CN109799267A - Plane humidity, ammonia gas sensor based on alkalization organ shape MXene sensitive material and preparation method thereof - Google Patents
Plane humidity, ammonia gas sensor based on alkalization organ shape MXene sensitive material and preparation method thereof Download PDFInfo
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Abstract
One kind is based on alkalization organ shape MXene (Ti3C2Tx, T represents surface DT group terminal, and x value is in each terminal ratio in surface) and the plane humidity of sensitive material, ammonia gas sensor and preparation method thereof, belong to air humidity dependent sensor technical field.By the Al for having Au/Ni interdigital electrode2O3The alkalization organ shape MXene (Ti of ceramic substrate and uniform drop coating in interdigital electrode and ceramic substrate3C2Tx) sensitive material composition.The present invention is achieved the purpose that remove surface F terminal and is inserted into sodium ion, compared the quick performance of air humidity of alkalization front and back, obtain the device with more high humility and ammonia sensitive property based on organ shape MXene material by basification organ shape MXene.The obtained sensor of the present invention has the current highest quick response of MXene air humidity, and has selectivity well.
Description
Technical field
The invention belongs to air humidity dependent sensor technical fields, and in particular to one kind is quick with novel alkalization organ shape MXene
The plane humidity and NH of sense electrode3Sensor and preparation method thereof is mainly used for ambient humidity and ammonia detection.
Background technique
Internet of Things (IoT) is one of information technology with fastest developing speed in the world.As the front end of information collection, sensor
Importance and demand become increasingly conspicuous.Currently, the sensor for environmental monitoring and physiological detection is various.Wherein, based on spy
The sensor of chemical gas of different testing mechanism is in the toxic and harmful gas and monitoring medical diagnosis treatment in monitoring atmospheric environment
Breathing symbolic gas in terms of be increasingly taken seriously.Therefore, the important information that gas sensor develops as big data era
Equipment is acquired, is had broad application prospects.
In order to obtain the high performance gas sensor of low-power consumption, people expect extensively graphene, transition metal two it is thio and
The two dimensions such as black phosphorus (2D) material.MXenes is a kind of New Two Dimensional material that Yury et al. is synthesized first, is two-dimentional transition metal
The abbreviation of carbide, nitride and carbonitride.Middle layer (such as aluminium, silicon, tin, indium) passes through hydrofluoric acid or lithium fluoride and hydrochloric acid
Mixture etching from MAX ceramic material remove, thus obtain layering MXene, molecular formula Mn+1XnTz, M represents transition metal
(such as titanium, vanadium, chromium, manganese), X represent C or N element, and T represents surface DT group terminal (such as O2-,OH-,F-NH2 -NH4 +Deng).MXene
Suffix " ene " highlight the similitudes of they and graphene.MXenes has large specific surface area, and good conductivity, element is flexible,
The advantages that nanometer layer thickness is adjustable is widely used in the fields such as lithium, sodium energy-storage system, electromagnetic interference (EMI) shielding, Water warfare.
Compared with other many two-dimensional materials, MXene gas sensor has the signal-to-noise ratio of superelevation.What our utilizations were most readily available
MAX ceramic material Ti3AlC2The most mature Ti of preparation route is synthesized3C2Tx。
With now widely used two-dimensional sheet Ti3C2TxIt compares, is not layered Ti with organ shape structure3C2TxWith compared with
High specific surface area, has biggish gas absorption surface, and this unique structure can be used as a kind of good gas sensitization
Material support.It can get finer and close layer structure, but its organ shape structure as the preparation method of etching liquid using villiaumite plus hydrochloric acid
It is unstable, it may partially be dispersed by shaking.Therefore, we select high concentration of hydrofluoric acid to etch, to obtain more stable organ
Shape structure.And the Ti of hydrofluoric acid preparation3C2TxSurface-F terminal content will account for significant proportion.According to work before, Ti3C2Tx's
Electric conductivity is influenced by humidity and gas.Ti more than surface-O and-OH terminal3C2TxThere can be better gas absorption performance,
Especially to ammonia.
Therefore, we develop and made based on plane ceramic substrate with organ shape Ti3C2TxFor the room temperature of sensitive material
Ammonia and humidity sensor.As far as we know, Ti3C2TxSensor first passage basic treatment realizes ammonia and humidity sensor
The improvement of performance.Alkalize organ shape Ti3C2TxIt is had potential application in terms of gas and humidity sensor.
Summary of the invention
The object of the present invention is to provide one kind based on alkalization organ shape MXene (Ti3C2Tx, T represents surface DT group terminal, x
Value is in each terminal ratio in surface) the plane humidity of sensitive material, ammonia gas sensor and preparation method thereof and the sensor
In the practical application of humidity and ammonia context of detection.The obtained sensor of the present invention has current highest MXene air humidity
Quick response, and there is selectivity well.
Plane humidity of the present invention and ammonia gas sensor, as shown in Figure 1, by having Au/Ni interdigital electrode
Al2O3The sensitive material composition of ceramic substrate and uniform drop coating in interdigital electrode and ceramic substrate；The sensitive material is
Alkalize organ shape MXene (Ti3C2Tx) sensitive material, it is prepared by the following method:
(1) Ti is weighed3AlC2It is slowly added into the reaction vessel containing 10~20mL hydrofluoric acid (mass fraction 40~45%)
In, be stirred to react under 40~60 DEG C of oil baths 20~24 hours, product after the reaction was completed washs repeatedly with deionized water, from
The heart, until supernatant pH is 6~7；
(2) lower sediment that step (1) obtains is dispersed in dehydrated alcohol, dry 8 in 80~90 DEG C of vacuum drying ovens
~12 hours, obtain Ti3C2TxPowder；
(3) Ti that step (2) obtains is weighed3C2TxPowder is added in concentration 2~10mol/L sodium hydroxide solution, magnetic force
Stirring 2~3 hours；Product is subjected to centrifuge washing with deionized water after stirring, until supernatant pH value is 7~8；Will under
Layer precipitating be dispersed in dehydrated alcohol 80~90 DEG C vacuum oven 8~12 hours, finally obtain alkalization organ shape Ti3C2Tx
Sensitive material powder.
Humidity of the present invention and the preparation step of ammonia gas sensor are as follows:
(1) Au/Ni interdigital electrode is made: first by Al2O3Ceramic substrate deionized water and dehydrated alcohol wash repeatedly, dry
Dry, then the interdigital mask plate complementary using shape with interdigitated electrode structure to be prepared is needed is exposure mask, first in Al2O3Ceramic substrate
Then the Ni layer electrode of upper one layer 0.5~2 micron thick of sputtering sputters the Au layer electricity of one layer of 80~150 nanometer thickness above it again
Pole；
(2) drop coating alkalization organ shape Ti3C2TxSensitive material: the Al with Au/Ni interdigital electrode that will be completed2O3Pottery
Porcelain substrate deionized water and dehydrated alcohol wash repeatedly, drying；Weigh alkalization organ shape Ti3C2TxSensitive material powder with go
Ionized water is uniformly mixed according to the ratio of (3~5) g:1mL, and after fully dispersed, uniform drop coating is having Au/Ni interdigital electrode
Al2O3It is then 30~40 minutes dry under 80~90 DEG C of vacuum conditions on ceramic substrate, to be prepared of the present invention
With the organ shape Ti that alkalizes3C2TxFor the plane humidity and ammonia gas sensor of sensitive material.
It is whole that the present invention reaches removal surface F based on organ shape MXene material, through basification organ shape MXene
The purpose at end and insertion sodium ion, the quick performance of air humidity of comparison alkalization front and back, obtaining has more high humility and ammonia sensitive property
Device.
Advantages of the present invention:
(1) sensor utilizes alkali process new material MXene, so that its wet sensitive and ammonia sensing capabilities are significantly promoted,
Raising for the quick performance of MXene material air humidity provides a kind of feasible solution.
(2) sensor works at room temperature, lower than the air humidities dependent sensor operating temperature such as conventional solid electrolyte, power consumption
It is small.
Detailed description of the invention
Fig. 1: alkalization organ shape Ti of the present invention3C2TxThe hydrone of plane room temperature humidity and ammonia gas sensor and
Ammonia Molecular Adsorption schematic diagram；Wherein, left-hand component is sensor structure schematic diagram, elaborates and sees Fig. 2, upper right portion is water
Molecular Adsorption schematic diagram, lower right-most portion are ammonia Molecular Adsorption schematic diagram.
As shown in Figure 1, the direct-insert sodium ion adsorbed water molecule of lamella, forms hydration sodium ion；Ammonia molecule is by oxygen
The be adsorbed on sheet surfaces of terminal.
Fig. 2: alkalization organ shape Ti of the present invention3C2TxThe structural representation of plane room temperature humidity and ammonia gas sensor
Figure；Wherein, Al2O3Ceramic substrate 1, Au/Ni interdigital electrode 2, Ti3C2TxSensitive material 3.
Fig. 3: the present invention obtained by alkalization before with organ shape Ti after alkalization3C2TxThe SEM of sensitive material schemes and TEM figure.Figure
Middle each section: Ti3C2Tx(10000 times of enlarged drawings a, 50000 times of enlarged drawing b) and alkalization Ti3C2Tx(10000 times of enlarged drawing f,
The SEM figure of 50000 times of enlarged drawing g)；Ti3C2Tx(single organ shape Ti3C2TxScheme c, organ shape Ti3C2TxLocal map d, Ti3C2Tx
Crystal lattice pattern e wherein represents TiO in dotted line frame2Lattice) and alkalization Ti3C2Tx(single alkalization organ shape Ti3C2TxScheme h, alkalize wind
Qin shape Ti3C2TxLocal map i, alkalize organ shape Ti3C2TxThe TEM of crystal lattice pattern j) schemes.
As shown in figure 3, can be observed with organ shape structure visible in detail, after basification from figure a and figure b
Scheme f and figure g, it can be seen that the increase in gap, comparison diagram d and figure i can see the disappearance of surface oxidation particle, illustrate lye at
Function acts on surface.
Fig. 4: the present invention obtained by alkalization before with organ shape Ti after alkalization3C2TxThe wet sensitive performance test chart of sensitive material.
Each section in figure: (a) it is based on Ti3C2TxWith alkalization Ti3C2TxDevice to the response-recovery curves of different relative humidity；(b,c)
Based on Ti3C2TxWith alkalization Ti3C2TxDevice to the responses of different relative humidity；(d) at 25 DEG C, based on alkalization Ti3C2Tx
Device in duplicate responses-recovery curve；(e) at 25 DEG C, based on alkalization Ti3C2TxDevice relative humidity 11%~
Response time and recovery time curve between 98%.
The response direction of humidity is changed as shown in figure 4, figure a presents alkalization context sensitive material, after alkalization
Ti3C2TxResistance value becomes apparent with humidity variation, from figure b and schemes the specific response of c it can also be seen that passing through alkalization place
Reason, the response in 95%RH environment increases to 302.30 from 1.2167, and device also maintains preferable weight in figure d
Multiple power of test, has the response time being exceedingly fast.
Fig. 5: the present invention obtained by alkalization before with organ shape Ti after alkalization3C2TxThe air-sensitive performance test chart of sensitive material.
Each section in figure: (a, b) is based on Ti3C2TxWith alkalization Ti3C2TxDevice under 38%RH humidity to 10ppm, 50ppm,
The response-recovery curve of the ammonia of 100ppm and 500ppm concentration；(c) alkalize Ti3C2TxDevice to 100ppm ammonia repeat ring
Answer-recovery curve；(d) it is based on Ti3C2TxWith alkalization Ti3C2TxDevice to concentration be 100ppm other gas (ethyl alcohol, second
Aldehyde, formaldehyde, methanol, acetone, methane, nitrogen dioxide) response.
The response direction of ammonia is changed as shown in figure 5, figure a and figure b present alkalization context sensitive material.Alkali
Ti after change3C2TxResistance value becomes apparent with ammonia concentration variation, and response is obviously improved, and alkalize Ti in figure c3C2Tx
Device maintains the ability preferably to 100ppm ammonia retest, and in figure d, alkalize Ti3C2TxDevice is shown to ammonia
Gas selectivity more outstanding reduces the interference of nitrogen dioxide, and the raising of ammonia response is so that the response of other gases can
To ignore.
Specific embodiment
Comparative example 1:
Organ shape Ti is prepared with hf etching method3C2TxMaterial, by untreated organ shape Ti3C2TxMaterial is as sensitive
Material makes plane room temperature wet sensitive and NH3Sensor, and the quick performance of sensor air humidity is tested, detailed process is as follows:
(1) organ shape Ti is prepared3C2Tx: weigh 1 gram of Ti3AlC2It is slowly added to hydrofluoric acid containing 20mL (mass fraction 45%)
100mL polytetrafluoroethylene (PTFE) bottle in, be stirred to react under 60 DEG C of oil baths 24 hours, product deionized water after the reaction was completed is anti-
After backwashing is washed, is centrifuged, until supernatant pH is 6.Finally lower sediment is dispersed in dehydrated alcohol and is done in 80 DEG C of vacuum drying ovens
Dry 12 hours, collect final organ shape Ti3C2TxPowder.
(2) Au/Ni interdigital electrode is made: first by the Al of 8.2mm*8.2mm2O3Ceramic substrate deionized water and anhydrous second
Alcohol washs repeatedly, drying, and then the interdigital mask plate complementary using shape with interdigitated electrode structure to be prepared is needed first exists as exposure mask
Al2O3The Ni layer electrode that one layer 1 micron thick is first sputtered on ceramic substrate, then sputters the Au of one layer of 100 nanometer thickness again above it
Layer electrode.
(3) drop coating organ shape Ti3C2Tx: the Al with Au/Ni interdigital electrode that will be completed2O3Ceramic substrate spend from
Sub- water and dehydrated alcohol wash repeatedly, drying.Weigh the organ shape Ti of 4mg3C2TxPowder is uniformly mixed with 1mL deionized water,
After fully dispersed, uniform drop coating is in Al2O3On ceramic substrate, it is then put in 80 DEG C of vacuum ovens 30 minutes.To be prepared
It is of the present invention with organ shape Ti3C2TxFor the plane temperature sensor of sensitive material.
Embodiment 1:
With the organ shape Ti after basification3C2TxMaterial makes humidity and ammonia gas sensor as sensitive electrode material,
Its manufacturing process are as follows:
(1) preparation alkalization organ shape Ti3C2Tx: weigh 1 gram of Ti3AlC2Being slowly added to hydrofluoric acid containing 20mL, (mass fraction is
45%) in 100mL polytetrafluoroethylene (PTFE) bottle, be stirred to react under 60 DEG C of oil baths 24 hours, product after the reaction was completed spend from
Sub- water is washed repeatedly, is centrifuged, until supernatant pH is 6.Finally lower sediment is dispersed in dehydrated alcohol and is dried in 80 DEG C of vacuum
It is 12 hours dry in case, collect final organ shape Ti3C2TxPowder.It is 2mol/L's that 100mL concentration is prepared in plastic beaker
High-concentration sodium hydroxide solution.Weigh 0.3 gram of organ shape Ti3C2TxPowder is added in sodium hydroxide solution, in magnetic agitation platform
On continuously stir 2 hours.Product is subjected to centrifuge washing with deionized water after stirring, until supernatant pH value be 8, will under
Layer precipitating be dispersed in dehydrated alcohol 80 DEG C vacuum oven 12 hours.Finally obtain alkalization organ shape Ti3C2TxSensitive material
Powder.
(2) by prepared alkalization organ shape Ti3C2TxMaking devices in drop coating to ceramic substrate, interdigital electrode production with
Device fabrication processes are identical as comparative example 1.
Wet sensitive test:
Sensor is connected on Fluke signal tester, respectively by sensor be placed in 11%RH, 33%RH, 54%RH,
Resistance signal test is carried out in the atmosphere of 75%RH, 85%RH and 95%RH.The test method of device is using traditional static survey
Examination method, detailed process is as follows:
1. sensor is connected on Fluke signal tester, device, which is placed in the test bottle that humidity is 11%RH, to be reached
Stablize, as resistance value (R of the device under 11%RH humidity11%).Test process is with R11%For benchmark resistance.
2. sensor is transferred quickly in the test bottle of other humidity, until response signal reaches stable, as device
Resistance value (R) under other humidity environments.
3. device is transferred back to again in the test bottle that humidity is 11%RH, stable until reaching, device completes primary ring
Answer recovery process.Resistance ratio R/R of the device under the atmosphere of 11%RH atmosphere and other humidity11%(comparative example), R11%/R
(embodiment) is the humidity response of device.
Air-sensitive test:
Sensor is connected on Fluke signal tester, respectively by sensor be placed in air, 10ppm, 50ppm,
Voltage signal test is carried out in the atmosphere of 100ppm and 500ppm ammonia.The test method of device uses traditional static test
Method, detailed process is as follows:
1. sensor is connected on Fluke signal tester, in the test bottle that it is 1L full of air volume that device, which is placed in,
Reach stable, as the aerial resistance value (R of deviceair)。
2. being transferred quickly to sensor in the test bottle equipped with concentration ammonia to be measured, until response signal reaches stable,
As resistance value (R) of the device in ammonia.
3. device is transferred back in air bottle again, stable until reaching, device completes a secondary response recovery process.Device
Resistance value ratio (Δ R/R in resistance difference Δ R and air in ammonia and airairIt * 100%) is device to the concentration ammonia
The response of gas.
Table 1 is with organ shape Ti3C2TxFor the R/R of the sensor of sensitive material11%With with the organ shape Ti that alkalizes3C2TxFor sensitivity
The R of the sensor of material11%The variation with humidity of/R
Table 2 is with organ shape Ti3C2TxIt is the sum of the sensor of sensitive material with the organ shape Ti that alkalizes3C2TxFor sensitive material
The Δ R/R of sensorair* 100% variation with humidity
It is listed in table 1 respectively with organ shape Ti3C2TxWith alkalization organ shape Ti3C2TxFor the plane of sensitive material production
Room temperature humidity sensor is in the ratio of the resistance value in different humidity atmosphere and the resistance value in 11%RH atmosphere with humidity
Changing value.It can be seen that, two kinds of devices have good response characteristic to humidity from table, wherein using alkalization organ shape
Ti3C2TxResponse for the device of sensitive material is higher.
It is listed in table 2 respectively with organ shape Ti3C2TxWith alkalization organ shape Ti3C2TxFor the plane of sensitive material production
The difference of resistance value and aerial resistance value of the room temperature ammonia gas sensor in various concentration ammonia and air resistance value
Ratio with ammonia concentration changing value.It can be seen that, after basification, the response of ammonia has greatly improved from table.
It can be seen that the alkalization organ shape Ti that we develop3C2TxThe device that sensitive material is constituted shows humidity and ammonia
Go out good sensitivity characteristic, obtains the plane room temperature humidity and ammonia gas sensor with highly sensitive, low operating temperature.
Claims (2)
1. a kind of plane humidity based on alkalization organ shape MXene sensitive material, ammonia gas sensor, by sensitive material and have
The Al of Au/Ni interdigital electrode2O3Ceramic wafer composition；By the Al for having Au/Ni interdigital electrode2O3Ceramic substrate and uniform drop coating
Sensitive material composition in interdigital electrode and ceramic substrate；It is characterized by: the sensitive material is alkalization organ shape
MXene sensitive material, and it is prepared by the following method,
(1) Ti is weighed3AlC2Be slowly added into containing 10~20mL, 40~45% hydrofluoric acid of mass fraction reaction vessel in,
It being stirred to react under 40~60 DEG C of oil baths 20~24 hours, product after the reaction was completed is washed repeatedly with deionized water, is centrifuged, until
Supernatant pH is 6~7；
(2) lower sediment that step (1) obtains is dispersed in dehydrated alcohol, dry 8~12 in 80~90 DEG C of vacuum drying ovens
Hour, obtain Ti3C2TxPowder；
(3) Ti that step (2) obtains is weighed3C2TxPowder is added in concentration 2~10mol/L sodium hydroxide solution, magnetic agitation
2~3 hours；Product is subjected to centrifuge washing with deionized water after stirring, until supernatant pH value is 7~8；Lower layer is sunk
Shallow lake be dispersed in dehydrated alcohol 80~90 DEG C vacuum oven 8~12 hours, finally obtain alkalization organ shape Ti3C2TxIt is sensitive
Material powder.
2. a kind of plane humidity based on alkalization organ shape MXene sensitive material described in claim 1, ammonia gas sensor
Preparation method, its step are as follows:
(1) Au/Ni interdigital electrode is made: first by Al2O3Ceramic substrate deionized water and dehydrated alcohol wash repeatedly, drying, so
The interdigital mask plate complementary using shape with interdigitated electrode structure to be prepared is needed is exposure mask afterwards, first in Al2O3It is sputtered on ceramic substrate
Then one layer 0.5~2 micron thick of Ni layer electrode sputters the Au layer electrode of one layer of 80~150 nanometer thickness above it again；
(2) drop coating alkalization organ shape Ti3C2TxSensitive material: the Al with Au/Ni interdigital electrode that will be completed2O3Ceramic base
Plate deionized water and dehydrated alcohol wash repeatedly, drying；Weigh alkalization organ shape Ti3C2TxSensitive material powder and deionization
Water is uniformly mixed according to the ratio of (3~5) g:1mL, and after fully dispersed, uniform drop coating is in the Al for having Au/Ni interdigital electrode2O3
On ceramic substrate, then dry 30~40 minutes under 80~90 DEG C of vacuum conditions, thus be prepared it is of the present invention with
Alkalize organ shape Ti3C2TxFor the plane humidity of sensitive material, ammonia gas sensor.
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| CN111017890A (en) * | 2019-12-30 | 2020-04-17 | 哈尔滨工业大学 | Method for rapidly preparing MXene film with high volume specific capacitance |
| CN111366615A (en) * | 2020-03-26 | 2020-07-03 | 电子科技大学 | Humidity sensor based on thin nano-flake MXene niobium carbide and preparation method thereof |
| CN112255278A (en) * | 2020-09-14 | 2021-01-22 | 重庆大学 | Based on Ti3C2Tx/WO3Room-temperature ammonia gas sensor made of composite nano material, and preparation method and application thereof |
| CN112254851B (en) * | 2020-10-16 | 2022-04-22 | 重庆大学 | Alk-Ti3C2Preparation method of PDMS flexible piezoresistive sensor |
| CN112254851A (en) * | 2020-10-16 | 2021-01-22 | 重庆大学 | Alk-Ti3C2Preparation method of PDMS flexible piezoresistive sensor |
| CN112229879A (en) * | 2020-10-21 | 2021-01-15 | 重庆大学 | TiO2-Ti3C2TxComposite film gas sensor and preparation method and application thereof |
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| CN113060734A (en) * | 2021-04-06 | 2021-07-02 | 郑州大学 | Infrared low-emissivity MXene film and preparation method thereof |
| CN113533449A (en) * | 2021-07-05 | 2021-10-22 | 广西师范大学 | Preparation method of MXene graphene composite structure gas sensor |
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| CN113447534A (en) * | 2021-07-06 | 2021-09-28 | 重庆大学 | Ammonia gas sensor and preparation method thereof |
| CN114137451A (en) * | 2021-11-30 | 2022-03-04 | 哈尔滨理工大学 | MXene and GMM cladding humidity and magnetic field measurement optical fiber sensor |
| CN114137451B (en) * | 2021-11-30 | 2023-09-26 | 哈尔滨理工大学 | MXene and GMM coated humidity and magnetic field measurement optical fiber sensor |
| CN115282786A (en) * | 2022-01-21 | 2022-11-04 | 浙江师范大学 | MXene modified composite separation membrane and preparation method and application thereof |
| CN115282786B (en) * | 2022-01-21 | 2023-12-08 | 浙江师范大学 | MXene modified composite separation membrane and preparation method and application thereof |
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