CN110261444A - A kind of preparation method of the gas sensitive material for acetone gas sensor - Google Patents
A kind of preparation method of the gas sensitive material for acetone gas sensor Download PDFInfo
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- CN110261444A CN110261444A CN201910546257.XA CN201910546257A CN110261444A CN 110261444 A CN110261444 A CN 110261444A CN 201910546257 A CN201910546257 A CN 201910546257A CN 110261444 A CN110261444 A CN 110261444A
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- 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
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Abstract
The present invention provides a kind of preparation methods of gas sensitive material for acetone gas sensor.0.3 g, six water indium acetate is dissolved in 35 mL deionized waters first, then under magnetic agitation effect, sequentially adds 0.015 g urea, 0.036g glucose.After 0.5 h of magnetic agitation, resulting mixed solution is transferred in the hydrothermal reaction kettle of 50 mL, reaction kettle is placed in 160o12 h are kept the temperature in C baking oven.Terminate, after reaction kettle cooled to room temperature wait react, white depositions are obtained by centrifugation, deionized water cleaning.Finally, white depositions are carried out to high-temperature process (500 in Muffle furnaceoC keeps 2h) obtain lurid In2O3Be cracked cube.In involved in the present invention2O3Cracking square sensitive material not only shows excellent acetone air-sensitive performance, but also its preparation process is simple, low in cost, environmentally protective, is suitble to industrialized production.
Description
Technical field
The invention belongs to gas sensor domain, it is related to a kind of acetone gas sensor high performance gas sensitive material
Preparation method.
Background technique
Various gas sensors are in necks such as industrial production, smart home, modern agriculture and space flight detections
Domain has played huge effect.In all kinds of gas sensors, metal-oxide semiconductor (MOS) base gas sensor, due in air
Feasible and reliability application in terms of quality testing, gas leakage and medical diagnosis receives greatly concern (J.H. Ma, Y.
Ren, X.R. Zhou, L.L. Liu, Y.H. Zhu, X.W. Cheng, P.C. Xu, X.X. Li, Y.H. Deng,
D.Y. Zhao, Pt nanoparticles sensitized ordered mesoporous WO3 semiconductor:
gas sensing performance and mechanism study, Advanced Functional Materials,
2018,28,1705268).For example, by analysis patient's exhaled gas composition and concentration information, doctor can soon,
Non-invasively it is diagnosed to be many recessive disorders.For diabetes patient, due to renal insufficiency, contain in the expiratory air of diabetes patient
There are more acetone gas.Therefore, by acetone gas sensor, can by it is real-time, quick, non-invasively detect in people's expiratory air
Acetone gas concentration tracks the state of an illness of diabetes patient.More importantly compared to traditional medical diagnosis technology (for example, blood
Fluid inspection and gas chromatographic analysis), metal-oxide semiconductor (MOS) base gas sensor has convenience, can carry and operate letter
The advantages such as just.Therefore, explore develop high performance gas sensor be it is necessary with it is vital.
As reported in the literature, metal-oxide semiconductor (MOS) (ZnO, In2O3、Co3O4、WO3) base sensitive material air-sensitive mistake
Journey includes gas absorption, surface chemical reaction, electronics transfer and Gas desorption process, and these processes with it is prepared quick
Structure, composition, exposure crystal face, surface defect of sense material etc. are closely related, and gas-sensing mechanisms are exposed to based on gas sensitive
When in different atmospheres, apparent variation occurs for the resistance of sensitive material.Therefore, improve air-sensitive process (such as far as possible
Gas absorption) it is the key that improve air-sensitive performance.So, rationally controllable to construct with specific morphology, structure and more multilist
Oxide semiconductor nano material more than the active site of face is the feasible path for promoting sensitive material air-sensitive performance.
In various metal-oxide semiconductor (MOS)s, indium oxide (In2O3) be typical N-shaped oxide semiconductor, by with
Detect various gases, such as ethyl alcohol, formaldehyde, acetone, hydrogen sulfide, hydrogen, chlorine, nitrogen dioxide (Y.S. Liu, X. Gao,
F. Li, G.Y. Lu, T. Zhang, N. Barsan, Pt-In2O3 mesoporous nanofibers with
enhanced gas sensing performance towards ppb-level NO2 at room temperature,
Sensors and Actuators B:Chemical, 2018, 260, 927-936).In indium oxide (In2O3) various systems
In standby strategy, since easy to operate, sample topography is controllable, hydrothermal method method is the most-often used technology of scientific research personnel.Thus,
It can be realized by accuracy controlling hydrothermal reaction condition (temperature, reaction time etc.) and type, concentration of reactant etc. specific
The controllable preparation of the oxidation phosphide material of pattern.
In this patent, subsequent annealing is combined using hydro-thermal technology of preparing, is successfully realized indium oxide (In2O3)
The controllable preparation of cracking cube.When by prepared indium oxide (In2O3) cracking cube be fabricated to heater-type gas sensor after,
Air-sensitive test result shows: indium oxide (In2O3) cracking cube has preferable selectivity, higher sensitive to acetone gas
The response speed and preferable stability spend, being exceedingly fast.Compared to the indium oxide cube of not crackle, indium oxide (In2O3) tortoise
Split cube and show faster resume speed and identical response speed: indium oxide cracking cube base gas sensor exists
200 oC is respectively 2 s and 116 s to response time, the recovery time of 100 ppm acetone；And the solid cube base gas of indium oxide
Body sensor is 200oC is respectively 1 s and 206 s to response time, the recovery time of 100 ppm acetone.
Summary of the invention
The object of the present invention is to provide a kind of sensitive materials that is environmentally protective, inexpensive, detecting easily to operate for acetone gas
The preparation method of material, to adapt to the needs of industrialized production.
Of the invention is technically characterized in that using appropriate indium acetate, urea, glucose, deionized water as reactant, passes through choosing
Appropriate hydrothermal temperature and reaction time are selected, realizes polygon indium oxide (In2O3) cube controllable preparation.It is made
Standby indium oxide cracking cube can not only provide bigger contact area for gas absorption, surface reaction, and being capable of structure
More loose sensitive material is built, and then prepared polygon indium oxide cube is made to show excellent acetone gas sensing property
Energy.
To achieve the above object, the invention discloses following technology contents:
A method of being used to prepare the preparation of the gas sensitive of high-performance acetone gas detection, it is characterised in that this method is pressed
Following steps carry out:
(1) 0.3 g, six water indium acetate is dissolved in 35 mL deionized waters, then under magnetic agitation effect, is sequentially added
0.015 g urea, 0.036 g glucose after 0.5 h of magnetic agitation, obtain milky mixed solution；
(2) milky mixed solution is transferred in the hydrothermal reaction kettle of 50 mL, then by reaction kettle as 160oIn C baking oven
Carry out hydro-thermal reaction.Oven temperature is set as 160oC keeps 12 h.Terminate, after reaction kettle cooled to room temperature wait react,
It is cleaned 3 times by centrifugation, deionized water, obtains white depositions.
(3) white depositions are subjected in Muffle furnace the high temperature anneal and obtain lurid In2O3Be cracked cube.
Annealing conditions are as follows: 500oC keeps 2h, and heating and cooling rate are 5oC/min.The surface of prepared indium oxide cube
Coarse, there are many crackles, and length is about 300-600 nm.There are many cubes to show explosion shape pattern.
The present invention, which is further disclosed, is preparing high performance acetone gas sensor gas sensitive using the method
The application of aspect.Air-sensitive test result is shown, 200oUnder the operating temperature of C, In2O3Cracking cube to acetone gas have compared with
High sensitivity (9.2), faster response/resume speed (2 s/116 s) and preferable stability.
Present invention mainly solves the prior art prepare acetone gas sensor in sensitive material when complicated for operation, environment
Pollution, it is with high costs, be difficult to industrialization, the problems such as sensitive material pattern prepared simultaneously is uncontrollable, sensitive material performance is poor,
Indium oxide (In disclosed by the invention2O3) cracking cube preparation method and prior art line exist than possessed good effect
In:
(1) hydrothermal technique advantage is made full use of, when by selecting suitable indium source, precipitating reagent, solvent, reaction temperature and reaction
Between, the indium oxide sensitive material of controllable preparation specific morphology.
(2) raw material sources for preparing indium oxide cracking cube are extensive and nontoxic, the non-flammable drugs such as explosive.
(3) during the preparation process, main equipment to be used includes baking oven, hydrothermal reaction kettle, Muffle furnace, these equipment are not only
Simple and easy to operate and maintenance cost is extremely low.The repeatability of sensitive material preparation simultaneously is high, is suitble to industrialized production.
Detailed description of the invention
Fig. 1 is the SEM figure of the indium oxide cracking cube gas sensitive prepared by the present invention for acetone gas sensor；
A therein is the SEM photograph of low power, and b, c are the SEM photographs of amplification, and d is the SEM photograph of high power；
Fig. 2 is the XRD diagram of the indium oxide cracking cube gas sensitive prepared by the present invention for acetone gas sensor；
Fig. 3 is indium oxide cracking cube gas sensitive prepared by the present invention 200oUnder C operating temperature, to 100 ppm acetone
Response/recovery curve of gas；
Fig. 4 is indium oxide cracking cube gas sensitive prepared by the present invention 200oUnder C operating temperature, it is exposed to different dense
Spend the resistance dynamic changing curve in acetone gas.
Specific embodiment
The present invention is described below by specific embodiment.Unless stated otherwise, technological means used in the present invention
It is method known in those skilled in the art.In addition, embodiment is interpreted as illustrative, it is not intended to limit the present invention
Range, the spirit and scope of the invention are limited only by the claims that follow.To those skilled in the art, without departing substantially from this
Under the premise of invention spirit and scope, in these embodiments various changes or change also belong to protection model of the invention
It encloses.The raw materials such as six water indium acetate therein, urea are commercially available.
Embodiment 1
(1) 0.3 g, six water indium acetate is dissolved in 35 mL deionized waters, then under magnetic agitation effect, is sequentially added
0.015 g urea, 0.036 g glucose after 0.5 h of magnetic agitation, obtain milky mixed solution；
(2) milky mixed solution is transferred in the hydrothermal reaction kettle of 50 mL, reaction kettle is then placed in 160oIn C baking oven
Carry out hydro-thermal reaction.Oven temperature is set as 160oC keeps 12 h.Terminate, after reaction kettle cooled to room temperature wait react,
It is cleaned 3 times by centrifugation, deionized water, obtains white depositions.
(3) white depositions are subjected in Muffle furnace the high temperature anneal and obtain lurid indium oxide (In2O3) cracking
Cube.Annealing conditions are as follows: 500oC keeps 2h, and heating and cooling rate are 5oC/min.Prepared indium oxide cube
The rough surface of body, there are many crackles.The length of cube is about 300-600 nm, shows explosion there are many cube
Shape pattern.Air-sensitive test data shows 200oUnder the operating temperature of C, In2O3Cracking cube has acetone gas higher
Sensitivity (9.2), faster response/resume speed (2 s/116 s) and preferable stability.
Embodiment 2
For the technical characterstic for further illustrating the method for the present invention, following comparative experiments is carried out:
(1) 0.3 g, six water indium acetate is dissolved in 35 mL deionized waters, then under magnetic agitation effect, is sequentially added
0.005 g sodium hydroxide, 0.18 g glucose after 0.5 h of magnetic agitation, obtain milky mixed solution；
(2) milky mixed solution is transferred in the hydrothermal reaction kettle of 50 mL, reaction kettle is then placed in 120oIn C baking oven
Carry out hydro-thermal reaction.Oven temperature is set as 120oC keeps 12 h.Terminate, after reaction kettle cooled to room temperature wait react,
It is cleaned 3 times by centrifugation, deionized water, obtains white depositions.
(3) white depositions are subjected in Muffle furnace the high temperature anneal and obtain lurid indium oxide (In2O3) solid
Cube.Annealing conditions are as follows: 500oC keeps 2h, and heating and cooling rate are 5oC/min.Obtained indium oxide (In2O3)
The rough surface of solid cube, without crackle, length is about 150-300 nm.Air-sensitive test result shows to compare
In the indium oxide cube of cracking, the solid cube of indium oxide is 200oUnder C operating temperature more to the resume speed of acetone gas
Slowly (recovery time is 206 s).
By the above comparative experiments it is found that when preparing acetone gas sensor sensitive material using the method for the present invention, preparation
Method is environmentally protective, low in cost, easily operated, is suitble to industrialized production.Indium oxide (In obtained simultaneously2O3) be cracked and stand
Cube shows excellent air-sensitive performance to acetone gas.Therefore, the method for the present invention is the acetone gas of a kind of high efficiency, low cost
The preparation method of body sensor gas sensitive.
Embodiment 3
Contain more acetone gas in the expiratory air of diabetes patient, therefore can be real-time, noninvasive, quick by gas sensor
Ground detects acetone concentration in diabetes patient's expiration, and then realizes the tracking to blood sugar in diabetic patients concentration.But common blood
Measuring method determines blood-sugar content in diabetes patient such as fasting blood-glucose (FBS), has invasive, and has to patient certain
Nocuity: before carrying out diabetes test, fasting at least 8-12 h is answered.If being lower than 100 mg/dl as the result is shown, then it represents that blood
It is sugared normal.If range is 100-125 mg/dl, then it represents that prediabetes are in, and when result is more than 126 mg/dl, then
Show with diabetes.Thus, the preparation method of sensitive material being capable of green in the acetone gas sensor that this patent is proposed
It is environmentally friendly, repeating, industrialized to prepare indium oxide cracking cube, and it is made into gas sensor, to apply
It is detected in diabetes.
Claims (2)
1. a kind of preparation method of the gas sensitive material for acetone gas sensor, it is characterised in that by following step into
Row:
(1) 0.3 g, six water indium acetate is dissolved in 35 mL deionized waters, then under magnetic agitation effect, is sequentially added
0.015 g urea, 0.036 g glucose after 0.5 h of magnetic agitation, obtain milky mixed solution；
(2) milky mixed solution is transferred in the hydrothermal reaction kettle of 50 mL, reaction kettle is then placed in 160oIn C baking oven
Carry out hydro-thermal reaction；Oven temperature is set as 160oC keeps 12 h, terminates, after reaction kettle cooled to room temperature wait react,
It is cleaned 3 times by centrifugation, deionized water, obtains white depositions；
(3) white depositions are subjected in Muffle furnace the high temperature anneal and obtain lurid In2O3Be cracked cube；Annealing
Condition are as follows: 500oC keeps 2h, and heating and cooling rate are 5oC/min；The surface of prepared indium oxide cube is thick
Rough, there are many crackle, length is about 300-600 nm, and cube shows explosion shape pattern.
2. application of the method described in claim 1 in terms of preparing high-performance acetone gas sensor gas sensitive；Wherein institute
The high-performance acetone gas sensor gas sensitive stated refers to: indium oxide is cracked cube 200oUnder C operating temperature, compared with
High sensitivity (9.2), faster response/resume speed (2 s/, 116 s) and preferable stability.
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Application publication date: 20190920 |