CN104792830A - Graphene/molybdenum disulfide compounding-based gas sensitive material and preparation method thereof - Google Patents
Graphene/molybdenum disulfide compounding-based gas sensitive material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a graphene/molybdenum disulfide compounding-based gas sensitive material and a preparation method thereof, relates to a gas sensitive material and a preparation method thereof, and aims at solving the technical problem that intrinsic graphene gas sensor nanoparticles only have high sensitivity for a few gases. The outer surface of graphene is coated by molybdenum disulfide. The preparation method comprises the following steps: I, cooling concentrated sulfuric acid, adding natural flake graphite and potassium permanganate, stirring, adding a mixed solution formed by hydrogen peroxide and distilled water, centrifuging and cleaning, and dissolving a precipitate in deionized water to obtain a solution; and II, dissolving sodium molybdate, cysteine and sodium hexadecyl benzene sulfonate in distilled water, adding the solution obtained in the step I, placing in a reaction kettle, and carrying out centrifugal cleaning and freeze drying to obtain the graphene/molybdenum disulfide compounding-based gas sensitive material. The composite material is high in selectivity and sensibility. The graphene/molybdenum disulfide compounding-based gas sensitive material and the preparation method thereof belong to the field of preparation of gas sensitive materials.
Description
Technical field
The present invention relates to a kind of gas sensitive material and preparation method thereof.
Background technology
What require quality of life along with people improves constantly, people for problem of environmental pollution growing interest, especially to the atmospheric pollution that human survival constitutes a threat to.Wherein, NO
2gas is to one of environment and the very serious pollutant of human health risk in air, NO especially in recent years
2the major sources of gas---the every annual growth rate of vehicle exhaust is surprising, makes NO
2monitoring become particularly important, therefore to know timely and accurately in environment and about the NO of pollution source
2the concentration of gas, is significant to environmental monitoring and environmental protection.
Because although traditional semiconductor gas sensor is widely used, due to its higher working temperature (being greater than 300 DEG C), usually limit the use of this type sensor.For this reason, researcher proposes the micro-scale by reducing semiconductor material, can reduce working temperature, consumes less energy and operate safer, therefore can be widely used in making gas sensor.Research in recent years finds that some characteristics of Graphene make it become very potential a kind of gas sensitive.Because Graphene is that each carbon atom of two-dimensional structure is exposed to surface, at room temperature there is very high electron mobility simultaneously, its electric transmission can reach 0.3um, when its binding molecule time, its electron transfer rate has change clearly, so it can be a kind of sensor sensing material had good prospects that Graphene has been proved to be.But research at present finds that the dissolubility of intrinsic Graphene gas sensitive nanoparticle own is poor, only there is high sensitivity to a few gases and often need to be desorbed by heating, limiting the widespread use of this kind of gas sensor to a certain extent.
Summary of the invention
The object of the invention is the technical matters only a few gases being had to high sensitivity in order to solve intrinsic Graphene gas sensitive nanoparticle, providing a kind of gas sensitive material based on Graphene/molybdenum disulfide compound and preparation method thereof.
Be 1 ﹕ 1 ~ 5 based on the mol ratio of molybdenum atom and carbon atom in the gas sensitive material of Graphene/molybdenum disulfide compound, molybdenum disulfide is wrapped in Graphene outside surface, and the number of plies of molybdenum disulfide is 5 ~ 20 layers, and every interlamellar spacing is 0.62 ~ 0.65nm.
Preparation method based on the gas sensitive material of Graphene/molybdenum disulfide compound carries out according to following steps:
One, 15 ~ 25ml concentrated sulphuric acid is cooled to-1 ~ 1 DEG C, adding 0.5 ~ 1.5g natural flake graphite and stir 30 ~ 50min, is that under the condition of less than 5 DEG C, in 25min, gradation adds 5 ~ 8g KMnO in temperature
4, stir 1 ~ 3h, obtain potpourri;
Two, by the stirred in water bath 30 ~ 60min of potpourri at 40 DEG C, the temperature to water-bath is 45 DEG C, stops stirring, and obtains slurries;
Three, slurries are forwarded to 80 DEG C of thermostat water baths to stir, treat that slurries are warmed up to 80 DEG C, adding 60 ~ 80ml distilled water in gradation 20min, to be stirred to reacting liquid temperature be 90 DEG C, then reactant liquor is shifted out water-bath and stir 15min, add 40 ~ 70ml distilled water diluting, add again 10 ~ 15ml by mass percent concentration be 30% hydrogen peroxide and the mixed solution that forms of 60ml distilled water to occurring golden yellow, centrifugal and washing to washing lotion pH value be 5 ~ 6, then the precipitation after centrifugal is dissolved in deionized water, obtains the solution that concentration is 1 ~ 3mg/ml;
Four, 0.5g sodium molybdate, 1g halfcystine and 0.3g cetyl benzenesulfonic acid sodium are dissolved in 60ml deionized water, then 20mL step 3 gained solution is added, again mixed solution is put into 100ml reactor, 18 ~ 24h is kept at 240 DEG C, eccentric cleaning, freeze drying, obtains the gas sensitive material based on Graphene/molybdenum disulfide compound.
Advantage of the present invention:
One, the gas sensitive based on Graphene/molybdenum disulfide compound substance of the present invention, lower relative to metal oxide gas sensitive working temperature, saves more multiple-energy-source;
Two, the gas sensitive based on Graphene/molybdenum disulfide compound substance of the present invention, preparation process is simple, easy to operate;
Three, the gas sensitive based on Graphene/molybdenum disulfide compound substance of the present invention, by load molybdenum disulfide nano particle, has higher selectivity and susceptibility relative to pure Graphene;
Four, the preparation method of the gas sensitive based on Graphene/molybdenum disulfide compound substance of the present invention, in the compound substance prepared by Graphene as electronic conduction path, overcome the shortcoming of the poorly conductive of molybdenum disulfide own.By molybdenum disulfide as gas sensor, drastically increase gas sensitization performance.
Accompanying drawing explanation
Fig. 1 is that the gas sensitive material based on Graphene/molybdenum disulfide compound prepared by experiment one carries out electron scanning micrograph;
Fig. 2 is the air-sensitive performance curve of the gas sensitive material based on Graphene/molybdenum disulfide compound prepared by experiment one, the air-sensitive performance curve of 1 expression Graphene in figure, the air-sensitive performance curve of 2 expression molybdenum disulfide, 3 represent the air-sensitive performance curve based on the gas sensitive material of Graphene/molybdenum disulfide compound.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the combination in any between each embodiment.
Embodiment one: present embodiment is 1 ﹕ 1 ~ 5 based on the mol ratio of molybdenum atom and carbon atom in the gas sensitive material of Graphene/molybdenum disulfide compound, molybdenum disulfide is wrapped in Graphene outside surface, the number of plies of molybdenum disulfide is 5 ~ 20 layers, and every interlamellar spacing is 0.62 ~ 0.65nm.
Embodiment two: present embodiment and embodiment one unlike described be 1 ﹕ 3 based on the mol ratio of molybdenum atom and carbon atom in the gas sensitive material of Graphene/molybdenum disulfide compound.Other is identical with embodiment one.
Embodiment three: one of present embodiment and embodiment one or two are 0.64nm unlike described every interlamellar spacing.Other is identical with one of embodiment one or two.
Embodiment four: carry out according to following steps based on the preparation method of the gas sensitive material of Graphene/molybdenum disulfide compound described in embodiment one:
One, 15 ~ 25ml concentrated sulphuric acid is cooled to-1 ~ 1 DEG C, adding 0.5 ~ 1.5g natural flake graphite and stir 30 ~ 50min, is that under the condition of less than 5 DEG C, in 25min, gradation adds 5 ~ 8g KMnO in temperature
4, stir 1 ~ 3h, obtain potpourri;
Two, by the stirred in water bath 30 ~ 60min of potpourri at 40 DEG C, the temperature to water-bath is 45 DEG C, stops stirring, and obtains slurries;
Three, slurries are forwarded to 80 DEG C of thermostat water baths to stir, treat that slurries are warmed up to 80 DEG C, adding 60 ~ 80ml distilled water in gradation 20min, to be stirred to reacting liquid temperature be 90 DEG C, then reactant liquor is shifted out water-bath and stir 15min, add 40 ~ 70ml distilled water diluting, add again 10 ~ 15ml by mass percent concentration be 30% hydrogen peroxide and the mixed solution that forms of 60ml distilled water to occurring golden yellow, centrifugal and washing to washing lotion pH value be 5 ~ 6, then the precipitation after centrifugal is dissolved in deionized water, obtains the solution that concentration is 1 ~ 3mg/ml;
Four, 0.5g sodium molybdate, 1g halfcystine and 0.3g cetyl benzenesulfonic acid sodium are dissolved in 60ml deionized water, then 20mL step 3 gained solution is added, again mixed solution is put into 100ml reactor, 18 ~ 24h is kept at 240 DEG C, eccentric cleaning, freeze drying, obtains the gas sensitive material based on Graphene/molybdenum disulfide compound.
Embodiment five: present embodiment and embodiment four are 95% ~ 98% unlike the mass percent concentration of the concentrated sulphuric acid described in step one.Other is identical with embodiment four.
Embodiment six: the concentrated sulphuric acid is cooled to 0 DEG C unlike in step one by present embodiment and embodiment four or five.Other is identical with embodiment four or five.
Embodiment seven: one of present embodiment and embodiment four to six stir 40min unlike adding 1g natural flake graphite in step one.Other is identical with one of embodiment one to six.
Embodiment eight: one of present embodiment and embodiment four to six are unlike being that gradation adds 6g KMnO in 25min under the condition of less than 5 DEG C in temperature in step one
4.Other is identical with one of embodiment one to six.
Embodiment nine: one of present embodiment and embodiment four to six unlike in step 2 by the stirred in water bath 30 ~ 60min of potpourri at 40 DEG C.Other is identical with one of embodiment one to six.
Embodiment ten: one of present embodiment and embodiment four to six keep 20h unlike in step 4 at 240 DEG C.Other is identical with one of embodiment one to six.
Adopt following experimental verification effect of the present invention:
Experiment one:
Preparation method based on the gas sensitive material of Graphene/molybdenum disulfide compound carries out according to following steps:
One, being that 98% concentrated sulphuric acid is cooled to-1 DEG C by 20ml mass percent concentration, adding 1g natural flake graphite and stir 30min, is divide under the condition of less than 2 DEG C to add 6g KMnO 3 times in 25min in temperature
4, stir 2h, obtain potpourri;
Two, by the stirred in water bath 60min of potpourri at 40 DEG C, the temperature to water-bath is 45 DEG C, stops stirring, and obtains slurries;
Three, slurries are forwarded to 80 DEG C of thermostat water baths to stir, treat that slurries are warmed up to 80 DEG C, 80ml is added (first few in gradation 20min, cumulative afterwards) distilled water (now reactant and thickness thereof, rapid stirring heat radiation as far as possible, if temperature is raised to 90 DEG C, then reactant liquor is shifted out water-bath to forward in air and stir 15min, add water gradually), add 50ml distilled water diluting, add again 15ml by mass percent concentration be 30% hydrogen peroxide and the mixed solution that forms of 60ml distilled water to occurring golden yellow, centrifugal and washing to washing lotion pH value be 5, then the precipitation after centrifugal is dissolved in deionized water, obtain the solution that concentration is 2mg/ml,
Four, 0.5g sodium molybdate, 1g halfcystine and 0.3g cetyl benzenesulfonic acid sodium are dissolved in 60ml deionized water, then 20mL step 3 gained solution is added, again mixed solution is put into 100ml reactor, 18h is kept at 240 DEG C, eccentric cleaning, freeze drying, obtains the gas sensitive material based on Graphene/molybdenum disulfide compound.
Gas sensitive material based on Graphene/molybdenum disulfide compound prepared by this experiment is carried out scanning electron microscope test, obtains Fig. 1.From Fig. 1, can observe the number of plies of molybdenum disulfide in compound clearly and be about about 5 ~ 20 layers, sheet interlayer spacing is about 0.64nm.
The gas sensitive material based on Graphene/molybdenum disulfide compound of employing CGS-1PT vapor sensitivity test macro to gained carries out the NO under room temperature condition
2vapor sensitivity is tested, and as shown in Figure 2, vapor sensitivity is defined as
wherein Rg is resistance when being exposed in gas, R
0for the initial resistance under nitrogen exposure.Wherein based on the NO of the gas sensitive material of Graphene/molybdenum disulfide compound
2vapor sensitivity is 200%, far above pure Graphene and pure molybdenum disulfide.
Claims (10)
1. based on the gas sensitive material of Graphene/molybdenum disulfide compound, it is characterized in that described is 1 ﹕ 1 ~ 5 based on the mol ratio of molybdenum atom and carbon atom in the gas sensitive material of Graphene/molybdenum disulfide compound, molybdenum disulfide is wrapped in Graphene outside surface, the number of plies of molybdenum disulfide is 5 ~ 20 layers, and every interlamellar spacing is 0.62 ~ 0.65nm.
2., according to claim 1 based on the gas sensitive material of Graphene/molybdenum disulfide compound, it is characterized in that described is 1 ﹕ 3 based on the mol ratio of molybdenum atom and carbon atom in the gas sensitive material of Graphene/molybdenum disulfide compound.
3., according to claim 1 based on the gas sensitive material of Graphene/molybdenum disulfide compound, it is characterized in that described every interlamellar spacing is 0.64nm.
4. described in claim 1 based on the preparation method of the gas sensitive material of Graphene/molybdenum disulfide compound, it is characterized in that the preparation method of the gas sensitive material based on Graphene/molybdenum disulfide compound carries out according to following steps:
One, 15 ~ 25ml concentrated sulphuric acid is cooled to-1 ~ 1 DEG C, adding 0.5 ~ 1.5g natural flake graphite and stir 30 ~ 50min, is that under the condition of less than 5 DEG C, in 25min, gradation adds 5 ~ 8g KMnO in temperature
4, stir 1 ~ 3h, obtain potpourri;
Two, by the stirred in water bath 30 ~ 60min of potpourri at 40 DEG C, the temperature to water-bath is 45 DEG C, stops stirring, and obtains slurries;
Three, slurries are forwarded to 80 DEG C of thermostat water baths to stir, treat that slurries are warmed up to 80 DEG C, adding 60 ~ 80ml distilled water in gradation 20min, to be stirred to reacting liquid temperature be 90 DEG C, then reactant liquor is shifted out water-bath and stir 15min, add 40 ~ 70ml distilled water diluting, add again 10 ~ 15ml by mass percent concentration be 30% hydrogen peroxide and the mixed solution that forms of 60ml distilled water to occurring golden yellow, centrifugal and washing to washing lotion pH value be 5 ~ 6, then the precipitation after centrifugal is dissolved in deionized water, obtains the solution that concentration is 1 ~ 3mg/ml;
Four, 0.5g sodium molybdate, 1g halfcystine and 0.3g cetyl benzenesulfonic acid sodium are dissolved in 60ml deionized water, then 20mL step 3 gained solution is added, again mixed solution is put into 100ml reactor, 18 ~ 24h is kept at 240 DEG C, eccentric cleaning, freeze drying, obtains the gas sensitive material based on Graphene/molybdenum disulfide compound.
5., according to claim 4 based on the preparation method of the gas sensitive material of Graphene/molybdenum disulfide compound, it is characterized in that the mass percent concentration of the concentrated sulphuric acid described in step one is 95% ~ 98%.
6. according to claim 4 or 5 based on the preparation method of the gas sensitive material of Graphene/molybdenum disulfide compound, it is characterized in that, in step one, the concentrated sulphuric acid is cooled to 0 DEG C.
7. according to claim 4 or 5 based on the preparation method of the gas sensitive material of Graphene/molybdenum disulfide compound, it is characterized in that adding in step one 1g natural flake graphite and stir 40min.
8. according to claim 4 or 5 based on the preparation method of the gas sensitive material of Graphene/molybdenum disulfide compound, to it is characterized in that in step one that gradation adds 6g KMnO in 25min under temperature is the condition of less than 5 DEG C
4.
9. according to claim 4 or 5 based on the preparation method of the gas sensitive material of Graphene/molybdenum disulfide compound, it is characterized in that the stirred in water bath 30 ~ 60min of potpourri at 40 DEG C in step 2.
10. according to claim 4 or 5 based on the preparation method of the gas sensitive material of Graphene/molybdenum disulfide compound, it is characterized in that in step 4 240 DEG C keep 20h.
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| CN106248735A (en) * | 2016-07-12 | 2016-12-21 | 电子科技大学 | A kind of humidity sensor based on ultra-thin sulfide film and preparation method thereof |
| CN107085020A (en) * | 2017-05-26 | 2017-08-22 | 黑龙江大学 | A kind of molybdenum disulfide/indium hydroxide composite air-sensitive sensing material and preparation method and application |
| CN107393721A (en) * | 2017-07-28 | 2017-11-24 | 浙江理工大学 | A kind of preparation method of the graphene zinc oxide nano tube array sensing material of molybdenum disulfide quantum dot modification |
| CN108680610A (en) * | 2018-06-13 | 2018-10-19 | 湘潭大学 | One kind being based on MoS2The room temperature NO of-PbS composite materials2Gas sensor and preparation method thereof |
| CN110208337A (en) * | 2019-06-28 | 2019-09-06 | 西南交通大学 | Compound humidity sensor of molybdenum disulfide/Nano diamond and preparation method thereof |
| CN111307876A (en) * | 2018-12-11 | 2020-06-19 | 有研工程技术研究院有限公司 | Gas sensor for detecting nitrogen dioxide and preparation method thereof |
| CN112903761A (en) * | 2021-01-19 | 2021-06-04 | 重庆大学 | Molybdenum disulfide-reduced graphene oxide-cuprous oxide ternary composite material and preparation method and application thereof |
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| CN111307876A (en) * | 2018-12-11 | 2020-06-19 | 有研工程技术研究院有限公司 | Gas sensor for detecting nitrogen dioxide and preparation method thereof |
| CN110208337A (en) * | 2019-06-28 | 2019-09-06 | 西南交通大学 | Compound humidity sensor of molybdenum disulfide/Nano diamond and preparation method thereof |
| CN110208337B (en) * | 2019-06-28 | 2022-02-08 | 西南交通大学 | Molybdenum disulfide/nano diamond composite humidity sensor and preparation method thereof |
| CN112903761A (en) * | 2021-01-19 | 2021-06-04 | 重庆大学 | Molybdenum disulfide-reduced graphene oxide-cuprous oxide ternary composite material and preparation method and application thereof |
| WO2023272664A1 (en) * | 2021-06-30 | 2023-01-05 | 苏州大学 | Graphene composite material, sensor and use thereof |
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