CN105136863A - Gas sensor based on CdIn2O4 nano film and preparation method of gas sensor - Google Patents

Gas sensor based on CdIn2O4 nano film and preparation method of gas sensor Download PDF

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CN105136863A
CN105136863A CN201510575958.8A CN201510575958A CN105136863A CN 105136863 A CN105136863 A CN 105136863A CN 201510575958 A CN201510575958 A CN 201510575958A CN 105136863 A CN105136863 A CN 105136863A
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cdin
nano
gas sensor
film
preparation
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CN105136863B (en
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王毓德
董成军
王莉红
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Yunnan University YNU
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Abstract

The invention relates to a gas sensor based on a CdIn2O4 nano film and a preparation method of the gas sensor, and belongs to the technical field of sensing of an inorganic porous material and gas. According to the gas sensor provided by the invention, the CdIn2O4 nano porous film is taken as a sensing layer of the sensor, and the CdIn2O4 nano porous film is prepared on the surface of a polished silicon chip sputtered with an Au-interdigital electrode by adopting a self-diffusion solvent evaporation self-assembly method, wherein used predecessors are block copolymer, cadmium acetate, indium tris acetylacetonate and absolute ethyl alcohol; the silicon chip is placed into a muffle furnace for heat treatment, and the obtained CdIn2O4 nano porous film has the film pore diameter of 20 to 30 nm. By adopting the CdIn2O4 nano porous film sensor to detect formaldehyde gas, the advantages of high sensitivity for the formaldehyde gas, low working temperature, small size and low power consumption and the like are achieved, and better practical application value is obtained.

Description

Based on CdIn 2o 4the gas sensor of nano thin-film and preparation method
Technical field
The present invention relates to a kind of based on CdIn 2o 4the gas sensor of nano thin-film and preparation method, belong to inorganic porous material and gas sensing techniques field.CdIn 2o 4nano-porous film detects formaldehyde gas as sensitive material, have highly sensitive, working temperature is low, volume is little, the advantage such as low in energy consumption.
Background technology
Formaldehyde in indoor air has become the major pollutants affecting human body health.The too high meeting of concentration of formaldehyde causes acute poisoning, shows as throat burning pain, expiratory dyspnea, pulmonary edema, anaphylactoid purpura, allergic dermatitis, liver transaminase rising, jaundice etc.For a long time, low concentration Formaldehyde Exposed can cause headache, dizziness, weak, sensory disturbance, immunity reduction, and can occur drowsiness, failure of memory or neurasthenia, mental depression; Slow poisoning is also huge to the harm of respiratory system, and Long Term Contact formaldehyde can cause respiratory dysfunction and hepatogenotoxicity pathology, shows as hepatocellular injury, liver radiation energy exception etc.In order to reduce and Control pollution, mould comfortable living environment, then require that PARA FORMALDEHYDE PRILLS(91,95) gas carries out detection control, even eliminate, this is with regard to the good formaldehyde sensor of inevitable requirement performance.So, develop a kind of highly sensitive formaldehyde gas sensor and there is very high practical significance.Gas sensitive device based on metal-oxide semiconductor (MOS) is widely used owing to having the advantage such as cheap, gas sensing property good, be easy to assembling, volume is little.Spinelle type composite oxides CdIn 2o 4be a kind of high degeneracy n-type semiconductor, to some gas, especially inflammable and explosive, toxic and harmful, as ethanol, NO, NO 2, Cl 2very sensitive.CdIn 2o 4pARA FORMALDEHYDE PRILLS(91,95) also has certain susceptibility, can obtain higher air-sensitive performance by improvement preparation technology and working sensor condition.But CdIn 2o 4the sensitivity of material PARA FORMALDEHYDE PRILLS(91,95) gas need further raising, to meet the requirement of practical application.In order to promote its gas sensing performance further, CdIn 2o 4the design of the nano-porous structure of gas sensitive becomes the important directions of development.It is large that nano-porous structure has surface area, and modifiable inside surface (modification, doping), be conducive to the diffusion of reactant, thus can effectively improve its air-sensitive performance and reduce the response time, turn avoid the drawback that these nano materials are easily reunited in application process simultaneously.The CdIn of current application 2o 4gas sensor, due to the many avtive spot feature of the Large ratio surface sum that do not possess nano-porous structure, is difficult to obtain PARA FORMALDEHYDE PRILLS(91,95) high air-sensitive property, therefore requires further improvement the appearance structure of material thus promote its air-sensitive performance.
Summary of the invention
Therefore, the present invention is to provide a kind of with nanoporous CdIn 2o 4film is gas sensor and the preparation method of gas sensitive.Simple one-pass film-forming technique is adopted to prepare CdIn 2o 4nano-porous film, as gas sensor sensing layer, utilizes CdIn 2o 4the topographical property of nano-porous film uniqueness and functional characteristic, it can be used as formaldehyde gas sensitive material, obtains highly sensitive formaldehyde gas sensor.
The present invention is achieved by following technical solution.
A kind of based on CdIn 2o 4the gas sensor of nano-porous film and preparation method, have following steps:
(1) CdIn 2o 4the preparation of colloidal sol: precursor be polyisobutylene- b-polyethylene oxide block copolymer, cadmium acetate, Indium Tris acetylacetonate, absolute ethyl alcohol, segmented copolymer is added (1 ~ 2:25 prepares colloidal sol in mass ratio) in ethanol solution, ultrasonic vibration 30min, obtain clear solution A, cadmium acetate, Indium Tris acetylacetonate are dissolved into respectively (mass ratio is respectively 1:4 and 1:8) in absolute ethyl alcohol, obtain solution B and C, in stirring, solution B is slowly added drop-wise in C, stir 30min, obtain solution D, in stirring, solution D is slowly added drop-wise in A, stirs 30min, obtain solution C dIn 2o 4colloidal sol;
(2) gained CdIn 2o 4colloidal sol is magnetic agitation (500r/min) 24h at room temperature, then at room temperature ageing 24h;
(3) step (2) gained colloidal sol is dripped to the silicon chip polished surface that sputtering has golden interdigital electrode, each colloidal sol consumption is 1 ~ 2, silicon chip product is at high temperature dried after whole silicon chip surface 1h until colloidal sol natural diffuseness, be placed in muffle furnace again to heat-treat, obtain CdIn at silicon substrate surface 2o 4nano-porous film, obtains CdIn 2o 4nano-porous film gas sensor element.
accompanying drawing illustrates:
The CdIn of Fig. 1 prepared by embodiment one 2o 4the X-ray diffractogram of nano-porous film, shows pure CdIn 2o 4characteristic diffraction peak peak position and standard card (JCPDS70-1680) completely the same, inclusion-free peak occurs, and peak type is sharp-pointed, shows that crystal structure degree is fine;
The CdIn of Fig. 2 prepared by embodiment one 2o 4the electron scanning micrograph figure of nano-porous film, photo shows that its pattern is nano-porous structure, and aperture is about 20nm;
The CdIn of Fig. 3 prepared by embodiment one 2o 4the sensitivity of nano-porous film sensor PARA FORMALDEHYDE PRILLS(91,95), CdIn 2o 4nano-porous film sensor is to having higher sensitivity;
The CdIn of Fig. 4 prepared by embodiment two 2o 4the electron scanning micrograph figure of nano-porous film, photo shows that its pattern is nano-porous structure, and aperture is about 20nm.
embodiment:
The present invention is raw materials used all adopts commercially available analytical reagent, and below in conjunction with specific embodiment, the present invention is further detailed explanation.
embodiment one:
(1) CdIn 2o 4the preparation of colloidal sol: precursor be polyisobutylene- b-polyethylene oxide block copolymer, cadmium acetate, Indium Tris acetylacetonate, absolute ethyl alcohol, segmented copolymer is added (1:25 prepares colloidal sol in mass ratio) in ethanol solution, ultrasonic vibration 30min, obtain clear solution A, cadmium acetate, Indium Tris acetylacetonate are dissolved into respectively (mass ratio is respectively 1:4 and 1:8) in absolute ethyl alcohol, obtain solution B and C, in stirring, solution B is slowly added drop-wise in C, stir 30min, obtain solution D, in stirring, solution D is slowly added drop-wise in A, obtains solution C dIn 2o 4colloidal sol;
(2) gained CdIn 2o 4colloidal sol is magnetic agitation (500r/min) 24h at room temperature, then at room temperature ageing 48h;
(3) keep relative air humidity to be 30%, step (2) gained colloidal sol being dripped to sputtering has the silicon chip polished surface of golden interdigital electrode, and each colloidal sol consumption is 1, after colloidal sol natural diffuseness to whole silicon chip surface 1h by silicon chip product 80 o24h drying and processing under C;
(4) by the sample silicon chip after step (3) drying and processing in muffle furnace during thermal treatment, heating rate is 1 oc/min, heat treatment temperature is 650 oc, heat treatment time is 2h;
(5) by CdIn prepared by step (4) 2o 4the sensitivity characteristic of its PARA FORMALDEHYDE PRILLS(91,95) gas of nano-porous film sensor test is 100 in working temperature oduring C, the sensitivity of 100ppm formaldehyde gas concentration is 16.0, and response, release time are respectively 1min, 5min.
embodiment two:
(1) CdIn 2o 4the preparation of colloidal sol: precursor be polyisobutylene- b-polyethylene oxide block copolymer, cadmium acetate, Indium Tris acetylacetonate, absolute ethyl alcohol, segmented copolymer is added (1.5:25 prepares colloidal sol in mass ratio) in ethanol solution, ultrasonic vibration 30min, obtain clear solution A, cadmium acetate, Indium Tris acetylacetonate are dissolved into respectively (mass ratio is respectively 1:4 and 1:8) in absolute ethyl alcohol, obtain solution B and C, in stirring, solution B is slowly added drop-wise in C, stir 30min, obtain solution D, in stirring, solution D is slowly added drop-wise in A, obtains solution C dIn 2o 4colloidal sol;
(2) gained CdIn 2o 4colloidal sol is magnetic agitation (500r/min) 24h at room temperature, then at room temperature ageing 48h;
(3) keep relative air humidity to be 20%, step (2) gained colloidal sol being dripped to sputtering has the silicon chip polished surface of golden interdigital electrode, and each colloidal sol consumption is 1, after colloidal sol natural diffuseness to whole silicon chip surface 1h by silicon chip product 85 o20h drying and processing under C;
(4) by the sample silicon chip after step (3) drying and processing in muffle furnace during thermal treatment, heating rate is 1 oc/min, heat treatment temperature is 700 oc, heat treatment time is 1.5h;
(5) by CdIn prepared by step (4) 2o 4the sensitivity characteristic of its PARA FORMALDEHYDE PRILLS(91,95) gas of nano-porous film sensor test is 100 in working temperature oduring C, the sensitivity of 100ppm gas concentration is 14.8, and response, release time are respectively 1min, 5.5min.
embodiment three:
(1) CdIn 2o 4the preparation of colloidal sol: precursor be polyisobutylene- b-polyethylene oxide block copolymer, cadmium acetate, Indium Tris acetylacetonate, absolute ethyl alcohol, segmented copolymer is added (2:25 prepares colloidal sol in mass ratio) in ethanol solution, ultrasonic vibration 30min, obtain clear solution A, cadmium acetate, Indium Tris acetylacetonate are dissolved into respectively (mass ratio is respectively 1:4 and 1:8) in absolute ethyl alcohol, obtain solution B and C, in stirring, solution B is slowly added drop-wise in C, stir 30min, obtain solution D, in stirring, solution D is slowly added drop-wise in A, obtains solution C dIn 2o 4colloidal sol;
(2) gained CdIn 2o 4colloidal sol is magnetic agitation (500r/min) 24h at room temperature, then at room temperature ageing 48h;
(3) keep relative air humidity to be 15%, step (2) gained colloidal sol being dripped to sputtering has the silicon chip polished surface of golden interdigital electrode, and each colloidal sol consumption is 1, after colloidal sol natural diffuseness to whole silicon chip surface 1h by silicon chip product 90 o12h drying and processing under C;
(4) by the sample silicon chip after step (3) drying and processing in muffle furnace during thermal treatment, heating rate is 1 oc/min, heat treatment temperature is 750 oc, heat treatment time is 1h;
(5) by CdIn prepared by step (4) 2o 4the sensitivity characteristic of its PARA FORMALDEHYDE PRILLS(91,95) gas of nano-porous film sensor test is 100 in working temperature oduring C, the sensitivity of 100ppm gas concentration is 15.4, and response, release time are respectively 1min, 5min.
The present invention adopts static volumetric method to measure CdIn 2o 4the sensitivity characteristic of nano-porous film sensor element PARA FORMALDEHYDE PRILLS(91,95) gas, the sensitivity of definition gas sensor β= r a/ r g, wherein r awith r gbe respectively the resistance value of sensor element in dry air and formaldehyde gas.

Claims (5)

1. based on CdIn 2o 4the gas sensor of nano thin-film and preparation method, is characterized in that having following preparation process and step:
(1) CdIn 2o 4the preparation of colloidal sol: precursor be polyisobutylene- b-polyethylene oxide block copolymer, cadmium acetate, Indium Tris acetylacetonate, absolute ethyl alcohol, segmented copolymer is added in ethanol solution, 1 ~ 2:25 prepares colloidal sol in mass ratio, ultrasonic vibration 30min, obtain clear solution A, cadmium acetate, Indium Tris acetylacetonate are dissolved in absolute ethyl alcohol respectively, mass ratio is respectively 1:4 and 1:8, obtain solution B and C, in stirring, solution B is slowly added drop-wise in C, stirs 30min, obtain solution D, in stirring, solution D is slowly added drop-wise in A, obtains solution C dIn 2o 4colloidal sol;
(2) gained CdIn 2o 4colloidal sol is magnetic agitation 24h at room temperature, and stir speed (S.S.) is 500r/min, then at room temperature ageing 48h;
(3) step (2) gained colloidal sol is dripped to the silicon chip polished surface that sputtering has golden interdigital electrode, each colloidal sol consumption is 1 ~ 2, silicon chip product is at high temperature dried after whole silicon chip surface 1h until colloidal sol natural diffuseness, be placed in muffle furnace again to heat-treat, obtain CdIn at silicon substrate surface 2o 4nano-porous film, obtains CdIn 2o 4nano-porous film gas sensor element.
2. according to claim 1 based on CdIn 2o 4the gas sensor of nano thin-film and preparation method, is characterized in that, preparation CdIn in described step (3) 2o 4during nano-porous film, relative air humidity is 15 ~ 30%.
3. according to claim 1 based on CdIn 2o 4the gas sensor of nano thin-film and preparation method, is characterized in that, in described step (3), the bake out temperature of silicon chip product is 80 ~ 90 oc, the time is 12 ~ 24h.
4. according to claim 1 based on CdIn 2o 4the gas sensor of nano thin-film and preparation method, is characterized in that, in described step (3), sample silicon chip is in muffle furnace during thermal treatment, and heating rate is 1 oc/min, heat treatment temperature is 650 ~ 750 oc, heat treatment time is 1 ~ 2h.
5. according to claim 1 based on CdIn 2o 4the gas sensor of nano thin-film and preparation method, is characterized in that, after the Thin-film anneal of described step (4), silicon chip forms the CdIn that aperture is 20 ~ 30nm 2o 4nano-porous film.
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