CN108007810A - A kind of QCM chemical sensors and preparation method thereof - Google Patents
A kind of QCM chemical sensors and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of chemical sensor based on quartz crystal microbalance (QCM) and preparation method thereof, including：Quartz crystal oscillator plate and coated in the sensitive layer on the quartz crystal oscillator plate, the material of the sensitive layer is quantum dot or quantum wire.Colloidal Quantum Dots or quantum wire are coated in quartz crystal oscillator surface homogeneous film formation, recycle appropriate salting liquid to carry out ligand processing, to remove the long-chain Ligand of quantum dot or quantum wire surface.By the use of Colloidal Quantum Dots or quantum wire as the QCM chemical sensors of sensitive layer compared with existing QCM chemical sensors, sensitive layer can be in room temperature film-forming and good crystallinity, simple process, the high-specific surface area and activity of nano material can be kept in the devices, response and recovery time are very fast, and respond height.
Description
Technical field
The invention belongs to sensor technical field, more particularly, to a kind of quartz crystal microbalance (Quartz
Crystal Microbalance, QCM) chemical sensor and preparation method thereof.
Background technology
QCM chemical sensors are a kind of sensors based on quality loading effect, when sensitive layer adsorption object gas
The quality on quartz crystal oscillator surface is caused to change so that the resonant frequency of quartz crystal oscillator changes, by target to be measured after molecule
The size of molecular concentration is converted into frequency signal output, so as to fulfill the detection of concentration of target molecules, it is easy to accomplish digitlization passes
It is defeated.QCM chemical sensors have the advantages that of simple structure and low cost, high sensitivity, stability are good, and operating temperature is
Room temperature, has become one of research hotspot of chemical sensor at present.
Up to the present, the sensitive membrane of obtained QCM chemical sensors is organic matter or organic matter composite wood mostly
Material, the humidity sensor that such as Zhen Yuan in 2016 et al. are prepared by the use of GO/PEI as sensitive membrane by spray-on process, when opposite
Humidity be 90% when, response and recovery time be respectively 53s/18s, due to humidity sensing film for composite material preparation process relatively
Difficulty, and the heat endurance of organic matter is relatively poor.Compared to organic matter humidity sensing film, the QCM chemistry prepared using inorganic matter is passed
Sensor responds and recovers slower, and such as Juan Xie in 2013 et al. are prepared for the QCM humidity based on ZnO using the mode of self assembly
Sensor, when relative humidity is 95%, response and recovery time are respectively 167.7s/62.2s, and response is relatively slow and humidity hysteresis is special
Property is poor.Chemical sensor Zhang Hongdi in 2015 et al. (CN 105203423A), which make use of, mixes the preparation of cerium zinc oxide nano fiber
QCM formula chemical sensors, materials synthesis technique is excessively complicated, and while preparing film needs 800 DEG C of high temperature drying, destroys
The high-specific surface area of nano-fiber material so that the response recovery characteristics of device are poor, and response is relatively low.
Zhang Jiaqi in 2013 et al. (103575865 A of CN) is prepared for a kind of being used to detect NH with ZnO nanorod3Sensor.
To sum up, the existing QCM chemical sensor preparation process based on organic matter or organic matter composite material is relative complex, and
The response of QCM chemical sensors and recovery based on inorganic matter sensitive membrane are slower.
The content of the invention
It is an object of the invention to solve the existing QCM chemical sensor systems based on organic matter or organic matter composite material
Standby process is relative complex, and the technology the shortcomings that response of the QCM chemical sensors based on inorganic matter sensitive membrane and slower recovery is asked
Topic.
To achieve the above object, in a first aspect, the present invention provides a kind of QCM chemical sensors, including：Quartz crystal shakes
Swing piece and coated in the sensitive layer on the quartz crystal oscillator plate, the material of the sensitive layer is Colloidal Quantum Dots or quantum
Line, the Colloidal Quantum Dots or quantum wire are to target gas molecules (such as H in environment2O, NO2, SO2, NH3Deng) sensitive, once ring
Target gas molecules component or concentration change in border causes the resonant frequency of the QCM chemical sensors to change immediately
Become.
Specifically, it make use of Colloidal Quantum Dots or quantum wire high as sensitive layer using Colloidal Quantum Dots or quantum wire
Specific surface area, thus have very high surface-active and very sensitive to target gas molecules, once adsorbed target gas molecule,
The resonant frequency of QCM chemical sensors can change immediately.
Present invention utilizes colloid quantum wire/quantum dot as sensitive material, can in strand DNA on Surface of Quartz crystal room temperature film-forming,
Its relatively large specific surface area is maintained in the devices, thus the QCM chemical sensors prepared have quickly response to recover
Characteristic, and response is of a relatively high.
Alternatively, the Colloidal Quantum Dots are PbS Colloidal Quantum Dots, ZnO colloid quantum dot, WO3Colloidal Quantum Dots or
In2O3Colloidal Quantum Dots；The quantum wire is SnO2Quantum wire.
Specifically, PbS Colloidal Quantum Dots, ZnO colloid quantum dot, WO3Colloidal Quantum Dots, In2O3Colloidal Quantum Dots and oxygen
Change tin SnO2The specific surface area of quantum wire is larger, therefore the time used in absorption or desorption target gas molecules is shorter, adsorbed target
Gas molecule is to respond, and desorption target gas molecules are to recover to normal condition.
Specifically, SnO is passed through2The selection of the generated time of quantum wire so that sensitive layer SnO2The QCM chemistry of quantum wire
Sensor can have response and recovery characteristics at room temperature so that QCM chemical sensors have preferable application prospect.
Second aspect, an embodiment of the present invention provides the preparation method of the QCM chemical sensors described in above-mentioned first aspect,
Including：(1) sensitive layer is coated into (such as spin coating, drop coating, spraying, brushing) on quartz crystal oscillator plate, makes its homogeneous film formation,
The material of the sensitive layer is Colloidal Quantum Dots or quantum wire, and the Colloidal Quantum Dots are PbS Colloidal Quantum Dots, ZnO colloid amount
Sub- point, WO3Colloidal Quantum Dots or In2O3Colloidal Quantum Dots or the quantum wire are SnO2Quantum wire；(2) it is molten using corresponding salt
The quartz crystal covered with sensitive layer that liquid processing step (1) obtains, to remove the surface coated long-chain of the sensitive layer, to institute
Sensitive layer is stated to be modified, easy to follow-up sensitive layer further in conjunction with and sensitive layer growth, the long-chain is oleyl amine or oil
Acid；(3) product obtained using absolute methanol solution soaking step (2), to remove remaining salting liquid, and it is molten to remove the salt
Liquid reacts generated accessory substance with the sensitive layer；(4) step (1) is repeated to step (3), until obtaining having required
The sensitive layer film of thickness, to obtain the QCM chemical sensors.
It should be noted that step (2) and step (3) be required to wait previous step after product drying after hold again
OK.
Alternatively, the Colloidal Quantum Dots are PbS, ZnO, In2O3Or WO3Colloidal Quantum Dots, the quantum wire is SnO2
Quantum wire.
Alternatively, the SnO2The preparation method of quantum wire is as follows：0.6g stannic chloride pentahydrates are added into 50ml beakers
SnCl4·5H2O powder, 20ml oleic acid OA, 2.5ml oleyl amine OLA and 10ml absolute ethyl alcohol are mixed, and make SnCl4·5H2O
It is completely dissolved；SnCl will be dissolved4·5H2Mixed solution after O powder is transferred in stainless steel water heating kettle, and keeps 3- at 180 DEG C
24h, obtains SnO2Quantum wire.
Alternatively, when the material of the sensitive layer is PbS Colloidal Quantum Dots, the salting liquid is sodium nitrite
(NaNO2) methanol solution；When the material of the sensitive layer is ZnO colloid quantum dot, the salting liquid is zinc chloride (ZnCl2)
Methanol solution；When the material of the sensitive layer is SnO2During quantum wire, the salting liquid is copper nitrate (Cu (NO3)2) methanol
Solution, when the sensitive layer is In2O3During Colloidal Quantum Dots, the salting liquid is copper acetate (Cu (CH3COO)2) methanol it is molten
Liquid, when the sensitive layer is WO3During quantum dot, then salting liquid processing is not required.
By the contemplated above technical scheme of the present invention compared with prior art, have the advantages that：
1st, using Colloidal Quantum Dots or quantum wire as sensitive layer, Colloidal Quantum Dots or the huge ratio table of quantum wire be make use of
Area, thus have very high surface-active and very sensitive to target gas molecules, once target gas molecules are adsorbed with,
The resonant frequency of QCM can change immediately.Further can from preparation process the selection of salting liquid and soaking time, quantum
Point/quantum wire synthesis temperature and the control of time etc. is regulated and controled, to obtain significant room temperature air-sensitive response signal.
2nd, QCM Colloidal Quantum Dots or quantum wire chemical sensor simplify device architecture and preparation process, and sensitive layer can be
At room temperature using technique direct formation of film at surface such as spin coating, spraying brushing, drop coatings, it is not necessary to by high-temperature process, device making technics letter
Single, energy consumption is small, and cost is low.
3rd, QCM chemical sensors provided by the invention, by the use of mineral colloid quantum dot or quantum wire as sensitive material,
Compared with the existing QCM chemical sensors prepared using organic matter, stability is more excellent.
4th, the present invention can oleic oil that effectively place to go Colloidal Quantum Dots or quantum wire surface are wrapped up with salting liquid processing
Amine long-chain, beneficial to the response speed of lifting QCM chemical sensors.
Brief description of the drawings
Fig. 1 is the flow diagram that spin-coating method prepares QCM chemical sensors；
Fig. 2 is QCM chemical sensors provided by the invention at room temperature to the response curve schematic diagram of different relative humidity.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, it is right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
It is an object of the invention to solve it is existing based on inorganic matter sensitive membrane QCM chemical sensors response and recover compared with
The shortcomings that slow, recovery characteristics are responded so using mineral colloid quantum dot or quantum wire to improve it.
Fig. 1 is the flow diagram that spin-coating method provided by the invention prepares QCM chemical sensors, as shown in Figure 1, the flow
Including：(1) sensitive layer is spin-coated on quartz crystal oscillator plate, makes its homogeneous film formation, the material of the sensitive layer is colloid amount
Son point or quantum wire；(2) quartz crystal covered with sensitive layer obtained using corresponding salting liquid processing step (1), to go
Except the surface coated long-chain of the sensitive layer, the sensitive layer is modified, easy to follow-up sensitive layer further in conjunction with and
The growth of sensitive layer, the long-chain are oleyl amine or oleic acid；(3) product obtained using absolute methanol solution soaking step (2), with
Remaining salting liquid is removed, and removes the salting liquid and reacts generated accessory substance with sensitive layer；(4) step is repeated
(1) to step (3), until the sensitive layer film with required thickness is obtained, to obtain the QCM chemical sensors.
QCM Colloidal Quantum Dots/quantum wire chemical sensor of the present invention includes quartz crystal oscillator plate and sensitive layer, sensitive
Layer is directly overlayed on quartz crystal, and sensitive layer is PbS Colloidal Quantum Dots, ZnO colloid quantum dot, WO3Colloidal Quantum Dots, In2O3
Colloidal Quantum Dots, SnO2Colloid quantum wire etc. is formed.Illustrate with reference to embodiments.
Embodiment 1
(1) quartz crystal oscillator plate is put into acetone first and cleaned, is then placed in ethanol, then with elevated pressure nitrogen air-blowing
It is dry.
(2) and then suitable SnO is taken2Quantum wire makes its homogeneous film formation coated on quartz crystal oscillator plate, recycles salt
The quartz crystal oscillator plate covered with quantum dot film that solution treatment obtains, it is right to remove the surface coated long-chain of quantum dot
Film is modified, easy to follow-up quantum dot further in conjunction with and film thickness growth；Finally use absolute methanol solution
Processing, to remove the accessory substance that remaining short chain ligand and short chain ligand solution and Colloidal Quantum Dots solution reaction are generated.
(3) step (2) is repeated, obtains the sensitive layer with required thickness, completes the preparation of chemical sensor.
Salting liquid in above-mentioned steps (2) is Cu (NO3)2Methanol solution.
Above-mentioned SnO2Colloid quantum wire is prepared as follows：
(1) 0.6g stannic chloride pentahydrates (SnCl is added into 50ml beakers4·5H2O) powder, 20ml oleic acid (OA), 2.5ml
Oleyl amine (OLA) and 10ml absolute ethyl alcohols are mixed, and make SnCl4·5H2O is completely dissolved.
(2) above-mentioned mixed solution is transferred in stainless steel water heating kettle, and 3-24h is kept at 180 DEG C.
(3) cleaned using organic solvent, centrifugation obtains SnO2Quantum wire, organic solvent are toluene and ethanol.
(4) gelatinous precipitate after cleaning is dissolved in 20ml toluene, just obtains SnO2Quantum wire solution.
Specifically, 0.6g SnCl are taken4·5H2O powder, is dispersed in 2.5ml OLA, 20ml OA, 10ml ethanol composition
In the mixed solvent, magnetic agitation makes it be uniformly dispersed, obtains mixed liquor；Mixed liquor is moved in the reaction kettle of 50ml, 180
When reaction 3-24 is small at a high temperature of DEG C, mixed liquor after reaction is poured into centrifuge tube, adds absolute ethyl alcohol and toluene to clean
And centrifuge.Specifically centrifugal process is：Ethanol in proper amount is first added into mixed liquor, is put into centrifuge and is revolved with the rotating speed of 8000rpm
Leave the heart 8 minutes, then pour out supernatant, leave sediment, first time cleaning process terminates；Added again into sediment appropriate
Toluene dissolves, then adds suitable alcohols thereto, is put into centrifuge with the rotating speed rotating centrifugal 8 minutes of 8000rpm, then falls
Go out supernatant, leave sediment；Take 20ml toluene to dissolve the sediment of above-mentioned acquisition, just obtain SnO2Quantum wire solution
Take suitable SnO2Quantum wire solution is spin-coated on quartz crystal oscillator plate with the rotating speed of 1000rpm, makes it
Homogeneous film formation, then adds Cu (NO successively3)2Methanol solution and absolute methanol handled, repeat spin coating 3 times, reach film
Required thickness, completes the preparation of chemical sensor.
Embodiment 2
0.9g (4mmol) PbO is dissolved into 3ml oleic acid (OA) and 17ml octadecylenes (ODE) and added in a nitrogen environment
Heat is to 90 DEG C of predecessors for preparing plumbi oleas, as lead source；Vacuumize, which is risen to 120 DEG C；By 180ul
(1mmol) TMS is dissolved into 10ml ODE, as sulphur source.
By in sulphur source injection lead source at 120 DEG C, solution is put into by (about 15s) after the complete blackening of question response system color
Temperature is set quickly to be down to room temperature in cold water；Acetone is added into solution after cooling, supernatant is removed after centrifugal mixer, is then passed through
Cross toluene disperse, acetone centrifugation repeatedly circulation until supernatant it is pure white；Final products therefrom is dried into powder and is dispersed in just
Vulcanized lead (PbS) quantum dot solution of 50mg/ml is obtained in octane.
Specific film formation step salting liquid same as Example 1 but used is 10mg/ml NaNO2Methanol solution.
Embodiment 3
Take 3.3g zinc acetates (Zn (OAc)2·2H2O) it is dissolved in 100ml absolute ethyl alcohols, and the ultrasound 2h at 80 DEG C, make
Its is dispersed, meanwhile, take 0.84g LiOHH2O is dissolved in 50ml absolute ethyl alcohols, is stirred at room temperature uniformly.Treat acetic acid
After zinc solution is cooled to room temperature, above two solution is mixed, and 10min is stirred at room temperature, just obtains the mixed of ZnO quantum dot
Liquid is closed, 2ml OA are then added into mixed liquor, precipitate ZnO quantum dot, sediment plus absolute ethyl alcohol and n-hexane are centrifuged
Cleaning 2 times.Finally ZnO quantum dot is dispersed in 50ml n-hexanes.
Specific film formation step salting liquid same as Example 1 but used is 10mg/ml zinc chloride (ZnCl2) methanol
Solution, and the quartz crystal after film is annealed 1h at 300 DEG C.
Embodiment 4
Specifically, 0.68g WCl are taken6Powder, be dispersed in 2.5ml oleyl amines (OLA), 20ml OA composition mixing it is molten
In agent, magnetic agitation makes it be uniformly dispersed, then adds 10ml ethanol thereto, obtains mixed liquor；Mixed liquor is moved to 50ml's
In reaction kettle, when reaction 3 is small at a high temperature of 180 DEG C, mixed liquor after reaction is poured into centrifuge tube, adds absolute ethyl alcohol
Clean and centrifuge with toluene.Specifically centrifugal process is：First ethanol in proper amount is added into mixed liquor, be put into centrifuge with
The rotating speed rotating centrifugal of 8000rpm 8 minutes, then pours out supernatant, leaves sediment, and first time cleaning process terminates；Again to
Q. s. toluene dissolving is added in sediment, then adds suitable alcohols thereto, is put into centrifuge and is rotated with the rotating speed of 8000rpm
Centrifugation 8 minutes, then pours out supernatant, leaves sediment；Take 12ml toluene to dissolve the sediment of above-mentioned acquisition, just obtain WO3
Quantum wire solution.
Specific film formation step is same as Example 1, but salting liquid processing is not required.
Embodiment 5
0.438g indium acetates (Inac3) and 5ml OLA mixed in three-necked bottle, vacuumize at room temperature, then in nitrogen
In atmosphere 30min is heated at 240 DEG C.After liquid cooled to room temperature to be mixed, mixed liquor is poured into centrifuge tube, is added appropriate
Ethanol centrifuges, finally dissolving by gained precipitation in hexane.Just In is obtained2O3Quantum dot.
Specific film formation step salting liquid same as Example 1 but used is 10mg/ml copper acetate methanol solutions.
Correspondingly, Fig. 2 be QCM chemical sensors provided in an embodiment of the present invention at room temperature to different humidity be response/
Recovery curve figure, sensitive material SnO2Colloid quantum wire (12h).It is 80% for relative humidity, the frequency shift of sensor
Δ f=1405Hz is measured, response recovery time is respectively that the QCM prepared using ZnO to report for work in 12s/6s, with background technology is sensed
Device is compared, and response and recovery characteristics substantially become excellent.
The quantum dot synthetic method used in the present invention, predecessor ratio, synthesis temperature and reaction time used are not
It is confined to the design parameter of proposition of the embodiment of the present invention, the selections of different parameters is to the quantum dot size, the gas-sensitive activity that synthesize
With extreme influence.
Annealing temperature in the present invention is not limited to the design parameter that present example provides, and annealing temperature determines quantum
The specific nature that point is shown in atmosphere, and then influence gas-selectively.
Salting liquid in the embodiment of the present invention, is not limited to NaNO2Solution, Cu (NO3)2Solution, zinc chloride (ZnCl2), can
Using NH4Cl solution, CuCl2Solution；Salting liquid can effectively remove the oleic acid oleyl amine long-chain of quantum dot surface parcel, improve quantum
Point gas absorption activity, and then improve gas-selectively and the sensitivity of sensor.
Since the physicochemical characteristic controllability of Colloidal Quantum Dots or quantum wire is strong, different short chain ligand solutions can be used to carry out
Doping or surface modification, are regulated and controled for the characteristic of different target gas, so as to improve the activity to object gas, reduction pair
The activity of other interference gas and improve stability, the optimization of incorporating quantum point component and its crystallite dimension further improves pair
The sensitivity of object gas and selectivity, reduce test limit.
QCM quantum wires/Colloidal Quantum Dots chemical sensor proposed by the present invention is prepared from sensitive layer and sensitive layer ligand
The optimization of processing；Different from the scheme of existing QCM measurement gases, had preferably to humidity using quantum dot or quantum wire measurement
Response and recovery characteristics；Compared with existing film forming scheme, preparation method provided by the invention, its film forming procedure takes shorter, nothing
Need another oil (gas) filling device is convenient to operate, film forming thickness is controllable better.
The invention discloses a kind of quartz crystal microbalance chemical sensor and preparation method thereof, it is vibrated by quartz crystal
Piece and Colloidal Quantum Dots sensitive layer are formed；Sensitive layer is evenly applied to quartz crystal oscillator plate surface, when its adsorbed gas should
Sensor mass changes so that the resonant frequency of quartz crystal oscillator plate changes, so as to carry out the other quality inspection of nanogram level
Survey；And preparation method proposed by the present invention be using spin-coating film with obtain uniformly, thickness is adjustable, adhesive force is excellent sensitivity
Layer；It is doped by salting liquid or surface modification, is regulated and controled for the characteristic of different target gas, further improved to mesh
The sensitivity of standard gas body and selectivity.
More than, it is only the preferable embodiment of the application, but the protection domain of the application is not limited thereto, and it is any
Those familiar with the art is in the technical scope that the application discloses, the change or replacement that can readily occur in, all should
Cover within the protection domain of the application.Therefore, the protection domain of the application should be subject to scope of the claims.
Claims (4)
- A kind of 1. QCM chemical sensors, it is characterised in that including：Quartz crystal oscillator plate and shake coated in the quartz crystal Swing the sensitive layer of on piece, the material of the sensitive layer is Colloidal Quantum Dots or quantum wire, the Colloidal Quantum Dots or quantum wire pair Gas molecule is sensitive, once gas componant or concentration change the resonant frequency of QCM chemical sensors can be caused to change.
- 2. QCM chemical sensors according to claim 1, it is characterised in that the Colloidal Quantum Dots are vulcanized lead (PbS), zinc oxide (ZnO), indium oxide (In2O3) or tungsten oxide (WO3) Colloidal Quantum Dots, the quantum wire is stannic oxide (SnO2) quantum wire.
- A kind of 3. preparation method of QCM chemical sensors as claimed in claim 1 or 2, it is characterised in that including：(1) sensitive layer is made into its homogeneous film formation, the material of the sensitive layer is colloid quantum coated on quartz crystal oscillator plate Point or quantum wire；(2) the quartz crystal oscillator plate covered with sensitive layer obtained using salting liquid processing step (1), to remove the sensitivity The organic matter long-chains such as the oleic acid oleyl amine of layer surface cladding, are modified the sensitive layer, easy to the knot again of follow-up sensitive layer Conjunction and the growth of sensitive layer, the long-chain is oleyl amine or oleic acid；(3) product obtained using absolute methanol solution soaking step (2), to remove the remaining salting liquid, and removes institute State salting liquid and react generated accessory substance with the sensitive layer；(4) step (1) is repeated to step (3), until the sensitive layer film with required thickness is obtained, it is described to obtain QCM chemical sensors.
- 4. the preparation method of QCM chemical sensors according to claim 3, it is characterised in that the Colloidal Quantum Dots are Vulcanized lead (PbS), zinc oxide (ZnO), indium oxide (In2O3) or tungsten oxide (WO3) Colloidal Quantum Dots, the quantum wire be two Tin oxide (SnO2) quantum wire.
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| CN113640169A (en) * | 2021-06-23 | 2021-11-12 | 南方医科大学皮肤病医院（广东省皮肤病医院、广东省皮肤性病防治中心、中国麻风防治研究中心） | WO based on doped Sb3Nanocrystalline QCM sensor and application thereof in monitoring of respiration and skin wound humidity |
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| CN114813877A (en) * | 2022-05-31 | 2022-07-29 | 华中科技大学 | Sensor for detecting glucose, preparation method and application thereof |
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