CN103884743A - Heterojunction NO2 gas sensor based on CuO-NiO core-shell structure as well as preparation method thereof - Google Patents
Heterojunction NO2 gas sensor based on CuO-NiO core-shell structure as well as preparation method thereof Download PDFInfo
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Abstract
The invention discloses a heterojunction NO2 gas sensor based on a CuO-NiO core-shell structure as well as a preparation method thereof, and belongs to the technical field of gas sensors. The sensor sequentially consists of an Al2O3 substrate, a Pd metal interpolation electrode and a CuO-NiO core-shell structured heterojunction nano microsphere sensitive layer prepared on the interpolation electrode from bottom to top, wherein the heterojunction nano microsphere sensitive layer has the thickness of 2-4 microns, and has the particle size of 600-800 nm; the metal interpolation electrode has the width and the interval of 0.15-0.20 mm, and has the thickness of 100-150 nm. A CuO/NiO core-shell structured nano microsphere is adopted as a sensitive material, and not only is the high specific surface area of the nano microsphere is utilized, but also the heterostructure of the CuO/NiO core-shell structured nano microsphere can be effectively utilized to improve the air-sensitive response. Meanwhile, the process provided by the invention is simple, and the prepared sensor is small in size, is suitable for mass production, and has important application value.
Description
Technical field
The invention belongs to gas sensor technical field, be specifically related to the nitrogen dioxide (NO that a kind of heterojunction Nano microsphere based on CuO-NiO nucleocapsid structure is gas sensitive material
2) gas sensor and preparation method thereof.
Background technology
Along with scientific and technological high speed development, people in enjoying the abundant material wealth of society, the harm that also brought to us by environmental pollution.In numerous pollutants, the problem that the discharge of gas pollutant brings is just increasingly sharpened.The burning of coal, motor vehicle exhaust emission, contains a large amount of sulphuric dioxide in these waste gas, carbon dioxide, nitrogen oxides etc., the discharge of these harmful gases to we environment and healthyly brought serious threat.Along with the reinforcement of people's environmental protection consciousness, the quick, intelligent detection of toxic gas (as oxides of nitrogen), flammable explosive gas (as ethanol, hydrogen, formaldehyde) and indoor organic effumability gas (as dimethylbenzene, formaldehyde) makes to develop high performance gas sensor to be become a kind of necessary.
Gas sensor is to utilize sensitive material directly to adsorb detection gas, and the electrical properties etc. of material is changed, and changes and detects gas concentration through detecting the output signal of peripheral circuit sensitive element.
Material for gas sensing has a lot, at present main application oxide semiconductor sensitive material.The oxide semiconductor sensitive material of different-shape has very large impact to air-sensitive performance, therefore often improves air-sensitive performance by the sensitive material of synthetic different-shape.In addition, the structure of sensitive material also has impact to air-sensitive performance.Among this, heterojunction structure is widely studied and applies.
Summary of the invention
The object of this invention is to provide a kind of heterojunction nitrogen dioxide gas sensor based on CuO-NiO nucleocapsid structure and preparation method thereof.
CuO-NiO nucleocapsid structure heterojunction Nano microsphere is a kind of sensitive material of porous surface, and CuO and NiO formation heterojunction structure, and this will improve its air-sensitive performance greatly.Adopt CuO-NiO nucleocapsid structure heterojunction Nano microsphere as sensitive material, not only applied its high specific surface area, the heterojunction structure that can also effectively utilize CuO-NiO nuclear shell structure nano microballoon improves air-sensitive response.Technique device volume simple, that make that simultaneously the present invention adopts is little, be suitable for producing in enormous quantities, thereby has important using value.
The heterojunction nitrogen dioxide gas sensor of CuO-NiO nucleocapsid structure of the present invention, from bottom to up successively by Al
2o
3substrate, Pd metal are inserted the CuO-NiO nucleocapsid structure heterojunction Nano microsphere sensitive layer composition that refers to electrode, adopts paint-on technique to prepare on slotting finger electrode; Wherein the thickness of CuO-NiO nuclear shell structure nano microballoon (CuO is core, and NiO is shell) sensitive layer is 2～4 μ m, and particle diameter is 600～800nm, and metal is inserted and referred to that width and the spacing of electrode are 0.15～0.20mm, and thickness is 100～150nm.
The preparation process of the nitrogen dioxide gas sensor based on CuO-NiO nucleocapsid structure heterojunction Nano microsphere of the present invention is as follows:
1, Pd metal is inserted the processing that refers to electrode
First the pd metal of preparing with screen printing technique with acetone, the wiping of ethanol cotton balls is respectively inserted the Al that refers to electrode
2o
3substrate is extremely clean, then by Al
2o
3substrate is placed in acetone, ethanol and deionized water successively, and ultrasonic cleaning 5～10 minutes is respectively finally dry under 100～120 DEG C of environment;
2, the preparation of CuO-NiO nucleocapsid structure heterojunction Nano microsphere
Adopt hydro-thermal method to prepare CuO-NiO nucleocapsid structure heterojunction Nano microsphere: under room temperature condition, first absolute ethyl alcohol, deionized water and normal butyl alcohol are mixed, stir and within 10～30 minutes, obtain mixed solvent, then in 20～40 milliliters of above-mentioned mixed solvents, add six water nickel chlorides, cupric sulfate pentahydrate, sodium citrate and urea, and continue to stir 10～30 minutes; In solvent, the volume ratio of absolute ethyl alcohol, deionized water and normal butyl alcohol is 50～100:20～40:1, the mol ratio of six water nickel chlorides, cupric sulfate pentahydrate, sodium citrate and urea is 1:0.5～2.5:0.5～1.75:2～7.5, and the usage ratio of six water nickel chlorides and absolute ethyl alcohol is 5～20g/L; Then the solution obtaining is transferred in reactor, at 100～180 DEG C, react 3～10h, be cooled to after room temperature product deionized water eccentric cleaning, after dry under room temperature, at 200～400 DEG C, calcine 1～3 hour again, thereby obtain taking CuO as core, NiO is the CuO-NiO nucleocapsid structure heterojunction Nano microsphere of shell;
3, the preparation of gas sensitive device
Dried CuO-NiO Nano microsphere is put into mortar, grind 20～30 points; Then in mortar, splash into deionized water (mass ratio of Nano microsphere and deionized water is 5:1～3), then continue to grind 20～30 points, obtain the slurry of sticky shape; Pick a small amount of slurry with spoon, be coated in Pd metal and insert and refer on electrode, then by it 60～80 DEG C of oven dry, obtaining thickness is the CuO-NiO nuclear shell structure nano microballoon sensitive layer of 2～4 μ m; Be finally that 40%RH, temperature are in the environment of 20～35 DEG C in relative humidity, by the device of preparation under the direct current of 40～80mA aging 24～72 hours, thereby obtain a kind of gas sensor that refers to electrode of inserting taking CuO-NiO nucleocapsid structure heterojunction Nano microsphere as sensitive layer, taking Pd as metal of the present invention.
CuO-NiO nucleocapsid structure heterojunction Nano microsphere gas sensor prepared by the present invention has the advantages that preparation method is simple, with low cost, response resume speed is fast, be expected to large-scale production, and nitrogen dioxide gas is had to good detection performance.
Brief description of the drawings
Fig. 1: the SEM shape appearance figure of CuO-NiO nucleocapsid structure heterojunction Nano microsphere, (b) figure is the part amplification of (a) figure, and wherein the enlargement factor of (a) figure is 25000 times, and (b) enlargement factor of figure is 65000 times;
Fig. 2: the prepared device architecture schematic diagram of the present invention;
Fig. 3: the XRD figure of CuO-NiO nuclear shell structure nano microballoon prepared by the present invention and XPS figure;
Fig. 3 (a) is the XRD figure of CuO-NiO nuclear shell structure nano microballoon;
Fig. 3 (b) is the XPS figure of CuO-NiO nuclear shell structure nano microballoon;
Fig. 4: device of the present invention is at 220 DEG C in working temperature, the sensitivity-NO of device
2grey density characteristics curve;
Fig. 5: device of the present invention is 220 DEG C, NO in working temperature
2concentration is under 100ppm, the corresponding recovery curve of device;
Fig. 6: device of the present invention is that 220 DEG C, gas concentration are under 100ppm in working temperature, the selectivity characteristic of device;
As shown in Figure 1, (a) in figure, find out that CuO-NiO nano-crystal with core-shell structure body forms multiple spheroidal aggravations, (b) figure finds out that the grain size of CuO-NiO nuclear shell structure nano microballoon is 600～800nm, and taking CuO as core, NiO is shell.
As shown in Figure 2, device is by Al
2o
3substrate 1, Pd metal are inserted and are referred to that electrode 3, CuO-NiO nuclear shell structure nano microballoon sensitive layer 2 form.
The XRD figure of the CuO-NiO nuclear shell structure nano microballoon that as shown in Figure 3, prepared by the present invention and XPS figure.XRD figure and XPS that Fig. 3 (a) and Fig. 3 (b) are respectively CuO-NiO nuclear shell structure nano microballoon prepared by the present invention scheme.From Fig. 3 (a), can find out, there is the characteristic peak of CuO and NiO in XRD spectra, and interpret sample comprises CuO and NiO crystal; The material that can further prove preparation from Fig. 3 (b) is CuO and NiO crystal.
As shown in Figure 4, when device is at 220 DEG C in working temperature, the sensitivity of device is with NO
2concentration increases and increases, and curve is at NO
2concentration range is that 10～100ppm presents good linear relationship.
As shown in Figure 5, when device is 220 DEG C, NO in working temperature
2concentration is under 100ppm, and the response time of device is 20s, and be 43s the release time of device.Show good response recovery characteristics, to NO
2there is good detection.
As shown in Figure 6, when device is that 220 DEG C, gas concentration are that under 100ppm, device is to NO in working temperature
2sensitivity be all greater than other detect gas.Device shows good selectivity.
Embodiment
Embodiment 1:
First the pd preparing with screen printing technique with acetone, the wiping of ethanol cotton balls respectively inserts the Al that refers to electrode
2o
3substrate is to clean, then will insert finger electrode and be placed in successively acetone, ethanol and deionized water, distinguishes ultrasonic cleaning 5 minutes, is finally put into drying for standby in 100 DEG C.
Adopt screen printing technique to prepare pd metal interdigital electrode, according to ink [good magnificent JX07500487]: pd powder: the ratio that the mass ratio of thinning agent is 1:1:2, stirs and is modulated into paste; Then paste is injected on the silk-screen plate with interdigital electrode pattern, under the angles of inclination of 30 °～45 ° and 5～10 Ns of pressure conditions, scrape paste, printed electrode is also dried, after ultraviolet light polymerization, complete the preparation of metal interdigital electrode, width and the electrode separation of metal interdigital electrode are 0.15～0.20mm, and thickness is 100～150nm.
Adopt hydro-thermal method to prepare CuO-NiO nucleocapsid structure heterojunction Nano microsphere: under room temperature condition, first absolute ethyl alcohol, deionized water and normal butyl alcohol are mixed, stir and within 10 minutes, obtain mixed solvent, then take out 20 milliliters of mixed solvents, and add wherein 0.2052 gram of six water nickel chloride, 0.086 gram of cupric sulfate pentahydrate, 0.10 gram of sodium citrate and 0.16 gram of urea, and continue to stir 10 minutes.In solvent, absolute ethyl alcohol, deionized water and normal butyl alcohol volume ratio are 100:40:1.Then blue solution is transferred in reactor, and react 8h at 160 DEG C, be cooled to after room temperature product deionized water eccentric cleaning, finally at room temperature dry, then dried product is carried out calcining 2 hours at 300 DEG C, the product finally obtaining is CuO-NiO nuclear shell structure nano microballoon.
Dried CuO-NiO Nano microsphere is put into mortar, grind 20 points; Then in mortar, splash into deionized water (mass ratio of CuO-NiO Nano microsphere and water is 5:2), then continue to grind 20 minutes, obtain the slurry of sticky shape; Pick a small amount of slurry with spoon, be coated in to insert and refer on electrode, then by it 60 DEG C of oven dry, the thickness of CuO-NiO nuclear shell structure nano microballoon sensitive layer is 2 μ m; Be finally that 40%RH, temperature are in the environment of 25 DEG C in relative humidity, by the device of preparation under the direct current of 60mA aging 72 hours, thereby obtain a kind of gas sensor that refers to electrode of inserting taking CuO-NiO nucleocapsid structure heterojunction Nano microsphere as sensitive layer, taking Pd as metal of the present invention.
The CuO-NiO nucleocapsid structure heterojunction Nano microsphere of preparing in above-described embodiment is sensitive layer, taking Pd as metal, the air-sensitive performance of the slotting gas sensor that refers to electrode is to test at the CGS-1TP type air-sensitive performance tester of Beijing Ai Lite Science and Technology Ltd..Air-sensitive performance index is as follows:
Sensitivity is 14.8(100ppm nitrogen dioxide);
Nitrogen dioxide gas test specification: 10～500ppm;
Response time is 20 seconds, 43 seconds release times.
Above said content, is only the specific embodiment of the present invention, can not limit scope of the invention process with it, and the impartial changes and improvements of generally carrying out according to patent claim of the present invention, all should still belong to the scope that patent of the present invention contains.
Claims (4)
1. the heterojunction NO based on CuO-NiO nucleocapsid structure
2gas sensor, is characterized in that: from bottom to up successively by Al
2o
3substrate (1), Pd metal interdigital electrode (3) and the composition of the CuO-NiO nuclear shell structure nano microballoon sensitive layer (2) taking CuO as core, taking NiO as shell.
2. a kind of heterojunction NO based on CuO-NiO nucleocapsid structure as claimed in claim 1
2gas sensor, it is characterized in that: the particle diameter of CuO-NiO nucleocapsid structure heterojunction Nano microsphere is 600～800nm, the thickness of CuO-NiO nuclear shell structure nano microballoon sensitive layer is 2～4 μ m, and width and the spacing of metal interdigital electrode are 0.15～0.20mm, and thickness is 100nm～150nm.
3. the heterojunction NO based on CuO-NiO nucleocapsid structure
2the preparation method of gas sensor, its step is as follows:
(1), Pd metal is inserted the processing that refers to electrode
First insert with acetone, the wiping of ethanol cotton balls the Al that refers to electrode with Pd metal respectively
2o
3substrate is extremely clean, then Pd metal is inserted and referred to that electrode is placed in acetone, ethanol and deionized water successively, and ultrasonic cleaning 5～10 minutes respectively is finally dried under 100～120 DEG C of environment;
(2), preparing under room temperature condition of CuO-NiO nucleocapsid structure heterojunction Nano microsphere, first absolute ethyl alcohol, deionized water and normal butyl alcohol are mixed, stir and within 10～30 minutes, obtain mixed solvent, then in 20～40 milliliters of above-mentioned mixed solvents, add six water nickel chlorides, cupric sulfate pentahydrate, sodium citrate and urea, and continue to stir 10～30 minutes; In solvent, the volume ratio of absolute ethyl alcohol, deionized water and normal butyl alcohol is 50～100:20～40:1, the mol ratio of six water nickel chlorides, cupric sulfate pentahydrate, sodium citrate and urea is 1:0.5～2.5:0.5～1.75:2～7.5, and the usage ratio of six water nickel chlorides and absolute ethyl alcohol is 5～20g/L; Then the solution obtaining is transferred in reactor, at 100～180 DEG C, react 3～10h, be cooled to after room temperature product deionized water eccentric cleaning, after dry under room temperature, at 200～400 DEG C, calcine 1～3 hour again, thereby obtain taking CuO as core, NiO is the CuO-NiO nucleocapsid structure heterojunction Nano microsphere of shell;
(3), the preparation of CuO-NiO Nano microsphere gas sensor
Dried CuO-NiO Nano microsphere is put into mortar, grind 20～30 points; Then in mortar, splash into deionized water, then continue to grind 20～30 points, obtain the slurry of sticky shape; Pick a small amount of slurry with spoon, be coated in Pd metal and insert and refer to, on electrode, then it be dried under 60～80 DEG C of conditions, obtaining thickness is the CuO-NiO nuclear shell structure nano microballoon sensitive layer of 2～4 μ m; Be finally that 40%RH, temperature are in the environment of 20～35 DEG C in relative humidity, under the direct current of 40～80mA aging 24～72 hours, thus obtain inserting taking CuO-NiO nucleocapsid structure heterojunction Nano microsphere as sensitive layer, taking Pd as metal the gas sensor that refers to electrode.
4. the preparation method of a kind of heterojunction gas sensor based on CuO-NiO nucleocapsid structure as claimed in claim 3, is characterized in that: in step (3), the mass ratio of Nano microsphere and deionized water is 5:1～3.
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