CN106770493B - A kind of acetone gas sensor and preparation method thereof based on CNTs@α-Fe2O3 heterojunction composite - Google Patents
A kind of acetone gas sensor and preparation method thereof based on CNTs@α-Fe2O3 heterojunction composite Download PDFInfo
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- G—PHYSICS
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- 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
Abstract
One kind being based on CNTs@a-Fe2O3Acetone gas sensor of heterojunction composite and preparation method thereof belongs to gas sensor technical field.The oxide aluminium earthenware outer substrate of 2 cyclic annular gold electrodes parallel to each other and discrete is had by outer surface, is formed coated in the metal oxide semiconductor gas sensitive material on oxide aluminium earthenware outer outer substrate surface and gold electrode and the nichrome heating coil being placed in ceramics pipe outer, platinum filament wire is had on each gold electrode；Sensitive material is CNTs and α-Fe2O3The compound hetero-junctions graded structure nano material of nanometer rods.Sensor of the present invention has the advantages that simple structure, cheap, small volume, durable and mass production, and the test result of gas-sensitive property shows that the sensor can carry out low concentration acetone to detect and have splendid long-time stability, so that it has important application prospect to the detection of acetone leakage in industrial production and alarm aspect and medical context of detection.
Description
Technical field
The invention belongs to oxide semiconductor gas sensor technical fields, and in particular to one kind is based on CNTs@α-Fe2O3
The acetone gas sensor and preparation method thereof of hetero-junctions graded structure composite material.
Background technique
With the concern of people's environmental pollution and industrial discharge, the real-time monitoring of toxic and harmful gas has been obtained greatly
Attention.Wherein, conductor oxidate formula gas sensor with its excellent performance and facilitates manufacture to obtain extensive concern.
In the past few decades, although achieving great successes for the research of the semiconductor-type gas-sensitive property of metal oxide, high-performance,
Highly selective, the research of the device of small size is still following challenge.The sensitivity of oxide semiconductor gas sensor
Mechanism is mainly react to each other caused semiconductor conductance of the semiconductor to the absorption of oxygen and object gas and between them
Variation.Therefore, the pattern of material, microstructure and crystalline size play a very important role gas-sensitive property.For having solely
The sensitive material of special structure and pattern is designed to for the main target of researcher.Recently, many research shows that compared to single
The hetero-junctions oxide semiconductor that monoxide is made of different chemical constituents shows excellent performance.
Carbon nanotube (Carbon Nanotubes, CNTs) with its excellent physics, chemistry, electrical and mechanical performance once
It was found that just causing the great interest of scientific research personnel.Past 20 years, people be explore CNTs application potential be put to it is huge
Effort.It can cause the change of its electrical properties when the different gas molecule of the adsorption of CNTs, this is also CNTs conduct
The basis of gas sensitive material.However, CNTs is used to also face some shortcomings, such as the suction to some gases as sensitive material
Attached energy is relatively low, lacks selectivity, and recovery time is long.With going deep into for research, it has been found that the surface defect of CNTs and residual
Pollutant is stayed to have very big influence to its air-sensitive property.Therefore, carrying out functionalization to CNTs with different material is considered as changing
Becoming its chemical property enhances the effective means of its gas-sensitive property.Although excellent sensitivity is special at noble metal decorated CNTs performance
Property, due to having used the catalytic selectivity of noble metal itself to result in high cost and limited monitoring range.In addition, CNTs
Synergistic effect is considered to have between oxide, with the carbon nano-tube modified gas sensor of can be improved of oxide semiconductor
Performance.Currently, synthesizing a variety of CNT base binary materials by different approaches has been achieved for remarkable progress.For example, Chen etc. makes
SnO2The hybrid material on the surface CNTs is dispersed at room temperature to NO2, CO and H2Good sound is shown at low concentrations
It answers.Asad etc. report CuO-SWCNT composite Nano wire material can detecte at room temperature concentration down to 100ppb H2S gas
Body.
Summary of the invention
The present invention is directed to by constructing based on CNTs@α-Fe2O3Hetero-junctions graded structure composite material, utilizes CNTs's
Bigger serface, longitudinal electric conductivity, to change composite material pattern, crystallite dimension, improve carrier concentration and formation potential barrier etc.,
The shortcomings that overcome low single metal oxide sensitivity, poor selectivity, realizes the detection to low concentration acetone gas.
The present invention first pre-processes CNTs using the mixed acid of the concentrated sulfuric acid and concentrated nitric acid.Commercially available CNTs is one
The pipe of kind hollow structure, pipe is closed at both ends, and surface roughness is small, and surface is unfavorable for crystal nucleation growth, and disperses in water
Property is very poor.Therefore it need to be pre-processed, defect is formed, is opened at end, increases surface roughness, increases dispersion in water
Property.Then, using Iron(III) chloride hexahydrate and acid treated CNTs as the raw material that sets out, water utilizes ferric trichloride as solvent
Solution is hydrolyzed when increasing temperature, generates presoma FeOOH (FeOOH) precipitating.Since CNTs is provided in crystal growth
Heterogeneous nucleation condition, crystal can around CNTs homoepitaxial, form CNTs@FeOOH composite material.And FeOOH is in height
α-Fe is converted under temperature2O3Crystal is to get having arrived CNTs@α-Fe2O3Hetero-junctions graded structure composite material.
Of the present invention is a kind of based on CNTs@α-Fe2O3The acetone gas of hetero-junctions graded structure composite material passes
Sensor has the oxide aluminium earthenware outer substrate of 2 cyclic annular gold electrodes parallel to each other and discrete by outer surface, is coated in absolutely
Metal oxide semiconductor gas sensitive material in edge alumina ceramic tube outer substrate surface and gold electrode is made pottery with insulation is placed in
Nichrome heating coil in porcelain tube forms, and platinum filament wire is had on each gold electrode；It is characterized by: semiconductor alloy
Oxide gas sensitive material is CNTs@α-Fe2O3Hetero-junctions graded structure composite material, and it is prepared by following steps
It arrives,
(1) mixed acid solution of pretreatment CNTs is prepared first, wherein the concentrated sulfuric acid (98wt%) and concentrated nitric acid (68wt%)
Volume ratio is 3:1；0.1~0.3g CNTs (diameter is 110~170nm, and length is 5~9 μm) is taken to be put into 30~50mL mixing
In acid, 30~60min of ultrasound keeps 4~6h at 70~100 DEG C, after cooled to room temperature, filtering, and use deionized water
It is alternately cleaned with ethyl alcohol, sample is labeled as F-CNTs, it is stand-by after drying；
(2) compound concentration is the FeCl of 0.8~1.2M3Aqueous solution, take 20~30mL FeCl3Aqueous solution, addition 8~
15mg F-CNTs, 10~30min of ultrasound；
(3) mixed liquor after step (2) ultrasound is placed in 80~90 DEG C of 5~10h of heating water bath, cooled to room temperature
Afterwards, it is centrifuged, and with ethyl alcohol and deionized water, alternately cleaning is centrifuged product, the precipitating being centrifuged is dried to get CNTs@is arrived
FeOOH composite material；
(4) the CNTs@FeOOH composite material that step (3) obtains is sintered 5~8 h at 400~450 DEG C to get arriving
CNTs@α-Fe2O3Hetero-junctions graded structure composite material, wherein α-Fe2O3To be rodlike, length is 110~180nm, and diameter is
40~80nm.
The present invention provides one kind to be based on CNTs@α-Fe2O3The acetone gas of hetero-junctions graded structure composite material senses
The preparation method of device.Device is heater-type gas sensor, and structure is as shown in Figure 4.Commercially available ceramics pipe range 4mm, outer diameter
1.2mm, internal diameter 0.8mm, by two close end with a pair of gold electrode separate, each electrode is connected to two platinum for outer surface
The preparation step of line, the sensor is as follows:
(1) the CNTs@α-Fe that will be prepared2O3Hetero-junctions graded structure composite material disperses in deionized water, shape
At grume slurry；
(2) slurry is picked with hairbrush form a thickness film coated in oxide aluminium earthenware outer and gold electrode surfaces, 200
~300 μm, 2~5h is sintered after drying at 350~450 DEG C；
(3) then nichrome heating coil is placed in oxide aluminium earthenware outer, and by oxide aluminium earthenware outer
It is welded on hexagonal tube socket, to obtain based on CNTs α-Fe2O3The acetone gas of hetero-junctions graded structure composite material passes
Sensor.
Heater-type acetone gas sensor of the present invention utilizes CNTs@α-Fe2O3Hetero-junctions graded structure composite wood
Material is used as sensitive material.Its mechanism are as follows: firstly, the CNTs chemical absorption of surface oxygen content of oxidation processes increases, so that composite wood
Material is than single α-Fe2O3There is nano material higher chemical oxygen to adsorb content, and the increase of chemisorption oxygen content can make its spirit
Sensitivity increases.Secondly, CNTs is as skeleton, α-Fe in this graded structure2O3Nanometer rods are uniform perpendicular to the surface CNTs
Distribution, forms a kind of stick bayonet fittings, has biggish specific surface area, so it is anti-with oxygen molecule to increase target gas molecules
The contact area answered greatly increases the utilization rate of sensitive material；On the other hand, unique heterojunction structure can also help improve
The gas sensitization characteristic of device.By theory analysis it may be concluded that the resistance value of sensitive material is strongly depend on its internal crystalline substance
Potential barrier at body interface.Material synthesized by us, CNTs and α-Fe2O3Contact between nanometer rods forms heterojunction gesture
It builds, increases barrier height, change greatly material resistance in reaction process, to facilitate the raising of gas-sensitive property；This three
The sensitivity of sensor greatly improved in the collective effect of aspect.Meanwhile heterojunction structure CNTs@α-Fe of the present invention2O3
The synthetic method environmental protection of stick thorn-like material, it is low in cost；The heater-type device technology of production is simple, small in size, is conducive to industrial
Batch production, therefore detected in medical treatment, industry security control etc. has broad application prospects.
Detailed description of the invention
Fig. 1 is the SEM figure before CNTs acid processing of the invention, wherein (a) figure is 9000 times of amplification factor, (b) figure is put
Big multiple is 20000 times, and (c) amplification factor of figure is 220000 times；1 refers to the closed port CNTs in figure.
Fig. 2 is CNTs acid of the invention treated SEM figure, wherein (a) figure is 20000 times of amplification factor, (b) figure
Amplification factor is 65000 times, and (c) amplification factor of figure is 30000 times；The port and surface corrosion that 1 finger CNTs is opened in figure
Hole.
Fig. 3 is CNTs@α-Fe of the invention2O3Hetero-junctions graded structure composite material is schemed as the SEM of sensitive material,
Its amplification factor is 20000 times；1 refers to α-Fe in figure2O3Nanometer rods, length are about 100nm, and 2 refer to CNTs.
Fig. 4 is CNTs@α-Fe of the invention2O3Acetone gas of the hetero-junctions graded structure composite material as sensitive material
The structural schematic diagram of body sensor；
Fig. 5 is spirit of sensor at a temperature of different operating to 100ppm acetone in comparative example and embodiment 1 of the invention
Sensitivity comparison diagram；
Fig. 6 is that comparative example and sensor in embodiment 1 of the invention are different to 100 ppm when operating temperature is 200 DEG C
The selective comparison diagram of gas；
Fig. 7 is sensor device sensitivity-the third when operating temperature is 200 DEG C in comparative example and embodiment 1 of the invention
Ketone concentration profiles.
As shown in Figure 1, by scheming (a), (b) and can be seen that CNTs diameter in (c) figure in 120nm or so, in sour processing
Before, surface roughness is small, port closed, as 1 is signified in figure.
As shown in Fig. 2, after peracid treatment, surface roughness increases, and port is opened by scheming 1 meaning in (a).Figure
(b) diameter is that the surface CNTs of 110nm or so has etch pit in；Scheme the CNTs that diameter in (c) is 200nm or so, port is opened,
And tube wall is also stripped.
As shown in figure 3, it can be seen that CNTs@α-Fe in (a) figure2O3Hetero-junctions graded structure composite material, homogeneity
It is good, good dispersion；(b) α-Fe is found out in figure2O3Nanometer rods (1 is signified in figure) are grown in CNTs surrounding (as shown in Figure 2), to
Outer diverging, α-Fe2O3The length of nanometer rods is 100~200nm.Wherein α-Fe2O3Nanorod growth constitutes and divides on the surface CNTs
Hierarchical organization, the two contact to form hetero-junctions.
As shown in figure 4, CNTs and α-Fe2O3Nanometer rods composite heterogenous junction graded structure nano material is as sensitive material
Gas sensor be heater-type structure, by sensitive material 1, gold electrode 2, Pt conducting wire 3, ceramic tube 4 and Ni-Cr heater strip 5
Composition.
As shown in figure 5, the optimum working temperature of sensor is 200 DEG C in comparative example and embodiment 1, device pair at this time
The sensitivity highest of 100ppm acetone, respectively 16 and 36.
As shown in fig. 6, testing gas compared to other, comparative example and 1 sensor of embodiment are with higher to acetone
Sensitivity.And compared with comparative example, the selectivity of 1 sensor of embodiment is greatly improved.
As shown in fig. 7, the sensitivity of all devices is with the increasing of acetone concentration when device operating temperature is 200 DEG C
Add and increase, and growth trend gradually slows down.Wherein, sensor sheet reveals optimal gas-sensitive property in embodiment 1.
The electric current of Ni-Cr heater strip is flowed through by change to regulate and control the operating temperature of sensor, at measurement sensor
Resistance value when in gas with various between two gold electrodes can obtain the sensitivity of sensor.Sensor is for acetone gas
Sensitivity S is defined as: S=Ra/Rg, wherein RgAnd RaWhen respectively sensor is in acetone gas and air between two gold electrodes
Resistance value.By sensitivity and gas concentration characteristic curve, the measurement to unknown acetone gas concentration may be implemented.
Specific embodiment
Comparative example:
With α-Fe2O3Nanometer rods make flat acetone gas sensor as sensitive material, and specific manufacturing process is such as
Under:
1. the FeCl that compound concentration is 0.1M3Solution, solvent are water.Take 20mL FeCl3Solution, ultrasonic 10min.
2. the mixed liquor after ultrasound is placed in 80 DEG C of heating water bath 5h.After natural cooling, by the brown color of generation precipitate from
Heart separation, and alternately cleaned with ethyl alcohol and deionized water.The precipitating being centrifuged is dried to get brick-red FeOOH nanometer rods are arrived
Material.
3. FeOOH nano-bar material to be sintered to 8h at 400 DEG C to get α-Fe is arrived2O3Nanometer rods powder.α-Fe2O3Nanometer
Stick length is 120~200nm, and diameter is 40~100nm, agglomeration occurs, and nanometer rods are agglomerated into having a size of 10 μm of magnitudes
It is irregular blocky.
4. by 5mg α-Fe2O3Powder is put into mortar, is added a little deionized water, grinds 10min, at grume slurry,
Insulating oxide aluminium of the slurry coated in commercially available outer surface with cyclic annular gold electrode a pair of parallel and separate is picked with hairbrush
The surface ceramic tube (long 4mm, outer diameter 1.2mm, internal diameter 0.8mm) is formed a thickness film (200~300 μm), at 400 DEG C after drying
Lower sintering 2h.Then nichrome heating coil (about 35 Ω of resistance) is placed in ceramic tube, and ceramic tube is welded on hexagonal
On tube socket, α-Fe is thus obtained2O3Nanometer rods acetone gas sensor.
Embodiment 1:
Sensitive material is CNTs@α-Fe2O3Hetero-junctions graded structure composite material acetone gas sensor, it is specific
Manufacturing process is as follows:
1. preparing the mixed acid solution of processing CNTs first, wherein the body of the concentrated sulfuric acid (98wt%) and concentrated nitric acid (68wt%)
Product is than being 3:1.0.1g CNTs (Sigma-Aldrich's sale, diameter are 110~170nm, and length is 5~9 μm) is taken to put
Enter in 30mL mixed acid, ultrasonic 30min, keep 5h at 100 DEG C, after cooled to room temperature (25 DEG C), filtering, and spend from
Sub- water and ethyl alcohol alternately clean, stand-by after drying.Sample is labeled as F-CNTs.
2. the FeCl that compound concentration is 0.1M3Solution, solvent are water.Take 20mL FeCl310mg F- is added in solution
CNTs, ultrasonic 10min.
3. the mixed liquor after ultrasound is placed in 80 DEG C of heating water bath 5h.After natural cooling, the black precipitate of generation is centrifuged
Separation, and alternately cleaned with ethyl alcohol and deionized water.The precipitating being centrifuged is dried to get CNTs@FeOOH composite material is arrived.
4. CNTs@FeOOH composite material to be sintered to 8h at 400 DEG C to get CNTs@α-Fe is arrived2O3Hetero-junctions graduation knot
Structure composite material, α-Fe2O3To be rodlike, length is 110~180nm, and diameter is 40~80 nm.
5. by 5mg CNTs and α-Fe2O3Composite powder is put into mortar, and a little deionized water is added, grinding
10min picks slurry coated in commercially available outer surface with a pair of ring-type parallel and separate with hairbrush at grume slurry
Surface oxide aluminium earthenware outer (long 4mm, outer diameter 1.2mm, 0.8 mm of internal diameter) of gold electrode, one thickness film of formation (200~
300 μm), 2h is sintered at 400 DEG C after drying.Then nichrome heating coil (about 35 Ω of resistance) is placed in ceramic tube,
And ceramic tube is welded on hexagonal tube socket, it thus obtains based on CNTs α-Fe2O3Hetero-junctions graded structure composite material
Acetone gas sensor.
Claims (2)
1. one kind is based on CNTs@α-Fe2O3The acetone gas sensor of heterojunction composite is put down by outer surface with 2 each other
The oxide aluminium earthenware outer substrate of capable and discrete cyclic annular gold electrode, be coated in oxide aluminium earthenware outer outer substrate surface and
Metal oxide semiconductor gas sensitive material on gold electrode is heated with the nichrome being placed in oxide aluminium earthenware outer
Coil forms, and platinum filament wire is had on each gold electrode；It is characterized by: metal oxide semiconductor gas sensitive material is
Based on CNTs@α-Fe2O3Hetero-junctions graded structure composite material, and it is prepared by following steps,
(1) mixed acid solution of pretreatment CNTs is prepared first, and wherein the volume ratio of the concentrated sulfuric acid and concentrated nitric acid is 3:1；Take 0.1~
0.3g CNTs is put into 30~50mL mixed acid, 30~60min of ultrasound, and 4~6h is kept at 70~100 DEG C, is naturally cooled to
After room temperature, filtering, and alternately cleaned with deionized water and ethyl alcohol, sample is labeled as F-CNTs, it is stand-by after drying；
(2) compound concentration is the FeCl of 0.8~1.2M3Aqueous solution, take 20~30mL FeCl38~15mg is added in aqueous solution
F-CNTs, 10~30min of ultrasound；
(3) mixed liquor after step (2) ultrasound is placed in 80~90 DEG C of 5~10h of heating water bath, after cooled to room temperature, from
The heart, and with ethyl alcohol and deionized water, alternately cleaning is centrifuged product, and the precipitating being centrifuged is dried to get compound to CNTs@FeOOH
Material；
(4) by the CNTs@FeOOH composite material that step (3) obtains be sintered at 400~450 DEG C 5~8h to get to CNTs and
α-Fe2O3Hetero-junctions graded structure composite material, wherein α-Fe2O3To be rodlike, the length is 110~180nm, diameters 40
~80nm.
2. as described in claim 1 a kind of based on CNTs@α-Fe2O3The system of the acetone gas sensor of heterojunction composite
Preparation Method, its step are as follows:
(1) by CNTs@α-Fe2O3Hetero-junctions graded structure composite material disperses in deionized water, to form grume slurry；
(2) slurry is picked with hairbrush form one layer of 200~300 μ m-thick coated in oxide aluminium earthenware outer and gold electrode surfaces
Film is sintered 2~5h at 350~450 DEG C after drying；
(3) then nichrome heating coil is placed in oxide aluminium earthenware outer, and oxide aluminium earthenware outer is welded
On hexagonal tube socket, to obtain based on CNTs α-Fe2O3The acetone gas sensor of hetero-junctions graded structure composite material.
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| CN108333226A (en) * | 2018-01-10 | 2018-07-27 | 长春理工大学 | Highly selective acetone gas sensor in high precision |
| CN111610234B (en) * | 2020-07-07 | 2021-09-07 | 上海大学 | Acetone gas sensor of field effect transistor and preparation method thereof |
| CN113731499B (en) * | 2021-09-08 | 2022-06-10 | 云南大学 | 1D/3D hierarchical heterojunction magnetic semiconductor and preparation method and application thereof |
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