CN110031512B - Single particle sensitive gas sensor and preparation method and application thereof - Google Patents
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Abstract
The invention relates to the technical field of gas sensors, in particular to a single particle sensitive gas sensor and a preparation method and application thereof, and the preparation method of the single particle sensitive gas sensor provided by the invention comprises the following steps: providing a sensor substrate; depositing single particles on the surface of the sensor substrate by adopting a single particle capture method to obtain a precursor of the single particle sensitive gas sensor; and annealing the precursor of the single particle sensitive gas sensor to obtain the single particle sensitive gas sensor. The preparation method has low cost and simple operation; the single particle sensitive gas sensor prepared by the preparation method can avoid particle aggregation and particle growth, thereby fully exerting the structural advantages of the nano particles, increasing the specific surface area, improving the sensitivity and being beneficial to the response recovery rate of gas in the processes of surface adsorption and desorption; the problem of instability caused by particle aggregation and secondary growth can be solved.
Description
Technical Field
The invention relates to the technical field of gas sensors, in particular to a single particle sensitive gas sensor and a preparation method and application thereof.
Background
The nano material has the characteristics of large specific surface area, rich surface defects and the like, and is widely applied to gas sensors. Generally, a semiconductor gas sensor is required to work at a higher temperature, but the continuous high-temperature work can damage the crystal structure of a semiconductor material, so that the performance of the sensor is unstable.
At present, ultraviolet enhancement and inhibition of sensitive particle growth are common ways for improving the problems, wherein ultraviolet enhancement mainly adopts a way of exciting a sensitive material by ultraviolet light to replace a way of thermally exciting the material by a heating element, and the way can improve the normal-temperature gas-sensitive property and the normal-temperature conductivity of the sensitive material; but the response recovery time is as high as several to tens of minutes, and the sensitivity is greatly reduced. Meanwhile, the inhibition of the growth of a single sensitive particle is mainly realized by preparing a hierarchical structure, but the operations from the preparation of the hierarchical structure to the preparation of the sensor, such as spin coating or coating, are needed to form a sensitive material thin film layer, and the sensitive material thin film layer usually forms a compact film due to the aggregation of the particles, which is not beneficial to the improvement and the stability of the gas-sensitive performance of the sensor.
On the basis, the prior art solves the problem of growth of single sensitive particles by preparing a single nano particle to construct a gas sensor; in the process of preparing a single nano particle gas sensor, the electrode deposition control is mainly realized by utilizing focused ion beam deposition, or the sensitive material control is realized by utilizing a contact atomic force microscope, so that the contact between the sensitive material and the electrode is realized, but the equipment used by the method is expensive and the operation is complex.
Disclosure of Invention
The invention aims to provide a preparation method of a single particle sensitive gas sensor, which is simple and low in cost.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a single particle sensitive gas sensor, which comprises the following steps:
providing a sensor substrate;
depositing single particles on the surface of the sensor substrate by adopting a single particle capture method to form a single particle sensitive layer, and obtaining a precursor of the single particle sensitive gas sensor;
and annealing the precursor of the single particle sensitive gas sensor to obtain the single particle sensitive gas sensor.
Preferably, the preparation method of the sensor substrate comprises the following steps:
and after the polymer fiber sacrificial layer and the electrode material layer are sequentially deposited on the sensor substrate, removing the polymer fiber sacrificial layer to obtain the sensor substrate.
Preferably, the polymer of the polymer fiber sacrificial layer is polyvinylpyrrolidone and/or polyvinyl alcohol.
Preferably, the electrode material layer comprises a base metal layer and a conductive metal layer;
the conductive metal layer is made of gold and/or platinum; the material of the underlying metal layer is tantalum;
the thickness of the conductive metal layer is 50-250 nm; the thickness of the underlying metal layer is 5-25 nm.
Preferably, the electrode material layer comprises two metal block regions;
the distance between the two metal block areas is 10-500 nm.
Preferably, the single particle capture method comprises the following steps: placing a sensor substrate in the single-particle dispersion liquid, applying voltage, and capturing single particles on the sensor substrate;
the single particles of the single particle dispersion liquid are metal oxides or metal sulfides;
the concentration of the single particle dispersion is 0.0001-1 g/mL.
Preferably, the voltage is 10-1000V.
Preferably, the annealing temperature is more than or equal to 300 ℃, and the annealing time is more than or equal to 1 h.
The invention also provides the single particle sensitive gas sensor prepared by the preparation method in the technical scheme.
The invention also provides the application of the single particle sensitive gas sensor in detecting inorganic gas or organic gas.
The invention provides a preparation method of a single particle sensitive gas sensor, which comprises the following steps: providing a sensor substrate; depositing single particles on the surface of the sensor substrate by adopting a single particle capture method to obtain a precursor of the single particle sensitive gas sensor; and annealing the precursor of the single particle sensitive gas sensor to obtain the single particle sensitive gas sensor. The preparation method has low cost and simple operation; the single particle sensitive gas sensor prepared by the preparation method can avoid particle aggregation and particle growth, thereby fully playing the structural advantages of the nano particles, on one hand, the specific surface area can be increased, the sensitivity is improved, and the response recovery rate of gas in the surface adsorption and desorption processes is improved; on the other hand, the problem of unstable performance caused by particle aggregation and secondary growth can be solved.
Drawings
FIG. 1 is a flow chart of the preparation of a sensor substrate;
FIG. 2 is a flow chart of the preparation of a single particle gas sensor;
fig. 3 is an SEM image of a polymer fiber sacrificial layer.
Detailed Description
The invention provides a preparation method of a single particle sensitive gas sensor, which comprises the following steps (as shown in figure 2):
providing a sensor substrate;
depositing single particles on the surface of the sensor substrate by adopting a single particle capture method to form a single particle sensitive layer, and obtaining a precursor of the single particle sensitive gas sensor;
and annealing the precursor of the single particle sensitive gas sensor to obtain the single particle sensitive gas sensor.
In the present invention, all the raw materials are commercially available products well known to those skilled in the art unless otherwise specified.
The invention provides a sensor substrate. In the present invention, the method for manufacturing the sensor substrate preferably includes the steps of:
after a polymer fiber sacrificial layer and an electrode material layer are sequentially deposited on the sensor substrate, the polymer fiber sacrificial layer is removed, and a sensor substrate is obtained (as shown in fig. 1). In the present invention, the sensor substrate is preferably an oxidized silicon wafer, a nitrided silicon wafer, a quartz glass wafer, or an alumina ceramic wafer.
In the present invention, the process of depositing the polymer fiber sacrificial layer on the sensor substrate preferably comprises the steps of:
mixing a polymer and a solvent to obtain an electrospinning solution;
and (3) placing the electrospinning solution into a syringe, and depositing a polymer fiber sacrificial layer on the sensor substrate by using electric field assisted ordered electrospinning.
According to the invention, the polymer and the solvent are mixed to obtain the electrospinning solution. In the present invention, the polymer is preferably polyvinylpyrrolidone and/or polyvinyl alcohol; when the polymers are two of the above specific choices, the invention does not have any special limitation on the proportion of the specific substances, and the specific substances can be mixed according to any proportion. In the invention, the solvent is preferably one or more of ethanol, deionized water and N, N-Dimethylformamide (DMF); when the solvent is more than two of the above specific choices, the invention has no special limitation on the proportion of the specific substances, and the specific substances can be mixed according to any proportion.
In the present invention, the ratio of the mass of the polymer to the volume of the solvent is preferably (0.1 to 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 is preferably performed under stirring; the stirring is preferably carried out in a magnetic stirrer. The stirring is not particularly limited in the present invention, and the stirring process known to those skilled in the art is adopted to stir and mix the components uniformly.
After the electrospinning solution is obtained, the electrospinning solution is placed in an injector, and the polymer fiber sacrificial layer is deposited on the sensor substrate by utilizing electric field-assisted ordered electrostatic spinning. In the invention, the voltage of the parallel electrode of the electric field assisted ordered electrostatic spinning is preferably-0.1-1 kV, more preferably 0.2-0.8 kV, and most preferably 0.4-0.6 kV; the distance between the parallel electrodes is preferably 0.5-1 cm. In the invention, the distance between the needle head of the injector and the sensor substrate is preferably 5-15 cm, and more preferably 8-12 cm; the voltage between the needle head of the injector and the sensor substrate is preferably 5-20 kV, and more preferably 10-15 kV; the liquid supply flow rate of the injector is preferably 0.1-0.5 mL/h, and more preferably 0.2-0.4 mL/h.
In the present invention, the polymer fibers in the polymer fiber sacrificial layer are arranged on the sensor substrate (as shown in fig. 3).
After depositing the polymer fiber sacrificial layer on the sensor substrate, the invention preferably adopts a physical vapor deposition method to deposit an electrode material layer on the polymer fiber sacrificial layer; the physical vapor deposition method is preferably a magnetron sputtering method or a thermal evaporation method; the present invention does not have any particular limitation on the specific process of the magnetron sputtering method or the thermal evaporation method, and the deposition can be performed by the magnetron sputtering method or the thermal evaporation method which are well known to those skilled in the art.
In the present invention, the electrode material layer preferably includes a primer metal layer and a conductive metal layer; the material of the conductive metal layer is preferably gold and/or platinum; more preferably one of the above specific materials; the material of the underlying metal layer is preferably tantalum. In the invention, the thickness of the conductive metal layer is preferably 50-250 nm, more preferably 50-100 nm, and most preferably 50-80 nm; the thickness of the bottom metal layer is preferably 5-25 nm, and more preferably 5-10 nm.
In the present invention, the electrode material layer preferably includes two metal block regions; the two metal block regions are arranged in the horizontal direction, and the distance between the two metal block regions is preferably 10-500 nm, more preferably 50-300 nm, and most preferably 100-200 nm.
In the invention, the process of removing the polymer fiber sacrificial layer is preferably to place the substrate after the electrode material layer is deposited in deionized water and carry out ultrasonic treatment; in the present invention, the power of the ultrasound is preferably >40W, more preferably >80W, most preferably > 100W; the invention does not have any special limitation on the time of the ultrasonic treatment, and the polymer fiber sacrificial layer and the attached metal (the part needing to be removed and deposited on the sacrificial layer) can be completely removed.
After the sensor substrate is prepared, the single particle capture method is adopted to deposit single particles on the surface of the sensor substrate, and a precursor of the single particle sensitive gas sensor is obtained. In the present invention, the single particle capture method preferably comprises the following steps:
and (3) placing the sensor substrate in the single particle dispersion liquid, applying voltage, and capturing single particles on the sensor substrate.
In the present invention, the single particle dispersion is preferably prepared by mixing a single particle material and a solvent to obtain a single particle dispersion. In the present invention, the single particle material is preferably a metal oxide or a metal sulfide; the metal oxide can be selected from ZnO and SnO2、Co3O4Or CuO; the metal sulfide may be specifically selected to be ZnS or PbS. In the invention, the solvent is preferably one or more of water, N-dimethylformamide and toluene; when the solvent is more than two of the above specific choices, the invention has no special limitation on the proportion of the specific substances, and the specific substances can be mixed according to any proportion. In the present invention, the mixing is preferably performed under the condition of ultrasound; in the present invention, the power of the ultrasound is preferably>40W, more preferably>80W, most preferably>100W; the time of the ultrasonic treatment is not limited in any way, and the ultrasonic treatment is carried out by adopting the ultrasonic time known by the technical personnel in the field and uniformly mixing the single particle dispersion liquid. In the present invention, the ultrasonication is preferably carried out in an ultrasonic cleaning machine.
In the present invention, the concentration of the single particle dispersion is preferably 0.0001 to 1g/mL, more preferably 0.001 to 0.1g/mL, and most preferably 0.01 to 0.05 g/mL.
In the present invention, the voltage is preferably 10 to 1000V, more preferably 200 to 800V, and most preferably 400 to 600V.
In the present invention, the single particle capturing method is preferably performed by a particle electrostatic capturing device; the particle electrostatic capturing device preferably comprises a direct current power supply and a gauge head; two poles of the direct current power supply are respectively connected with two metal block regions of the sensor substrate electrode.
In the present invention, the particle trapping process ends when current flows through the head of the meter.
After the precursor of the single particle sensitive gas sensor is obtained, the precursor of the single particle sensitive gas sensor is annealed to obtain the single particle sensitive gas sensor. In the present invention, the temperature of the annealing treatment is preferably not less than 300 ℃, more preferably not less than 400 ℃, and most preferably not less than 500 ℃; the time of the annealing treatment is preferably not less than 1 hour, more preferably not less than 2 hours, and most preferably not less than 4 hours. In the present invention, the annealing treatment can enhance the contact of the single particles with the electrode and can also stabilize the properties of the sensitive material.
The invention also provides a single particle sensitive gas sensor prepared by the preparation method in the technical scheme; the single particle sensitive gas sensor includes a sensor substrate and a single particle sensitive layer.
The invention also provides application of the single particle sensitive gas sensor in detecting inorganic gas or organic gas.
The following detailed description of the single particle sensitive gas sensor and its preparation method and application will be made with reference to the examples, but they should not be construed as limiting the scope of the invention.
Example 1
Mixing 0.8g of polyvinylpyrrolidone with 10mL of ethanol, and stirring in a magnetic stirrer until a uniform solution is formed to obtain an electrospinning solution;
placing the electrospinning solution in an injector, and depositing orderly-arranged polyvinylpyrrolidone fiber sacrificial layers on the nitrided silicon wafer by using an electric field-assisted ordered electrospinning method (under the condition of the electric field-assisted ordered electrospinning method, the distance between a needle head of the injector and the silicon wafer is 10cm, the voltage is 11kV, the liquid supply flow of the injector is 0.3mL/h, the voltage of parallel electrodes of an electric field is 0.5kV, and the distance between the parallel electrodes is 1 cm);
sequentially depositing base metal tantalum (with the thickness of 5nm) and gold (with the thickness of 50nm) by magnetron sputtering to form an electrode material layer;
placing the sensor substrate deposited with the polyvinylpyrrolidone fiber sacrificial layer and the electrode material layer in deionized water, and carrying out ultrasonic treatment under the ultrasonic frequency of 60W until the polyvinylpyrrolidone fiber sacrificial layer and the attached metal are completely removed to obtain a sensor substrate;
mixing 0.3g of ZnO with 10mL of water, and carrying out ultrasonic treatment under the condition of 60W until uniform single particle dispersion liquid is formed;
placing the sensor substrate in the single particle dispersion, applying voltage (1000V), and performing single particle capture on the sensor substrate to obtain a precursor of the single particle sensitive gas sensor;
and annealing the precursor of the single particle sensitive gas sensor for 4 hours at 500 ℃ to obtain the single particle sensitive gas sensor.
Example 2
Mixing 0.6g of polyvinyl alcohol and 10mL of ethanol, and stirring in a magnetic stirrer until a uniform solution is formed to obtain an electrospinning solution;
placing the electrospinning solution in an injector, and depositing orderly-arranged polyvinyl alcohol fiber sacrificial layers on the nitrided silicon wafer by using an electric field assisted ordered electrospinning method (the conditions of the electric field assisted ordered electrospinning method are that the distance between a needle head of the injector and the silicon wafer is 13cm, the voltage is 10.5kV, the liquid supply flow of the injector is 0.2mL/h, the voltage of parallel electrodes of an electric field is-0.1 kV, and the distance of the parallel electrodes is 0.5 cm);
sequentially depositing a base metal tantalum (with the thickness of 10nm) and platinum (with the thickness of 100nm) by magnetron sputtering;
placing the sensor substrate deposited with the polyvinyl alcohol fiber sacrificial layer and the electrode material layer in deionized water, and carrying out ultrasonic treatment under the condition that the ultrasonic frequency is 100W until the polyethylene fiber sacrificial layer and the attached metal are completely removed to obtain a sensor substrate;
mixing 0.1g of ZnS and 10mL of water, and carrying out ultrasonic treatment under the condition of 100W until a uniform single particle dispersion liquid is formed;
placing the sensor substrate in the single particle dispersion, applying voltage (500V), and performing single particle capture on the sensor substrate to obtain a precursor of the single particle sensitive gas sensor;
and annealing the precursor of the single particle sensitive gas sensor for 3h at the temperature of 400 ℃ to obtain the single particle sensitive gas sensor.
The preparation method provided by the invention is simple and low in cost; the single particle sensitive gas sensor prepared by the preparation method can avoid particle aggregation and particle growth, thereby fully playing the structural advantages of the nano particles, on one hand, the specific surface area can be increased, the sensitivity is improved, and the response recovery rate of gas in the surface adsorption and desorption processes is improved; on the other hand, the problem of unstable performance caused by particle aggregation and secondary growth can be solved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. A method of making a single particle sensitive gas sensor comprising the steps of:
providing a sensor substrate;
depositing single particles on the surface of the sensor substrate by adopting a single particle capture method to form a single particle sensitive layer, and obtaining a precursor of the single particle sensitive gas sensor;
annealing the precursor of the single particle sensitive gas sensor to obtain the single particle sensitive gas sensor;
the preparation method of the sensor substrate comprises the following steps:
after a polymer fiber sacrificial layer and an electrode material layer are sequentially deposited on a sensor substrate, removing the polymer fiber sacrificial layer to obtain the sensor substrate;
the electrode material layer comprises a bottom metal layer and a conductive metal layer;
the conductive metal layer is made of gold and/or platinum; the material of the underlying metal layer is tantalum;
the thickness of the conductive metal layer is 50-250 nm; the thickness of the underlying metal layer is 5-25 nm;
the electrode material layer comprises two metal block regions; the two metal block regions are arranged in the horizontal direction; the distance between the two metal block areas is 10-500 nm;
the single particle capture method is carried out in an ion static capture device, and the particle static capture device comprises a direct current power supply and a gauge outfit; two poles of the direct current power supply are respectively connected with two metal block regions of the sensor substrate electrode;
the single particle capture method comprises the following steps: placing a sensor substrate in the single-particle dispersion liquid, applying voltage, performing single-particle capture on the sensor substrate, and finishing the particle capture process when current flows through a meter head;
the single particles of the single particle dispersion liquid are metal oxides or metal sulfides;
the concentration of the single particle dispersion liquid is 0.0001-1 g/mL;
the voltage is 10-1000V.
2. The method of claim 1, wherein the polymer of the polymer fiber sacrificial layer is polyvinylpyrrolidone and/or polyvinyl alcohol.
3. The preparation method according to claim 1, wherein the annealing temperature is equal to or higher than 300 ℃ and the annealing time is equal to or higher than 1 h.
4. A single particle sensitive gas sensor prepared by the preparation method of any one of claims 1 to 3.
5. Use of a single particle sensitive gas sensor as claimed in claim 4 for detecting inorganic or organic gases.
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