CN111307884B - Heterojunction sensitive device, preparation method thereof and gas sensor comprising same - Google Patents
Heterojunction sensitive device, preparation method thereof and gas sensor comprising same Download PDFInfo
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- CN111307884B CN111307884B CN202010392076.9A CN202010392076A CN111307884B CN 111307884 B CN111307884 B CN 111307884B CN 202010392076 A CN202010392076 A CN 202010392076A CN 111307884 B CN111307884 B CN 111307884B
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- C01B32/198—Graphene oxide
Abstract
The invention discloses a heterojunction sensitive device, a preparation method thereof and a gas sensor comprising the sensitive device, and belongs to the technical field of semiconductor devices and sensing. The preparation method comprises three steps: carrying out controllable coating on the surfaces of the magnetic submicron spheres sequentially by using the carbon nano tubes and the graphene oxide to form a heterojunction; in the sample dropping process, a magnetic field is utilized to control the three-dimensional magnetic carbon nanotube/reduced graphene oxide heterojunction to form a chain-shaped multi-conduction channel which is arranged in an oriented manner between electrodes; and (4) carrying out reduction treatment on the graphene oxide to complete the construction of the gas sensing device. Compared with the prior art, the method can effectively solve the problems of low sensitivity of sensitive nano material devices, poor uniformity of sensitive materials, poor performance stability of devices in the same batch and the like in the construction process of the gas sensor by utilizing the in-situ formation of the carbon-based heterojunction and the magnetic field control technology, and is simple and efficient in construction method and suitable for large-scale production.
Description
Technical Field
The invention belongs to the technical field of semiconductor devices and sensing (G03F), and particularly relates to a method for controllably constructing a high-performance gas sensor by in-situ preparation of a three-dimensional magnetic carbon nanotube/reduced graphene oxide heterojunction and magnetic field induced arrangement.
Background
The reduced graphene oxide has the specific performance different from that of a conventional material due to the huge specific surface area, the unique size effect, the macroscopic quantum tunneling effect and the like, the huge specific surface area provides a great number of active sites, different gas-sensitive response characteristics can be easily realized through a functional group modification method, and meanwhile, the reduced graphene oxide has the characteristic of working at room temperature and is a nano gas-sensitive material with great development potential. However, when a reduced graphene oxide sensor is constructed, the phenomena of overlapping, agglomeration and uneven distribution of sensitive nano materials are easily generated in the process of dripping sample drying on the surface of an electrode, so that the advantages of the gas-sensitive nano materials, such as huge surface area and rich active sites, are seriously limited, the performance stability of the device and the random difference of the performance of the device in the same batch are large, and the reduced graphene oxide is relatively low in sensitivity compared with other materials, so that the problem seriously hinders the industrialization process of the reduced graphene oxide sensor.
A group of topics of Shanghai university of transportation has studied that the utilization of specific surface area and active sites can be improved by converting the stacking mode of sensitive nanomaterials from two-dimensional to three-dimensional, and simultaneously, the usage amount of the sensitive nanomaterials is reduced. Earlier researches prove that the multi-channel gas sensor is formed by uniformly coating the magnetic microspheres with the nano gas-sensitive material and realizing chain-shaped directional arrangement of three-dimensional magnetic microspheres by a magnetic induction arrangement technology. However, when pure reduced graphene oxide is used as a gas sensitive material, due to the existence of a large number of structural defects or functional groups, the recombination probability of carriers is very high, and the further improvement of the sensitivity of the gas sensitive device and the shortening of the response/recovery time are limited.
Disclosure of Invention
The purpose of the invention is as follows: a heterojunction sensitive device, a preparation method thereof and a gas sensor comprising the same are provided to solve the problems involved in the background art.
The technical scheme is as follows: the invention provides a preparation method of a three-dimensional carbon nanotube/reduced graphene oxide heterojunction sensitive device, which comprises the following steps:
s1, electrostatic self-assembly of heterojunction:
the carbon nano tube and the graphene oxide are sequentially coated on the surface of the magnetic submicron sphere in a controllable manner to form a three-dimensional magnetic carbon nano tube/reduced graphene oxide heterojunction;
s2, orientation arrangement of heterojunction:
in the sample dropping process, the three-dimensional magnetic carbon nanotube/reduced graphene oxide heterojunction is controlled by a magnetic field to form directional arrangement between electrodes to form a chain-shaped multi-conduction channel;
s3, reduction treatment:
and (4) carrying out reduction treatment on the graphene oxide to complete the construction of the gas sensing device.
As a preferable scheme, the carbon nanotube/graphene oxide sequential coating is electrostatic self-assembly coating, and the coating order can be changed.
As a preferable scheme, the magnetic submicron sphere takes a magnetic material as a core and silicon dioxide as a shell; the magnetic submicron spheres at least comprise Fe3O4@SiO2、γ-Fe2O3@SiO2、Ni@SiO2、NiO@SiO2One kind of (1).
As a preferable scheme, the carbon nanotube at least comprises one of a carboxylated single-wall carbon nanotube, a carboxylated double-wall carbon nanotube and a carboxylated multi-wall carbon nanotube.
As a preferable scheme, the coating time of the carbon nano tube or the reduced graphene oxide is 1-12 hours.
Preferably, before the electrostatic self-assembly of the heterojunction, the SiO2And (3) carrying out HCl activation treatment on the surface of the layer, and carrying out ultrasonic soaking for 10-40 minutes.
As a preferable scheme, the magnetic field intensity of the magnetic field operated arrangement is 200-3000 gauss.
Preferably, the reduction treatment is thermal reduction or chemical reduction.
The invention also provides a three-dimensional carbon nanotube/reduced graphene oxide heterojunction sensitive device, which comprises: the gas-sensitive material is a three-dimensional carbon nanotube/reduced graphene oxide heterojunction formed by coating a carbon nanotube and graphene oxide on the surface of a magnetic submicron sphere through electrostatic self-assembly.
As a preferable scheme, the carbon nanotube/graphene oxide sequential coating is electrostatic self-assembly coating, and the coating order can be changed.
As a preferable scheme, the magnetic submicron sphere takes a magnetic material core and silicon dioxide as a shell; the magnetic submicron spheres at least comprise Fe3O4@SiO2、γ-Fe2O3@SiO2、Ni@SiO2、NiO@SiO2One kind of (1).
As a preferable scheme, the carbon nanotube at least comprises one of a carboxylated single-wall carbon nanotube, a carboxylated double-wall carbon nanotube and a carboxylated multi-wall carbon nanotube.
The invention also provides an application of the three-dimensional carbon nanotube/reduced graphene oxide heterojunction sensitive device in preparing a gas sensor, which comprises the following steps:
s1, electrostatic self-assembly of heterojunction:
the carbon nano tube and the graphene oxide are sequentially coated on the surface of the magnetic submicron sphere in a controllable manner to form a three-dimensional magnetic carbon nano tube/reduced graphene oxide heterojunction;
s2, orientation arrangement of heterojunction:
in the sample dropping process, the three-dimensional magnetic carbon nanotube/reduced graphene oxide heterojunction is controlled by a magnetic field to form directional arrangement between electrodes to form a chain-shaped multi-conduction channel;
s3, reduction treatment:
and (4) carrying out reduction treatment on the graphene oxide to complete the construction of the gas sensing device.
S4, welding and packaging
Finally, the sensor device is welded and packaged, and therefore the sensor is obtained.
As a preferable scheme, the carbon nanotube/graphene oxide sequential coating is electrostatic self-assembly coating, and the coating order can be changed.
As a preferable scheme, the magnetic submicron sphere takes a magnetic material as a core and silicon dioxide as a shell; the magnetic submicron spheres at least comprise Fe3O4@SiO2、γ-Fe2O3@SiO2、Ni@SiO2、NiO@SiO2One kind of (1).
As a preferable scheme, the carbon nanotube at least comprises one of a carboxylated single-wall carbon nanotube, a carboxylated double-wall carbon nanotube and a carboxylated multi-wall carbon nanotube.
As a preferable scheme, the coating time of the carbon nano tube or the reduced graphene oxide is 1-12 hours.
Preferably, before the electrostatic self-assembly of the heterojunction, the SiO2And (3) carrying out HCl activation treatment on the surface of the layer, and carrying out ultrasonic soaking for 10-40 minutes.
As a preferable scheme, the magnetic field intensity of the magnetic field operated arrangement is 200-3000 gauss.
Preferably, the reduction treatment is thermal reduction or chemical reduction.
Has the advantages that: the invention relates to a heterojunction sensitive device, a preparation method thereof and a gas sensor containing the same. The gas-sensitive device ensures that active sites on the huge specific surface area of the carbon nano tube/reduced graphene oxide are utilized to the maximum, and meanwhile, on the basis that the multiple conducting channels which are uniformly distributed ensure stable performance of the device and uniform performance of the devices in the same batch, the controllable heterojunction can further improve the gas-sensitive responsivity of the device and shorten the response time.
Compared with the prior art, the invention has the following advantages:
1. the magnetic submicron ball is used as a support, and the carbon nano tube and the graphene oxide can be sequentially and uniformly wrapped on the surface of the magnetic submicron material to form a heterojunction in an electrostatic self-assembly mode, so that the contact mode and the charge separation mode of a conductive main body and gas to be detected can be effectively changed, and the performance of a device can be effectively improved.
2. On the premise of ensuring that the active sites are utilized to the maximum, the device stability and the performance uniformity of devices in the same batch are ensured, the simple and controllable carbon nanotube/reduced graphene heterojunction can further effectively improve the responsiveness of gas sensitivity and shorten the response time.
3. The construction method is simple, efficient and suitable for large-scale production.
Drawings
Fig. 1 is a schematic diagram of a three-dimensional magnetic carbon nanotube/reduced graphene oxide heterojunction according to the present invention.
FIG. 2 is a scanning electron micrograph of a multi-channel device obtained in example 1.
Fig. 3 is a comparison curve of performances of the three-dimensional carbon nanotube @ silica composite gas sensor prepared in example 1 and a two-dimensional carbon nanotube network gas sensor.
FIG. 4 shows the gas sensor made of the three-dimensional carbon nanotube @ silica composite material prepared in example 1 for different concentrations of NO2Response-recovery curve of gas.
The reference signs are: the magnetic submicron sphere comprises a magnetic submicron sphere 1 with a core-shell structure, a carbon nanotube 2 and reduced graphene 3.
Detailed Description
The invention will now be further described with reference to the following examples, which are intended to be illustrative of the invention and are not to be construed as limiting the invention.
Example 1
With magnetic Fe of 500nm diameter3O4@SiO2Submicron spheres with core-shell structures are taken as a support body, and an electrostatic self-assembly method is adopted to firstly carry out magnetic Fe3O4@SiO2Assembling the carboxylated multi-walled carbon nano-tube assembled on the surface of the submicron sphere with the core-shell structure for 1 hour; then, putting the magnetic submicron spheres coated with the carboxylated carbon nanotubes on the surface into the graphene oxide dispersion liquid, and stirring and assembling for 12 hours; dispersing the three-dimensional magnetic carbon nano tube/reduced graphene oxide heterojunction gas-sensitive material in isopropanol solution, and concentrating in the manufacturing process of a gas-sensitive deviceAnd (3) carrying out directional arrangement on the sensitive material solution with the temperature of 0.2mg/mL under the condition of a transverse magnetic field (as shown in figure 1) with the strength of 2000 gauss, after a solvent is evaporated and the magnetic field is removed, carrying out heat treatment at 200 ℃ in an air atmosphere for 90 minutes, and thus completing the construction of the multi-channel sensitive device. The arrangement of the sensitive material between the pairs of interdigitated electrodes is shown in figure 2.
Example 2
Using magnetic gamma-Fe with diameter of 600nm2O3@SiO2The submicron ball with the core-shell structure is taken as a support body, and a carboxylated single-walled carbon nanotube is assembled on the surface of the submicron ball with the magnetic core-shell structure by adopting an electrostatic self-assembly method for 5 hours; then, putting the magnetic submicron spheres coated with the carboxylated carbon nanotubes on the surface into the graphene oxide dispersion liquid, and stirring and assembling for 8 hours; dispersing a three-dimensional magnetic carbon nanotube/reduced graphene oxide heterojunction gas-sensitive material in an isopropanol solution, in the manufacturing process of a gas-sensitive device, carrying out directional arrangement on the sensitive material solution with the concentration of 0.2mg/mL under the condition of a transverse magnetic field with the strength of 200 gauss, after a solvent is evaporated and the magnetic field is removed, carrying out chemical reduction treatment in a hydrazine hydrate solution for 90 minutes, and then completing the construction of the multi-channel sensitive device.
Example 3
Magnetic Ni @ SiO with the diameter of 800nm2The submicron ball with the core-shell structure is taken as a support body, a layer of carboxylated single-walled carbon nanotubes is firstly assembled on the surface of the submicron ball with the magnetic core-shell structure by adopting an electrostatic self-assembly method, and the assembly time is 10 hours; then, placing the magnetic submicron spheres with the surfaces wrapped with the carboxylated single-walled carbon nanotubes into the graphene oxide dispersion liquid for stirring and assembling for 6 hours; dispersing a three-dimensional magnetic carbon nanotube/reduced graphene oxide heterojunction gas sensitive material in an isopropanol solution, in the manufacturing process of a gas sensitive device, carrying out directional arrangement on the sensitive material solution with the concentration of 0.2mg/mL under the condition of a transverse magnetic field with the strength of 3000 gauss, after a solvent is evaporated and the magnetic field is removed, carrying out heat treatment at 250 ℃ in the air atmosphere for 90 minutes, and thus completing the construction of the multi-channel sensitive device.
Example 4
By magnet with diameter of 600nmNiO @ SiO 22The submicron ball with the core-shell structure is taken as a support body, a layer of carboxylated double-wall carbon nano tube is assembled on the surface of the submicron ball with the magnetic core-shell structure by adopting an electrostatic self-assembly method, and the assembly time is 3 hours; then, putting the magnetic submicron spheres with the surface wrapped by the carboxylated double-walled carbon nanotubes into the graphene oxide dispersion liquid for stirring and assembling, wherein the assembling time is 8 hours; dispersing a three-dimensional magnetic carbon nanotube/reduced graphene oxide heterojunction gas sensitive material in an isopropanol solution, in the manufacturing process of a gas sensitive device, carrying out directional arrangement on the sensitive material solution with the concentration of 0.2mg/mL under the condition of a transverse magnetic field with the strength of 3000 gauss, after a solvent is evaporated and the magnetic field is removed, carrying out heat treatment in an ascorbic acid solution at 100 ℃ for 12 hours, and completing the construction of the multi-channel sensitive device.
Example 5
With magnetic Fe of 600nm diameter3O4@SiO2Submicron spheres with core-shell structures are taken as a support body, and an electrostatic self-assembly method is adopted to firstly carry out magnetic Fe3O4@SiO2Assembling a layer of graphene oxide on the surface of the core-shell structure submicron sphere for 3 hours; then, putting the magnetic submicron spheres coated with the graphene oxide on the surface into the dispersion liquid of the carboxylated single-walled carbon nanotubes, and stirring and assembling for 8 hours; dispersing a three-dimensional magnetic carbon nanotube/reduced graphene oxide heterojunction gas sensitive material in an isopropanol solution, in the manufacturing process of a gas sensitive device, carrying out directional arrangement on the sensitive material solution with the concentration of 0.2mg/mL under the condition of a transverse magnetic field with the strength of 1000 gauss, after a solvent is evaporated and the magnetic field is removed, carrying out heat treatment at 200 ℃ in the air atmosphere for 90 minutes, and thus completing the construction of the multi-channel sensitive device.
Example of detection
And (3) welding and packaging the multi-channel sensitive device obtained in the embodiment 1 to obtain the three-dimensional carbon nanotube @ silicon dioxide composite material gas sensor, and performing performance test on the performance of the gas sensor and the performance of the existing two-dimensional carbon nanotube network gas sensor. The specific experimental data are shown in FIG. 3 and FIG. 4, wherein the gas sensitivity responsivity
(ii) a Delta I is the difference between the current value of the gas sensor in the gas to be measured and the current value in the air, IaThe current value of the sensor in the air.
In a word, the self-assembly scheme of the invention with the silicon dioxide nanometer spheres as the supports enables the carbon nanometer tubes to be uniformly wrapped on the surfaces of the silicon dioxide nanometer spheres, the three-dimensional carbon nanometer tube @ silicon dioxide composite material gas sensor prepared by the method can effectively utilize the large-area carbon nanometer tubes and control the thickness of the sensing network, and the gas-sensitive performance is greatly improved after the multi-walled carbon nanometer tube network is converted from two dimensions to three dimensions as shown in the attached figure 3 (the comparison curve of the performances of the three-dimensional carbon nanometer tube @ silicon dioxide composite material gas sensor prepared by the invention and the two-dimensional carbon nanometer tube network gas sensor), thereby highlighting the innovation of the invention. From FIG. 4 (gas sensor for different concentrations of NO)2Response-recovery curve of gas), the gas sensor based on the three-dimensional carbon nanotube network also exhibits excellent gas sensing performance, high sensitivity, good repeatability and NO sensitivity2Excellent selectivity of gas.
It should be noted that, for those skilled in the art, the device performance can be effectively improved by changing the coating sequence, coating time, magnetic field distribution, reduction treatment method, and the like of the carbon nanotubes and the graphene oxide. The various features described in the foregoing detailed description may be combined in any suitable manner without departing from the scope of the invention. The invention is not described in detail in order to avoid unnecessary repetition.
Claims (9)
1. A preparation method of a three-dimensional carbon nanotube/reduced graphene oxide heterojunction sensitive device is characterized by comprising the following steps:
s1, electrostatic self-assembly of heterojunction
The carbon nano tube and the graphene oxide are sequentially coated on the surface of the magnetic submicron sphere in a controllable manner to form a three-dimensional magnetic carbon nano tube/reduced graphene oxide heterojunction; the magnetic submicron sphere takes a magnetic material core and silicon dioxide as a shell;
s2, alignment of heterojunctions
In the sample dripping process, a transverse magnetic field is used for controlling the three-dimensional magnetic carbon nanotube/reduced graphene oxide heterojunction to form directional arrangement between electrodes to form a chain-shaped multi-conduction channel, and the magnetic field intensity of the arrangement controlled by the magnetic field is 200-3000 gauss;
s3, reduction treatment
And (4) carrying out reduction treatment on the graphene oxide to complete the construction of the gas sensing device.
2. The method of claim 1, wherein the sequential coating of the carbon nanotubes/graphene oxide is electrostatic self-assembly coating, and the coating order is changeable.
3. The method for preparing a three-dimensional carbon nanotube/reduced graphene oxide heterojunction sensitive device as claimed in claim 1, wherein the magnetic submicron spheres at least comprise Fe3O4@SiO2、g-Fe2O3@SiO2、Ni@SiO2、NiO@SiO2One kind of (1).
4. The method as claimed in claim 1, wherein the carbon nanotubes include at least one of carboxylated single-walled carbon nanotubes, carboxylated double-walled carbon nanotubes, and carboxylated multi-walled carbon nanotubes.
5. The method for preparing the three-dimensional carbon nanotube/reduced graphene oxide heterojunction sensitive device according to claim 1, wherein the coating time of the carbon nanotube or the reduced graphene oxide is 1-12 hours.
6. The three-dimensional carbon nanotube/reduced graphite oxide of claim 1The preparation method of the alkene heterojunction sensitive device is characterized in that before the electrostatic self-assembly of the heterojunction, SiO is carried out2And (3) carrying out HCl activation treatment on the surface of the layer, and carrying out ultrasonic soaking for 10-40 minutes.
7. The method for preparing the three-dimensional carbon nanotube/reduced graphene oxide heterojunction sensitive device according to claim 1, wherein the reduction treatment is thermal reduction or chemical reduction.
8. A heterojunction sensitive device obtained by the preparation method of the three-dimensional carbon nanotube/reduced graphene oxide heterojunction sensitive device according to any one of claims 1 to 7, comprising: the gas-sensitive material is a three-dimensional carbon nanotube/reduced graphene oxide heterojunction formed by coating a carbon nanotube and graphene oxide on the surface of a magnetic submicron sphere through electrostatic self-assembly.
9. The application of the three-dimensional carbon nanotube/reduced graphene oxide heterojunction sensitive device in preparing the gas sensor is characterized by comprising the following steps of:
s1, electrostatic self-assembly of heterojunction
The carbon nano tube and the graphene oxide are sequentially coated on the surface of the magnetic submicron sphere in a controllable manner to form a three-dimensional magnetic carbon nano tube/reduced graphene oxide heterojunction; the magnetic submicron sphere takes a magnetic material core and silicon dioxide as a shell;
s2, alignment of heterojunctions
In the sample dripping process, a transverse magnetic field is used for controlling the three-dimensional magnetic carbon nanotube/reduced graphene oxide heterojunction to form directional arrangement between electrodes to form a chain-shaped multi-conduction channel, and the magnetic field intensity of the arrangement controlled by the magnetic field is 200-3000 gauss;
s3, reduction treatment
Carrying out reduction treatment on the graphene oxide to complete the construction of the gas sensing device;
s4, welding and packaging
Finally, the sensor device is welded and packaged, and therefore the sensor is obtained.
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