CN105510398A - Film-type alcohol gas-sensitive sensor and preparation method thereof - Google Patents
Film-type alcohol gas-sensitive sensor and preparation method thereof Download PDFInfo
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- CN105510398A CN105510398A CN201510563473.7A CN201510563473A CN105510398A CN 105510398 A CN105510398 A CN 105510398A CN 201510563473 A CN201510563473 A CN 201510563473A CN 105510398 A CN105510398 A CN 105510398A
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Abstract
The invention discloses a ZnSnO-based amorphous oxide semiconductor film-based film-type alcohol gas-sensitive sensor and a preparation method thereof. The alcohol gas-sensitive sensor comprises an insulation substrate layer, an electrode layer and a sensing layer. The sensing layer is an amorphous oxide semiconductor film. The invention also provides a preparation method of the alcohol gas-sensitive sensor. The preparation method comprises insulation substrate layer preparation, metal electrode preparation and gas-sensitive sensing layer ZnSnO amorphous film preparation. The sensing layer is prepared through a solution chemical method. The preparation method has simple processes and a low cost. The alcohol gas-sensitive sensor utilizing the amorphous oxide semiconductor film as a sensing layer has the advantages of high detection sensitivity, simple preparation processes and good repeatability and has important application value in fields of military and civilian use.
Description
Technical field
The present invention relates to gas sensor field, particularly relate to a kind of amorphous oxide semiconductor film-type alcohol gas sensor and preparation method thereof.
Background technology
Along with rapid economic development, the quality of life of people improves rapidly, and environmental protection consciousness strengthens gradually, and the demand of people to gas sensor is outstanding day by day.The principle of work of gas sensor is: gas molecule has an impact to sensing layer surface and internal resistance, reflects response to gas and detection by the change of resistance, thus realizes the detection to gas concentration and composition.Find that metal-oxide semiconductor (MOS) has gas sensitive effect since 20 beginnings of the century, its development obtains the extensive concern of researcher.Mainly be applied in the fields such as traffic, food, safety, mine and industrial automation monitoring on a large scale at present, the multiple gases such as detection methane, carbon monoxide, hydrogen, alcohol, serve the effect do not replaced.
The gas sensitive be widely studied at present comprises ZnO, SnO
2, Fe
2o
3deng semiconductor material.Be generally that the powder gas sensitive of preparation is coated on insulated substrate in actual applications, the more annealed step such as aging form gas sensing layer, applies in the related art after the miniaturization and intellectuality of device.But this kind of sensing material is the bonding by nano particle, grain boundaries trapping centre is many, chemical stability is not high, causes the sensitivity of sensor not high.Although monodimension nanometer material is based on its higher specific surface area and stronger sensitivity in decades recently, show extraordinary development prospect.But well-known, monodimension nanometer material makes material itself extremely unstable due to its huge specific surface area, be unfavorable for that the long-term stability of sensor uses.At present, the gas sensor that people develop is substantially all based on nano material, but the feature of nano material self and preparation flow thereof determine it is difficult to realize large scale integration and produces, also with existing microelectric technique and integrated technique incompatible.
Amorphous oxide semiconductor semiconductive thin film is a kind of very important semiconductor oxide materials, between more than ten nearest years, obtain large development, and its special electric property makes this kind of material be hopeful very much to be applied in optoelectronic information and sensory field.At present, amorphous oxide semiconductor semiconductive thin film has obtained Preliminary Applications in fields such as display techniques of new generation, as the channel layer as thin film transistor (TFT) (TFT); Also there is report amorphous oxide semiconductor semiconductive thin film in document for the achievement in research of ultraviolet detection, bio-sensing etc., but yet there are no and utilize amorphous oxide semiconductor semiconductor as gas sensing layer to be applied in gas sensor field.As amorphous oxide semiconductor semiconductive thin film, it possesses the performance not available for general nano material, such as, do not have that crystal boundary trapping centre, chemical stability are high, radiation resistance advantages of higher.Particularly, utilize amorphous oxide semiconductor semiconductor film film production gas sensor, with existing microelectric technique and planar technology mutually compatible, the microminiaturization of device and integrated can be realized, thus the intellectuality and the portability that realize gas sensor is also easy to, to wearable production development, this is and the maximum difference of the existing gas sensor based on nano material and advantage.Therefore, the gas sensor based on amorphous oxide semiconductor semiconductive thin film will be a kind of novel gas detector, represents following developing direction, has huge potential market application prospect.
Summary of the invention
For overcoming the problems of the prior art, the present invention aims to provide a kind of film-type alcohol gas sensor based on amorphous oxide semiconductor film and preparation method thereof, carries out the exploration of Novel air dependent sensor.
The invention provides a kind of film-type alcohol gas sensor, described film-type alcohol gas sensor, comprises dielectric substrate layers, electrode layer and sensing layer; Wherein electrode layer is placed on bottom containing two electrodes be oppositely arranged, dielectric substrate, sensing layer and electrode layer to be placed in dielectric substrate layers and to be that levels is arranged; Wherein said sensing layer is amorphous oxide semiconductor film.
Further, electrode layer is arranged at dielectric substrate layers upper surface, and sensing layer is covered on electrode layer.
Further, amorphous oxide semiconductor film as sensing layer is ZnSnO base amorphous oxide semiconductor film, wherein can add a small amount of metallic element and comprise the sensing capabilities that the units such as Al, Ga, Si, Nb, In, Hf, Zr usually regulate and control its chemical composition and film.
Further, the chemical formula of described ZnSnO base amorphous oxide semiconductor film is Zn
xsn
yo
x+2y, wherein 0.1≤x≤0.5,0.5≤y≤0.9, and x+y=1.
Further, the described amorphous oxide semiconductor film thickness as sensing layer is 50nm ~ 800nm.
Present invention also offers a kind of preparation method of alcohol gas sensor, the method comprises the following steps:
select dielectric substrate layers, and dielectric substrate layers is thoroughly cleaned, dry after cleaning;
electrode layer is prepared on dielectric substrate layers surface; And etch, form two electrodes be oppositely arranged;
electrode layer is prepared amorphous oxide semiconductor film, as the sensing layer of alcohol gas sensor.
Or the making step order of this alcohol gas sensor is
, thus the film-type alcohol gas sensor formed is followed successively by dielectric substrate layers, the sensing layer of amorphous oxide semiconductor film, electrode layer from bottom to up.
Further, step
the middle amorphous oxide semiconductor as sensing layer is by a kind of ZnSnO base amorphous oxide semiconductor film prepared in solution chemical processes.
Beneficial effect of the present invention is:
1) the film-type alcohol gas sensor based on ZnSnO base amorphous oxide semiconductor film that the present invention makes is a kind of novel sensor, and its detection sensitivity is high, is expected to realize its application in various fields such as military and civilians.
2) amorphous oxide semiconductor film-type alcohol gas sensor, there is the current performance not available for nano material sensor device, such as there is not the nano effect of nano material, substantially reduce the generation of defect, and chemical stability is higher, radiation resistance is higher.Utilize amorphous oxide semiconductor film to make gas sensor, the gas sensor overcome based on nano material is difficult to realize large scale integration produces, is difficult to and the shortcoming such as existing microelectric technique and integrated process compatible.Amorphous oxide semiconductor film type sensor can with existing microelectric technique and planar technology mutually compatible, the microminiaturization of device and integrated can be realized, be thus also easy to the intellectuality and the portability that realize gas sensor, to wearable production development.Amorphous oxide semiconductor film-type alcohol gas sensor prepared by the present invention, confirms the possibility that amorphous oxide semiconductor film is applied on gas sensor.
3) the invention provides the preparation method of amorphous oxide semiconductor alcohol gas sensor, wherein preparation method's dirigibility of sensing layer amorphous oxide semiconductor film is strong, traditional film-forming method can be selected, comprise conventional magnetic control, the physical methods such as pulsed laser deposition; Also can select chemical solution method, this method preparation technology is simple, cost is low, and can realize the low-temperature epitaxy of film, can considerably increase the chance industrially applied.
4) the invention provides the preparation method of amorphous oxide semiconductor film-type alcohol gas sensor in addition, wherein obtained amorphous oxide semiconductor film-sensing layer surfacing, distributed components, be easy to corrosion, can large area prepare, and yield rate is high.
5) the amorphous oxide semiconductor film-type alcohol gas sensor for preparing of the present invention, for Conventional nano material, its specific surface area is extremely little, but the sensor that the performance of sensor but can be prepared with nano material is suitable.
Accompanying drawing explanation
Fig. 1 is the structural representation of film-type alcohol gas sensor of the present invention.
Fig. 2 is the schematic cross-section in A-A direction in Fig. 1.
Fig. 3 is another structural representation of film-type alcohol gas sensor of the present invention.
Fig. 4 be in example 1 film-type alcohol gas sensor to the response diagram of the alcohol content of 20ppm concentration.
Fig. 5 be in example 1 film-type alcohol gas sensor to the response diagram of the alcohol content of 100ppm concentration.
Fig. 6 be in example 1 film-type alcohol gas sensor to the response diagram of the alcohol content of 500ppm concentration.
Wherein, in figure: 1 is dielectric substrate layers, 2 is electrode layer, and 3 is sensing layer.
Embodiment
The present invention is further illustrated below in conjunction with accompanying drawing and instantiation.Be illustrated in figure 1 film-type alcohol gas sensor of the present invention, Fig. 2 is the sectional view of Fig. 1 along A-A direction, can see in figure, film-type alcohol gas sensor of the present invention comprises dielectric substrate layers, electrode layer and sensing layer, wherein electrode layer is relatively arranged on the electrode of substrate top surface containing two, and sensing layer is covered on electrode layer.A kind of preferred structure being only film-type alcohol gas sensor of the present invention shown in Fig. 1 and Fig. 2, this structure is owing to being placed in the top of electrode layer by sensing layer, at the skin of whole sensor, therefore can increase effective contact area of induction gas and sensing layer, therefore effectively can improve the detectivity of sensor.Film alcohol gas sensor of the present invention, also can adopt the structure as Fig. 3, sensing layer is arranged at the upper surface of substrate, and electrode layer covers the top of sensing layer.Dielectric substrate layers of the present invention can be any one in sapphire, quartz, glass, pottery, polycarbonate or polyethylene terephthalate.And the preparation of alcohol gas sensor sensing layer of the present invention can be the chemical methodes such as traditional magnetron sputtering, pulsed laser deposition physical method and solution chemical processes; The sensing layer of alcohol gas sensor of the present invention is ZnSnO base amorphous oxide semiconductor film, can add the sensing capabilities that the units such as appropriate Al, Ga, Si, Nb, In usually regulate and control its chemical composition and film according to suitably requiring in ZnSnO base film; The present invention as the amorphous oxide semiconductor film thickness of alcohol gas sensor preferably between 50 ~ 800nm.The material of the electrode layer of alcohol gas sensor of the present invention can be the good conducting metals of resistance to elevated temperatures such as Pd, Ag, the material of two electrodes can be identical, also different metals can be adopted, for preparing simple consideration, preferably two electrodes adopt the metal electrode of identical material, and the present invention is preferably Ag electrode, and two electrodes are oppositely arranged in the middle of substrate and sensing layer, interdigital shape as shown in Figure 1 can arrange, also can adopt other forms be oppositely arranged; Operationally, alcohol molecule can provide electronics to enter sensing layer to alcohol gas sensor of the present invention, thus causes surface resistance to change, and produces response.Can see from the present invention, amorphous oxide semiconductor film ZnSnO base film type alcohol gas sensor has very strong response to alcohol, and amorphous oxide semiconductor film is as the sensing layer of alcohol sensor, compare nano material and there is no nano effect, therefore chemical stability is high, radiation resistance is high, and there is not crystal boundary trapping centre in this kind of material.
The preparation method of film-type alcohol gas sensor of the present invention, step comprises substrate preparation process, prepared by metal electrode and the sensing layer forming step of etching step and amorphous oxide semiconductor film.
First carrying out substrate preparation process, choose substrate, carry out the selection of substrate according to subsequent sensor part, can be sapphire, quartz, glass, pottery, polycarbonate or polyethylene terephthalate etc.; Substrate is cleaned thoroughly, dry after cleaning.
Then in the preparation of the enterprising row metal electrode of substrate, in the present invention, the formation of metal electrode can adopt magnetron sputtering method, electron beam evaporation technique etc., preferred electron beam evaporation technology of the present invention, and its technology controlling and process is the general knowledge of those skilled in the art; Then etched by the metal electrode of formation, the selection of etching also can carry out wet method or dry etching.Two electrodes of alcohol sensor of the present invention do not limit it and whether use material of the same race, whether adopt same formation method, and the present invention is preferably two electrodes and is electron-beam vapor deposition method and prepares Ag electrode.
Finally carry out the preparation of sensing layer, common method for making has magnetron sputtering method, pulsed laser deposition, chemical solution method etc., preferably using chemical solution method in the present invention, is a kind of cryochemistry reaction method, and use the method technique is simple, cost is low, be easy to large area preparation; Adopt preferred method preparation of the present invention as the ZnSnO base amorphous oxide semiconductor film of sensing layer, control the material characteristic of this film by controlling its fabrication process parameters, such as, select the solvent of suitable both Zn, Sn source material and proportioning thereof, the concentration of control Zn, Sn precursor solution, spin speed when controlling spin-coating film and follow-up annealing temperature and time etc.; In preparation process, can add according to suitably requiring the sensing capabilities that the units such as appropriate Al, Ga, Si, Nb, In usually regulate and control its chemical composition and film in ZnSnO base film.
Certainly, more than the preferred preparation method of the present invention, also by the preparation process reversed order of the preparation process of electrode in above-mentioned preparation method and amorphous oxide semiconductor film-sensing layer, substrate first can carry out the preparation of sensing layer, sensing layer makes electrode layer again.
Below for ZnSnO base amorphous oxide semiconductor film prepared by chemical solution method, its preparation as film-type alcohol gas sensor and the application in alcohol detection thereof are described.
Example 1
I) prepare quartz substrate, thoroughly cleaning substrate is also dry;
II) in above-mentioned quartz substrate, the electrode of alcohol gas sensor is made: the present invention adopts electron beam evaporation technique to deposit the Ag metal of one deck 100nm as electrode; Etch afterwards, between electrode, be spaced apart 400 μm.As shown in Figure 1;
III) then on above-mentioned obtained Ag electrode layer, chemical solution method is utilized to prepare the sensing layer of alcohol sensor.This example adopts chemical solution method to prepare ZnSnO base noncrystal membrane as sensing layer, and this example selects Zn (NO
3)
26H
2o and SnCl
2as the source material of both Zn, Sn, dimethoxy-ethanol, diacetone and ammonia spirit, as the solvent of both Zn, Sn source material, join to obtain precursor solution, and by spin-coating film and annealing in process, obtaining chemical formula is Zn
0.36sn
0.64o
1.64amorphous oxide semiconductor film.Carry out thickness measuring to obtained film, test result is: film thickness is about 120nm.
To Zn obtained above
0.36sn
0.64o
1.64amorphous oxide semiconductor film carries out alcohol-detection characteristic test as alcohol sensor, and probe temperature is 450 DEG C, and wherein the content of alcohol is respectively 20ppm, 100ppm and 500ppm, the response obtained and restorability as follows:
1), during alcohol content 20ppm, response and release time, detection sensitivity was 3.21, as shown in Figure 4 within 10s;
2), during alcohol content 100ppm, response and release time, detection sensitivity was 4.76, as shown in Figure 5 within 10s;
3), during alcohol content 500ppm, response and release time, detection sensitivity was 31.18, as shown in Figure 6 within 10s.
Example 2
I) Sapphire Substrate is prepared; Thorough cleaning substrate is also dry; Different from example 1 sapphire has been selected to be substrate for this example;
II) in above-mentioned quartz substrate, the Ag electrode of alcohol gas sensor is made: just the same with the electrode fabrication of example 1;
III) then on above-mentioned obtained Ag electrode layer, chemical solution method is utilized to prepare the sensing layer of alcohol sensor.This example this step and example 1 unlike, when making the presoma in Zn and Sn source, the Zn:Sn=0.1:0.9 that both proportioning adopts.The molecular formula of the amorphous oxide semiconductor film finally obtained is: Zn
0.1sn
0.9o
1.9; Carry out thickness measuring to obtained film, test result is: film thickness is about 50nm.
To Zn obtained above
0.1sn
0.9o
1.9amorphous oxide semiconductor film carries out alcohol-detection characteristic test as alcohol sensor, and probe temperature is 450 DEG C, and wherein the content of alcohol is respectively 20ppm, 100ppm and 500ppm, the response obtained and restorability as follows:
1), during alcohol content 20ppm, response and release time, detection sensitivity was 4.12 within 10s;
2), during alcohol content 100ppm, response and release time, detection sensitivity was 6.53 within 10s;
3), during alcohol content 500ppm, response and release time, detection sensitivity was 46.27 within 10s.
Example 3
I) quartz substrate is prepared; Thorough cleaning substrate is also dry; The same with example 1;
II) in above-mentioned quartz substrate, make the Ag electrode of alcohol gas sensor; Just the same with the electrode fabrication of example 1;
III) then on above-mentioned obtained Ag electrode layer, chemical solution method is utilized to prepare the sensing layer of alcohol sensor.This example this step and example 1 unlike, when making the presoma in Zn and Sn source, the Zn:Sn=0.5:0.5 that both proportioning adopts.The molecular formula of the amorphous oxide semiconductor film finally obtained is: Zn
0.5sn
0.5o
1.5; Carry out thickness measuring to obtained film, test result is: film thickness is about 800nm.
To Zn obtained above
0.5sn
0.5o
1.5amorphous oxide semiconductor film carries out alcohol-detection characteristic test as alcohol sensor, and probe temperature is 450 DEG C, and wherein the content of alcohol is respectively 20ppm, 100ppm and 500ppm, the response obtained and restorability as follows:
1), during alcohol content 20ppm, response and release time, detection sensitivity was 3.51 within 10s;
2), during alcohol content 100ppm, response and release time, detection sensitivity was 5.37 within 10s;
3), during alcohol content 500ppm, response and release time, detection sensitivity was 37.09 within 10s.
The sensing capabilities that the units such as appropriate Al, Ga, Si, Nb, In usually regulate and control its chemical composition and film can be added according to demand in sensing layer in preparation process in above-mentioned each example.
Claims (7)
1. a film-type alcohol gas sensor, described film-type alcohol gas sensor, comprises dielectric substrate layers, electrode layer and sensing layer; Wherein electrode layer is placed on bottom containing two electrodes be oppositely arranged, dielectric substrate, sensing layer and electrode layer to be placed in dielectric substrate layers and to be that levels is arranged; It is characterized in that: described sensing layer is amorphous oxide semiconductor film.
2. a kind of film-type alcohol gas sensor according to claim 1, is characterized in that: electrode layer is arranged at dielectric substrate layers upper surface, and sensing layer is covered on electrode layer.
3. a kind of film-type alcohol gas sensor according to claim 1, is characterized in that: the amorphous oxide semiconductor film as sensing layer is ZnSnO base amorphous oxide semiconductor film.
4. a kind of film-type alcohol gas sensor according to claim 3, is characterized in that: the chemical formula of described ZnSnO base amorphous oxide semiconductor film is Zn
xsn
yo
x+2y, wherein 0.1≤x≤0.5,0.5≤y≤0.9, and x+y=1.
5. a kind of film-type alcohol gas sensor according to claim 1, is characterized in that: the described amorphous oxide semiconductor film thickness as sensing layer is 50nm ~ 800nm.
6. prepare a method for film-type alcohol gas sensor described in any one of Claims 1 to 5, it is characterized in that comprising the following steps:
1. select dielectric substrate layers, and dielectric substrate layers is thoroughly cleaned, dry after cleaning;
2. electrode layer is prepared on dielectric substrate layers surface; And etch, form two electrodes be oppositely arranged;
3. on electrode layer, amorphous oxide semiconductor film is prepared, as the sensing layer of alcohol gas sensor;
Or its making step order is
, thus the film-type alcohol gas sensor formed is followed successively by dielectric substrate layers, the sensing layer of amorphous oxide semiconductor film, electrode layer from bottom to up.
7. the preparation method of a kind of film-type alcohol gas sensor according to claim 6, is characterized in that: step 3. in be the ZnSnO base amorphous oxide semiconductor film prepared by solution chemical processes as the amorphous oxide semiconductor of sensing layer.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2018014719A1 (en) * | 2016-07-20 | 2018-01-25 | 广州易活生物科技有限公司 | Detection electrode structure, detection aperture plate, and prefabricated detection aperture plate |
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