CN105548274A - In-situ synthesis of cadmium oxide nanometer gas-sensitive element with secondary pore structure - Google Patents
In-situ synthesis of cadmium oxide nanometer gas-sensitive element with secondary pore structure Download PDFInfo
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- CN105548274A CN105548274A CN201510909360.8A CN201510909360A CN105548274A CN 105548274 A CN105548274 A CN 105548274A CN 201510909360 A CN201510909360 A CN 201510909360A CN 105548274 A CN105548274 A CN 105548274A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00349—Creating layers of material on a substrate
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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
Abstract
The invention discloses a cadmium oxide nanometer gas-sensitive element with a secondary pore structure. The cadmium oxide nanometer gas sensitive element is synthesized through the following steps: with ethylene glycol monomethyl ether as a solvent, preparing a mixed solution of 0.1 M of zinc acetate and 0.2 M of ethanolamine, soaking a glass slide into the mixed solution, and carrying out annealing treatment; preparing a mixed solution of 0.025 M of zinc nitrate and 0.025 M of hexamethylene tetramine, soaking the above-mentioned glass slide into the mixed solution, and carrying out heat-preserving so as to obtain a nanorod array of zinc oxide, wherein the nanorod array is used as a seed layer for growing cadmium oxide; placing cadmium sulfide (CdS) powder into an evacuated tubular furnace, placing an above-mentioned zinc oxide-grown substrate at a position 30 cm below the cadmium sulfide (CdS) powder, then introducing nitrogen and air, carrying out heating to 650 DEG C so as to obtain a nanosheet array of cadmium (Cd), and carrying out heat-preserving at 360 to 440 DEG C for 30 min so as to obtain a nanometer structure of cadmium oxide; and cutting the glass slide into a rectangular shape with a size of 0.5 cm * 1.0 cm, and carrying out coating with electrodes so as to prepare the gas-sensitive element. The gas-sensitive element provided by the invention has the following advantages: at a temperature of 215 DEG C, sensitivity to diethyl ether with a concentration 100 ppm is 138%, and response time and recovery time are 15 seconds and 27 seconds, respectively; meanwhile, the synthetic process is simple, safe and controllable, has low cost and is applicable to large-scale production.
Description
Technical field
The invention relates to gas sensor, particularly relate to a kind of cadmium oxide nanometer gas sensor adopting the method fabricated in situ of chemical vapor deposition to have secondary pore space structure.
Background technology
Ether is a kind of colourless flammable liquid with special odor, is widely used in commercial production and scientific research.The molecular formula C of ether
2h
5oC
2h
5, be a kind of liquid of colourless, inflammable, highly volatile, its smell band is irritant, is taken as Splenectomy, is also common drugs.Ether fume can form explosive mixture with air, when it runs into spark, high temperature, oxygenant, perchloric acid, chlorine, oxygen, ozone etc., just there is the danger that combustion explosion occurs, sometimes also (explosion limits 1.9% ~ 36%, V/V) on fire because of electrostatic.Due to its highly volatile, inevitably infiltrate in the life of people, endanger the healthy of people, long-term low concentration sucks, there are headache, dizziness, albuminuria, polycythemia, see XueliYu, ChangshengXie, LiYang.SensorsandActuatorsB:Chemical, 2014, (195): therefore, in order to the safety of human life and property, realize detection effectively to ether gas is a urgent and significant research to 439-445..
Gas sensor is a kind of sensor gas componant detected and concentration being converted to electric signal, wherein semiconductor transducer is the gas sensor adopting semiconductor material to make, produce adsorption or reaction when interacting with gas, cause carrier moving to be the change of the conductivity of feature, volt-ampere characteristic or surface potential.(see He Daoqing. sensor and sensor technology. Beijing: Science Press, 2003.) metal oxide semiconductor gas sensor has that structure is simple, with low cost, highly sensitive, response rapidly, the advantage of long service life, therefore most widely used.The most important characterisitic parameter of gas sensor has working temperature, sensitivity, selectivity, response-recovery time, stability etc.See KawasakiH, UedaT, SudaY, etal.SensorsandActuatorsB, 2004,100:266-269.
Existing ether detecting material is mostly the hierarchical structure nano material of metal oxide semiconductor, as the Nano dendritic crystal of CdO, see Xiangqian, Fu, Jinyun, Liu, Tianli, Han.SensorsandActuatorsB:Chemical, 2013, (184): 260-267, TiO2 porous nanometer thin films, see XueliYu, ChangshengXie, LiYang.SensorsandActuatorsB:Chemical, 2014, (195): 439-445, SnO2 nano flower etc., see Yang, Liu, Yang, Jiao, Zhenglin, Zhang.ACSAppl.Mater.Interfaces, 2014, (6): 2174-2184.Method for making many employings solvent heat of these materials adds the method for sintering, and process is comparatively complicated, and preparation temperature is high, and power consumption is large, and is not suitable for large-scale low-cost production.And in the process of assembly device, the technique used also more complicated, have impact on promoting the use of of late device greatly.At aspect of performance, this kind of gas sensitive generally all has response to many combustible gases, so more weak to the selectivity of ether, can not more efficiently realize must detecting for ether is effective fast and accurately.
Summary of the invention
Object of the present invention, easily reunite when being used as gas sensitive for existing two-dimensional material, the research of fabricated in situ gas sensitive device is few, especially ether sensitive detection parts complicated process of preparation, to problems such as the poor selectivity of ether, utilize nanometic zinc oxide rod array as Seed Layer, grow in zinc oxide nano rod Seed Layer by the method for chemical vapor deposition and obtain cadmium nano-chip arrays, oxidation obtains having fabricated in situ gas sensor after the cadmium oxide nano-chip arrays of secondary pore space structure in atmosphere, realize, to ether, there is high selectivity and the gas sensor compared with short response time.Structure of the present invention is ingenious, technique simple, safety is controlled, with low cost.The gas sensitive device that the present invention obtains can realize the selective response for ether effectively, and propose secondary hole this has the nanostructured of good responding ability for air-sensitive.
The present invention is achieved by following technical solution:
Fabricated in situ has a cadmium oxide nanometer gas sensor for secondary pore space structure, has following steps:
(1) synthesis of nanometic zinc oxide rod array Seed Layer
1. using ethylene glycol monoemethyl ether as solvent, configuration concentration is the mixed solution of the zinc acetate of 0.1M and the monoethanolamine of 0.2M; Immerse 30s in above-mentioned solution using microslide as substrate, then microslide substrate is placed in baking oven drying process; After repetition aforesaid operations twice, by above-mentioned microslide substrate in atmosphere in 500 DEG C of annealing in process 1h, make Seed Layer and microslide substrate rigid contact;
2. using deionized water as solvent, configuration concentration is the mixed solution of the zinc nitrate of 0.025M and the hexamethylene tetramine of 0.025M;
Get the above-mentioned mixed solution of 60-80ml in reactor, and the reactor filling mixed solution is put in above-mentioned microslide substrate, have one of Seed Layer to face down, the height of mixed solution did not have substrate just;
3. reactor is put into baking oven, at the temperature of 100 DEG C, be incubated 9 hours, then take out above-mentioned microslide substrate, carefully suprabasil for microslide white depositions is rinsed well with deionized water, obtain the nanometer stick array of zinc paste;
(2) synthesis of cadmium oxide nanostructured and the preparation of gas sensitive device
1. the CdS powder of 0.05g is placed in the central authorities of vacuum tube furnace, then above-mentioned length is had the microslide substrate of the nanometer stick array of zinc paste to be positioned over distance CdS powder 30cm place;
2. vacuum tube furnace is evacuated to 100mTorr, then the nitrogen simultaneously passed into and air, and overpressure is adjusted to 9Torr, be warming up to 650 DEG C, insulation 30min, naturally cools to room temperature, obtains the nano-chip arrays of Cd;
3. at 360 ~ 440 DEG C of temperature, be incubated 30min in atmosphere to the microslide substrate of the nano-chip arrays of Cd obtained above, oxidation obtains the nanostructured of cadmium oxide;
4. there is the microslide substrate of composite structure to be cut into the rectangle that size is 0.5cm × 1cm growth, and apply two strip electrodes with silver slurry at two ends, then be incubated 6 hours at 100 DEG C, the obtained cadmium oxide nanometer gas sensitive device with secondary pore space structure.
The specification of described step (1) microslide substrate is 1. 2cm × 4cm.
The flow of the air that described step (2) 2. passes into is 250sccm, and the flow of nitrogen is 45sccm.
The optimum working temperature of air-sensitive original paper of the present invention is 215 DEG C.
Beneficial effect of the present invention is as follows:
Instant invention overcomes the problem that existing two-dimensional semiconductor gas sensitive device is easily reunited in manufacturing process, adopt nanometic zinc oxide rod array as Seed Layer, the synthesis carrying out original position has the cadmium oxide of secondary hole, the impact using the membrane structure that produces below cadmium oxide nanometer sheet of chemical gaseous phase depositing process for air-sensitive performance can be got rid of, and the technique of follow-up making devices is simple, is conducive to promoting on a large scale.The device that the cadmium oxide with secondary pore space structure prepares reaches 138% for the response of the ether of 100ppm at the temperature of 215 DEG C, responds and is respectively 15 seconds and about 27 seconds release time, and achieving the high selectivity to ether.Structure of the present invention is ingenious, technique simple, safety is controlled, with low cost, is applicable to large-scale production.
Accompanying drawing explanation
Fig. 1 is the sectional view of cadmium oxide length on zinc oxide nano rod that embodiment 1 has secondary hole;
Fig. 2 is pattern and the thing phase phenogram of cadmium oxide:
A () is the shape appearance figure of embodiment 2 cadmium oxide nano-chip arrays;
B () is the shape appearance figure that embodiment 1 has secondary hole cadmium oxide;
C () is the shape appearance figure of embodiment 3 reticulate texture cadmium oxide.
Embodiment
Below in conjunction with concrete embodiment, the invention will be further described.
Embodiment 1
(1) synthesis of nanometic zinc oxide rod array Seed Layer
1. using ethylene glycol monoemethyl ether as solvent, configuration concentration is the mixed solution of the zinc acetate of 0.1M and the monoethanolamine of 0.2M; Immerse 30s in above-mentioned solution using microslide as substrate, then microslide substrate is placed in baking oven drying process; After repetition aforesaid operations twice, by above-mentioned microslide substrate in atmosphere in 500 DEG C of annealing in process 1h, make Seed Layer and microslide substrate rigid contact;
2. using deionized water as solvent, configuration concentration is the mixed solution of the zinc nitrate of 0.025M and the hexamethylene tetramine of 0.025M;
Get the above-mentioned mixed solution of 80ml in reactor, and the reactor filling mixed solution is put in above-mentioned microslide substrate, have one of Seed Layer to face down, the height of mixed solution did not have substrate just;
3. reactor is put into baking oven and be incubated 9 hours at the temperature of 100 DEG C, then take out above-mentioned microslide substrate, carefully suprabasil for microslide white depositions is rinsed well with deionized water, obtain the nanometer stick array of zinc paste; The top of zinc oxide nano rod is comparatively evenly sparse, such structure is advantageously for the growth of Cd nano-chip arrays.Because structure sparse is like this conducive to the deposition of the Cd steam group in vacuum tube furnace, namely relative to ganoid substrate, structure sparse like this can stop that more Cd steam carries out nucleation and growth.In addition, owing to being by the gap evenly existed between nanometer rods, such skeleton can avoid the formation of Seed Layer thereon when realizing Cd nanometer sheet and growing.
(2) synthesis of cadmium oxide nanostructured and the preparation of gas sensitive device
1. the CdS powder of 0.05g is placed in the central authorities of vacuum tube furnace, then above-mentioned length is had the microslide substrate of the nanometer stick array of zinc paste to be positioned over distance CdS powder 30cm place; The specification of glass sheet is 2cm × 4cm;
2. vacuum tube furnace is evacuated to 100mTorr, then the nitrogen simultaneously passed into and air, and overpressure is adjusted to 9Torr, be warming up to 650 DEG C, insulation 30min, naturally cools to room temperature, obtains the nano-chip arrays of Cd; The flow of the air passed into is 250sccm, and the flow of nitrogen is 45sccm;
3. at 400 DEG C of temperature, be incubated 30min in atmosphere to the microslide substrate of the nano-chip arrays of Cd obtained above, oxidation obtains the nanostructured of the cadmium oxide with secondary pore space structure; The pattern of its nanostructured, as shown in Fig. 2-b, can be seen by figure, the basic pattern of the nanostructured obtained also in store nano-chip arrays, but some holes have appearred in each nanometer sheet.The nano-chip arrays that each nanometer sheet is formed is first order hole, and the porous in each nanometer sheet constitutes the hole of the second level, and the existence of second level hole is that it has the major reason of excellent air-sensitive performance.And can be seen by Fig. 1, the nano-chip arrays of this double-decker top CdO obtained has good contacting with the ZnO nano-rod array of bottom.Can be seen by careful observation, in the interface of contact, the bottom of nanometer sheet directly and the tip contact of the nanometer rods of bottom, and is direct contact, there is not a visible film existence.The existence of adopting and comparatively perfectly can solve the Seed Layer bottom CdO nano-chip arrays is in this way described, and then eliminates its impact for air-sensitive performance.
4. there is the microslide substrate of composite structure to be cut into the rectangle that size is 0.5cm × 1cm growth, and apply two strip electrodes with silver slurry at two ends, then be incubated 6 hours at 100 DEG C, the obtained cadmium oxide nanometer gas sensitive device with secondary pore space structure.
Best air-sensitive performance is obtained under this Parameter Conditions.Under the oxidizing temperature of 400 DEG C, the device obtained has air-sensitive performance the most excellent, and under the working temperature of 215 DEG C, the sensitivity for the ether of 100ppm is 138%, and response and release time are 15s and 27s respectively, and have best selectivity.So the cadmium oxide with secondary hole obtained under the oxidizing temperature of 400 DEG C has air-sensitive performance the most excellent.
Embodiment 2
The present embodiment is similar to embodiment 1, and difference is: step (2) 3. in the oxidizing temperature of cadmium oxide be 360 DEG C, can be seen by Fig. 2-a, under this working temperature, the pattern of the cadmium oxide obtained is complete nano-chip arrays.Under this oxidizing temperature, obtaining double-decker under the same terms for the sensitivity of ether is 36%, and response and release time are 22s and 51s respectively.
Embodiment 3
The present embodiment is similar to embodiment 1, and difference is: step (2) 3. in the oxidizing temperature of cadmium oxide be 440 DEG C.Can be seen by Fig. 2-c, under this working temperature, the pattern of the cadmium oxide obtained is for having spongiform cadmium oxide.At this temperature, obtaining double-decker under the same terms for the sensitivity of ether is 43%, and response and release time are 44s and 57s respectively.
Claims (4)
1. fabricated in situ has a cadmium oxide nanometer gas sensor for secondary pore space structure, has following steps:
(1) synthesis of nanometic zinc oxide rod array Seed Layer
1. using ethylene glycol monoemethyl ether as solvent, configuration concentration is the mixed solution of the zinc acetate of 0.1M and the monoethanolamine of 0.2M; Immerse 30s in above-mentioned solution using microslide as substrate, then microslide substrate is placed in baking oven drying process; After repetition aforesaid operations twice, by above-mentioned microslide substrate in atmosphere in 500 DEG C of annealing in process 1h, make Seed Layer and microslide substrate rigid contact;
2. using deionized water as solvent, configuration concentration is the mixed solution of the zinc nitrate of 0.025M and the hexamethylene tetramine of 0.025M;
Get the above-mentioned mixed solution of 60-80ml in reactor, and the reactor filling mixed solution is put in above-mentioned microslide substrate, have one of Seed Layer to face down, the height of mixed solution did not have substrate just;
3. reactor is put into baking oven, at the temperature of 100 DEG C, be incubated 9 hours, then take out above-mentioned microslide substrate, carefully suprabasil for microslide white depositions is rinsed well with deionized water, obtain the nanometer stick array of zinc paste.
(2) synthesis of cadmium oxide nanostructured and the preparation of gas sensitive device
1. the CdS powder of 0.05g is placed in the central authorities of vacuum tube furnace, then above-mentioned length is had the microslide substrate of the nanometer stick array of zinc paste to be positioned over distance CdS powder 30cm place;
2. vacuum tube furnace is evacuated to 100mTorr, then the nitrogen simultaneously passed into and air, and overpressure is adjusted to 9Torr, be warming up to 650 DEG C, insulation 30min, naturally cools to room temperature, obtains the nano-chip arrays of Cd;
3. at 360 ~ 440 DEG C of temperature, be incubated 30min in atmosphere to the microslide substrate of the nano-chip arrays of Cd obtained above, oxidation obtains the nanostructured of cadmium oxide;
4. there is the microslide substrate of composite structure to be cut into the rectangle that size is 0.5cm × 1cm growth, and apply two strip electrodes with silver slurry at two ends, then be incubated 6 hours at 100 DEG C, the obtained cadmium oxide nanometer gas sensitive device with secondary pore space structure.
2. fabricated in situ according to claim 1 has the gas sensitive device of secondary hole cadmium oxide nanostructured, it is characterized in that, the specification of described step (1) microslide substrate is 1. 2cm × 4cm.
3. fabricated in situ according to claim 1 has the gas sensitive device of secondary hole cadmium oxide nanostructured, it is characterized in that, the flow of the air that described step (2) 2. passes into is 250sccm, and the flow of nitrogen is 45sccm.
4. fabricated in situ according to claim 1 has the gas sensitive device of secondary hole cadmium oxide nanostructured, it is characterized in that, the optimum working temperature of air-sensitive original paper of the present invention is 215 DEG C.
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Cited By (2)
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| CN106556623A (en) * | 2016-08-15 | 2017-04-05 | 华南师范大学 | A kind of gas-liquid interface processing method of semiconductor gas sensor |
| US10809216B2 (en) | 2017-10-23 | 2020-10-20 | Boe Technology Group Co., Ltd. | Gas sensor and method for manufacturing the same, and detection device |
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