption capacity of gas is increased, and the gas-sensitive performance of the gas-sensitive nanorod is improved.
FIG. 2b shows MoO prepared in water as solvent without surfactant3(P) a morphology of the nano powder, and transmission electron microscope analysis of a sample can find that the prepared molybdenum trioxide nano particles are in irregular shapes. It can be seen that the molybdenum trioxide without the surfactant is in the form of a granular block.
Example 4 MoO3Gas sensitivity of nano powder device
The invention is based on MoO3The sensitivity of the sensing element of (R) to 100ppm ethanol at different temperatures was investigated.
The component test was performed using a special instrument, model: WS-30A, manufacturer: zhengzhou Weisheng electronics technology Co Ltd
The preparation steps of the gas sensor are as follows:
step 1, inserting a metal resistance wire into a gas sensor ceramic tube, and assembling into a set of six contacts with three independent circuits. Welding the assembled element and the gas sensitive element base together by using an advanced welding table;
step 2, taking a proper amount of prepared MoO3Placing the powder in agate mortar, adding appropriate amount of ethanol, grinding for 30min counterclockwise, collecting pasty material, and adding MoO with clean brush pen for three times3The paste is uniformly coated on the outer surface of the gas-sensitive element ceramic tube, dried at room temperature and sealed for later use.
The results are shown in FIG. 3. From FIG. 3, it can be seen that MoO was observed in the temperature range of 190-310 deg.C3The sensitivity detection degree of the (R) nano-rod to 100ppm ethanol gradually rises, reaches the maximum value at 310 ℃, and MoO is carried out when the temperature continues to rise to 370 DEG C3The sensitivity of (R) nanorods to 100ppm ethanol gradually decreased. The results show that at 310 ℃ the MoO3The sensitivity detection degree of the (R) nano rod to 100ppm ethanol reaches the highest, and the maximum sensitivity Ra/RgA value of 30, and therefore MoO at 310 ℃3(R) optimum sensitive operating temperature of the nanomaterial.
After the optimal working temperature is determined, the invention continues to work on MoO3(R) and MoO3(P) sensitivity was studied at 310 ℃ for different concentrations (10-1000ppm) of ethanol gas. MoO at 310 ℃ as shown in FIG. 43(R) and MoO3(P) As the concentration of ethanol gas (10-1000ppm) is increased, the sensitivity is also greatly increased, and the sensitivity R is increased under the gas concentration of 1000ppma/RgThe value reaches the highest. Wherein, during the increasing of the concentration of the ethanol gas, the MoO3Sensitivity increase ratio MoO of (R) nanomaterial3The sensitivity of the (P) nano material is increased more remarkably, and the increase range in the ethanol concentration range of 500-1000ppm is more obvious. A more pronounced change in response was seen when the ethanol concentration was in the range of 100-1000 ppm. MoO3(R) R at ethanol concentrations of 100, 200, 500 and 1000ppma/RgValues 35, 45, 90 and 160, respectively; and MoO3(P) R at ethanol concentrations of 100, 200, 500 and 1000ppma/RgThe values are 18, 25, 50 and 100, respectively. The results show that the MoO basis is in the range of ethanol concentration of 100-3R of gas sensor of (R) for ethanola/RgAll values are higher than those based on MoO3R of gas sensor of (P) to ethanola/RgThe difference is more obvious with the increasing of the ethanol concentration.
FIG. 5 is an enlarged view of the low concentration range of 0-50ppm of ethanol gas, and it can be found that MoO is present at a low ethanol concentration3(R) and MoO3The change in the response value of (P) to ethanol is not very clear, but tends to be high. As is evident from the figure, MoO3(R) nanorods R corresponding to ethanol concentrations of 5, 10 and 50ppma/RgThe values are respectively 6, 9 and 20, and the change of the response value is obvious; and MoO3(P) R at ethanol concentrations of 5, 10 and 50ppma/RgThe values are 2, 3 and 7, respectively, and the response value changes less. The results show that in the ethanol concentration range from 0 to 50ppm, based on MoO3The response values of the sensors of (R) to ethanol are all higher than those based on MoO3(P) response value of sensor to ethanol, and MoO3(R) is MoO3The sensitivity increase tendency of (P) is more remarkable.
FIG. 6 shows MoO3(R) and MoO3(P) trend plot of sensitivity to different concentrations (10-1000ppm) of ethanol at 310 deg.C, MoO can be seen3(R) and MoO3(P) shows an ascending state for ethanol trend graphs of different concentrations, and MoO3(R) ratio MoO3The increase in (P) is more pronounced. Thus, MoO can be obtained3After the (R) nano-rod is added with the surfactant, the MoO is reduced3The agglomeration phenomenon of the powder and the rod-shaped structure further increase the specific surface area of the powder, increase the gas adsorption capacity, increase the reaction speed and greatly improve the gas-sensitive performance of the powder.
As shown in fig. 7, the present application is also directed to MoO3(R) and MoO3(P) acetone was detected with sensitivity at 310 ℃ at different concentrations (10-1000 ppm). It was found that at an optimum sensitive working temperature of 310 ℃, MoO3(R) and MoO3(P) R for acetone gases of different concentrations (10-1000ppm)a/RgThe values all show rising trend, which is similar to the sensitive detection trend graph of ethanol; and MoO3(R) sensitivity R to acetone concentrations of 100, 200, 500 and 1000ppma/RgValues of 10, 15, 30 and 60, MoO, respectively3(R) R for acetone concentrationa/RgValue ratio MoO3(P) R to acetone concentrationa/RgThe trend of the value is more obvious, and the phenomenon is the same as the change of the response value of the ethanol gas. The results show that the method has the advantages of high yield,MoO3(R) and MoO3(P) sensitive detection of acetone gas the tendency of the degree of change is similar to that of ethanol gas, but R for ethanol gasa/RgThe magnitude of the increase in value is more pronounced.
FIG. 8 shows MoO3(R) and MoO3(P) trend graph of sensitivity to different concentrations (10-1000ppm) of acetone at 310 ℃. As can be seen from FIG. 8, MoO3(P) R for acetone gases of different concentrationsa/RgThe variation curve of the value is relatively gentle, and MoO3(R) R for acetone gases of different concentrationsa/RgThe trend of the value change is obviously increased, which indicates that MoO3Sensitivity ratio of (R) to acetone gas MoO3(P) sensitivity to acetone gas Ra/RgThe value is good. Meanwhile, MoO can be seen by comparing the MoO with a sensitive detection change chart of ethanol with different concentrations3(R) and MoO3(P) R for ethanol gasa/RgValue ratio R to acetone gasa/RgThe value is good.
Example 5 MoO3Sensitivity detection of gas sensitive material to multiple organic gases
The application carries out sensitivity detection on various organic gases at the optimal working temperature of 310 ℃. FIG. 9 shows MoO3(R) and MoO3(P) sensitivity profile at 310 ℃ for 100ppm concentrations of ethanol, ethylene glycol, toluene, acetic acid, benzene, and acetone gases. It can be found that MoO3(R) and MoO3(P) has certain response to the six gases, but the response to ethanol is far higher than that of other gases, MoO3(R) R for ethanol gasa/RgValues of up to 30. The results show that MoO3(R) and MoO3(P) high selectivity to ethanol gas and MoO3(R) R for these gasesa/RgAll values are higher than MoO3(P) R for these gasesa/RgThe value is obtained. Thus indicating a MoO-based3The gas sensor of (R) has great potential in practical applications.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.

Claims (6)

1. MoO (MoO)3A method for preparing a gas sensitive material, comprising:
1) adding a proper amount of Na2MoO4·2H2Dissolving O in deionized water, and uniformly mixing to obtain a solution A;
2) adding a proper amount of EDTA (ethylene diamine tetraacetic acid) powder into the solution A, and stirring and dissolving uniformly to obtain a solution B;
3) adding a hydrochloric acid solution into the solution B under a stirring state, and obtaining a solution C after the solution is transparent;
4) placing the solution C in a reaction kettle, sealing the reaction kettle, placing the reaction kettle in an oven, reacting for 5.5h at 150 ℃, and cooling for 15h at room temperature after the reaction is finished;
6) standing in a container after complete cooling, removing supernatant, centrifuging the suspension and collecting precipitate;
7) putting the precipitate in an oven, and drying at 95 ℃ for 24h to obtain MoO3And (3) nano powder.
2. The method of claim 1, wherein in step 1), the step
Na2MoO4·2H2O is in powder form, Na2MoO4·2H2The concentration of O dissolved in deionized water is 0.1-1 mmol/ml.
3. The method of claim 1, wherein the EDTA and Na are present2MoO4·2H2The mass ratio of O is 1-10: 40.
4. The method of claim 1, wherein the hydrochloric acid is reacted with Na2MoO4·2H2The molar ratio of O is 2: 1.
5. MoO prepared according to the preparation method of any one of claims 1 to 43A gas sensitive material.
6. The MoO of claim 53The application of the gas sensitive material in preparing a gas sensor.
CN202010843648.0A 2020-08-20 2020-08-20 MoO (MoO)3Gas-sensitive material and preparation method and application thereof Pending CN111994954A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010843648.0A CN111994954A (en) 2020-08-20 2020-08-20 MoO (MoO)3Gas-sensitive material and preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010843648.0A CN111994954A (en) 2020-08-20 2020-08-20 MoO (MoO)3Gas-sensitive material and preparation method and application thereof

Publications (1)

Publication Number Publication Date
CN111994954A true CN111994954A (en) 2020-11-27

Family

ID=73473637

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010843648.0A Pending CN111994954A (en) 2020-08-20 2020-08-20 MoO (MoO)3Gas-sensitive material and preparation method and application thereof

Country Status (1)

Country Link
CN (1) CN111994954A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112730531A (en) * 2020-12-24 2021-04-30 宁波大学 Preparation method of hydrogen sulfide gas sensor based on molybdenum trioxide nanosheets
CN116046852A (en) * 2023-01-17 2023-05-02 云南民族大学 High-performance ethanol gas sensor of ZnO nanoparticle modified alpha-molybdenum trioxide heterojunction

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102139923A (en) * 2011-04-29 2011-08-03 西安工程大学 Method for preparing molybdenum trioxide material with orthorhombic phase single crystal nano belt structure
CN103771516A (en) * 2014-01-24 2014-05-07 天津理工大学 Preparation method of hexagonal-phase molybdenum trioxide microrod
CN105301061A (en) * 2015-09-23 2016-02-03 西南交通大学 Self-assembled latticed alpha-MoO3 nanoribbon gas-sensitive sensor
WO2017133616A1 (en) * 2016-02-01 2017-08-10 武汉清琪科技有限公司 Gas-sensitive component, gas-sensitive device and system
CN107337473A (en) * 2017-07-25 2017-11-10 济南大学 The growth in situ MoO on earthenware3The method and gas sensor of nanometer sheet
CN108950734A (en) * 2018-08-24 2018-12-07 济南大学 A kind of gully shape MoO3Synthetic method and products thereof
CN108996549A (en) * 2018-10-10 2018-12-14 金堆城钼业光明（山东）股份有限公司 A kind of MoO3The network structure nanometer material and preparation method thereof of piece assembling

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102139923A (en) * 2011-04-29 2011-08-03 西安工程大学 Method for preparing molybdenum trioxide material with orthorhombic phase single crystal nano belt structure
CN103771516A (en) * 2014-01-24 2014-05-07 天津理工大学 Preparation method of hexagonal-phase molybdenum trioxide microrod
CN105301061A (en) * 2015-09-23 2016-02-03 西南交通大学 Self-assembled latticed alpha-MoO3 nanoribbon gas-sensitive sensor
WO2017133616A1 (en) * 2016-02-01 2017-08-10 武汉清琪科技有限公司 Gas-sensitive component, gas-sensitive device and system
CN107337473A (en) * 2017-07-25 2017-11-10 济南大学 The growth in situ MoO on earthenware3The method and gas sensor of nanometer sheet
CN108950734A (en) * 2018-08-24 2018-12-07 济南大学 A kind of gully shape MoO3Synthetic method and products thereof
CN108996549A (en) * 2018-10-10 2018-12-14 金堆城钼业光明（山东）股份有限公司 A kind of MoO3The network structure nanometer material and preparation method thereof of piece assembling

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
苟中平: "纳米MoO3的水热合成及气敏性能研究", 《中国优秀硕士学位论文全文数据库》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112730531A (en) * 2020-12-24 2021-04-30 宁波大学 Preparation method of hydrogen sulfide gas sensor based on molybdenum trioxide nanosheets
CN112730531B (en) * 2020-12-24 2022-11-04 宁波大学 Preparation method of hydrogen sulfide gas sensor based on molybdenum trioxide nanosheets
CN116046852A (en) * 2023-01-17 2023-05-02 云南民族大学 High-performance ethanol gas sensor of ZnO nanoparticle modified alpha-molybdenum trioxide heterojunction

Similar Documents

Publication Publication Date Title
Wang et al. Synthesis and gas sensitivities of SnO2 nanorods and hollow microspheres
Wang et al. Horseshoe-shaped SnO2 with annulus-like mesoporous for ethanol gas sensing application
Wang et al. Hierarchical flower-like WO3 nanostructures and their gas sensing properties
Wu et al. Construction of MoS2/Si nanowire array heterojunction for ultrahigh-sensitivity gas sensor
Hao et al. Controllable synthesis and enhanced gas sensing properties of a single-crystalline WO 3–rGO porous nanocomposite
CN102275981B (en) Preparation method of self-substrate SnO2 nanorod array
Jin et al. Synthesis of hierarchical SnO2 nanoflowers with enhanced acetic acid gas sensing properties
Li et al. Ionic liquid-assisted synthesis of WO 3 particles with enhanced gas sensing properties
CN111994954A (en) MoO (MoO)3Gas-sensitive material and preparation method and application thereof
Liu et al. Fabrication and CO sensing properties of mesostructured ZnO gas sensors
Zeng et al. Hydrothermal synthesis and gas sensing properties of variety low dimensional nanostructures of SnO2
Wu et al. The effective determination of Cd (ii) and Pb (ii) simultaneously based on an aluminum silicon carbide-reduced graphene oxide nanocomposite electrode
Li et al. Porous In2O3 microstructures: hydrothermal synthesis and enhanced Cl2 sensing performance
Li et al. Ionic liquid-assisted synthesis of SnO 2 particles with nanorod subunits for enhanced gas-sensing properties
Nie et al. The 3D crystal morphologies of NiO gas sensor and constantly improved sensing properties to ethanol
Zhang et al. On-chip surface modified nanostructured ZnO as functional pH sensors
Xu et al. Synthesis, characterization and gas sensing properties of porous flower-like indium oxide nanostructures
Hu et al. The hydrothermal evolution of the phase and shape of ZnS nanostructures and their gas-sensing properties
Li et al. Synthesis and gas-sensing properties of ZnO particles from an ionic liquid precursor
Zhang et al. Construction of hierarchical ZnO flower-like structure for boost H2S detection at low temperature
CN110455873B (en) Method for improving performance of MoS2 gas sensor by adopting W doping
Li et al. In (OH) 3 particles from an ionic liquid precursor and their conversion to porous In 2 O 3 particles for enhanced gas sensing properties
Gao et al. Hydrothermal synthesis of agglomerating TiO 2 nanoflowers and its gas sensing
Wang et al. Room temperature sensing performance of graphene-like SnS2 towards ammonia
Zhu et al. Highly sensitive sensor based on NaBi (MoO4) 2/MWCNT composites

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20201127