CN115541666B - Heterojunction composite material for trimethylamine gas sensor and preparation method thereof - Google Patents
Heterojunction composite material for trimethylamine gas sensor and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a heterojunction composite material for a trimethylamine gas sensor and a preparation method thereof, wherein the heterojunction composite material is Cu 3 Mo 2 O 9 /MoO 3 Heterojunction composite material, cu 3 Mo 2 O 9 /MoO 3 The heterojunction composite material is Cu 3 Mo 2 O 9 Nanoparticles are bonded to MoO in an in situ growth manner 3 Formed on a nanoribbon; the preparation method comprises the following steps: (1) Adding MoO 3 Adding the nanobelt, sodium molybdate and copper salt into a solvent, and stirring until the nanobelt, the sodium molybdate and the copper salt are fully dissolved and dispersed to obtain a precursor; (2) Transferring the precursor into a reaction kettle, putting the reaction kettle into an oven for reaction for a period of time, cooling, centrifuging, and drying and precipitating to obtain an intermediate product; (3) Putting the intermediate product into a muffle furnace, and performing heat treatment to obtain Cu 3 Mo 2 O 9 /MoO 3 A heterojunction composite material. The invention is prepared by mixing Cu 3 Mo 2 O 9 In situ growth of nanoparticles to MoO 3 A heterojunction is constructed on the nanobelt, a charge depletion layer is formed at an interface, a conductive channel is reduced, the initial resistance is improved, and the gas adsorption capacity is enhanced, so that the working temperature is reduced, and the TMA detection capacity is improved.
Description
Technical Field
The invention belongs to the technical field of gas-sensitive material preparation, and particularly relates to a heterojunction composite material for a trimethylamine gas sensor and a preparation method thereof.
Background
Trimethylamine (TMA) is a toxic gaseous organic amine, is volatile at normal temperature, and is flammable and explosive. The limit of exposure to TMA for a long time (10 hours) is 10 ppm and for a short time (15 minutes) is 15 ppm, otherwise health problems such as headache, nausea, cough, upper respiratory system irritation and pulmonary edema may occur. TMA gas is generated during the storage of fish, shrimp and meat, and the concentration thereof increases as the freshness thereof decreases, so that the presence and concentration of TMA become important indicators for evaluating the freshness of meat, fish and shrimp. Therefore, the method has strong practical significance for realizing the rapid and accurate detection of TMA. Many detection methods such as gas chromatography, colorimetry, photometry, etc. suffer from the disadvantages of cumbersome instruments, long test sample preparation times, and high requirements on operator proficiency. However, the gas-sensitive test method using the gas sensor has the advantages of simple and convenient manufacture, portability, capability of realizing rapid detection, real-time response and the like.
At present, based on MoO 3 The gas sensor made of the nano material has good selectivity on TMA, and has good development and application potential in the aspect of TMA detection. In practical applications, however, based on pure MoO 3 TMA sensors made of nano materials generally have high working temperature (300 to 450 ℃) and higher detection limit (>1 ppm). On the one hand, the high working temperature leads to poor device stability and high overall energy consumption, and simultaneously increases hidden fire detonation risk in the TMA detection process, and on the other hand, in the real-time monitoring of TMA, the high detection limit leads to low device resolution ratio, and more accurate detection can not be realized for TMA.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a Cu used for a trimethylamine gas sensor 3 Mo 2 O 9 /MoO 3 Heterojunction composite materials and methods of making the same. By designing Cu 3 Mo 2 O 9 In situ growth of nanoparticles to MoO 3 A heterojunction is constructed on the nanobelt, a charge depletion layer is formed at an interface, a conductive channel is reduced, the initial resistance is improved, and the gas adsorption capacity is enhanced, so that the working temperature is reduced, and the TMA detection capacity is improved.
In order to achieve the purpose, the invention is realized by the following technical scheme:
in one aspect, the invention provides a heterojunction composite material for a trimethylamine gas sensor, wherein the heterojunction composite material is Cu 3 Mo 2 O 9 /MoO 3 Heterojunction composite material, said Cu 3 Mo 2 O 9 /MoO 3 The heterojunction composite material is Cu 3 Mo 2 O 9 Nanoparticles are bonded to MoO in an in situ growth manner 3 Formed on a nanoribbon.
Preferably, the Cu 3 Mo 2 O 9 The diameter of the nanoparticles is 50 to 200nm, and the most preferable is 50 nm.
Preferably, the Cu 3 Mo 2 O 9 /MoO 3 Cu in heterojunction composite 3 Mo 2 O 9 The loading of the nano particles is 1-20wt%.
Preferably, the Cu 3 Mo 2 O 9 /MoO 3 The optimal working temperature of the heterojunction composite material is below 180 ℃, and the detection limit of trimethylamine gas is less than or equal to 0.05ppm.
In another aspect, the present invention provides a method for preparing a heterojunction composite material for a trimethylamine gas sensor, comprising the steps of:
(1) Adding MoO 3 Adding the nanobelt, sodium molybdate and copper salt into a solvent, and stirring until the nanobelt, the sodium molybdate and the copper salt are fully dissolved and dispersed to obtain a precursor;
(2) Transferring the precursor into a reaction kettle, putting the precursor into an oven for reaction for a period of time, cooling, centrifuging, and drying and precipitating to obtain an intermediate product;
(3) Putting the intermediate product into a muffle furnace, and performing heat treatment to obtain Cu 3 Mo 2 O 9 /MoO 3 A heterojunction composite material.
The reaction mechanism is as follows: in step (2)
And
combined to form basic copper molybdate
Basic copper molybdate adhered to MoO 3 Dehydrating the basic copper molybdate to form copper molybdate Cu on the surface of the nanobelt after the high-temperature heat treatment in the step (3) 3 Mo 2 O 9 Simultaneously bound to MoO 3 Obtaining Cu from the surface of the nanobelt 3 Mo 2 O 9 /MoO 3 A heterojunction composite material.
Preferably, in step (1), the MoO is 3 The mass ratio of the nanobelt to the sodium molybdate to the copper salt is 1 (0.01-0.26) to (0.0140-0.28), the mass ratio of the nanobelt to the sodium molybdate to the copper salt is more preferably 1 (0.02-0.12) to (0.03-0.13), and the mass ratio of the nanobelt to the sodium molybdate to the copper salt is most preferably 1:0.03: 0.04.
Preferably, in step (1), the copper salt is one of copper acetate, copper nitrate and copper sulfate, and most preferably, the copper salt is copper acetate.
Preferably, in the step (1), the solvent is a mixed solution of water, ethanol and ethylene glycol.
Preferably, in the step (2), the oven temperature is 100 to 150 ℃, the reaction time is 2 to 12 hours, and most preferably, the oven temperature is 120 ℃, and the reaction time is 5 hours.
Preferably, in the step (3), the heat treatment temperature is 300 to 500 ℃ and the time is 1 to 5 hours, and most preferably, the heat treatment temperature is 350 ℃ and the time is 2 hours.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention adopts a hydrothermal method to prepare Cu 3 Mo 2 O 9 /MoO 3 Heterojunction composite material of Cu 3 Mo 2 O 9 Nanoparticles attached to MoO 3 On the nanoribbons, heterostructures are formed.
(2) Based on Cu 3 Mo 2 O 9 /MoO 3 Gas sensor of heterojunction composite material and pure MoO 3 、Cu 3 Mo 2 O 9 Compared with the prior art, the gas-sensitive performance is obviously improved, the optimal working temperature is reduced to be below 180 ℃, the detection limit of TMA gas reaches 0.05ppm, and the gas-sensitive material has good response-recovery performance on low-concentration TMA.
(3) The invention designs Cu 3 Mo 2 O 9 In situ growth of nanoparticles to MoO 3 Heterojunction is constructed on the nano-band due to Cu 3 Mo 2 O 9 Is a p-type semiconductor, has a unique spatial structure, and unsaturated coordination of Cu and Mo in the structure increases the potential Lewis acid active adsorption sites for trimethylamine, so that Cu 3 Mo 2 O 9 Has certain amine sensitive application potential. When MoO 3 Nanobelt and Cu 3 Mo 2 O 9 When the nano particles are constructed to form a p-n type heterojunction, the Fermi levels of two different semiconductor materials are different, so that the Fermi levels are relatively moved, a charge depletion layer is formed at an interface, a conductive channel is reduced, the initial resistance is improved, the gas adsorption capacity is enhanced, the working temperature is reduced, and the detection capacity on TMA is improved.
(4) The preparation method disclosed by the invention is simple in process and low in cost, and meets the environmental requirements.
Drawings
FIG. 1 is a MoO prepared in comparative example 1 3 SEM image characterization of nanobelts (control 1);
FIG. 2 is Cu prepared in comparative example 2 3 Mo 2 O 9 SEM image characterization of nanoparticles (control 2);
FIG. 3 shows Cu prepared in example 1 of the present invention 3 Mo 2 O 9 /MoO 3 SEM image characterization of the heterojunction composite material;
FIG. 4 shows Cu prepared in example 1 of the present invention 3 Mo 2 O 9 /MoO 3 TEM image characterization of the heterojunction composite material;
FIG. 5 shows Cu prepared in example 1 of the present invention 3 Mo 2 O 9 /MoO 3 HRTEM image characterization of the heterojunction composite material;
FIG. 6 shows Cu prepared according to example 1 of the present invention 3 Mo 2 O 9 /MoO 3 Heterojunction composite, moO prepared in comparative example 1 3 Cu prepared in nanoribbon comparative sample 1 and comparative example 2 3 Mo 2 O 9 Gas-sensitive response plots of the gas sensor of nanoparticle control 2 for different concentrations of TMA;
FIG. 7 shows Cu prepared according to example 1 of the present invention 3 Mo 2 O 9 /MoO 3 The gas sensor of the heterojunction composite material has gas-sensitive response graphs for TMA with different concentrations at different temperatures;
FIG. 8 shows Cu prepared according to example 1 of the present invention 3 Mo 2 O 9 /MoO 3 The response and recovery of a gas sensor of heterojunction composite material to low concentrations of TMA at the optimum operating temperature is plotted.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention, the following description of the preferred embodiments of the present invention is provided in connection with the specific examples, but the present invention should not be construed as being limited thereto, and only by way of example.
The test methods or test methods described in the following examples are conventional methods unless otherwise specified; the reagents and materials, unless otherwise indicated, are conventionally obtained commercially or prepared by conventional methods.
Example 1
The embodiment provides a preparation method of a heterojunction composite material for a trimethylamine gas sensor, which comprises the following steps:
(1) Adding MoO 3 Adding the nanobelt, sodium molybdate and copper acetate into ethanol and ethylene glycol according to the mass ratio of 1Stirring the mixed solvent until the mixed solvent is fully dissolved to obtain a precursor;
(2) Transferring the precursor into a reaction kettle, putting the reaction kettle into an oven to react for 5 hours at 120 ℃, cooling and centrifuging, alternately washing the obtained product with ethanol and deionized water for several times, and drying at 80 ℃ to obtain an intermediate product;
(3) Putting the intermediate product into a muffle furnace, and carrying out heat treatment at 350 ℃ for 2h to obtain Cu 3 Mo 2 O 9 /MoO 3 A heterojunction composite material.
Example 2
The embodiment provides a preparation method of a heterojunction composite material for a trimethylamine gas sensor, which comprises the following steps:
(1) Adding MoO 3 Adding the nanobelt, sodium molybdate and copper nitrate into a mixed solvent of ethanol and ethylene glycol according to the mass ratio of 1: 0.011: 0.0140, and stirring until the mixture is fully dissolved to obtain a precursor;
(2) Transferring the precursor into a reaction kettle, putting the precursor into an oven to react for 12 hours at 100 ℃, cooling and centrifuging, alternately washing the obtained product with ethanol and deionized water for several times, and drying at 80 ℃ to obtain an intermediate product;
(3) Putting the intermediate product into a muffle furnace, and carrying out heat treatment at 300 ℃ for 5h to obtain Cu 3 Mo 2 O 9 /MoO 3 A heterojunction composite material.
Example 3
The embodiment provides a preparation method of a heterojunction composite material for a trimethylamine gas sensor, which comprises the following steps:
(1) Adding MoO 3 Adding the nanobelts, sodium molybdate and copper sulfate into a mixed solvent of ethanol and ethylene glycol according to the mass ratio of 1: 0.26: 0.28, and stirring until the mixture is fully dissolved to obtain a precursor;
(2) Transferring the precursor into a reaction kettle, putting the precursor into an oven to react for 2h at 150 ℃, cooling and centrifuging, alternately washing the obtained product with ethanol and deionized water for several times, and drying at 80 ℃ to obtain an intermediate product;
(3) Putting the intermediate product into a muffle furnace, and carrying out heat treatment at 450 ℃ for 1 h to obtain Cu 3 Mo 2 O 9 /MoO 3 A heterojunction composite material.
Comparative example 1
This example uses MoO 3 Nanobelt as comparative sample 1, this example prepared MoO 3 The method of the nanobelt is the same as that of the embodiment 1, and specifically comprises the following steps:
adding 0.8000 g of molybdenum powder into 19.0 mL of deionized water, mechanically stirring until the molybdenum powder is completely and uniformly dispersed in the water, and slowly adding 6.0 mL of 30% hydrogen peroxide in the stirring process; after the dropwise addition, stirring is continued for 3 hours to obtain orange-yellow molybdenum peroxide sol. Transferring the sol into a hydrothermal reaction kettle, placing the sol into an oven, keeping the temperature at 180 ℃ for 24 hours, stopping the reaction, naturally cooling to room temperature, alternately washing the obtained product with ethanol and deionized water for a plurality of times, and finally drying at 80 ℃ to obtain white or light blue MoO 3 A nanoribbon; as shown in FIG. 1, the MoO generated 3 The nanoribbon has the width of 200 to 400 nm, the thickness of 20 to 50 nm, the length of 2 to 10 mu m, smooth surface and similar appearance.
Comparative example 2
The present example uses Cu 3 Mo 2 O 9 Nanoparticles as comparative 2, this example prepared Cu 3 Mo 2 O 9 The method of nanoparticles is the same as in example 1, specifically:
adding sodium molybdate and copper acetate into a mixed solvent of ethanol and ethylene glycol according to a molar ratio of 2 3 Mo 2 O 9 Nanoparticles as shown in figure 2.
Examples 1 to 3 of the present invention use Cu 3 Mo 2 O 9 Nanoparticles are bonded to MoO in situ growth 3 Preparing on a nanobelt to obtain Cu 3 Mo 2 O 9 /MoO 3 Heterojunction composite, exemplified by the product of example 1, in combination with comparative examples 1 and 2, for Cu of the invention 3 Mo 2 O 9 /MoO 3 Analysis of the microstructure and material performance test data for the heterojunction composite was as follows:
FIG. 3 shows Cu prepared in example 1 of the present invention 3 Mo 2 O 9 /MoO 3 SEM image characterization of the heterojunction composite material; FIG. 4 and FIG. 5 are each a Cu film prepared in example 1 of the present invention 3 Mo 2 O 9 /MoO 3 TEM and HRTEM image representation of the heterojunction composite material; as can be seen from FIG. 3, FIG. 4 and FIG. 5, the preparation method provided by the present invention is applied to MoO 3 On the nanobelt successfully loads Cu 3 Mo 2 O 9 Nanoparticles, cu obtained by preparation 3 Mo 2 O 9 /MoO 3 The composite material has a heterostructure.
FIG. 6 shows Cu prepared according to example 1 of the present invention 3 Mo 2 O 9 /MoO 3 Heterojunction composite, moO prepared in comparative example 1 3 Cu prepared in nanoribbon comparative sample 1 and comparative example 2 3 Mo 2 O 9 Gas-sensitive response plots of the gas sensor of nanoparticle control 2 for different concentrations of TMA; as can be seen from FIG. 6, and based on pure MoO 3 Nanobelt comparative sample 1, pure Cu 3 Mo 2 O 9 Nanoparticles in comparison to gas sensor of reference 2, cu 3 Mo 2 O 9 /MoO 3 The gas sensitive response of the heterojunction composite material to TMA is obviously improved.
FIG. 7 shows Cu prepared according to example 1 of the present invention 3 Mo 2 O 9 /MoO 3 The gas sensor of the heterojunction composite material has gas-sensitive response graphs for TMA with different concentrations at different working temperatures; as can be seen from fig. 7, the response of the device to TMA increases with increasing gas concentration, with an optimum operating temperature of 168 ℃.
FIG. 8 shows Cu prepared according to example 1 of the present invention 3 Mo 2 O 9 /MoO 3 HeterojunctionThe response and recovery curves of the composite gas sensor to low concentrations of TMA at an optimum operating temperature of 168 ℃; as can be seen from FIG. 8, at this temperature, cu is present 3 Mo 2 O 9 /MoO 3 The heterojunction composite material has good response-recovery characteristics to 0.05-1 ppm TMA, the detection limit to the TMA reaches 0.05ppm, the heterojunction composite material has good response-recovery performance to low-concentration trimethylamine, and the heterojunction composite material has wide application prospect in the field of trimethylamine detection.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and it is obvious to those skilled in the art that the present invention is not limited to the details of the above-mentioned exemplary embodiments, and that the present invention can be embodied in any other specific form without departing from the spirit or essential characteristics thereof. Thus, the present embodiments are merely exemplary and non-limiting. The scope of the invention is indicated by the appended claims rather than the foregoing description, and all changes that come within the meaning and range of equivalency of the claims are intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (6)
1. A preparation method of a heterojunction composite material for a trimethylamine gas sensor is characterized by comprising the following steps:
the heterojunction composite material is Cu 3 Mo 2 O 9 /MoO 3 Heterojunction composite material, said Cu 3 Mo 2 O 9 /MoO 3 The heterojunction composite material is Cu 3 Mo 2 O 9 Nanoparticles are bonded to MoO in an in situ growth manner 3 Formed on a nanoribbon;
the preparation method of the heterojunction composite material comprises the following steps:
(1) Adding MoO 3 Adding the nanobelt, sodium molybdate and copper salt into a solvent, and stirring until the nanobelt, the sodium molybdate and the copper salt are fully dissolved and dispersed to obtain a precursor;
(2) Transferring the precursor into a reaction kettle, putting the precursor into an oven for reaction for a period of time, cooling, centrifuging, and drying and precipitating to obtain an intermediate product;
(3) Putting the intermediate product into a muffle furnace, and performing heat treatment to obtain Cu 3 Mo 2 O 9 /MoO 3 A heterojunction composite material;
the copper salt is one of copper acetate, copper nitrate and copper sulfate; the solvent is a mixed solution of water, ethanol and glycol; the Cu 3 Mo 2 O 9 /MoO 3 The optimal working temperature of the heterojunction composite material is below 180 ℃, and the detection limit of trimethylamine gas is less than or equal to 0.05ppm.
2. The method for preparing a heterojunction composite material for a trimethylamine gas sensor according to claim 1, wherein: the Cu 3 Mo 2 O 9 The diameter of the nano-particles is 50-200 nm.
3. The method for preparing a heterojunction composite material for a trimethylamine gas sensor according to claim 1, wherein: the Cu 3 Mo 2 O 9 /MoO 3 Cu in heterojunction composite 3 Mo 2 O 9 The loading of the nano particles is 1-20wt%.
4. The method for preparing a heterojunction composite material for a trimethylamine gas sensor according to claim 1, wherein: in the step (1), the MoO 3 The mass ratio of the nano-belt, the sodium molybdate and the copper salt is 1 (0.01-0.26) to 0.01-0.28.
5. The method for preparing a heterojunction composite material for a trimethylamine gas sensor according to claim 1, wherein: in the step (2), the temperature of the oven is 100-150 ℃, and the reaction time is 2-12 h.
6. The method for preparing a heterojunction composite material for a trimethylamine gas sensor according to claim 1, wherein: in the step (3), the heat treatment temperature is 300-500 ℃ and the time is 1-5 h.
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