CN110845152A - Surface acoustic wave gas sensor of modified colloidal quantum dot film and preparation method thereof - Google Patents
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Abstract
The invention discloses a surface acoustic wave gas sensor of a modified colloidal quantum dot film and a preparation method thereof, wherein the method comprises the following steps: A. providing a surface acoustic wave delay line, and coating a colloidal quantum dot solution on a delay area of the surface acoustic wave delay line to form a colloidal quantum dot film; B. and irradiating the colloidal quantum dot film by adopting an ion beam or plasma to obtain the surface acoustic wave gas sensor of the modified colloidal quantum dot film. According to the invention, the colloid quantum dot film is irradiated by the ion beam or the plasma, so that residual long-chain oleic acid and residual oleylamine in the colloid quantum dot film can be removed, the porosity of the colloid quantum dot film is improved, the specific surface area of the colloid quantum dot film is increased, the contact area of the colloid quantum dot and the detected gas is increased, the gas-sensitive response of the colloid quantum dot surface acoustic wave gas sensor is greatly improved, the high sensitivity and the rapid detection at the sub-ppm level can be realized, and the colloid quantum dot surface acoustic wave gas sensor has a wide application prospect in the aspect of bionic olfaction of an intelligent sensor.
Description
Technical Field
The invention relates to the technical field of intelligent sensors, in particular to a surface acoustic wave gas sensor of a modified colloidal quantum dot film and a preparation method thereof
Background
The Surface Acoustic Wave (SAW) sensing technology is one of the popular technologies in the wireless sensor technology, does not need a power supply, utilizes the high-frequency characteristic of a SAW device and the piezoelectric characteristic of a substrate, receives a radio wave signal through an antenna, converts the radio wave signal into a surface acoustic wave signal, transmits the surface acoustic wave signal on the sensor, and converts the processed surface acoustic wave signal into the radio wave signal again to be transmitted back.
A sensitive film for selectively identifying gas molecules is coated on a propagation path of the SAW device to form the SAW gas sensor, and the changes of mass, conductance or elastic parameters before and after the sensitive film adsorbs gas are utilized to influence the propagation of surface acoustic waves (wave velocity or phase position), so that the passive wireless detection of target gas is realized.
One of the key technologies in the research of SAW gas sensors is the analysis of the sensing mechanism and the preparation of sensitive thin film materials of the detection interface of the sensor. Therefore, the preparation and development of highly sensitive gas-sensitive materials become a research hotspot of the SAW gas sensor in the past decades. However, the existing sensitive film material has the problems of low sensitivity, overlong response recovery time and the like in the practical application process, and the practical application of the sensitive film material is limited. Therefore, the SAW gas sensor with high sensitivity and quick response is developed, and has very important significance and wide market prospect.
The colloidal quantum dot is a zero-dimensional inorganic semiconductor nano material, and the particle size of the nano particle is smaller than or close to the exciton Bohr radius, so that a series of novel physicochemical effects are shown. The colloidal quantum dots have higher specific surface area, can provide a large number of active sites for adsorbing target gas molecules, and simultaneously, the grain size of the colloidal quantum dots is similar to the Debye length, thereby being beneficial to the rapid transfer of charges and accelerating the response speed of the gas. The characteristics are favorable for the application of the colloidal quantum dots in a high-performance gas sensor, and a novel surface acoustic wave gas sensor based on the colloidal quantum dot film can be manufactured. However, long-chain oleic acid and oleylamine are generally needed in the synthesis process of the colloidal quantum dots, and although a part of high-molecular oleic acid and oleylamine can be removed in the treatment process after film formation by cleaning and heating, a part of long-chain high-molecular oleic acid and oleylamine still exist to wrap around the colloidal quantum dots, so that the contact between the colloidal quantum dots and gas is blocked, and the gas-sensitive response cannot be further improved.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a surface acoustic wave gas sensor of modified colloidal quantum dots and a preparation method thereof, and aims to solve the problem of low gas-sensitive response of the existing surface acoustic wave gas sensor.
The technical scheme of the invention is as follows:
a method for preparing a surface acoustic wave gas sensor of a modified colloidal quantum dot film comprises the following steps:
A. providing a surface acoustic wave delay line, and coating a colloidal quantum dot solution on a delay area of the surface acoustic wave delay line to form a colloidal quantum dot film;
B. and irradiating the colloidal quantum dot film by adopting ion beams or plasmas to obtain the surface acoustic wave gas sensor of the modified colloidal quantum dots.
In the preparation method, in the step A, the colloidal quantum dot solution is obtained by dissolving one or more colloidal quantum dots in a solvent, and the colloidal quantum dots are prepared by a wet chemical method.
The preparation method is characterized in that the colloidal quantum dots are II-VI compounds, III-V compounds, IV-VI compounds or II-VI compounds.
The preparation method comprises the step of preparing the colloidal quantum dots by using a solvent, wherein the colloidal quantum dots are SnS, PbS, SnSe or PbSe.
In the preparation method, in the step a, the coating mode is selected from one of blade coating, spray coating, spin coating, drop coating and dip coating.
In the preparation method, in the step A, the surface acoustic wave delay line comprises a substrate, an input interdigital transducer and an output interdigital transducer which are convexly arranged on the substrate, and the delay area is an area between the input interdigital transducer and the output interdigital transducer.
In the preparation method, in the step B, the ion beam is an argon ion beam or a nitrogen ion beam, and the plasma is an oxygen plasma.
In the preparation method, in the step B, the energy of the ion beam or the plasma is 0.1-0.6KV, and/or the irradiation time is 1-10 s.
The preparation method is characterized in that the thickness of the colloidal quantum dot film is 0.1-1 μm.
A surface acoustic wave gas sensor of a modified colloidal quantum dot film is prepared by the preparation method.
Has the advantages that: according to the invention, the colloid quantum dot film is irradiated by the ion beam or the plasma, so that residual long-chain oleic acid and residual oleylamine in the colloid quantum dot film can be removed, the porosity of the colloid quantum dot film is improved, the specific surface area of the colloid quantum dot film is increased, the contact area of the colloid quantum dot and the detected gas is increased, the gas-sensitive response of the colloid quantum dot surface acoustic wave gas sensor is enhanced, the high sensitivity and the rapid detection at the sub-ppm level can be realized, and the colloid quantum dot surface acoustic wave gas sensor has a wide application prospect in the aspect of bionic olfaction of an intelligent sensor.
Drawings
Fig. 1 is a schematic structural diagram of a surface acoustic wave gas sensor with modified colloidal quantum dots according to embodiment 1 of the present invention.
Fig. 2 is an SEM image of the surface of the SnS colloidal quantum dot film without ion beam irradiation in example 1 of the present invention.
FIG. 3 is an SEM image of the surface of an SnS colloidal quantum dot film irradiated by 0.4kV argon ion beams in example 1 of the present invention.
FIG. 4 is a diagram showing a surface acoustic wave gas sensor pair with 2ppm of NO, which is a modified SnS colloidal quantum dot thin film obtained by irradiation of argon ion beams with different energy levels in embodiment 4 of the present invention2Transient response curve of gas.
Detailed Description
The invention provides a preparation method of a surface acoustic wave gas sensor of a modified colloidal quantum dot film, which is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a preparation method of a surface acoustic wave gas sensor of a modified colloidal quantum dot film, which comprises the following steps:
A. providing a surface acoustic wave delay line, and coating a colloidal quantum dot solution on a delay area of the surface acoustic wave delay line to form a colloidal quantum dot film;
B. and irradiating the colloidal quantum dot film by adopting ion beams or plasmas to obtain the surface acoustic wave gas sensor of the modified colloidal quantum dot film.
Specifically, in the step A, an input interdigital transducer and an output interdigital transducer are prepared on a substrate, a delay area is arranged between the input interdigital transducer and the output interdigital transducer to form a double-port surface acoustic wave delay line, a colloid quantum dot solution is coated on the delay area of the surface acoustic wave delay line, and after a solvent is volatilized, the colloid quantum dot film is washed twice by methanol to form the colloid quantum dot film.
In one embodiment, the colloidal quantum dot solution is obtained by dissolving one or more colloidal quantum dots in a solvent, and the colloidal quantum dots are prepared by a wet chemical method.
In one embodiment, the colloidal quantum dots may be, but are not limited to, group II-VI compounds, group III-V compounds, group IV-VI compounds, or group II-VI compounds. Further, the colloidal quantum dots may be, but are not limited to, SnS, PbS, SnSe, or PbSe.
In one embodiment, the coating may be selected from, but is not limited to, one of knife coating, spray coating, spin coating, drop coating, and dip coating.
Specifically, in the step B, the sensor coated with the colloidal quantum dot film is placed in an ion beam or plasma irradiation system, a mask technology is adopted to shield a non-to-be-irradiated area of the sensor, the ion beam or plasma irradiation energy and irradiation time are adjusted, and the colloidal quantum dot film in the delay area is irradiated by the ion beam or plasma, so that the surface acoustic wave gas sensor of the modified colloidal quantum dot film is prepared.
In the embodiment, the irradiation energy of the adopted ion beam/plasma is accurate and controllable, the environmental temperature is controllable during irradiation, the beam directivity is high, and the repeatability is good. The energy-carrying ion beam or plasma can be used for further removing residual long-chain oleic acid and oleylamine in the colloidal quantum dot film, the porosity of the colloidal quantum dot film is improved, the specific surface area of the colloidal quantum dot film is increased, the contact area of the colloidal quantum dot and the detected gas is increased, the gas-sensitive response of the colloidal quantum dot surface acoustic wave gas sensor is enhanced, high sensitivity and rapid detection at the sub-ppm level are realized, and the method has a wide application prospect in the bionic olfaction aspect of an intelligent sensor.
In one embodiment, the ion beam is an argon ion beam or a nitrogen ion beam and the plasma is an oxygen plasma.
In one embodiment, the ion beam or plasma has an energy of 0.1-0.6KV and/or the irradiation time is 1-10 s. Wherein, the residual long chain oleic acid and oleylamine molecules in the colloid quantum dot film cannot be removed due to too low irradiation energy of the ion beam or the plasma, and the colloid quantum dot film is damaged due to too high irradiation energy, so that the gas-sensitive response is poor; residual long-chain oleic acid and oleylamine molecules in the colloidal quantum dot film cannot be removed due to too short irradiation time of the ion beam or the plasma, and the colloidal quantum dot film is damaged due to too long irradiation energy or irradiation time, so that the gas-sensitive response is poor.
In one embodiment, the colloidal quantum dot thin film has a thickness of 0.1 to 1 μm. The film is too thin, the number of colloid quantum dots is small, and the sensitivity is low; the film is too thick to facilitate gas to enter the film to react with the colloidal quantum dots.
The embodiment of the invention provides a surface acoustic wave gas sensor of a modified colloidal quantum dot film, wherein the surface acoustic wave gas sensor is prepared by adopting the preparation method.
The preparation and performance of the surface acoustic wave gas sensor of the modified colloidal quantum dot film of the present invention are described in detail by several embodiments.
Example 1
(1) Preparation of SnS colloidal quantum dot solution
(1.1) Anhydrous tin chloride powder (SnCl)2380mg) was charged into a 50mL three-necked flask, evacuated, charged with 1-octadecene (1-ODE, 5mL), trioctylphosphine (TOP, 3mL) and oleic acid (OA, 4.5mL), heated to 60 deg.C, and magnetically stirred for 1h to obtain a precursor of Sn.
(1.2) Thioacetamide (TAA, 75mg), oleylamine (OLA, 5mL) and trioctylphosphine (TOP, 3mL) were added to a glass bottle to make the precursor of S.
(1.3) then raising the temperature of the Sn precursor to 100 ℃, quickly adding the S precursor prepared in the step (1.2) into a three-neck bottle, and magnetically stirring for 5min for reaction. And after the reaction is finished, washing the SnS quantum dots twice by using n-octane and absolute ethyl alcohol, setting the centrifugal rotation speed to be 8000r/min and the time to be 10min, and carrying out centrifugal separation to obtain the SnS colloidal quantum. And (3) dispersing the SnS colloidal quantum into n-octane to prepare a 100mg/mL SnS colloidal quantum dot solution.
(2) Preparation of surface acoustic wave gas sensor of modified SnS colloidal quantum dot film
(2.1) carrying out magnetron sputtering of an aluminum layer on an ST-cut quartz crystal (substrate), and preparing an input interdigital transducer (IDT) and an output interdigital transducer by adopting a traditional photoetching process; in this case, the periodicity of IDT was 15.8 μm and the thickness was 200 nm. A delay area is arranged between the input interdigital transducer and the output interdigital transducer, and the area of the delay area is 3.6mm2Forming a surface acoustic wave delay line; the SAW delay line has a center frequency of 200.02MHz and an insertion loss of-12.82 dB.
(2.2) adopting a spin coating mode, dropping the SnS colloidal quantum dot solution on a delay area of the surface acoustic wave delay line by using a pipette, adjusting the spin coating speed to be 2000r/min, rotating for 45s to form a SnS colloidal quantum dot film, after drying, washing twice by using pure methanol to remove residues, finally placing the SnS colloidal quantum dot film in an ion beam irradiation system, shielding the part except the SnS colloidal quantum dot film by adopting a mask technology, irradiating the surface of the SnS colloidal quantum dot film by adopting an argon ion beam with irradiation energy of 0.4kV, and obtaining the surface acoustic wave gas sensor of the modified colloidal quantum dot (SnS) film, wherein the structure of the surface acoustic wave gas sensor is shown in figure 1 and comprises the following steps: the device comprises an ST-cut quartz substrate 1, an input interdigital transducer 2, an output interdigital transducer 3 and SnS colloidal quantum dots 4.
(2.3) observing the morphology of the colloidal quantum dot film in the surface acoustic wave gas sensor of the modified SnS colloidal quantum dot film prepared in the above embodiment before and after irradiation by using a Scanning Electron Microscope (SEM), wherein the morphology of the SnS colloidal quantum dot film before irradiation is shown in fig. 2, and the morphology of the SnS colloidal quantum dot film after irradiation by using a 0.4kV argon ion beam is shown in fig. 3. Comparing fig. 2 and fig. 3, it can be seen that before the ion beam irradiation, the SnS quantum dot film is flat and dense, and at the same time, a part of the area is covered with long chain oleylamine and oleic acid molecules; after irradiation of 0.4kV argon ion beams, residual long-chain oleylamine and oleic acid molecules on the surface of the SnS colloidal quantum dot film are removed, and the surface becomes loose and porous.
Example 2
A surface acoustic wave gas sensor of a modified SnS colloidal quantum dot film was prepared according to the preparation procedure in example 1, except that the energy of the argon ion beam irradiation used was 0.2 kV.
Example 3
A surface acoustic wave gas sensor of a modified SnS colloidal quantum dot film was prepared according to the preparation procedure in example 1, except that the energy of the argon ion beam irradiation used was 0.6 kV.
Surface acoustic wave gas sensors using the modified SnS colloidal quantum dot films obtained by the preparation steps of example 1 without argon ion beam irradiation and the modified SnS colloidal quantum dot films obtained in examples 1 to 3 were used for 2ppm of NO, respectively2Testing the frequency drift amount of the gas; acoustic surface wave gas sensor pair with modified SnS colloidal quantum dot films and 2ppm of NO2The transient response curve of the gas is shown in fig. 4. Therefore, the maximum frequency drift amount of the SnS colloidal quantum dot film surface acoustic wave gas sensor without ion beam irradiation is 2.5 KHz. After the ion beams with the intensities of 0.2kV, 0.4kV and 0.6kV are adopted to irradiate the surface of the SnS colloid quantum dot film, the maximum frequency drift amounts of the sensors respectively reach 5.7KHz, 6.3KHz and 4.2KHz, and compared with the sensor which is not irradiated, the frequency drift amount of the sensor which is irradiated by the ion beams can be improved by 152 percent at most. Therefore, after ion beam irradiation treatment, the gas-sensitive response of the colloidal quantum dot film surface acoustic wave gas sensor is enhanced.
In conclusion, the colloid quantum dot film is irradiated by the ion beam or the plasma, residual long-chain oleic acid and residual oleylamine in the colloid quantum dot film can be further removed by utilizing the energy-carrying ion beam or the plasma, the porosity of the colloid quantum dot film is improved, the specific surface area of the colloid quantum dot film is increased, the contact area of the colloid quantum dot and the gas to be detected is increased, the gas-sensitive response of the colloid quantum dot surface acoustic wave gas sensor is enhanced, the high sensitivity and the quick detection of the sub-ppm level can be realized, and the colloid quantum dot surface acoustic wave gas sensor has wide application prospect in the bionic olfaction aspect of intelligent sensors.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A surface acoustic wave gas sensor of a modified colloid quantum dot film and a preparation method thereof are characterized by comprising the following steps:
A. providing a surface acoustic wave delay line, and coating a colloidal quantum dot solution on a delay area of the surface acoustic wave delay line to form a colloidal quantum dot film;
B. and irradiating the colloidal quantum dot film by adopting ion beams or plasmas to obtain the surface acoustic wave gas sensor of the modified colloidal quantum dot film.
2. The preparation method according to claim 1, wherein in the step A, the colloidal quantum dot solution is prepared by dissolving one or more colloidal quantum dots in a solvent, and the colloidal quantum dots are prepared by a wet chemical method.
3. The method of claim 2, wherein the colloidal quantum dot is a group II-VI compound, a group III-V compound, a group IV-VI compound, or a group II-VI compound.
4. The preparation method according to claim 2, wherein the colloidal quantum dot is SnS, PbS, SnSe or PbSe.
5. The method according to claim 1, wherein in step a, the coating is performed by one selected from blade coating, spray coating, spin coating, drop coating, and dip coating.
6. The manufacturing method according to claim 1, wherein in step a, the surface acoustic wave delay line includes a substrate, and an input interdigital transducer and an output interdigital transducer that are protruded on the substrate, and the delay region is a region between the input interdigital transducer and the output interdigital transducer.
7. The method according to claim 1, wherein in the step B, the ion beam is an argon ion beam or a nitrogen ion beam, and the plasma is an oxygen plasma.
8. The method according to claim 1, wherein in step B, the energy of the ion beam or plasma is 0.1-0.6KV, and/or the irradiation time is 1-10 s.
9. The method according to claim 1, wherein the colloidal quantum dot film has a thickness of 0.1 to 1 μm.
10. A surface acoustic wave gas sensor of a modified colloidal quantum dot film, characterized by being manufactured by the manufacturing method of any one of claims 1 to 9.
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| US20180312749A1 (en) * | 2017-04-26 | 2018-11-01 | National Tsing Hua University | Combination solution of colloidal quantum dots and method for making the same |
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