CN107817279A - A kind of NO based on electrode surface growth in situ NiO nano thin-films2Sensor - Google Patents
A kind of NO based on electrode surface growth in situ NiO nano thin-films2Sensor Download PDFInfo
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Abstract
Invention is related to a kind of NO based on electrode surface growth in situ NiO nano thin-films2Sensor and preparation method thereof, belong to the gas sensor technical field of one-dimensional metal oxide semi-conducting material.A kind of NO based on electrode surface growth in situ NiO nano thin-films2Sensor, the sensor are made up of electrode member and uniform growth in situ in the NiO films of electrode element surface, wherein, the NiO films are made up of NiO crystal grains, and the NiO crystal grains are face-centered cubic phase crystal structure, a diameter of 20~30nm.The gas sensor is obtained to NO when operating temperature is 150 DEG C2Peak response, response and recovery time are short, and selectivity is high, and long-time stability are good, the deficiencies of INVENTIONConventional metal-oxide semiconductor-type gas sensor preparation technology flow is complicated, selectivity and long-time stability are poor is efficiently solved, is the NO with good development prospect2Gas sensor.
Description
Technical field
The present invention relates to a kind of NO based on electrode surface growth in situ NiO nano thin-films2Sensor and preparation method thereof,
Belong to the gas sensor technical field of one-dimensional metal oxide semi-conducting material.
Background technology
With society development and science and technology progress, the quality of life of people there occurs revolutionary change, but with
This various negative issue brought simultaneously also constantly highlights.In recent years, haze, greenhouse effects, acid rain etc. threaten people's body to be good for
The phenomenon of health is constantly aggravated, and gas leak, gas explosion, gassing etc. threaten the accident of people's life security to occur again and again,
So that people are constantly lifted for pollution, dangerous, pernicious gas detection with the demand alarmed, so as to be sensed to high performance gas
The development of device proposes the more urgently requirement with harshness.
The species of gas sensor is many at present, can be divided into semiconductor-type gas sensing according to gas sensitive and action effect
Device, electrochemical gas sensor, solid electrolyte formula gas sensor, catalytic combustion type gas sensor, optical type gas
Sensor, high score minor gas sensor etc..Wherein, metal-oxide semiconductor (MOS) formula gas sensor is due to response speed
It hurry up, the advantages that high sensitivity, detection gas concentration limit are low, all solid state, small volume, be a kind of gas being most widely used at present
Body sensor.The working environment of gas sensor is complicated, usually contains a variety of toxic and harmful gas, is partly led for metal oxide
For body gas sensor, its poor gas-selectively is always to restrict an important factor for it further develops.
NiO is a kind of p-type broad stopband metal oxide semiconductor material, and its energy gap is in 3.6~4.0eV or so.NiO
Material has very excellent electronic transmission performance and chemical stability, in electrochromism, catalysis, magnetic material, battery, gas sensing
The fields such as device have all shown good application prospect.Because it has higher gas sensitivity, low cost and various micro-nanos
The advantages that rice technology is preferably compatible, had been considered as once one of best candidate of gas sensitive.Gas sensor at present
Preparation method is substantially the gas sensitive that will be prepared in advance and is manually applied on electrode so that gas sensitive and substrate knot
It is poor with joint efforts, so as to cause the long-time stability of gas sensor poor.
The content of the invention
For current metal-oxide semiconductor (MOS) formula gas sensor in terms of gas-selectively and long-time stability not
Foot, the present invention provide a kind of NO based on electrode surface growth in situ NiO nano thin-films2Sensor and preparation method thereof.Purpose
It is to lift coating method by sol-gel to go out in electrode surface growth in situ that surface topography is homogeneous, property is stable, loose porous
NiO nano thin-films, and it is prepared into the NO with high selectivity, excellent long-time stability2Sensor, to overcome existing sensor to select
The deficiencies of selecting property is not high, long-time stability are poor.
A kind of NO2Sensor, the sensor are thin in the NiO of electrode element surface by electrode member and uniform growth in situ
Film forms,
Wherein, the NiO films are made up of NiO crystal grains, and the NiO crystal grains are face-centered cubic phase crystal knot
Structure, a diameter of 20~30nm.
NO of the present invention2Sensor, the NiO nano thin-films are detection NO2The gas sensitive of gas.
In above-mentioned technical proposal, the NiO nano thin-films have the architectural characteristic that surface topography is homogeneous, loose porous.
In above-mentioned technical proposal, the material of preferably described electrode member is Al2O3Ceramic material or gold.
In above-mentioned technical proposal, preferably described electrode member is shaped as tubulose or plane.
Further, most preferably described electrode member is tubular ceramic element or plane gold dollar part.
In above-mentioned technical proposal, preferably described sensor is by electrode element surface growth in situ NiO nano thin-films
Gained.
Further, the method for the growth in situ NiO nano thin-films is：Using lifting coating method in electrode element surface
NiO colloidal sols are coated, are dried；Electrode member of the surface coated with NiO colloidal sols is heat-treated, condition is：With 3 DEG C/min liter
Warm speed is heated to 500 DEG C and keeps 1h；Aging 24h at 250~300 DEG C, both.
Further, the NiO colloidal sols are made as follows：At room temperature, second two is added into nickel acetate tetrahydrate
Alcohol methyl ether, stirring, makes nickel acetate tetrahydrate be completely dissolved among ethylene glycol monomethyl ether；The solution formed is stirred into 2h in 60 DEG C,
And 25~28wt.% ammoniacal liquor is added dropwise dropwise into solution；Sealing, is aged 24h at room temperature, filters, obtains NiO colloidal sols,
Wherein, nickel acetate tetrahydrate, ammoniacal liquor, the mol ratio of ethylene glycol monomethyl ether are 5~7:5~7:100.
In above-mentioned technical proposal, the nickel acetate tetrahydrate, ammoniacal liquor, ethylene glycol monomethyl ether mol ratio in ammoniacal liquor amount with ammonia
Solute meter in water.
Further, the lifting film is carried out in pulling coating machine, is dried after film, the lifting film
Machine arrange parameter is：Stroke 6cm, decrease speed 300~500 μm/s, 30~60s of quiescent time, 300~400 μm of the rate of climb/
s；Such as need to increase the film number of plies, then repeat the above steps.
Compared with prior art, the features of the present invention and excellent effect are：
The invention provides one kind to be based on simple electrode surface growth in situ, preparation method, selectivity height, long-time stability
The NiO nano thin-films NO of the advantages that good2Sensor and preparation method thereof.From preparation method, the present invention first by colloidal sol-
Gel method has gone out layer of Ni O nano thin-films in electrode surface growth in situ, is then prepared into gas sensor by burin-in process.
The gas sensor is obtained to NO when operating temperature is 150 DEG C2Peak response, response and recovery time it is short, selectivity
Height, long-time stability are good, efficiently solve INVENTIONConventional metal-oxide semiconductor-type gas sensor preparation technology flow complexity, choosing
The deficiencies of selecting property and poor long-time stability, be the NO with good development prospect2Gas sensor.
Brief description of the drawings
Fig. 1 is the NO based on tubular ceramic electrode surface growth in situ NiO nano thin-films in embodiment 1 and embodiment 22Pass
The structural representation of sensor.Wherein, 1：Al2O3Earthenware；2：NiO air-sensitive coatings；3：Resistive heater；4：Gold electrode；5：Platinum
Lead.
Fig. 2 is the X ray diffracting spectrum of NiO nano thin-films prepared by the present invention；
Fig. 3 is (a) low range and (b) high magnification electron scanning micrograph of NiO nano thin-films prepared by the present invention；
Fig. 4 is the transmission electron microscope figure of the NiO crystal grain of composition NiO nano thin-films prepared by the present invention；
Fig. 5 is the gas sensor of the invention prepared to 20ppm NO2Sensitivity and operating temperature between graph of a relation；
Fig. 6 be the gas sensor for preparing of the present invention when operating temperature is 150 DEG C to various concentrations NO2Dynamic response
Curve map；
Fig. 7 is the gas sensor prepared sensitivity and NO when operating temperature is 150 DEG C of the invention2Between gas concentration
Graph of a relation；
Fig. 8 be the gas sensor for preparing of the present invention when operating temperature is 150 DEG C to the sensitive of different detected gas
Degree figure；
Fig. 9 be the gas sensor for preparing of the present invention when operating temperature is 150 DEG C to 20ppm NO2Sensitivity at any time
Between variation diagram；
Figure 10 is the NO based on plane gold electrode surfaces growth in situ NiO nano thin-films in embodiment 3 and embodiment 42Pass
Sensor component schematic diagram；Wherein：6：Plane Al2O3Ceramic substrate；7：NiO air-sensitive coatings；8：Adding thermal resistance；9：Gold electrode；10：
Platinum lead.
Embodiment
Following non-limiting examples can make one of ordinary skill in the art be more fully understood the present invention, but not with
Any mode limits the present invention.
Test method described in following embodiments, it is conventional method unless otherwise specified；The reagent and material, such as
Without specified otherwise, commercially obtain.
Air-sensitive test system described in following embodiments contains scientific and technological WS-30A types air-sensitive test system to be bright；The agingtable
Scientific and technological TS-60 types agingtable is contained to be bright.
NO described in following embodiments2Sensor is obtained by following preparation methods：
(1) weigh quantitative nickel acetate tetrahydrate with electronic balance to be put into triangular flask, added with pipette into triangular flask
Enter quantitative ethylene glycol monomethyl ether, then mixing 3h with magnetic stirring apparatus at room temperature makes nickel acetate tetrahydrate be completely dissolved in second
Among glycol methyl ether.The solution formed is stirred into 2h in 60 DEG C of constant temperature water baths, and is added dropwise dropwise into solution a certain amount of
Ammoniacal liquor as stabilizer/complexing agent.Wherein, nickel acetate tetrahydrate, ammoniacal liquor, the mol ratio of ethylene glycol monomethyl ether are 5~7:5~7:
100.Triangular flask sealing is taken out afterwards, is aged 24h at room temperature and is obtained NiO colloidal sols.The qualitative filter of NiO colloidal sol middling speeds that will be obtained
Paper filters, and sealing is stand-by.
(2) electrode member for treating film is cleaned up with deionized water and ethanol solution respectively, be then fixed in
The substrate bearing of pulling coating machine, while the beaker for filling stand-by NiO colloidal sols is put into the material cup rest area of pulling coating machine.
(3) relevant parameter of pulling coating machine is set：Stroke 6cm, 300~500 μm/s of decrease speed, quiescent time 30~
60s, 300~400 μm/s of the rate of climb, then proceeds by lifting film.After lifting film terminates, electrode is placed in electric heating drum
In wind drying box, 30min is dried under the conditions of 80 DEG C, takes out be cooled to room temperature afterwards.Such as need to increase the film number of plies, then repeat
State step (3).
(4) electrode for scribbling NiO films is put into tube furnace, with 3 DEG C/min heating rate heated Tube-furnace to 500
DEG C and keep 1h.After tube furnace is cooled to room temperature, layer of Ni O nano thin-films can be obtained on electrode.
(5) electrode member is soldered in the detection pedestal of air-sensitive test system, be placed on agingtable in 300 DEG C of conditions
Lower aging 24h, produces final gas sensor.
Embodiment 1
NO based on tubular ceramic electrode surface growth in situ NiO nano thin-films2Sensor element, its structural representation is such as
Shown in Fig. 1, by Al2O3Earthenware, gold electrode, platinum lead, resistive heater and air-sensitive material layer composition.Gold electrode is overlayed on
Al2O3Ceramic pipe surface forms ceramic electrode, and platinum lead is welded on gold electrode surfaces, and resistive heater is transverse in Al2O3Ceramics
Guan Zhong, gas sensitive are grown in whole Al2O3Earthenware and gold electrode surfaces.Described gas sensitive composition is NiO nanometer thins
Film, it, which is evenly distributed, is grown in ceramic electrode surface, NiO nano thin-films by a diameter of 20~30nm face-centered cubic phase NiO
Crystal grain is formed, and film surface appearance is homogeneous, loose porous.
A kind of NO based on tubular ceramic electrode surface growth in situ NiO nano thin-films2Sensor and preparation method thereof, press
Carried out according to following steps：
(1) weigh quantitative nickel acetate tetrahydrate with electronic balance to be put into triangular flask, added with pipette into triangular flask
Enter quantitative ethylene glycol monomethyl ether, then mixing 3h with magnetic stirring apparatus at room temperature makes nickel acetate tetrahydrate be completely dissolved in second
Among glycol methyl ether.The solution formed is stirred into 2h in 60 DEG C of constant temperature water baths, and is added dropwise dropwise into solution a certain amount of
Ammoniacal liquor as stabilizer/complexing agent.Wherein, nickel acetate tetrahydrate, ammoniacal liquor, the mol ratio of ethylene glycol monomethyl ether are 1:1:20 (ammonia
For the amount of water in terms of solute, other embodiment is same).Triangular flask sealing is taken out afterwards, is aged 24h at room temperature and is obtained NiO colloidal sols.Will
Obtained NiO colloidal sol middling speeds qualitative filter paper filtering, sealing are stand-by.
(2) by the ceramic electrode for treating film, (gold electrode overlays on Al2O3The electrode member that ceramic pipe surface is formed) spend respectively
Ionized water and ethanol solution clean up, and are then fixed in the substrate bearing of pulling coating machine, while will fill stand-by
The beaker of NiO colloidal sols is put into the material cup rest area of pulling coating machine.
(3) relevant parameter of pulling coating machine is set：Stroke 6cm, decrease speed 500 μm/s, quiescent time 30s, rise
400 μm/s of speed, then proceeds by lifting film.After lifting film terminates, ceramic electrode is placed in electric drying oven with forced convection
In, 30min is dried under the conditions of 80 DEG C, takes out be cooled to room temperature afterwards.Repeat step (3) carries out film next time.
(4) ceramic electrode for scribbling 2 layers of NiO films is put into tube furnace, with 3 DEG C/min heating rate heated Tube
Stove is to 500 DEG C and keeps 1h.After tube furnace is cooled to room temperature, layer of Ni O nano thin-films can be obtained on ceramic electrode.
(5) ceramic electrode element is soldered in the detection pedestal of air-sensitive test system, be placed on agingtable at 300 DEG C
Under the conditions of aging 24h, produce final gas sensor.
The X ray diffracting spectrum of NiO nano thin-films is as shown in Figure 2.It can be seen that the NiO of electrode surface growth
For face-centered cubic phase crystal structure, diffraction maximum peak shape is sharp, and halfwidth is smaller, and the diffraction maximum without any other impurity, shows
NiO crystallinity is preferably and purity is higher.The scanning electron microscope (SEM) photograph of NiO nano thin-films is as shown in Figure 3.It can be seen that NiO receives
Rice film is made up of small NiO crystal grain, and surface topography is homogeneous and loose porous.Fig. 4 is the NiO crystalline substances for forming NiO nano thin-films
The transmission electron microscope figure of grain.As can be seen from the figure a diameter of 20~30nm of the NiO crystal grain of NiO nano thin-films is formed.
NO based on ceramic electrode surface in situ growth NiO nano thin-films2Sensor is to 20ppm NO2Sensitivity and work
The relation for making temperature is as shown in Figure 5.It can be seen that the sensor is obtained to NO when operating temperature is 150 DEG C2Most
Atmospheric sensitivity.Fig. 6 be the sensor in 150 DEG C of operating temperature to various concentrations NO2Dynamic response curve.From figure
As can be seen that the sensor response/recovery time is shorter and has good invertibity and stability, at the same increased resistance value with
NO2The reduction of concentration and reduce, show its sensitivity and NO2Concentration correlation, the sensor as shown in Figure 7 exist
Sensitivity and NO when operating temperature is 150 DEG C2Relation between concentration more can clearly be found out.
NO based on tubular ceramic electrode surface growth in situ NiO nano thin-films2Sensitivity of the sensor to gas with various
As shown in Figure 8.As can be seen from Figure 8, the sensor is to 10ppm NO2Sensitivity far above to 1000ppm, other are common
The sensitivity of toxic and harmful gas, show preferable gas-selectively.This shows gaseous environment of the sensor in complexity
In can be to NO2Effectively differentiated, show preferable actual application prospect.Fig. 9 is the sensor to 20ppm NO2's
Sensitivity versus time curve.It can be seen that the sensor its change of sensitivity scope in 30 days is smaller, table
Reveal good stability, can preferably overcome the shortcomings of that existing sensor long-time stability are poor.
Embodiment 2
NO based on tubular ceramic electrode surface growth in situ NiO nano thin-films2Sensor element, its structural representation is such as
Shown in Fig. 1, by Al2O3Earthenware, gold electrode, platinum lead, resistive heater and air-sensitive material layer composition.Gold electrode is overlayed on
Al2O3Ceramic pipe surface forms ceramic electrode, and platinum lead is welded on gold electrode surfaces, and resistive heater is transverse in Al2O3Ceramics
Guan Zhong, gas sensitive are grown in whole Al2O3Earthenware and gold electrode surfaces.Described gas sensitive composition is NiO nanometer thins
Film, it, which is evenly distributed, is grown in ceramic electrode surface, NiO nano thin-films by a diameter of 20~30nm face-centered cubic phase NiO
Crystal grain is formed, and film surface appearance is homogeneous, loose porous.
A kind of NO based on tubular ceramic electrode surface growth in situ NiO nano thin-films2Sensor and preparation method thereof, press
Carried out according to following steps：
(1) weigh quantitative nickel acetate tetrahydrate with electronic balance to be put into triangular flask, added with pipette into triangular flask
Enter quantitative ethylene glycol monomethyl ether, then mixing 3h with magnetic stirring apparatus at room temperature makes nickel acetate tetrahydrate be completely dissolved in second
Among glycol methyl ether.The solution formed is stirred into 2h in 60 DEG C of constant temperature water baths, and is added dropwise dropwise into solution a certain amount of
Ammoniacal liquor as stabilizer/complexing agent.Wherein, nickel acetate tetrahydrate, ammoniacal liquor, the mol ratio of ethylene glycol monomethyl ether are 7:7:100.It
Triangular flask sealing is taken out afterwards, is aged 24h at room temperature and is obtained NiO colloidal sols.The NiO colloidal sol middling speed qualitative filter paper mistakes that will be obtained
Filter, sealing are stand-by.
(2) by the ceramic electrode for treating film, (gold electrode overlays on Al2O3The electrode member that ceramic pipe surface is formed) spend respectively
Ionized water and ethanol solution clean up, and are then fixed in the substrate bearing of pulling coating machine, while will fill stand-by
The beaker of NiO colloidal sols is put into the material cup rest area of pulling coating machine.
(3) relevant parameter of pulling coating machine is set：Stroke 6cm, decrease speed 300 μm/s, quiescent time 60s, rise
300 μm/s of speed, then proceeds by lifting film.After lifting film terminates, ceramic electrode is placed in electric drying oven with forced convection
In, 30min is dried under the conditions of 80 DEG C, takes out be cooled to room temperature afterwards.
(4) ceramic electrode for scribbling 1 layer of NiO film is put into tube furnace, with 3 DEG C/min heating rate heated Tube
Stove is to 500 DEG C and keeps 1h.After tube furnace is cooled to room temperature, layer of Ni O nano thin-films can be obtained on ceramic electrode.
(5) ceramic electrode element is soldered in the detection pedestal of air-sensitive test system, be placed on agingtable at 300 DEG C
Under the conditions of aging 24h, produce final gas sensor.
After testing, the NO manufactured in the present embodiment based on NiO nano thin-films2Sensor is in 100~200 DEG C of bars of operating temperature
To NO under part2With good gas-sensitive property
Embodiment 3
NO based on plane gold electrode surfaces growth in situ NiO nano thin-films2Sensor element, its structural representation is as schemed
Shown in 10, by plane Al2O3Ceramic substrate, gold electrode, platinum lead, adding thermal resistance and air-sensitive material layer composition.Gold electrode is covered
In plane Al2O3Ceramic base plate surface forms plane gold electrode, and platinum lead is welded on gold electrode surfaces, and adding thermal resistance overlays on flat
Face Al2O3The ceramic substrate back side, gas sensitive are grown in whole plane Al2O3Ceramic substrate and gold electrode surfaces.Described air-sensitive
Material composition is NiO nano thin-films, and its uniform distribution is grown in electrode element surface, NiO nano thin-films by a diameter of 20~
30nm face-centered cubic phase NiO crystal grains are formed, and film surface appearance is homogeneous, loose porous.
A kind of NO based on plane gold electrode surfaces growth in situ NiO nano thin-films2Sensor and preparation method thereof, according to
Following steps are carried out：
(1) weigh quantitative nickel acetate tetrahydrate with electronic balance to be put into triangular flask, added with pipette into triangular flask
Enter quantitative ethylene glycol monomethyl ether, then mixing 3h with magnetic stirring apparatus at room temperature makes nickel acetate tetrahydrate be completely dissolved in second
Among glycol methyl ether.The solution formed is stirred into 2h in 60 DEG C of constant temperature water baths, and is added dropwise dropwise into solution a certain amount of
Ammoniacal liquor as stabilizer/complexing agent.Wherein, nickel acetate tetrahydrate, ammoniacal liquor, the mol ratio of ethylene glycol monomethyl ether are 1:1:20.It
Triangular flask sealing is taken out afterwards, is aged 24h at room temperature and is obtained NiO colloidal sols.The NiO colloidal sol middling speed qualitative filter paper mistakes that will be obtained
Filter, sealing are stand-by.
(2) by the plane gold electrode for treating film, (gold electrode overlays on plane Al2O3The electrode member that ceramic base plate surface is formed)
Cleaned up respectively with deionized water and ethanol solution, be then fixed in the substrate bearing of pulling coating machine, simultaneously will
The beaker for filling stand-by NiO colloidal sols is put into the material cup rest area of pulling coating machine.
(3) relevant parameter of pulling coating machine is set：Stroke 6cm, decrease speed 500 μm/s, quiescent time 30s, rise
400 μm/s of speed, then proceeds by lifting film.After lifting film terminates, electrode is placed in electric drying oven with forced convection,
30min is dried under the conditions of 80 DEG C, takes out be cooled to room temperature afterwards.Repeat step (3) carries out film next time.
(4) the plane gold electrode for scribbling 2 layers of NiO films is put into tube furnace, with 3 DEG C/min heating rate heating tube
Formula stove is to 500 DEG C and keeps 1h.After tube furnace is cooled to room temperature, layer of Ni O nanometer thins can be obtained on plane gold electrode
Film.
(5) plane gold electrode element is soldered in the detection pedestal of air-sensitive test system, be placed on agingtable 300
Aging 24h under the conditions of DEG C, produce final gas sensor.
After testing, the NO manufactured in the present embodiment based on NiO nano thin-films2Sensor is in 100~200 DEG C of bars of operating temperature
To NO under part2With good gas-sensitive property.
Embodiment 4
NO based on plane gold electrode surfaces growth in situ NiO nano thin-films2Sensor element, its structural representation is as schemed
Shown in 10, by plane Al2O3Ceramic substrate, gold electrode, platinum lead, adding thermal resistance and air-sensitive material layer composition.Gold electrode is covered
In plane Al2O3Ceramic base plate surface forms plane gold electrode, and platinum lead is welded on gold electrode surfaces, and adding thermal resistance overlays on flat
Face Al2O3The ceramic substrate back side, gas sensitive are grown in whole plane Al2O3Ceramic substrate and gold electrode surfaces.Described air-sensitive
Material composition is NiO nano thin-films, and its uniform distribution is grown in electrode element surface, NiO nano thin-films by a diameter of 20~
30nm face-centered cubic phase NiO crystal grains are formed, and film surface appearance is homogeneous, loose porous.
A kind of NO based on plane gold electrode surfaces growth in situ NiO nano thin-films2Sensor and preparation method thereof, according to
Following steps are carried out：
(1) weigh quantitative nickel acetate tetrahydrate with electronic balance to be put into triangular flask, added with pipette into triangular flask
Enter quantitative ethylene glycol monomethyl ether, then mixing 3h with magnetic stirring apparatus at room temperature makes nickel acetate tetrahydrate be completely dissolved in second
Among glycol methyl ether.The solution formed is stirred into 2h in 60 DEG C of constant temperature water baths, and is added dropwise dropwise into solution a certain amount of
Ammoniacal liquor as stabilizer/complexing agent.Wherein, nickel acetate tetrahydrate, ammoniacal liquor, the mol ratio of ethylene glycol monomethyl ether are 7:7:100.It
Triangular flask sealing is taken out afterwards, is aged 24h at room temperature and is obtained NiO colloidal sols.The NiO colloidal sol middling speed qualitative filter paper mistakes that will be obtained
Filter, sealing are stand-by.
(2) by the plane gold electrode for treating film, (gold electrode overlays on plane Al2O3The electrode member that ceramic base plate surface is formed)
Cleaned up respectively with deionized water and ethanol solution, be then fixed in the substrate bearing of pulling coating machine, simultaneously will
The beaker for filling stand-by NiO colloidal sols is put into the material cup rest area of pulling coating machine.
(3) relevant parameter of pulling coating machine is set：Stroke 6cm, decrease speed 300 μm/s, quiescent time 60s, rise
300 μm/s of speed, then proceeds by lifting film.After lifting film terminates, electrode is placed in electric drying oven with forced convection,
30min is dried under the conditions of 80 DEG C, takes out be cooled to room temperature afterwards.
(4) the plane gold electrode for scribbling 1 layer of NiO film is put into tube furnace, with 3 DEG C/min heating rate heating tube
Formula stove is to 500 DEG C and keeps 1h.After tube furnace is cooled to room temperature, layer of Ni O nanometer thins can be obtained on plane gold electrode
Film.
(5) plane gold electrode element is soldered in the detection pedestal of air-sensitive test system, be placed on agingtable 300
Aging 24h under the conditions of DEG C, produce final gas sensor.
After testing, the NO manufactured in the present embodiment based on NiO nano thin-films2Sensor is in 100~200 DEG C of bars of operating temperature
To NO under part2With good gas-sensitive property.
Claims (7)
- A kind of 1. NO based on electrode surface growth in situ NiO nano thin-films2Sensor, it is characterised in that：The sensor is by electricity Pole element and uniform growth in situ form in the NiO films of electrode element surface,Wherein, the NiO films are made up of NiO crystal grains, and the NiO crystal grains are face-centered cubic phase crystal structure, directly Footpath is 20~30nm.
- 2. sensor according to claim 1, it is characterised in that：The material of the electrode member is Al2O3Ceramic material or Gold.
- 3. sensor according to claim 1, it is characterised in that：The electrode member is shaped as tubulose or plane.
- 4. sensor according to claim 1, it is characterised in that：The sensor is by situ in electrode element surface Grow obtained by NiO nano thin-films.
- 5. sensor according to claim 4, it is characterised in that：The method of the growth in situ NiO nano thin-films is：Adopt NiO colloidal sols are coated in electrode element surface with lifting coating method, are dried；Electrode member of the surface coated with NiO colloidal sols is carried out Heat treatment, condition are：500 DEG C are heated to 3 DEG C/min heating rate and keep 1h；Aging 24h at 250~300 DEG C, both .
- 6. sensor according to claim 4, it is characterised in that：The NiO colloidal sols are made as follows：At room temperature, ethylene glycol monomethyl ether is added into nickel acetate tetrahydrate, stirs, nickel acetate tetrahydrate is completely dissolved in ethylene glycol first Among ether；The solution formed is continued to stirring 2h in 60 DEG C, and 25~28wt.% ammoniacal liquor is added dropwise dropwise into solution；It is close Envelope, is aged 24h at room temperature, filters, obtains NiO colloidal sols,Wherein, nickel acetate tetrahydrate, ammoniacal liquor, the mol ratio of ethylene glycol monomethyl ether are 5~7:5~7:100.
- 7. sensor according to claim 4, it is characterised in that：The lifting film is carried out in pulling coating machine, is applied It is dried after film, the pulling coating machine arrange parameter is：Stroke 6cm, 300~500 μm/s of decrease speed, quiescent time 30 ~60s, 300~400 μm/s of the rate of climb；Such as need to increase the film number of plies, then repeat the above steps.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710897155.3A CN107817279B (en) | 2017-09-28 | 2017-09-28 | A kind of NO based on electrode surface growth in situ NiO nano thin-film2Sensor |
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| CN201710897155.3A CN107817279B (en) | 2017-09-28 | 2017-09-28 | A kind of NO based on electrode surface growth in situ NiO nano thin-film2Sensor |
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| CN107817279B CN107817279B (en) | 2019-10-29 |
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| CN110514700A (en) * | 2019-09-27 | 2019-11-29 | 西安电子科技大学 | A kind of copper oxide and cobaltosic oxide heterogeneous structural nano line composite sensitive material, ethylene glycol sensor and preparation method |
| CN113376191A (en) * | 2021-06-08 | 2021-09-10 | 中国科学院上海应用物理研究所 | In-situ-based device and method for high-throughput crystal culture and rapid sample loading |
| CN113433171A (en) * | 2021-06-24 | 2021-09-24 | 兰州大学 | Gas-sensitive material, gas-sensitive sensor, and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110514700A (en) * | 2019-09-27 | 2019-11-29 | 西安电子科技大学 | A kind of copper oxide and cobaltosic oxide heterogeneous structural nano line composite sensitive material, ethylene glycol sensor and preparation method |
| CN110514700B (en) * | 2019-09-27 | 2021-09-07 | 西安电子科技大学 | Copper oxide and cobaltosic oxide heterostructure nanowire composite sensitive material, ethylene glycol sensor and preparation method |
| CN113376191A (en) * | 2021-06-08 | 2021-09-10 | 中国科学院上海应用物理研究所 | In-situ-based device and method for high-throughput crystal culture and rapid sample loading |
| CN113433171A (en) * | 2021-06-24 | 2021-09-24 | 兰州大学 | Gas-sensitive material, gas-sensitive sensor, and preparation method and application thereof |
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