CN105486723A - Preparation method for room temperature NO2 sensor with ceramic-based vanadium oxide nanorod structure - Google Patents
Preparation method for room temperature NO2 sensor with ceramic-based vanadium oxide nanorod structure Download PDFInfo
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- CN105486723A CN105486723A CN201510807930.2A CN201510807930A CN105486723A CN 105486723 A CN105486723 A CN 105486723A CN 201510807930 A CN201510807930 A CN 201510807930A CN 105486723 A CN105486723 A CN 105486723A
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- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
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Abstract
The invention discloses a preparation method for a room temperature NO2 sensor with a ceramic-based vanadium oxide nanorod structure. The preparation method comprises the following steps: cleaning of a ceramic substrate; weighing of V2O5 powder; preparation of a ceramic-based vanadium oxide nanorod by using a single vapor transport method; and preparation of a ceramic-based vanadium oxide nanorod gas-sensitive sensor element. The ceramic substrate used in the invention has a rough bottom surface, is low in cost and can easily realize large-area preparation of the vanadium oxide nanorod. The ceramic-based vanadium oxide nanorod gas-sensitive sensor element is simple in structure, low in preparation cost, easy in operation and time-saving and can work at room temperature. Thus, the prepared gas-sensitive sensor element can detect NO2 gas at room temperature and has the advantages of high sensitivity, rapid response, short recovery time and repeatable detection.
Description
Technical field
The present invention relates to a kind of gas sensor element method for making, be specifically related to a kind of detection NO being applicable to working and room temperature
2the preparation method of the ceramic base vanadium oxide nanorod structure gas sensor of gas.
Background technology
Mankind's daily life is closely connected with the environment of surrounding with activity in production, and such as, in mining area, chemical enterprise, family etc., the change of atmosphere has great impact to the production work of the mankind and health.In recent years, the existence of acid rain, greenhouse effect, depletion of the ozone layer, inflammable, explosive, poisonous harmful gas, has all become serious human health problems, wherein oxides of nitrogen (NO
x) gas is the main cause causing acid rain and photo-chemical smog, research and development is used for oxides of nitrogen (NO
x) sensor construction of gas detect is significant.
Along with the enhancing of mankind's environmental consciousness, people are to NO
2the performance requirement of gas sensor also improves gradually, as: sensitivity, response recovery time, working temperature, gas concentration etc.In a word, from now on gas sensor will, working and room temperature, low concentration sensing fast towards high sensitivity, response recovery time, can the future development such as duplicate detection.
At present, the simple NO of structure
2gas sensor is in order to increase chemical mobility of the surface to improve sensitivity, and working temperature, generally higher than room temperature, works under the high temperature conditions for a long time and not only greatly can increase the power consumption of sensor, can cause the bad stability of sensor simultaneously.But the NO that can at room temperature work at present
2gas sensor mostly is composite structure, and method for making cost height is consuming time and complicated.So it is simple to work out a kind of structure, the low operation again of preparation cost is easy, can in the NO of working and room temperature
2gas sensor has great importance.
Vanadium oxide, as a kind of important broad stopband N-type semiconductor metal oxide sensitive material, is a kind of surface conductance (resistance) control type gas sensitive.VO
2film is polycrystalline structure, and its inside exists a large amount of crystal boundary, crystal structure surface in atmosphere time can adsorb a large amount of oxygen molecules, oxygen molecule has very strong electronegativity, can from semiconductor conduction band trapped electron, as catalytic oxidation gas NO
2time, NO
2capture the electronics in semiconductor conduction band further, grain boundaries barrier height is increased, resistance becomes large, shows gas-sensitive property.Vanadium oxide nanometer rods has larger specific surface area, and namely more gas absorption position and gas diffusion paths, fully can contact NO
2gas, and then make that Charger transfer occurs between Semiconductor gas sensors material and gas and form heterojunction.In addition namely vanadium oxide nanometer rods at room temperature has stronger chemical mobility of the surface and stronger gas sorption ability, can realize gas sensor working and room temperature.It should be noted that single ceramic base vanadium oxide nanometer rods gas sensor, under can realizing room temperature, air-sensitive is tested, and structure is simple, and cost of manufacture is low and operation is easy.
Substrate at present for the preparation of vanadium oxide nanometer rods mostly is ganoid quartz, silicon chip (SiO
2), prepared nanometer rods is embedded in substrate strongly and density is low, is unsuitable for large area and prepares vanadium oxide nanometer rods.
Summary of the invention
In order to solve problems of the prior art, the invention provides a kind of ceramic base vanadium oxide nanorod structure room temperature NO
2the preparation method of sensor, overcomes vanadium oxide nanorod structure room temperature NO in prior art
2the problem that gas sensor cost is high, operation is loaded down with trivial details.
Technical scheme of the present invention is: a kind of ceramic base vanadium oxide nanorod structure room temperature NO
2the preparation method of sensor, comprises the steps:
(1) cleaning of ceramic substrate:
By potsherd substrate ultrasonic cleaning 5 ~ 20min in acetone and ethanol respectively, to remove the greasy dirt of ceramic substrate surface, organic impurities and surface oxide layer, cleaned rear taking-up ceramic substrate and blown away the liquid of substrate surface with inhaling that ball, to be put in after sucking liquid on filter paper and in the vacuum drying chamber of 60 ~ 80 DEG C dry 5-10min for subsequent use;
(2) V is weighed
2o
5powder:
Weigh V
2o
5powder is for subsequent use;
(3) single Vapor Transport prepares ceramic base vanadium oxide nanometer rods:
By the V of step (2)
2o
5powder evaporation source is evenly laid on the ceramic substrate of step (1), and entirety puts into quartz ampoule, is then holding V
2o
5the ceramic substrate of a slice step (1) is placed in the argon gas stream direction, side of ceramic powder substrate, quartz ampoule entirety being put into programmable type high-temperature vacuum tubular type furnace apparatus (GSL-1400X type), by controlling unitary variant method, change working temperature 850 ~ 1000 DEG C being set to change the surface topography of vanadium oxide nanometer rods; Meanwhile, along with the rising density of nanorods table of temperature is large, Size Distribution trend evenly.
(4) ceramic base vanadium oxide nanometer rods gas sensor element is prepared:
The ceramic base vanadium oxide nanometer rods obtained in step (3) is placed in the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment (DSP-III), utilize mask depositing a pair platinum point electrode in ceramic base vanadium oxide nanorod surfaces, make and can be used for room temperature detection NO
2gas sensor element.
The evaporation source of described step (2) to be quality purity be 99.999% V
2o
5powder.
The condition of described step (3) high-temperature vacuum tubular type stove is: using the argon gas of quality purity 99.999% as working gas, cleaning burner hearth 5 ~ 10min before experiment, vacuum tightness in stove is made to reach below 20Pa, then flowmeter is adjusted to " opening " shelves, regulate the Ar airshed 20sccm needed for experiment, regulate operating pressure 1.5Torr, working time 2h is set.
Described step (4) ultrahigh vacuum facing-target magnetron sputtering system equipment adopts the metal platinum of quality purity 99.99% as target, and using the argon gas of quality purity 99.999% as working gas, argon gas flow is 24sccm, and body vacuum tightness is 4 × 10
-4pa ~ 5 × 10
-4pa, sputtering operating pressure is 2 ~ 4Pa, and sputtering power is 100W, and sputtering time is 2min.
Described step (3) in tubular furnace, grow vanadium oxide nanometer rods with single Vapor Transport, can to form free growing diameter on the surface of ceramic base be 100 ~ 150nm after experiment terminates, length is the nanometer rods of 10 ~ 15 μm.
A kind of prepared gas sensor element detects NO in room temperature
2the application of gas-sensitive property.
Beneficial effect of the present invention is: provide and a kind ofly low cost can prepare the method for ceramic base vanadium oxide nanometer rods, single Vapor Transport operation is comparatively simple, and the process conditions of required control are few, and environmentally safe.Further, prepared ceramic base vanadium oxide nanometer rods has comparatively bigger serface and gas diffusion paths.In primary study of the present invention nanometer rods preparation process, working temperature is on the impact of ceramic base vanadium oxide nanometer rods gas-sensitive property, and under same temperature ceramic base vanadium oxide nanometer rods to different N O
2the gas-sensitive property of concentration.Result shows, ceramic base vanadium oxide nanometer rods at room temperature detects the NO of low concentration
2gas, has highly sensitive, that response recovery time is short advantage.Meanwhile, this gas sensor volume is little, easy to use, has important practice and Research Significance.
Ceramic bases rough surface used in the present invention, and cost is low, is easy to large area and prepares vanadium oxide nanometer rods.Ceramic base vanadium oxide nanometer rods gas sensor element, structure is simple, and preparation cost is low to save time and operation is easy, can realize working and room temperature.And then produce one and can detect NO at ambient temperature
2gas and have high sensitivity, fast response recovery time, can the gas sensor element of repeated test.
Accompanying drawing explanation
Fig. 1 is ceramic base vanadium oxide nanometer rods gas sensor part drawing;
Fig. 2 is the ceramic base vanadium oxide nanorod surfaces electron scanning micrograph prepared by embodiment 1;
Fig. 3 is the ceramic base vanadium oxide nanometer rods X-ray diffraction photo prepared by embodiment 1;
Fig. 4 is that ceramic base vanadium oxide nanorod structure gas sensor element prepared by embodiment 1 is to 1 ~ 5ppmNO
2the dynamic response curve of gas;
Fig. 5 is sensitivity and the NO of ceramic base vanadium oxide nanorod structure gas sensor element prepared by embodiment 1
2the corresponding relation figure of gas concentration;
Fig. 6 is that ceramic base vanadium oxide nanorod structure gas sensor element prepared by embodiment 1 is to 5ppmNO
2reperformance test schematic diagram.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
The present invention is raw materials used all adopts commercially available chemically pure reagent.
Embodiment 1
(1) cleaning of ceramic substrate
It is rectangular-shaped that potsherd a slice being of a size of 2cm*2cm cuts into the two panels being of a size of 2cm*1cm, then complete for a slice is put into glass cylinder with the potsherd after two panels cutting, ultrasonic cleaning 5 ~ 20min in acetone and ethanol respectively, cleaned rear taking-up ceramic substrate and with the liquid inhaling your ball and blow away substrate surface, to be put in after sucking liquid on filter paper and in the vacuum drying chamber of 60 ~ 80 DEG C drying 5 ~ 10min for subsequent use;
(2) V is weighed
2o
5powder
Weigh 0.15gV
2o
5powder is for subsequent use;
(3) single Vapor Transport prepares ceramic base vanadium oxide nanometer rods
By the V of step (2)
2o
5powder evaporation source is evenly laid on the ceramic substrate of the 2cm*2cm of step (1), and entirety puts into quartz ampoule, then holds V in distance
2o
5the ceramic substrate of the two panels 2cm*1cm of step (1) is placed at ceramic substrate 0.5cm and the 3cm place of powder respectively, quartz ampoule entirety is put into programmable type high-temperature vacuum tubular type stove (GSL-1400X type) equipment, using the argon gas of quality purity 99.999% as working gas, flowmeter is adjusted to " cleaning " shelves, cleaning burner hearth 5 ~ 10min, then flowmeter is adjusted to " closedown " shelves, vacuum tightness in stove is made to reach below 20Pa, then flowmeter is adjusted to " opening " shelves, regulate the Ar airshed 20sccm needed for experiment, regulate operating pressure 1.5Torr, heating curve is set, working time 2h is set, working temperature 1000 DEG C is set, final step occurs that "-121 " are namely provided with, test, as shown in Figure 2, record mean diameter is 150nm to ceramic base vanadium oxide nanorod surfaces topography scan electron microscopic analysis result prepared by embodiment 1, and average length is the nanometer rods of 15 μm.Ceramic base vanadium oxide nanometer rods X-ray diffraction analysis result prepared by embodiment 1 as shown in Figure 3;
(4) ceramic base vanadium oxide nanometer rods gas sensor element is prepared
The ceramic base vanadium oxide nanometer rods obtained in step (3) is placed in the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, adopt the metal platinum of quality purity 99.99% as target, using the argon gas of quality purity 99.999% as working gas, argon gas flow is 24sccm, and body vacuum tightness is 4.010
-4pa, sputtering operating pressure is 2Pa, and sputtering power is 100W, and sputtering time is 2min, and be of a size of the platinum electrode of 0.2cm*0.2cm for a pair in ceramic base vanadium oxide nanorod surfaces deposition, electrode separation is 8mm.
The ceramic base vanadium oxide nanorod structure gas sensor element that embodiment 1 obtains is at room temperature to the NO of 1 ~ 5ppm
2the dynamic response curve of gas as shown in Figure 4.Its sensitivity at room temperature and NO
2the corresponding relation schematic diagram of gas concentration as shown in Figure 5, wherein to 1,2,3,4,5ppmNO
2the sensitivity of gas is respectively 1.80,1.96,2.04,2.17 and 2.42.
Ceramic base vanadium oxide nanorod structure gas sensor element obtained by embodiment 1 is at room temperature to 5ppmNO
2carry out 5 reperformance tests, as shown in Figure 6, the ceramic base vanadium oxide nanorod structure gas sensor element obtained by explanation has good repeatability to test result.
Embodiment 2
The difference of the present embodiment and embodiment 1 is: in step (3), single Vapor Transport prepares the working temperature that arranges of ceramic base vanadium oxide nanometer rods is 950 DEG C, and obtained ceramic base vanadium oxide nanorod structure gas sensor element is at room temperature to 3ppmNO
2the sensitivity of gas is 1.73.
Embodiment 3
The difference of the present embodiment and embodiment 1 is: in step (3), single Vapor Transport prepares the working temperature that arranges of ceramic base vanadium oxide nanometer rods is 900 DEG C, and obtained ceramic base vanadium oxide nanorod structure gas sensor element is at room temperature to 3ppmNO
2the sensitivity of gas is 1.62.
Embodiment 4
The difference of the present embodiment and embodiment 1 is: in step (3), single Vapor Transport prepares the working temperature that arranges of ceramic base vanadium oxide nanometer rods is 850 DEG C, and obtained ceramic base vanadium oxide nanorod structure gas sensor element is at room temperature to 3ppmNO
2the sensitivity of gas is 1.31.
Although invention has been described by reference to the accompanying drawings above; but the present invention is not limited to above-mentioned embodiment; above-mentioned embodiment is only schematic; be not restrictive; those of ordinary skill in the art is under enlightenment of the present invention; do not departing under the ambit that present inventive concept and claim protect, can also make a lot of form, these all belong within protection scope of the present invention.
Claims (5)
1. a ceramic base vanadium oxide nanorod structure room temperature NO
2the preparation method of sensor, is characterized in that, comprises the steps:
(1) cleaning of ceramic substrate:
By potsherd substrate ultrasonic cleaning 5 ~ 20min in acetone and ethanol respectively, to remove the greasy dirt of ceramic substrate surface, organic impurities and surface oxide layer, cleaned rear taking-up ceramic substrate and blown away the liquid of substrate surface with inhaling that ball, to be put in after sucking liquid on filter paper and in the vacuum drying chamber of 60 ~ 80 DEG C dry 5-10min for subsequent use;
(2) V is weighed
2o
5powder:
Weigh V
2o
5powder is for subsequent use;
(3) single Vapor Transport prepares ceramic base vanadium oxide nanometer rods:
By the V of step (2)
2o
5powder evaporation source is evenly laid on the ceramic substrate of step (1), and entirety puts into quartz ampoule, is then holding V
2o
5the ceramic substrate of a slice step (1) is placed in the argon gas stream direction, side of ceramic powder substrate, quartz ampoule entirety being put into programmable type high-temperature vacuum tubular type furnace apparatus, by controlling unitary variant method, change working temperature 850 ~ 1000 DEG C being set to change the surface topography of vanadium oxide nanometer rods;
(4) ceramic base vanadium oxide nanometer rods gas sensor element is prepared:
The ceramic base vanadium oxide nanometer rods obtained in step (3) is placed in the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, utilizes mask depositing a pair platinum point electrode in ceramic base vanadium oxide nanorod surfaces, make and can be used for room temperature detection NO
2gas sensor element.
2. ceramic base vanadium oxide nanorod structure room temperature NO according to claim 1
2the preparation method of sensor, is characterized in that, the evaporation source of described step (2) to be quality purity be 99.999% V
2o
5powder.
3. ceramic base vanadium oxide nanorod structure room temperature NO according to claim 1
2the preparation method of sensor, it is characterized in that, the condition of described step (3) high-temperature vacuum tubular type stove is: using the argon gas of quality purity 99.999% as working gas, cleaning burner hearth 5 ~ 10min before experiment, make vacuum tightness in stove reach below 20Pa, then flowmeter is adjusted to " opening " shelves, regulate the Ar airshed 20sccm needed for experiment, regulate operating pressure 1.5Torr, working time 2h is set.
4. ceramic base vanadium oxide nanorod structure room temperature NO according to claim 1
2the preparation method of sensor, it is characterized in that, described step (4) ultrahigh vacuum facing-target magnetron sputtering system equipment adopts the metal platinum of quality purity 99.99% as target, using the argon gas of quality purity 99.999% as working gas, argon gas flow is 24sccm, and body vacuum tightness is 4 × 10
-4pa ~ 5 × 10
-4pa, sputtering operating pressure is 2 ~ 4Pa, and sputtering power is 100W, and sputtering time is 2min.
5. the sensor element prepared by a claim 1 detects NO in room temperature
2the application of gas-sensitive property.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106187318A (en) * | 2016-07-15 | 2016-12-07 | 天津大学 | A kind of preparation method of the ceramic base Vanadium dioxide nanometer rod structure of freedom and on-plane surface growth |
| CN106248743A (en) * | 2016-07-15 | 2016-12-21 | 天津大学 | A kind of gold doping vanadium dioxide nano chip architecture room temperature CH4the preparation method of gas sensor |
| CN106501322A (en) * | 2016-10-28 | 2017-03-15 | 中国石油大学(华东) | One kind is based on nanometer grid structure V2O5Gas sensor of thin film and preparation method thereof |
| CN107764872A (en) * | 2017-09-25 | 2018-03-06 | 天津大学 | The nitrogen dioxide gas sensor preparation method of gold modification vanadium dioxide nanowire |
| CN110243874A (en) * | 2019-07-02 | 2019-09-17 | 上海应用技术大学 | A kind of method of solid electrolyte resistivity under measurement high temperature |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106187318A (en) * | 2016-07-15 | 2016-12-07 | 天津大学 | A kind of preparation method of the ceramic base Vanadium dioxide nanometer rod structure of freedom and on-plane surface growth |
| CN106248743A (en) * | 2016-07-15 | 2016-12-21 | 天津大学 | A kind of gold doping vanadium dioxide nano chip architecture room temperature CH4the preparation method of gas sensor |
| CN106501322A (en) * | 2016-10-28 | 2017-03-15 | 中国石油大学(华东) | One kind is based on nanometer grid structure V2O5Gas sensor of thin film and preparation method thereof |
| CN106501322B (en) * | 2016-10-28 | 2019-01-01 | 中国石油大学(华东) | One kind being based on nanometer grid structure V2O5Gas sensor of film and preparation method thereof |
| CN107764872A (en) * | 2017-09-25 | 2018-03-06 | 天津大学 | The nitrogen dioxide gas sensor preparation method of gold modification vanadium dioxide nanowire |
| CN110243874A (en) * | 2019-07-02 | 2019-09-17 | 上海应用技术大学 | A kind of method of solid electrolyte resistivity under measurement high temperature |
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Application publication date: 20160413 |