CN105067670A - Ordered Cu-doped nano-porous tin oxide sensing device - Google Patents
Ordered Cu-doped nano-porous tin oxide sensing device Download PDFInfo
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Abstract
The invention discloses an ordered Cu-doped nano-porous tin oxide sensing device. The sensing device is produced through the following steps: 1, producing an interdigital electrode-based graphene oxide film through adopting a spin coating method; 2, producing a device coated with a composite sensing film through a spin coating method, drying, and carrying out hot steam treatment; 3, removing a template from the device obtained in step 2; and 4, carrying out a reduction reaction on the device obtained in step 3 under an ultraviolet radiation condition to obtain the nano-porous tin oxide sensing device. The ordered Cu-doped nano-porous tin oxide sensing device has an excellent sensing performance, and the response time and the recovery time to low concentration H2S gas are shorter than 20s respectively.
Description
Technical field
The present invention relates to a kind of gas sensor, be specifically related to a kind of room temperature H of the film-type high selectivity that ordered nano hole tin oxide is sensing material of mixing with cupric oxide Erbium-doped
2s gas-sensitive sensor device.
Background technology
Along with scientific and technical high speed development, modern industry also brings safety and environmental problem while bringing great economic benefit and civilization and progress for the mankind, particularly there is inflammable and explosive and noxious material in a large number in oil coal equal energy source industry production run.In the face of so serious safety and environmental problem, national governments' increasing is to the input of sensor technology and research and development.U.S. government pays much attention to the research and development support to sensor technology always, and plan development of new sensor put into effect by the needs for energy security, for detecting toxic and harmful.China in 2011 issue national medium-term and long-term plans clearly using enviromental monitoring equipment gas sensor as main development object.But the detection sensitivity that traditional gas sensor exists low concentration feeble signal is on the low side, the shortcomings such as poor selectivity.In order to realize quick response, mostly adopting type of heating, improving senor operating temperature (working temperature 200-600 DEG C).The introducing of heating system not only increases energy consumption, and easily ignites inflammable gas, brings huge potential safety hazard.It is 240 DEG C as patent CN104502413 prepares the mix best sensing detection temperature of tin oxide base sulfuretted hydrogen gas sensitive of gained cupric oxide Erbium-doped.
Summary of the invention
The object of the invention is, in order to solve the defect existed in prior art, to provide one at room temperature, can to low concentration H
2the senser element that S responds fast.
In order to achieve the above object, the invention provides a kind of nano-pore tin oxide sensors part of orderly Cu doping, prepared by following steps:
(1) graphene oxide/interdigital electrode preparation: preparation concentration is that (preferred concentration is 1mg/ml for the polar graphite oxide alkene solution of 0.01-10mg/ml,), the pH value regulating graphene oxide polar solvent is 9-10, adopts spin-coating method preparation based on the graphene oxide film of interdigital electrode;
(2) the device preparation of sensing material is coated with: get mantoquita and pink salt (preferred molar ratio is 4:100) that mass ratio is 1:100-8:100, be dissolved in polar solvent, then add surfactant, adjust ph is to obtaining settled solution; Plated film on the device adopting spin-coating method to prepare in step (1) gained settled solution, must be coated with the device of sensing material; After gained being coated with the device drying of sensing material, through vapours process 1-4 days; The mass ratio of described surfactant and pink salt is 0.4:100-6:100(preferred molar ratio is 0.48:100).
(3) surfactant in removal step (2) obtained device;
(4) reduce: step (3) obtained device is carried out reduction reaction under ultraviolet irradiation condition, obtains described nano-pore tin oxide sensors part.
Wherein, step (1) Semi-polarity graphene oxide solution is graphene oxide water solution; Polar solvent in described step (2) adopts absolute ethyl alcohol.
The method of vapours process is as follows in step (2): dried device is put into closed container, regulates the relative humidity 70%-95% in container, then container is put into air dry oven and regulate temperature to be 100 ~ 150 DEG C.
The method removing template in step (3) is as follows: step (2) device after vapours process is placed in UV-O
324-48h is processed under environment.
Mantoquita adopts cupric chloride, copper nitrate or copper sulphate, preferred cupric chloride; Pink salt adopts anhydrous stannic chloride, nitric acid tin or STANNOUS SULPHATE CRYSTALLINE, preferred anhydrous stannic chloride; Interdigital electrode adopts gold electrode or platinum electrode, preferred interdigital gold electrode.
In step (1), spin-coating method adopts spin speed to be 2000-4000rpm, each spin-coating time 30-60s; In step (2), spin-coating method step is: in sol evenning machine, and be 5% ~ 50% by controlling the humidity of sol evenning machine cavity, the speed of spin coating is 2000-4000rpm, and each spin-coating time is 30-60s, and the multiplicity of plated film is 1-10 time.
The present invention has the following advantages compared to existing technology:
1, the ordered nano hole Cu Erbium-doped of the present invention sensing capabilities of nano tin dioxide senser element of mixing is excellent, to low concentration H
2s gas response time and release time are all lower than 20s.
2, the preparation of composite sensing material and sensor production are synchronously carried out by the preparation process of senser element of the present invention, simplify experimental procedure, strengthen repeatability prepared by sensing material, improve the specific surface area of sensing material, form high-quality p-n junction, for carrier transport provides excellent passage, activation grain surface adsorptive power, promote surface reaction activity, improve sensitivity and shorten the response time, by near for sensing detection temperature room temperature, the work of the gas sensor greatly strengthened uses range, and is conducive to reducing energy consumption.
3, the present invention uses hot steaming method gained ordered nano hole tin oxide sensing material, and structurally ordered, thermal stability is strong; Use UV-O
3method removes surfactant, avoids the destruction of method to membrane structure of traditional roasting; Use UV reducing process fully to use the reducing power of burst of ultraviolel tin oxide, carried out effective reduction to graphene oxide, compared with traditional method of reducing, the method environmental friendliness, easy to operate, cost is low.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the senser element of preparation in the embodiment of the present invention 1;
Fig. 2 steams after method process and through UV-O through heat in the embodiment of the present invention 1
3the one dimension SAXS scatter diagram of the sensing membrane after process;
Fig. 3 is the TEM figure of the senser element surface sensing membrane of preparation in the embodiment of the present invention 1;
Fig. 4 is the sensing capabilities figure of the senser element of preparation in the embodiment of the present invention 1.
In Fig. 1,1-Graphene, 2-interdigital electrode.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
1, at room temperature, configuration graphene oxide solution (solvent is deionized water) 1mg/ml, adjust ph is 9-10, and start sol evenning machine, pipettor gets 100ul solution, and the rotating speed controlling sol evenning machine is 2000rpm, and spin-coating time is 30s.
2, by dry under 60 DEG C of conditions for the device (interdigital gold electrode) scribbling graphene oxide.Take 0.04g cupric chloride and 1g anhydrous stannic chloride, be dissolved in absolute ethyl alcohol, add the surfactant F127 of 0.4g, then add 1ml concentrated hydrochloric acid, mix and obtain settled solution.Start sol evenning machine, be fixed on by the device scribbling graphene oxide in sol evenning machine cavity, the humidity controlling cavity is 10%, and spin speed is 4000rpm, and spin-coating time is 30s, and spin coating repeats 1 time.By above-mentioned brand-new for after the device drying of sensing material, device is put into closed container, regulate the relative humidity 70% in container, then container is put into air dry oven and regulate temperature to be 100 DEG C, the reaction time is 4 days.
3, at UV/O
336h under environment, finally penetrates lower lasting 8h in UV illumination, obtains preparing ordered nano hole Cu Erbium-doped based on Graphene/gold electrode and to mix SnO
2senser element.
Fig. 1 prepares orderly Cu Erbium-doped to mix nano-pore SnO for preparing gained Graphene/gold electrode
2the SEM figure of senser element, as can be seen from the figure by the bridging of Graphene 1, makes the performance of interdigital electrode 2 obtain huge lifting.
Fig. 2 is after step 2 processes and through UV-O
3the SAXS figure of the sensing membrane after process, as can be seen from the figure, both all have good structural order.
Fig. 3 prepares orderly Cu Erbium-doped to mix nano-pore SnO for preparing gained Graphene/gold electrode
2the transmission electron microscope photo of senser element surface sensing membrane, as can be seen from the figure nano particle diameter is about 5nm, and nano-pore is along the arrangement of 110 crystal face long-range orders, and average pore size is about 10nm.
Fig. 4 prepares orderly Cu Erbium-doped to mix nano-pore SnO for preparing gained Graphene/gold electrode
2senser element air-sensitive performance test pattern at room temperature, as can be seen from the figure, sensitivity is along with H
2s concentration changes from 20ppm-200ppm, then by the near 20ppm of 200ppm.Response time and the release time of sensor are all less than 20s.
Embodiment 2
1, at room temperature, configuration graphene oxide solution 5mg/ml, adjust ph is 9-10, and start sol evenning machine, pipettor gets 100ul solution, and the rotating speed controlling sol evenning machine is 2000rpm, and spin-coating time is 45s.
2, by scribble graphene oxide device 60 DEG C of conditions under dry.Take 0.08g copper nitrate and 1.5g tetra-nitrification tin, be dissolved in absolute ethyl alcohol, add the surfactant P123 of 0.36g, then add 1ml concentrated hydrochloric acid, mix and obtain settled solution.Start sol evenning machine, be fixed on by the device scribbling graphene oxide in sol evenning machine cavity, the humidity controlling cavity is 30%, and spin speed is 4000rpm, and spin-coating time is 45s, and spin coating repeats 5 times.By above-mentioned brand-new for after the device drying of sensing material, device is put into closed container, regulate the relative humidity 80% in container, then container is put into air dry oven and regulate temperature to be 120 DEG C, the reaction time is 2 days.
3, at UV/O
336h under environment, finally penetrates lower lasting 8h in UV illumination, obtains preparing orderly Cu Erbium-doped based on Graphene/gold electrode and to mix nano-pore SnO
2senser element.
SAXS figure shows the orderly sensing membrane after step 2 process, and through UV-O
3sensing membrane after process has good structural order.The transmission electron microscope photo preparing gained senser element surface sensing membrane shows, nano particle diameter is about 5nm, and nano-pore is along the arrangement of 110 crystal face long-range orders, and average pore size is about 7nm.At room temperature carry out air-sensitive performance test to preparing gained senser element, sensitivity is along with H
2s concentration changes from 20ppm-200ppm, then by the near 20ppm of 200ppm, response time and the release time of sensor are all less than 20s.
Embodiment 3
1, at room temperature, configuration graphene oxide solution 10mg/ml, adjust ph is 9-10, and start sol evenning machine, pipettor gets 100ul solution, and the rotating speed controlling sol evenning machine is 2000rpm, and spin-coating time is 60s.
2, by scribble graphene oxide device 60 DEG C of conditions under dry.Take 0.042g copper sulphate and 1.3g sulphation tin, be dissolved in absolute ethyl alcohol, add the surfactant F127 of 0.36g, then add 1ml concentrated hydrochloric acid, mix and obtain settled solution.Start sol evenning machine, be fixed on by the device scribbling graphene oxide in sol evenning machine cavity, the humidity controlling cavity is 50%, and spin speed is 4000rpm, and spin-coating time is 60s, repeats spin coating 10 times.By above-mentioned brand-new for after the device drying of sensing material, device is put into closed container, regulate the relative humidity 95% in container, then container is put into air dry oven and regulate temperature to be 150 DEG C, the reaction time is 1 day.
3, at UV/O
348h under environment, finally penetrates lower lasting 8h in UV illumination, obtains preparing orderly Cu Erbium-doped based on Graphene/gold electrode and to mix nano-pore SnO
2senser element.
SAXS figure shows the orderly sensing membrane after the process of hot steaming method, and through UV-O
3sensing membrane after process has good structural order.The transmission electron microscope photo preparing gained senser element surface sensing rete shows, nano particle diameter is about 5nm, and nano-pore is along the arrangement of 110 crystal face long-range orders, and average pore size is about 9nm.At room temperature carry out air-sensitive performance test to preparing gained senser element, sensitivity is along with H
2s concentration changes from 20ppm-200ppm, then by the near 20ppm of 200ppm, response time and the release time of sensor are all less than 20s.
Preparation method of the present invention gives full play to hot steaming method, and by preparation sol solution, then realize crystallization by subsequent treatment low temperature, and achieve self assembly in the process of crystallization, the order of gained film is improved.Crystal grain has nano-grade size, and mean grain size is about 5nm, and passes through UV/O
3the order of process rear film further improves; Preparation technology of the present invention is simple, less demanding to equipment, is easy to large-scale production; The compact structure of the ordered nano hole sensing material that the present invention obtains, nano-pore arrangement long-range order, and there is good sensing capabilities.
Claims (6)
1. the nano-pore tin oxide sensors part of an orderly Cu doping, it is characterized in that, described nano-pore tin oxide sensors part is prepared by following steps: (1) graphene oxide/interdigital electrode preparation: preparation concentration is the polar graphite oxide alkene solution of 0.01-10mg/ml, the pH value regulating graphene oxide polar solvent is 9-10, adopts spin-coating method preparation based on the graphene oxide film of interdigital electrode; (2) the device preparation of sensing material is coated with: get mantoquita and pink salt that mass ratio is 1:100-8:100, be dissolved in polar solvent, then add surfactant, adjust ph is to obtaining settled solution; Plated film on the device adopting spin-coating method to prepare in step (1) gained settled solution, must be coated with the device of sensing material; After device drying, through vapours process 1 ~ 4 day; The mass ratio of described surfactant and pink salt is 0.4:100-6:100; (3) surfactant in removal step (2) obtained device; (4) reduce: step (3) obtained device is carried out reduction reaction under ultraviolet irradiation condition, obtains described nano-pore tin oxide sensors part.
2. nano-pore tin oxide sensors part according to claim 1, is characterized in that, described step (1) Semi-polarity graphene oxide solution is graphene oxide water solution; Polar solvent in described step (2) adopts absolute ethyl alcohol.
3. nano-pore tin oxide sensors part according to claim 1 and 2, is characterized in that, the method removing template in described step (3) is as follows: process 24-48h under step (2) obtained device is placed in UV-O3 environment.
4. nano-pore tin oxide sensors part according to claim 1 and 2, it is characterized in that, vapours disposal route in described step (2) is as follows: dried device is put into closed container, regulate the relative humidity 70%-95% in container, then container is put into air dry oven and regulate temperature to be 100 ~ 150 DEG C.
5. nano-pore tin oxide sensors part according to claim 3, is characterized in that, described mantoquita adopts cupric chloride, copper nitrate or copper sulphate; Described pink salt adopts anhydrous stannic chloride, nitric acid tin or STANNOUS SULPHATE CRYSTALLINE; Described interdigital electrode adopts gold electrode or platinum electrode.
6. nano-pore tin oxide sensors part according to claim 3, is characterized in that, in described step (1), spin-coating method adopts spin speed to be 2000-4000rpm, each spin-coating time 30-60s; In described step (2), spin-coating method step is: in sol evenning machine, and be 5% ~ 50% by controlling the humidity of sol evenning machine cavity, the speed of spin coating is 2000-4000rpm, and each spin-coating time is 30-60s, and the multiplicity of plated film is 1-10 time.
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| CN107085027A (en) * | 2017-05-25 | 2017-08-22 | 福州大学 | A kind of composite nano materials of room temperature detection hydrogen sulfide and its preparation method and application |
| CN107831195A (en) * | 2017-10-30 | 2018-03-23 | 上海应用技术大学 | A kind of animal flesh metal doping nano graphene olfactory sensor |
| CN107831269A (en) * | 2017-10-19 | 2018-03-23 | 上海纳米技术及应用国家工程研究中心有限公司 | The method of the tin dioxide gas-sensitive material stability of lifting vulcanization hydrogen sensitive |
| CN108333225A (en) * | 2017-12-24 | 2018-07-27 | 苏州南尔材料科技有限公司 | A kind of preparation method of graphene tin oxide sensing material |
| CN110530941A (en) * | 2019-07-17 | 2019-12-03 | 济南大学 | A kind of Cu doping Sn3O4Gas sensitive and its formaldehyde gas sensor and preparation method, application |
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| CN107831269A (en) * | 2017-10-19 | 2018-03-23 | 上海纳米技术及应用国家工程研究中心有限公司 | The method of the tin dioxide gas-sensitive material stability of lifting vulcanization hydrogen sensitive |
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| CN108333225A (en) * | 2017-12-24 | 2018-07-27 | 苏州南尔材料科技有限公司 | A kind of preparation method of graphene tin oxide sensing material |
| CN110530941A (en) * | 2019-07-17 | 2019-12-03 | 济南大学 | A kind of Cu doping Sn3O4Gas sensitive and its formaldehyde gas sensor and preparation method, application |
| CN110530941B (en) * | 2019-07-17 | 2022-01-14 | 济南大学 | Cu doped Sn3O4Gas sensitive material, formaldehyde gas sensor, preparation method and application thereof |
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