CN110031512A - A kind of single particle sensitive gas sensor and its preparation method and application - Google Patents
A kind of single particle sensitive gas sensor and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to gas sensor technical field more particularly to a kind of single particle sensitive gas sensor and its preparation method and application, a kind of preparation method of single particle sensitive gas sensor provided by the invention, comprising the following steps: sensor substrate is provided;Single-particle is deposited in the sensor substrate surface using single-particle prize law, obtains single particle sensitive gas sensor presoma;The single particle sensitive gas sensor presoma is made annealing treatment, single particle sensitive gas sensor is obtained.Preparation method of the present invention is at low cost, easy to operate;The single particle sensitive gas sensor being prepared using the preparation method can be to avoid particle buildup and particle growth, to give full play to the structural advantage of nanoparticle, it is capable of increasing specific surface area, sensitivity is improved, facilitates response regeneration rate of the gas in adsorption and desorption process;Also particle buildup and diauxic growth bring instability problem be can solve.
Description
Technical field
The present invention relates to gas sensor technical field more particularly to a kind of single particle sensitive gas sensor and its systems
Preparation Method and application.
Background technique
Since nano material has the characteristics that large specific surface area, surface defect are abundant, it is widely used in gas sensor
Device.Usual semiconductor gas sensor generally requires to work at a higher temperature, but lasting hot operation can make partly to lead
The crystal structure of body material is destroyed, and the unstable problem of sensor performance is in turn resulted in.
Currently, ultraviolet enhancing and inhibition sensitive particles growth are the usual ways for improving the above problem, wherein ultraviolet enhancing
Mainly using ultraviolet excitation sensitive material replace heating element to the thermal excitation of material by the way of, which can improve quick
Feel the room temperature gas-sensitive property and room temperature electric conductivity of material;But its response recovery time is but up to a few to tens of minutes, sensitivity
It is greatly reduced.Meanwhile single sensitive particles growth being inhibited mainly to realize by preparing hierarchical structure, but tied from preparation classification
The preparation of structure to sensor also needs just form sensitive material film layer by operations such as spin coating or coatings, the sensitivity material
Material film layer would generally due to particle aggregation and form dense film, be unfavorable for the raising and stabilization of sensor air-sensitive performance.
On the basis of the above, the prior art solves single sensitivity by preparing single nanoparticle building gas sensor
The problem of particle growth;It is mainly real using focused ion beam deposition during preparing single nanoparticle gas sensor
Existing electrode deposition control, or realize sensitive material control by contact atomic force microscope, thus realize sensitive material with
The contact of electrode, but equipment used in the method is more expensive, operates also more complicated.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of single particle sensitive gas sensor, the method letters
It is single, it is at low cost.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of preparation methods of single particle sensitive gas sensor, comprising the following steps:
Sensor substrate is provided;
Single-particle is deposited on the surface of the sensor substrate using single-particle prize law, forms single particle sensitive layer,
Obtain single particle sensitive gas sensor presoma;
The single particle sensitive gas sensor presoma is made annealing treatment, single particle sensitive gas biography is obtained
Sensor.
Preferably, the preparation method of the sensor substrate, comprising the following steps:
After being sequentially depositing polymer fiber sacrificial layer and electrode material layer in sensor base, removal polymer fiber is sacrificial
Domestic animal layer, obtains sensor substrate.
Preferably, the polymer of the polymer fiber sacrificial layer is polyvinylpyrrolidone and/or polyvinyl alcohol.
Preferably, the electrode material layer includes bottoming metal layer and conductive metal layer;
The material of the conductive metal layer is gold and/or platinum;The material of the bottoming metal layer is tantalum;
The conductive metal layer with a thickness of 50~250nm;The bottoming metal layer with a thickness of 5~25nm.
Preferably, the electrode material layer includes two metal block areas;
The spacing in two metal block area is 10~500nm.
Preferably, the process of the single-particle prize law are as follows: sensor substrate is placed in single-particle dispersion liquid, applies electricity
Pressure carries out single-particle capture in sensor substrate;
The single-particle of the single-particle dispersion liquid is metal oxide or metal sulfide;
The concentration of the single-particle dispersion liquid is 0.0001~1g/mL.
Preferably, the voltage is 10~1000V.
Preferably, temperature >=300 DEG C of the annealing, time >=1h of the annealing.
The present invention also provides the single particle sensitive gas biographies that the preparation method described in above-mentioned technical proposal is prepared
Sensor.
The present invention also provides the single particle sensitive gas sensors in detection inorganic gas or organic gas
Application.
The present invention provides a kind of preparation methods of single particle sensitive gas sensor, comprising the following steps: provides biography
Sensor substrate;Single-particle is deposited in the sensor substrate surface using single-particle prize law, obtains single particle sensitive gas
Sensor precursor;The single particle sensitive gas sensor presoma is made annealing treatment, single particle sensitivity is obtained
Gas sensor.Preparation method of the present invention is at low cost, easy to operate;It is prepared using the preparation method single
Particle-sensitive gas sensor can to avoid particle buildup and particle growth, to give full play to the structural advantage of nanoparticle,
On the one hand it is capable of increasing specific surface area, sensitivity is improved, helps to improve response of the gas in adsorption and desorption process
Regeneration rate;On the other hand particle buildup and diauxic growth bring performance instability problem also be can solve.
Detailed description of the invention
Fig. 1 is the preparation flow figure of sensor substrate;
Fig. 2 is the preparation flow figure of single-particle gas sensor;
Fig. 3 is that the SEM of polymer fiber sacrificial layer schemes.
Specific embodiment
The present invention provides a kind of preparation method of single particle sensitive gas sensor, include the following steps (such as Fig. 2 institute
Show):
Sensor substrate is provided;
Single-particle is deposited in the sensor substrate surface using single-particle prize law, single particle sensitive layer is formed, obtains
To single particle sensitive gas sensor presoma;
The single particle sensitive gas sensor presoma is made annealing treatment, single particle sensitive gas biography is obtained
Sensor.
In the present invention, if without specified otherwise, all raw materials are commercial product well known to those skilled in the art.
The present invention provides sensor substrate.In the present invention, the preparation method of the sensor substrate preferably includes following
Step:
After being sequentially depositing polymer fiber sacrificial layer and electrode material layer in sensor base, removal polymer fiber is sacrificial
Domestic animal layer, obtains sensor substrate (as shown in Figure 1).In the present invention, the sensor base is preferably silicon wafer, the nitrogen after aoxidizing
Silicon wafer, quartz glass plate or alumina ceramic plate after change.
In the present invention, the process of deposition polymerization fibres sacrificial layer preferably includes following steps in sensor base:
Polymer and solvent are mixed, electrospun solution is obtained;
The electrospun solution is placed in syringe, is deposited in sensor base using the orderly electrostatic spinning of electric field-assisted
Polymer fiber sacrificial layer.
The present invention mixes polymer and solvent, obtains electrospun solution.In the present invention, the polymer is preferably poly- second
Alkene pyrrolidone and/or polyvinyl alcohol;When the polymer is two kinds in above-mentioned specific choice, the present invention is to described specific
The no any special restriction of proportion of substance, is mixed by any proportion.In the present invention, the solvent is preferably
One or more of ethyl alcohol, deionized water and N,N-dimethylformamide (DMF);When the solvent is in above-mentioned specific choice
It is two or more when, proportion no any special restriction of the present invention to the specific substance is mixed by any proportion
?.
In the present invention, the quality of the polymer and the volume ratio of the solvent are preferably (0.1~1) g:(1~10)
ML, more preferably (0.2~0.8) g:(2~8) mL, most preferably (0.4~0.6) g:(4~6) mL.
In the present invention, the mixing preferably carries out under stirring conditions;The stirring is preferably in magnetic stirring apparatus
It carries out.The present invention carries out the no any special restriction of stirring using whipping process well known to those skilled in the art
It stirs and is uniformly mixed each component.
After obtaining electrospun solution, the electrospun solution is placed in syringe by the present invention, utilizes the orderly electrostatic of electric field-assisted
Spinning deposition polymerization fibres sacrificial layer in sensor base.In the present invention, the electric field-assisted orderly electrostatic spinning
Parallel pole voltage is preferably -0.1~1kV, more preferably 0.2~0.8kV, most preferably 0.4~0.6kV;The parallel electricity
The spacing of pole is preferably 0.5~1cm.In the present invention, the syringe needle of the syringe and the spacing of sensor base be preferably 5~
15cm, more preferably 8~12cm;Voltage between the syringe needle and sensor base of the syringe is preferably 5~20kV, more preferably
For 10~15kV;The syringe is preferably 0.1~0.5mL/h for flow quantity, more preferably 0.2~0.4mL/h.
In the present invention, the ordered arrangement in sensor base of the polymer fiber in the polymer fiber sacrificial layer
(as shown in Figure 3).
In sensor base after deposition polymerization fibres sacrificial layer, present invention preferably employs physical vaporous depositions poly-
Close deposition of electrode material layer on fibres sacrificial layer;The physical vaporous deposition is preferably magnetron sputtering method or thermal evaporation;
The present invention does not have any special restriction to the detailed process of the magnetron sputtering method or thermal evaporation, using those skilled in the art
Magnetron sputtering method known to member or thermal evaporation are deposited.
In the present invention, the electrode material layer preferably includes bottoming metal layer and conductive metal layer;The conductive metal
The material of layer is preferably gold and/or platinum;One of more preferably above-mentioned specific material;The material of the bottoming metal layer is preferred
For tantalum.In the present invention, the thickness of the conductive metal layer is preferably 50~250nm, more preferably 50~100nm, most preferably
For 50~80nm;The thickness of the bottoming metal layer is preferably 5~25nm, more preferably 5~10nm.
In the present invention, the electrode material layer preferably includes two metal block areas;Two metal block area is in the horizontal direction
The spacing of upper arrangement, two metal block area is preferably 10~500nm, more preferably 50~300nm, most preferably 100~
200nm。
In the present invention, the process of the removal polymer fiber sacrificial layer is preferably by the lining after deposition of electrode material layer
Bottom is placed in deionized water, carries out ultrasound;In the present invention, the power of the ultrasound it is preferred > 40W, more preferably > 80W, most preferably
>100W;The present invention does not have any special restriction to the time of the ultrasound, makes polymer fiber sacrificial layer and its adhesion metal
(being deposited on the part for needing to remove on sacrificial layer) can be completely removed.
It is prepared after sensor substrate, the present invention is deposited using single-particle prize law in the sensor substrate surface
Single-particle obtains single particle sensitive gas sensor presoma.In the present invention, the process of the single-particle prize law is preferred
Are as follows:
Sensor substrate is placed in single-particle dispersion liquid, voltage is applied, single-particle capture is carried out in sensor substrate.
In the present invention, the preparation method of the single-particle dispersion liquid preferably mixes single-particle material and solvent, obtains
To single-particle dispersion liquid.In the present invention, the single-particle material is preferably metal oxide or metal sulfide;The metal
Oxide can be selected specifically to ZnO, SnO2、Co3O4Or CuO;The metal sulfide can be selected specifically to ZnS or PbS.
In the present invention, the solvent is preferably one or more of water, n,N-Dimethylformamide and toluene;When the solvent is
When two or more in above-mentioned specific choice, proportion no any special restriction of the present invention to the specific substance, by appointing
Meaning proportion is mixed.In the present invention, the mixing preferably carries out under conditions of ultrasound;In the present invention, described
Ultrasound power it is preferred > 40W, more preferably > 80W, most preferably > 100W;It is any special that the present invention does not have the time of the ultrasound
Restriction, using ultrasonic time well known to those skilled in the art carry out ultrasound and make single-particle homogeneous dispersion mix.
In the present invention, the ultrasound carries out preferably in supersonic cleaning machine.
In the present invention, the concentration of the single-particle dispersion liquid is preferably 0.0001~1g/mL, more preferably 0.001~
0.1g/mL, most preferably 0.01~0.05g/mL.
In the present invention, the voltage is preferably 10~1000V, more preferably 200~800V, most preferably 400~
600V。
In the present invention, the single-particle prize law preferably passes through the progress of particle electrostatic capture device;The particle electrostatic
Acquisition equipment preferably includes DC power supply and gauge outfit;The two poles of the earth of the DC power supply are separately connected two of sensor substrate electrode
Metal block area.
In the present invention, when gauge outfit has electric current to flow through, particle-capture process terminates.
After obtaining single particle sensitive gas sensor presoma, the present invention is by the single particle sensitive gas sensor
Presoma is made annealing treatment, and single particle sensitive gas sensor is obtained.In the present invention, the temperature of the annealing is excellent
>=300 DEG C of choosing, more preferably >=400 DEG C, most preferably >=500 DEG C;Time of the annealing preferably >=1h, more preferably
>=2h, most preferably >=4h.In the present invention, contact of the single particle with electrode can be enhanced in the annealing, can also be with
Stablize the property of sensitive material.
The present invention also provides the single particle sensitive gas biographies that the preparation method described in above-mentioned technical proposal is prepared
Sensor;The single particle sensitive gas sensor includes sensor substrate and single particle sensitive layer.
The present invention also provides the single particle sensitive gas sensors in detection inorganic gas or organic gas
Using.
Below with reference to embodiment to a kind of single particle sensitive gas sensor provided by the invention and preparation method thereof and
Using being described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
0.8g polyvinylpyrrolidone and 10mL ethyl alcohol are mixed, are stirred in magnetic stirring apparatus uniform to being formed
Solution obtains electrospun solution;
The electrospun solution is placed in syringe, using the orderly method of electrostatic spinning of electric field-assisted on the silicon wafer after nitridation
Deposit the polyvinyl pyrrolidone fibers sacrificial layer (condition of the orderly method of electrostatic spinning of electric field-assisted: syringe of ordered arrangement
The spacing of syringe needle and silicon wafer is 10cm, voltage 11kV;Syringe is 0.3mL/h for flow quantity;The parallel pole electricity of electric field
Pressure is 0.5kV, and the spacing of parallel pole is 1cm);
Bottoming metal tantalum (with a thickness of 5nm) and golden (with a thickness of 50nm), formation electrode material are sequentially depositing using magnetron sputtering
The bed of material;
By the above-mentioned sensor base for being deposited with polyvinyl pyrrolidone fibers sacrificial layer and electrode material layer be placed in from
In sub- water, ultrasound is carried out under conditions of supersonic frequency is 60W, until polyvinyl pyrrolidone fibers sacrificial layer and adhesion metal
It is completely removed, obtains sensor substrate;
0.3gZnO and 10mL water is mixed, is ultrasonically treated under conditions of 60W, until forming uniform single-particle point
Dispersion liquid;
The sensor substrate is placed in above-mentioned single-particle dispersion liquid, is applied voltage (1000V), in sensor substrate
Single-particle capture is carried out, single particle sensitive gas sensor presoma is obtained;
The single particle sensitive gas sensor presoma is annealed 4h under conditions of 500 DEG C, obtains single particle
Sensitive gas sensor.
Embodiment 2
0.6g polyvinyl alcohol and 10mL ethyl alcohol are mixed, are stirred in magnetic stirring apparatus to the uniform solution of formation,
Obtain electrospun solution;
The electrospun solution is placed in syringe, using the orderly method of electrostatic spinning of electric field-assisted on the silicon wafer after nitridation
Deposit ordered arrangement vinal sacrificial layer (condition of the orderly method of electrostatic spinning of electric field-assisted: the syringe needle of syringe with
The spacing of silicon wafer is 13cm, voltage 10.5kV;Syringe is 0.2mL/h for flow quantity;The parallel pole voltage of electric field be-
0.1kV, the spacing of parallel pole are 0.5cm);
It is sequentially depositing bottoming metal tantalum (with a thickness of 10nm) and platinum using magnetron sputtering (with a thickness of 100nm);
The above-mentioned sensor base for being deposited with vinal sacrificial layer and electrode material layer is placed in deionized water,
Ultrasound is carried out under conditions of supersonic frequency is 100W, until polyethylene fibre sacrificial layer and adhesion metal are completely removed, is obtained
To sensor substrate;
0.1gZnS and 10mL water is mixed, is ultrasonically treated under conditions of 100W, until forming uniform single-particle point
Dispersion liquid;
The sensor substrate is placed in above-mentioned single-particle dispersion liquid, is applied voltage (500V), in sensor substrate
Single-particle capture is carried out, single particle sensitive gas sensor presoma is obtained;
The single particle sensitive gas sensor presoma is annealed 3h under conditions of 400 DEG C, obtains single particle
Sensitive gas sensor.
As seen from the above embodiment, preparation method provided by the invention is simple, at low cost;It is prepared into the preparation method
The single particle sensitive gas sensor arrived can be to avoid particle buildup and particle growth, to give full play to the knot of nanoparticle
On the one hand structure advantage is capable of increasing specific surface area, improves sensitivity, helps to improve gas in adsorption and desorption process
Response regeneration rate;On the other hand particle buildup and diauxic growth bring performance instability problem also be can solve.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of single particle sensitive gas sensor, comprising the following steps:
Sensor substrate is provided;
Single-particle is deposited on the surface of the sensor substrate using single-particle prize law, single particle sensitive layer is formed, obtains
Single particle sensitive gas sensor presoma;
The single particle sensitive gas sensor presoma is made annealing treatment, single particle sensitive gas sensing is obtained
Device.
2. preparation method as described in claim 1, which is characterized in that the preparation method of the sensor substrate, including it is following
Step:
After being sequentially depositing polymer fiber sacrificial layer and electrode material layer in sensor base, polymer fiber sacrifice is removed
Layer, obtains sensor substrate.
3. preparation method as claimed in claim 2, which is characterized in that the polymer of the polymer fiber sacrificial layer is poly- second
Alkene pyrrolidone and/or polyvinyl alcohol.
4. preparation method as claimed in claim 2 or claim 3, which is characterized in that the electrode material layer include bottoming metal layer and
Conductive metal layer;
The material of the conductive metal layer is gold and/or platinum;The material of the bottoming metal layer is tantalum;
The conductive metal layer with a thickness of 50~250nm;The bottoming metal layer with a thickness of 5~25nm.
5. preparation method as claimed in claim 4, which is characterized in that the electrode material layer includes two metal block areas;
The spacing in two metal block area is 10~500nm.
6. preparation method as described in claim 1, which is characterized in that the process of the single-particle prize law are as follows: by sensor
Substrate is placed in single-particle dispersion liquid, applies voltage, and single-particle capture is carried out in sensor substrate;
The single-particle of the single-particle dispersion liquid is metal oxide or metal sulfide;
The concentration of the single-particle dispersion liquid is 0.0001~1g/mL.
7. preparation method as claimed in claim 6, which is characterized in that the voltage is 10~1000V.
8. preparation method as described in claim 1, which is characterized in that temperature >=300 DEG C of the annealing, the annealing when
Between >=1h.
9. the single particle sensitive gas sensor that preparation method according to any one of claims 1 to 8 is prepared.
10. application of the single particle sensitive gas sensor as claimed in claim 9 in detection inorganic gas or organic gas.
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