CN106546635A - Preparation method based on p n abnormal shape heterojunction semiconductor nitrogen dioxide gas sensing layers - Google Patents
Preparation method based on p n abnormal shape heterojunction semiconductor nitrogen dioxide gas sensing layers Download PDFInfo
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- CN106546635A CN106546635A CN201610930445.9A CN201610930445A CN106546635A CN 106546635 A CN106546635 A CN 106546635A CN 201610930445 A CN201610930445 A CN 201610930445A CN 106546635 A CN106546635 A CN 106546635A
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- 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
- G01N27/129—Diode type sensors, e.g. gas sensitive Schottky diodes
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- 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
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Abstract
The present invention relates to the preparation method based on p n abnormal shape heterojunction semiconductor nitrogen dioxide gas sensing layers.The present invention is using monocrystalline silicon piece Si as insulating body, interdigitated electrodes and terminals are prepared in insulating body front, the mixed-powder for weighing zinc nitrate and copper nitrate respectively is dissolved in deionized water or organic solvent, stirring obtains homogeneous solution as presoma, the flame stream produced by plasma gun is sent to by non-atomized nozzle, through evaporation, decomposition, nucleation, heating and acceleration, impinged upon with molten particles and prepare directly over interdigitated electrodes Semiconductor gas sensors coating.Instant invention overcomes in the past because crystal grain is grown up, caused coating performance declines and fails etc. defect present in lubricant coating.Quick preparation nanometer of the invention, porous p n abnormal shape heterojunction semiconductor gas sensing layers, it is reproducible, it is possible to achieve various p n-type semiconductors are combined, to low concentration of NO2Response have the advantages that sensitivity is high, response speed is very fast.
Description
Technical field
The present invention relates to a kind of engineering and materials science field, more particularly to based on p-n abnormal shape heterojunction semiconductors
The preparation method of nitrogen dioxide gas sensing layer.
Background technology
Nitrogen dioxide (NO2) it is a kind of relatively conventional, the harmful gas with contaminative and toxicity in atmosphere pollution
Body, is a kind of highly active gaseous material, is that acid rain and photochemical fog primarily form reason.Further, since NO2Gas with
The acidifying of water reaction and combustion-supporting property, which has very big potential safety hazard in the industrial production.In addition, NO2Gas has to human body
Very big harm.Make one in NO2The very short time in atmosphere, pulmonary function can be also damaged, if long-time is in NO2Atmosphere
In enclosing, then may cause the permanent organic disease of pulmonary.Therefore, to NO2The monitoring and monitoring of gas just seems extremely important.
At this stage, metal-oxide base semiconductor due to with low cost, sensitivity it is high and respond it is fast with resume speed
The advantages of, it is commonly used for NO2Gas sensitive.But traditional metal-oxide base semiconductor is generally needed under conditions of high temperature
Energy normal work, this will play very big restriction to the use of metal-oxide base semiconductor, for example, increase power consumption, reduce which
The shortcomings of job security.Therefore, for sensor semiconductor, reduce its operating temperature and be just particularly important.Using
Radiation of visible light is the method for a replacement high-temperature heating.But for wide band gap semiconducter, due to its wider band gap,
Visible ray can not be allowed to excite, therefore, wide band gap semiconducter can not be worked under visible light illumination.
As most of p-type semiconductors are narrow gap semiconductor, and most n-type quasiconductor is wide band gap semiconducter, because
This builds the irradiation of the p-n abnormal shape heterojunction composites that are made up of the narrower p-type of band gap and wider n-type semiconductor in visible ray
Under can realize the response of preferable room temperature, than INVENTIONConventional metal-oxide base semiconductor sensor, p-n abnormal shape heterojunction semiconductors
In interface as the electronics on high level and hole can form a broader space-charge region to low-lying level transfer, cause
Energy band bends.It is passed through NO2Afterwards, space-charge region broadens, band curvature aggravation, and electronics transport channel just narrows, so as to reality
Now to NO2Gas is preferably responded.
Before the present invention makes, at present can be by method systems such as the multistep such as hydro-thermal method and sol-gal process synthesis
Standby p-n abnormal shapes heterojunction semiconductor gas sensitive, but these methods are present, and synthesis step is complicated, combined coefficient is low and repetitive rate
The hydrothermal reaction kettle of low shortcoming, such as 50mL can only prepare several milligrams of powder, and the material morphology being synthesized every time and
Granular size cannot guarantee that completely the same, therefore be badly in need of that a kind of alternative method of exploitation can simple and practical ground be extensive prepares p-n
Special-shaped heterojunction semiconductor gas sensitive.
CN1424779 is a kind of manufacture method of the semiconductor transducer gas sensor of detection nitrogen dioxide, and the method adopts
The oxidation of indium stannum is prepared in the quartz substrate of manufactured gold electrode and ruthenium oxide resistance zone of heating with ultrasonic spray pyrolysis
Thing thin film, and made by nitrogen dioxide all table of the nitrogen dioxide gas sensor gas sensor to 0.1ppm to 5ppm concentration ranges
Reveal good gas-sensitive property.
CN105092654A is a kind of self-driven gas sensor based on p-n heterojunction, and its structure includes quasiconductor
Substrate, the insulating barrier being formed in substrate and the first metal electrode layer, formation the second metal on the insulating layer that material is formed
Electrode layer and the single wall carbon nano-tube film layer being formed on the second metal electrode layer, wherein, the insulating barrier arranges at least one
Individual window, second metal electrode layer surround the window, and the single wall carbon nano-tube film layer fills the window, with
The substrate contact.
CN104195499A is a kind of method that plasma spraying with liquid feedstock prepares micro-nano compound structure coating, and the method includes
Following steps：(1) solution salt, suspension particle are added in solvent, obtain suspension；(2) suspension is passed through into non-atomized
Nozzle is sent in the flame stream of plasma gun generation, and the flame stream that plasma gun is produced sprays to pretreated matrix surface,
Composite structure coating is obtained on matrix.The method can solve the problem that or part solves thermal barrier coating, SOFC electricity
The caused painting because crystal grain is grown up present in pole coating, high temperature gas sensor gas sensing layer, high-temperature wearable and lubricant coating
Layer hydraulic performance decline and Problem of Failure.
The content of the invention
The purpose of the present invention is that and overcomes drawbacks described above, develops based on p-n abnormal shape heterojunction semiconductor titanium dioxide nitrogen
The preparation method of photosensitive layer.
The technical scheme is that：
Based on the preparation method of p-n abnormal shape heterojunction semiconductor nitrogen dioxide gas sensing layers, which is mainly characterized by, bag
Containing following steps：
(1) using monocrystalline silicon piece Si as insulating body；
(2) interdigitated electrodes and wiring are prepared in insulating body front by silk screen printing, sputtering, evaporation or spraying method
End；
(3) mixed-powder for weighing zinc nitrate and copper nitrate respectively is dissolved in deionized water or organic solvent, using magnetic force
Agitator or other agitating devices obtain homogeneous solution as presoma；
(4) preparation-obtained solution presoma is sent to into the flame produced by plasma gun by non-atomized nozzle
Stream；
(5) precursor solution is through evaporation, decomposition, nucleation, heating and accelerates, and impinges upon interdigitated electrodes with molten particles
Surface prepares Semiconductor gas sensors coating.
Monocrystalline silicon piece Si in the step (1) is to adopt aluminium oxide Al2O3Or through surface oxidation treatment.
Advantages of the present invention and effect are：
First, it is heterogeneous nanometer, porous p-n abnormal shapes directly can quickly to be prepared with solution presoma plasma spraying
Pn junction p n gas sensing layer, preparation process are quick and easy and reproducible.
Second, p-n abnormal shape heterojunction semiconductor gas sensing layer can realize that various p-n junction semi-conducting materials are combined, and make
The standby gas sensitive for obtaining is to low concentration of NO2Response have the advantages that sensitivity is high, response speed is very fast.
Indium sesquioxide. gas sensitive is prepared using ultrasonic spray pyrolysis compared to patent CN1424779, what this patent was adopted
It is the gas sensitive of solution plasma spraying preparation.It is served only for preparing Indium sesquioxide. compared to patent CN1424779, this patent can be made
Standby is all of p-n abnormal shapes heterojunction semiconductor, therefore, the species of the gas sensitive that this patent can be prepared is more, is suitable for model
Enclose wider.
Compared to patent CN105092654A, the p-type material that this patent is adopted for single wall carbon nano-tube film, this patent institute
The p-type material for adopting is for quasiconductor, and relative to the multiple structure of patent CN105092654A, this patent is made using mixed solution
For presoma, the complicated synthesis step needed for without the need for CN105092654A, additionally, the gas sensing layer technology of preparing of this patent is operated more
Plus it is simple, with deposition velocity it is fast, coating porosity is controllable the characteristics of.
Prepared by patent CN104195499A is micro-nano compound structure coating, and prepared by this patent is nano composite structure
Coating, and patent CN104195499A uses suspension and solution mixing feeding, this patent uses mixed solution, makes
It is different with spraying raw material.In addition, prepared by this patent be nitrogen dioxide gas sensitive, it is more clear and definite to prepare material category,
Using specifically.
Describe the present invention below in conjunction with the drawings and specific embodiments, but it is not as a limitation of the invention.
Description of the drawings
The scanning electron microscope schematic diagram of the CuO@ZnO coatings of Fig. 1 --- the embodiment of the present invention 1.
The sensor of Fig. 2 --- the embodiment of the present invention 1 is to NO2The response schematic diagram of gas.
Specific embodiment
The present invention technical thought be：
To solve a difficult problem of the pure wide band gap semiconducter under visible light illumination without response, there is provided a kind of different based on p-n abnormal shapes
The preparation method of matter pn junction p n nitrogen dioxide gas sensing layer, it is therefore an objective to overcome pure wide band gap semiconducter not absorb lacking for visible ray
Point, prepares p-n abnormal shape heterojunction semiconductor air-sensitive coatings by solution plasma spraying, as p-type semiconductor is mostly arrowband
Gap semiconductor, therefore the visible absorption scope of spraying state coating can be greatly widened, additionally, the electron transfer of p-n storerooms
Also gas sensing layer air-sensitive performance at room temperature can significantly be improved.
With reference to specific embodiment, the invention will be further described, it is clear that described embodiment is the present invention one
Section Example, rather than whole embodiments.Based on embodiments of the invention, one of ordinary skill in the art is not making
The every other embodiment obtained under the premise of creative work, belongs to the scope of protection of the invention.
Chemical raw material required for the present invention is commercially available, or is obtained using conventional method.
The matrix that the present invention is adopted can be buied from market for pure zirconia aluminium flake or the monocrystalline silicon piece through oxidation processes.
The present invention measures gas sensor to NO using Devince By Dynamic Gas Ration Method2The response performance of gas, total gas flow rate is
1000mL/min, sensitivity definition are Rg/Ra, wherein RgAnd RaIt is air-sensitive film in NO2With the resistance under synthesis of air atmosphere.
Embodiment 1：
1. using aluminium oxide as insulating body, by 30 × 20 × 1mm alumina wafers successively in deionized water and ethanol
In, and aid in, with ultrasound, cleaning 5 minutes, 80 DEG C of dry for standby.
2., using the method for vacuum coating, using metal mask pattern, one layer of chromium, 0.3 μm of thickness, for improving first are prepared
Bond strength, then one layer 0.5 μm of evaporation is golden, obtains interdigitated electrodes.
3. 14.87 and 1.21g lenticular zinc nitrate (Zn (NO are weighed respectively3)2) and copper nitrate (Cu (NO3)2), it is dissolved in
In 250mL deionized waters, blue-tinted transparent mixed solution presoma is obtained using magnetic agitation mode.
4., using the method for solution presoma plasma spraying, CuO@ZnO coatings, spray are sprayed directly over interdigitated electrodes
Apply apart from 100mm, it is 40L/min argon and 2L/min hydrogen that plasma generates gas, and substrate temperature is room temperature (25 DEG C), sprays work(
Rate is 25kW, and the CuO@ZnO coatings that thickness is 5.0 μm are obtained on interdigitated electrodes.
5. the CuO@ZnO coatings for preparing are passed through the table of X-ray diffraction XRD and x-ray photoelectron spectroscopy XPS
Levy, as a result show coating for the hexagonal wurtzite ZnO and CuO of Emission in Cubic
6. the CuO@ZnO coatings for preparing are analyzed by field emission scanning electron microscope FE-SEM, coating presents porous
Nanostructured, as shown in Figure 1.
7. the CuO@ZnO sensors obtained by carry out air-sensitive test, as a result show, spray the CuO@ZnO gas sensitives of state
To NO2The gas-sensitive property of n-type semiconductor is shown, 0.2ppm and 1.0ppm NO are passed through2When, the sensitivity of sensor is respectively
1.2 and 4.8 (as shown in Figure 2).
Embodiment 2：
The present embodiment with the difference of embodiment 1 is：Weigh 25.13 and 1.42g lenticular chlorinations in step 3 respectively
Tungsten (WCI6) and copper nitrate (Cu (NO3)2), be dissolved in 500mL deionized waters, blue-tinted transparent is obtained using magnetic agitation mode molten
Liquid presoma；In step 4, using the method for solution plasma spraying, CuO@WO are sprayed directly over interdigitated electrodes3Apply
Layer, spray distance 100mm, it is 45L/min argon and 3L/min hydrogen that plasma generates gas, and substrate temperature is 25 DEG C, sprays work(
Rate is 27kW, and the CuO@WO that thickness is 20.0 μm are obtained on interdigitated electrodes3Coating；In step 7, coating to 0.1ppm and
0.3ppm NO2When, the sensitivity of sensor is respectively 1.9 and 5.1.
Embodiment 3：
The present embodiment with the difference of embodiment 1 is：Weigh 27.15 and 2.31g lenticular chlorinations in step 3 respectively
Stannum (SnCl4) and copper nitrate (Cu (NO3)2) be dissolved in 500mL dehydrated alcohol, solution presoma is obtained using magnetic agitation mode；
In step 4, using the method for solution plasma spraying, CuO@SnO are sprayed directly over interdigitated electrodes2Coating, spray away from
From 90mm, it is 40L/min argon and 2L/min hydrogen that plasma generates gas, and substrate temperature is 50 DEG C, and spray power is 25kW,
The CuO@SnO that thickness is 10.0 μm are obtained on interdigitated electrodes2Coating；In step 7, coating is to 0.4ppm and 1.2ppm NO2
When, the sensitivity of sensor is respectively 1.8 and 4.7.
Embodiment 4：
The present embodiment with the difference of embodiment 1 is：Weigh 26.8 and 1.63g lenticular metatitanic acids in step 3 respectively
Butyl ester ((CH3CH2CH2CH2O)4) and copper nitrate (Cu (NO Ti3)2) be dissolved in 500mL dehydrated alcohol, followed by magnetic agitation
Mode obtains solution presoma；In step 4, using the method for solution plasma spraying, spray directly over interdigitated electrodes
CuO@TiO2Coating, spray distance 100mm, it is 50L/min argon and 3L/min hydrogen that plasma generates gas, and substrate temperature is 25
DEG C, spray power is 27kW, and the CuO@TiO that thickness is 10.0 μm are obtained on interdigitated electrodes2Coating；In step 7, coating
To 0.3ppm and 1.0ppm NO2When, the sensitivity of sensor is respectively 2.1 and 7.3.
Embodiment 5：
The present embodiment with the difference of embodiment 1 is：Weigh 32.16 and 4.35g lenticular chlorinations in step 3 respectively
Indium (InCl3) and copper nitrate (Cu (NO3)2) be dissolved in 500mL deionized waters, obtain before solution followed by magnetic agitation mode
Drive body；In step 4, using the method for solution plasma spraying, CuO@In are sprayed directly over interdigitated electrodes2O3Coating, spray
Apply apart from 110mm, it is 50L/min argon and 2L/min hydrogen that plasma generates gas, and substrate temperature is 25 DEG C, and spray power is
26kW, obtains the CuO@In that thickness is 15.0 μm on interdigitated electrodes2O3Coating；In step 7, coating to 0.1ppm and
0.5ppm NO2When, the sensitivity of sensor is respectively 0.6 and 4.1.
Claims (2)
1. the preparation method based on p-n abnormal shape heterojunction semiconductor nitrogen dioxide gas sensing layers, it is characterised in that comprising following step
Suddenly：
(1) using monocrystalline silicon piece Si as insulating body；
(2) interdigitated electrodes and terminals are prepared in insulating body front by silk screen printing, sputtering, evaporation or spraying method；
(3) mixed-powder for weighing zinc nitrate and copper nitrate respectively is dissolved in deionized water or organic solvent, using magnetic agitation
Device or other agitating devices obtain homogeneous solution as presoma；
(4) preparation-obtained solution presoma is sent to into the flame stream produced by plasma gun by non-atomized nozzle；
(5) precursor solution is through evaporation, decomposition, nucleation, heating and accelerates, and impinges upon interdigitated electrodes with molten particles and just goes up
Side prepares Semiconductor gas sensors coating.
2. the preparation method based on p-n abnormal shape heterojunction semiconductor nitrogen dioxide gas sensing layers according to claim 1, which is special
Levy be monocrystalline silicon piece Si in the step (1) be to adopt aluminium oxide Al2O3Or through surface oxidation treatment.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115389570A (en) * | 2022-08-02 | 2022-11-25 | 昌吉学院 | Composite material gas sensor and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115389570A (en) * | 2022-08-02 | 2022-11-25 | 昌吉学院 | Composite material gas sensor and preparation method thereof |
| CN115389570B (en) * | 2022-08-02 | 2024-05-31 | 昌吉学院 | Composite material gas sensor and preparation method thereof |
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Application publication date: 20170329 |