CN103616413A - Gas sensor based on reduction-oxidation graphene and preparation method of gas sensor - Google Patents
Gas sensor based on reduction-oxidation graphene and preparation method of gas sensor Download PDFInfo
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Abstract
The invention belongs to the technical field of sensors, and discloses a gas sensor based on reduction-oxidation graphene and a preparation method of the gas sensor. The gas sensor based on reduction-oxidation graphene is obtained by assembling dispersion liquid of large-size oxidation graphene on an amination electrode surface and performing in-situ reduction on the assembled oxidation graphene by adopting a liquid reducing agent. The gas sensor based on reduction-oxidation grapheme, prepared by the method disclosed by the invention, has excellent sensing property to ammonia molecules, and the preparation method is simple in process, controllable and suitable for large-scale preparation of the gas sensor.
Description
Technical field
The invention belongs to sensor technical field, relate to a kind of gas nanosensor and preparation method thereof, be specifically related to a kind of gas sensor based on redox graphene and preparation method thereof.
Background technology
Gas sensor is being brought into play more and more important effect in fields such as environmental monitoring, chemical industry monitoring, food security, health cares.Development along with nanometer technology, nanometer organic semiconductor, metal-oxide semiconductor (MOS) nano particle, carbon nanomaterial and two-dimensional nano film etc. have all been used as sensitive material and have formed gas sensor, compare have more excellent detection performance with traditional sensors.
Graphene, as the individual layer bi-dimensional cellular structural carbon in carbon family, has the irreplaceable advantage of many conventional sensors materials, and therefore, it has development prospect widely as sensing material at aspects such as biology, chemistry, machinery, aviation, military affairs.The preparation method of Graphene mainly contains three kinds: mechanical stripping method, chemical gaseous phase deposition method and chemistry or thermal reduction graphite oxide method, the Graphene of preparation all shows good response performance to gas molecule.Wherein, the Graphene that prepared by the relative additive method of electronation graphene oxide has the advantage of the following aspects: (1) preparation method is simple; (2) low without specific installation, cost, be convenient to extensive preparation; (3) by functional molecular design, be beneficial to Graphene and disperse in solution, be convenient to the making of device; (4) MOLECULE DESIGN can improve the selective response performance of sensor to gas molecule.Inventor writes articles and points out the 107th page of the 1st phase in 2012 in Sensors and Actuators B:Chemicals, and the redox graphene that p-phenylenediamine (PPD) reduction is prepared has good selective response performance to DMMP gas molecule.Therefore, electronation graphene oxide gas sensor has caused research widely.
In order to realize the application of redox graphene material in gas detects, conventionally need the senser element of preparation based on redox graphene sensitive material.The preparation of device has two kinds of methods conventionally: (1) adopts micro fabrication directly on sensitive material film surface, to prepare electrode, and the device obtaining has good electrically contacting, thereby can improve signal to noise ratio (S/N ratio).Yet the method has changed existing standard technology flow process, process is more loaded down with trivial details, and cost is relatively high.(2) first adopt the micro fabrication of standard to prepare electrode, then redox graphene solution is dropped on electrode, drying and forming-film, well behaved senser element meets with a response.Although this kind of method is simple to operate, be convenient to extensive preparation.Yet the repeatability of the method is poor, be unfavorable for the popularization of Standardization Process.For extensive controlled preparation is based on redox graphene gas sensing device, be necessary to seek new preparation technology, extensive controlled electronation graphene oxide gas sensor gas molecule to good response performance of preparing.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of gas sensor based on redox graphene and controllable method for preparing thereof that ammonia is shown to extremely sensitive response performance.
For achieving the above object, the invention provides following technical scheme:
The present invention is by large scale graphene oxide dispersion liquid is assembled in to amidized electrode surface, and adopts liquid reducer to carry out in-situ reducing to the graphene oxide of assembling, thereby obtains redox graphene gas sensor, specifically comprises the steps:
(1) preparation of large scale graphene oxide dispersion liquid
The graphene oxide that is of a size of 10～50 μ m is placed in to water, and ultrasonic processing 1min～3h under the frequency of 40～80kHz, forms the suspending liquid that monolithic disperses, and in described suspending liquid, graphene oxide concentration is 0.25～3mg/mL;
Described graphene oxide prepares by Brodie method, Staudenmaier method or Hummers method.
(2) amination of electrode is processed
Electrode is placed in after mercaptoethylmaine aqueous solution immersion treatment 1～48h, and water and alcohol flushing are clean, obtain being assembled with amino electrode;
Preferably, the concentration of described mercaptoethylmaine aqueous solution is 1～5mM.
Preferably, described electrode adopts photoetching and the lift-off technology in micro-processing technology to prepare, and the spacing of controlling positive and negative electrode is 100 μ m～800 μ m, and the spacing of adjacent electrode is 1 μ m～10 μ m.
(3) graphene oxide is in the assembling of electrode surface
The amino electrode that is assembled with that step (2) is obtained is placed in the described graphene oxide dispersion liquid of step (1) and soaks 1～24h, carries out graphene oxide in the assembling of electrode surface;
(4) preparation of redox graphene gas sensor
The electrode that is assembled with graphene oxide that step (3) is obtained is placed in closed container, in closed container, add liquid reducer simultaneously, add thermosetting reductive agent steam, realize the in-situ reducing of graphene oxide, thereby obtain redox graphene gas sensor;
Wherein, described liquid reducer is one or more the potpourri in pyrroles, hydrazine hydrate, ethylenediamine.
Preferably, the volume ratio of described closed container and liquid reducer is 100:1～0.05.
Preferably, described liquid reducer is heated to 60～200 ℃ and forms steam.
Preferably, by described graphene oxide at reductive agent steam atmosphere situ reduction 12～24h.
The present invention also provides a kind of gas sensor based on redox graphene that adopts said method to make.
The redox graphene gas sensor of preparing by said method has excellent sensing capabilities to ammonia molecule, and this preparation method's technique is simple, and controlled, is suitable for a large amount of preparations of gas sensor.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme in the embodiment of the present invention, below the accompanying drawing of required use during embodiment is described is briefly described, apparently, accompanying drawing relevant of the present invention in the following describes is only some embodiments of the present invention, for those of ordinary skills, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is the electrode scanning electron microscope (SEM) photograph of the gas sensor that makes of the embodiment of the present invention 1;
Fig. 2 is the response curve of the gas sensor that makes of the embodiment of the present invention 1 to 50ppb ammonia molecule.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is described in detail, obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Embodiment based in the present invention, the every other embodiment that those of ordinary skills obtain under the prerequisite of not making creative work, belongs to the scope of protection of the invention.
The present invention's each raw material used all can be buied by market.
Embodiment 1
(1), by 10 μ m left and right large scale graphite oxide 0.1g ultrasonic in water (45KHz) 1h that obtain by Hummers method, form the dispersion liquid of 0.5mg/mL.
(2) adopt photoetching and lift-off technology in micro-processing technology to prepare gold electrode, the spacing of controlling positive and negative electrode is 800 μ m, and the spacing of adjacent electrode is 1 μ m.Electrode is placed in after 1mM mercaptoethylmaine aqueous solution immersion treatment 24h, and water and alcohol flushing are clean, obtain being assembled with amino electrode.
(3) by being assembled with amino electrode, being placed in graphene oxide dispersion liquid and soaking 24h, water and alcohol flushing are clean, thereby realize graphene oxide in the assembling of electrode surface.
(4) electrode that is assembled with graphene oxide is placed in the closed container of 100mL, in closed container, add 0.06mL pyrroles simultaneously, 90 ℃ add thermosetting pyrroles steam, reaction 24h, thereby realize the in-situ reducing of graphene oxide, obtain redox graphene gas sensor, resistance is 28K Ω.
Embodiment 2
(1), by 10 μ m left and right large scale graphite oxide 0.1g ultrasonic in water (45KHz) 1h that obtain by Hummers method, form the dispersion liquid of 0.25mg/mL.
(2) adopt photoetching and lift-off technology in micro-processing technology to prepare gold electrode, the spacing of controlling positive and negative electrode is 800 μ m, and the spacing of adjacent electrode is 1 μ m.Electrode is placed in after 1mM mercaptoethylmaine aqueous solution immersion treatment 24h, and water and alcohol flushing are clean, obtain being assembled with amino electrode.
(3) by being assembled with amino electrode, being placed in graphene oxide dispersion liquid and soaking 24h, water and alcohol flushing are clean, thereby realize graphene oxide in the assembling of electrode surface.
(4) electrode that is assembled with graphene oxide is placed in the closed container of 100mL, in closed container, add 0.06mL pyrroles simultaneously, 90 ℃ add thermosetting pyrroles steam, reaction 24h, thereby realize the in-situ reducing of graphene oxide, obtain redox graphene gas sensor, resistance is 8.3M Ω.
Embodiment 3
(1), by 10 μ m left and right large scale graphite oxide 0.1g ultrasonic in water (45KHz) 1h that obtain by Hummers method, form the dispersion liquid of 1.0mg/mL.
(2) adopt photoetching and lift-off technology in micro-processing technology to prepare gold electrode, the spacing of controlling positive and negative electrode is 800 μ m, and the spacing of adjacent electrode is 1 μ m.Electrode is placed in after 1mM mercaptoethylmaine aqueous solution immersion treatment 24h, and water and alcohol flushing are clean, obtain being assembled with amino electrode.
(3) by being assembled with amino electrode, being placed in graphene oxide dispersion liquid and soaking 24h, water and alcohol flushing are clean, thereby realize graphene oxide in the assembling of electrode surface.
(4) electrode that is assembled with graphene oxide is placed in the closed container of 100mL, in closed container, add 0.06mL pyrroles simultaneously, 90 ℃ add thermosetting pyrroles steam, reaction 24h, thereby realize the in-situ reducing of graphene oxide, obtain redox graphene gas sensor, resistance is 14K Ω.
Embodiment 4
(1), by 10 μ m left and right large scale graphite oxide 0.1g ultrasonic in water (45KHz) 1h that obtain by Hummers method, form the dispersion liquid of 0.5mg/mL.
(2) adopt photoetching and lift-off technology in micro-processing technology to prepare gold electrode, the spacing of controlling positive and negative electrode is 800 μ m, and the spacing of adjacent electrode is 1 μ m.Electrode is placed in after 1mM mercaptoethylmaine aqueous solution immersion treatment 24h, and water and alcohol flushing are clean, obtain being assembled with amino electrode.
(3) by being assembled with amino electrode, being placed in graphene oxide dispersion liquid and soaking 24h, water and alcohol flushing are clean, thereby realize graphene oxide in the assembling of electrode surface.
(4) electrode that is assembled with graphene oxide is placed in the closed container of 100mL, in closed container, add 1.0mL pyrroles simultaneously, 90 ℃ add thermosetting pyrroles steam, reaction 24h, thereby realize the in-situ reducing of graphene oxide, obtain redox graphene gas sensor, resistance is 5K Ω.
Embodiment 5
(1), by 10 μ m left and right large scale graphite oxide 0.1g ultrasonic in water (45KHz) 1h that obtain by Hummers method, form the dispersion liquid of 0.5mg/mL.
(2) adopt photoetching and lift-off technology in micro-processing technology to prepare gold electrode, the spacing of controlling positive and negative electrode is 800 μ m, and the spacing of adjacent electrode is 1 μ m.Electrode is placed in after 1mM mercaptoethylmaine aqueous solution immersion treatment 24h, and water and alcohol flushing are clean, obtain being assembled with amino electrode.
(3) by being assembled with amino electrode, being placed in graphene oxide dispersion liquid and soaking 24h, water and alcohol flushing are clean, thereby realize graphene oxide in the assembling of electrode surface.
(4) electrode that is assembled with graphene oxide is placed in the closed container of 100mL, in closed container, add 0.06mL pyrroles simultaneously, 200 ℃ add thermosetting pyrroles steam, reaction 24h, thereby realize the in-situ reducing of graphene oxide, obtain redox graphene gas sensor, resistance is 2K Ω.
Embodiment 6
(1), by 10 μ m left and right large scale graphite oxide 0.1g ultrasonic in water (45KHz) 1h that obtain by Hummers method, form the dispersion liquid of 0.5mg/mL.
(2) adopt photoetching and lift-off technology in micro-processing technology to prepare gold electrode, the spacing of controlling positive and negative electrode is 800 μ m, and the spacing of adjacent electrode is 1 μ m.Electrode is placed in after 1mM mercaptoethylmaine aqueous solution immersion treatment 24h, and water and alcohol flushing are clean, obtain being assembled with amino electrode.
(3) by being assembled with amino electrode, being placed in graphene oxide dispersion liquid and soaking 24h, water and alcohol flushing are clean, thereby realize graphene oxide in the assembling of electrode surface.
(4) electrode that is assembled with graphene oxide is placed in the closed container of 100mL, in closed container, add 0.06mL pyrroles simultaneously, 60 ℃ add thermosetting pyrroles steam, reaction 24h, thereby realize the in-situ reducing of graphene oxide, obtain redox graphene gas sensor, resistance is 100K Ω.
Embodiment 7
(1), by 10 μ m left and right large scale graphite oxide 0.1g ultrasonic in water (45KHz) 1h that obtain by Hummers method, form the dispersion liquid of 0.5mg/mL.
(2) adopt photoetching and lift-off technology in micro-processing technology to prepare gold electrode, the spacing of controlling positive and negative electrode is 800 μ m, and the spacing of adjacent electrode is 1 μ m.Electrode is placed in after 1mM mercaptoethylmaine aqueous solution immersion treatment 24h, and water and alcohol flushing are clean, obtain being assembled with amino electrode.
(3) by being assembled with amino electrode, being placed in graphene oxide dispersion liquid and soaking 24h, water and alcohol flushing are clean, thereby realize graphene oxide in the assembling of electrode surface.
(4) electrode that is assembled with graphene oxide is placed in the closed container of 100mL, in closed container, add 0.06mL hydrazine hydrate simultaneously, 90 ℃ add thermosetting hydrazine hydrate steam, reaction 24h, thereby realize the in-situ reducing of graphene oxide, obtain redox graphene gas sensor, resistance is 15K Ω.
Embodiment 8
(1), by 10 μ m left and right large scale graphite oxide 0.1g ultrasonic in water (45KHz) 1h that obtain by Hummers method, form the dispersion liquid of 0.5mg/mL.
(2) adopt photoetching and lift-off technology in micro-processing technology to prepare gold electrode, the spacing of controlling positive and negative electrode is 800 μ m, and the spacing of adjacent electrode is 1 μ m.Electrode is placed in after 1mM mercaptoethylmaine aqueous solution immersion treatment 24h, and water and alcohol flushing are clean, obtain being assembled with amino electrode.
(3) by being assembled with amino electrode, being placed in graphene oxide dispersion liquid and soaking 24h, water and alcohol flushing are clean, thereby realize graphene oxide in the assembling of electrode surface.
(4) electrode that is assembled with graphene oxide is placed in the closed container of 100mL, in closed container, add 0.06mL ethylenediamine simultaneously, 90 ℃ add thermosetting ethylenediamine steam, reaction 24h, thereby realize the in-situ reducing of graphene oxide, obtain redox graphene gas sensor, resistance is 20K Ω.
The gas sensor that the embodiment 1 of take makes is illustrated as example contrasts accompanying drawing.
Fig. 1 is the electrode scanning electron microscope (SEM) photograph of the gas sensor that makes of the embodiment of the present invention 1, can see that redox graphene has been overlapped between electrode, to form galvanic circle.
Fig. 2 is the response curve of the gas sensor that makes of the embodiment of the present invention 1 to 50ppb ammonia molecule, can find out that described gas sensor shows extremely sensitive response performance to ammonia molecule.
In sum, the redox graphene gas sensor of preparing by said method has excellent sensing capabilities to ammonia molecule, and this preparation method's technique is simple, is suitable for a large amount of preparations of gas sensor.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and in the situation that not deviating from spirit of the present invention or essential characteristic, can realize the present invention with other concrete form.Therefore, no matter from which point, all should regard embodiment as exemplary, and be nonrestrictive, scope of the present invention is limited by claims rather than above-mentioned explanation, is therefore intended to include in the present invention dropping on the implication that is equal to important document of claim and all changes in scope.
In addition, be to be understood that, although this instructions is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of instructions is only for clarity sake, those skilled in the art should make instructions as a whole, and the technical scheme in each embodiment also can, through appropriately combined, form other embodiments that it will be appreciated by those skilled in the art that.
Claims (7)
1. a preparation method for the gas sensor based on redox graphene, is characterized in that, comprises the steps:
(1) preparation of large scale graphene oxide dispersion liquid
The graphene oxide that is of a size of 10～50 μ m is placed in to water, and ultrasonic processing 1min～3h under the frequency of 40～80kHz, forms the suspending liquid that monolithic disperses, and in described suspending liquid, graphene oxide concentration is 0.25～3mg/mL;
(2) amination of electrode is processed
Electrode is placed in after mercaptoethylmaine aqueous solution immersion treatment 1～48h, and water and alcohol flushing are clean, obtain being assembled with amino electrode;
(3) graphene oxide is in the assembling of electrode surface
The amino electrode that is assembled with that step (2) is obtained is placed in the described graphene oxide dispersion liquid of step (1) and soaks 1～24h, carries out graphene oxide in the assembling of electrode surface;
(4) preparation of redox graphene gas sensor
The electrode that is assembled with graphene oxide that step (3) is obtained is placed in closed container, in closed container, add liquid reducer simultaneously, add thermosetting reductive agent steam, realize the in-situ reducing of graphene oxide, thereby obtain redox graphene gas sensor;
Wherein, described liquid reducer is one or more the potpourri in pyrroles, hydrazine hydrate, ethylenediamine.
2. preparation method according to claim 1, is characterized in that: the concentration of described mercaptoethylmaine aqueous solution is 1～5mM.
3. preparation method according to claim 1, is characterized in that: described electrode adopts photoetching and the lift-off technology in micro-processing technology to prepare, and the spacing of controlling positive and negative electrode is 100 μ m～800 μ m, and the spacing of adjacent electrode is 1 μ m～10 μ m.
4. preparation method according to claim 1, is characterized in that: described closed container and the volume ratio of liquid reducer are 100:1～0.05.
5. preparation method according to claim 1, is characterized in that: described liquid reducer is heated to 60～200 ℃ and forms steam.
6. preparation method according to claim 1, is characterized in that: by described graphene oxide at reductive agent steam atmosphere situ reduction 12～24h.
7. the gas sensor based on redox graphene, is characterized in that: described gas sensor is prepared by the preparation method described in claim 1～6 any one.
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Application publication date: 20140305 |