CN113292041A - Based on SnSe2Semiconductor multifunctional intelligent sensor and preparation method thereof - Google Patents
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Abstract
The invention provides a multifunctional intelligent sensor based on a SnSe2 semiconductor and a preparation method thereof, belonging to the field of multifunctional sensors. Comprises a substrate, a first area sensor, a second area sensor and a third area sensor; the substrate is of a semi-Mo metal-semi-glass structure, and the first area sensor and the second area sensor are positioned on a Mo metal layer on the substrate, are communicated with a Mo metal film and are respectively a photoelectric sensor and a methane gas sensor; the third area sensor is located at the glass position on the substrate and is a pressure sensor. The invention utilizes SnSexThe two-dimensional material grows on the same substrate and has the advantage of multiple functions, so that one sensor can measure simultaneouslyThe multifunctional sensor has the advantages of small size, strong function, centralized acquired information, convenience in processing and profound significance and influence on future semiconductor integration technology.
Description
Technical Field
The invention belongs to the field of multifunctional sensors, and particularly relates to a sensor based on SnSe2A semiconductor multifunctional intelligent sensor and a preparation method thereof.
Background
Whether in the security fields such as security, monitoring and health, or in the mobile electronic field such as smart phones, the multifunctional sensor is undoubtedly a new research direction in the current sensor technology development.
In order to be able to detect multiple signals simultaneously with higher sensitivity and smaller granularity, the miniature digital three-port sensor can simultaneously adopt a thermosensitive element, a photosensitive element and a magnetosensitive element; the sensor in the assembly mode can output not only an analog signal, but also a frequency signal and a digital signal. In general, the various functions of a sensor can be realized by different physical (or chemical) effects of a sensing element and different characteristics thereof. With the development of sensors and micromachining technology, people can also manufacture several sensitive elements on the same material or silicon chip to manufacture an integrated multifunctional sensor, the multifunctional sensor can measure several parameters simultaneously, and the sensor has high integration level and small volume. Meanwhile, because the sensors are integrated on one chip, the working conditions of all sensitive elements are the same, mutual compensation and correction are easy to realize, and the sensor is one direction of development of multi-functional sensors.
Compared with the traditional semiconductor material, the multifunctional sensor array based on the two-dimensional film material has the advantages that the unique quantum confinement effect and surface effect (larger specific surface area) of the nanoscale, strong absorption response to gas and unique rough structure of the gas are benefited, the two-dimensional film material can play multiple functions through the design of the sensor structure and the preparation method, the industrialization process of the next-generation multifunctional intelligent sensor is expected to be promoted, and the ever-increasing market demand and national defense safety and health demand on the high-sensitivity detector are met.
Disclosure of Invention
In view of the above, the present invention provides a method based on SnSe2The multifunctional intelligent sensor of the semiconductor and the preparation method thereof can simultaneously detect pressure, gas and photoelectricity on the premise of ensuring the performance stability and the service life of a device, and has high integration level and high detection precision under the volume.
In order to achieve the purpose, the invention adopts the following technical scheme:
one of the purposes of the invention is to provide a SnSe-based chip2The semiconductor multifunctional intelligent sensor comprises a substrate, a first area sensor, a second area sensor and a third area sensor; the substrate is of a semi-Mo metal-semi-glass structure, and the first area sensor and the second area sensor are positioned on the Mo metal layer on the substrate and are communicated with the Mo metal film; a third area sensor is located at a glass position on the substrate;
the first area sensor is a photoelectric sensor and sequentially comprises a Mo metal layer, a vertical SnSex nanosheet layer after glue homogenizing and a Ni-Al-Ni forked electrode layer from bottom to top;
the second area sensor is a methane gas sensor and sequentially comprises a Mo metal layer, a vertical SnSex nanosheet layer after glue homogenizing and a Ni-Al-Ni full electrode layer from bottom to top;
the third area sensor is a pressure sensor and sequentially comprises a glass substrate layer, a vertical SnSex nanosheet layer after glue homogenizing, an Au metal layer and a PDMS/Au microstructure layer from bottom to top.
Another object of the present invention is to provide the SnSe-based chip2Semiconductor multifunction intelligenceThe preparation method of the sensor comprises the following steps:
(1) substrate pretreatment: dividing the Mo-plated glass substrate into two parts, and utilizing H to make use of Mo metal film on half of the glass substrate2O2Wiping off the solution to ensure that one half of the substrate is a glass substrate and the other half of the substrate is a Mo-plated glass substrate;
(2) two-dimensional material growth: dividing a substrate into three areas by using a mask plate, wherein the first area and the second area are positioned on the Mo-plated glass substrate, and the third area is positioned on the non-Mo-plated glass substrate; growing vertical SnSex nanosheets on the substrates of the three regions by using molecular beam epitaxy equipment, wherein x is 1.6-2.2;
(3) thermal annealing: preserving the heat for 30-60 min at the temperature of 200-280 ℃ under the atmosphere of 2% H2S and 98% N2;
(4) glue homogenizing: glue is homogenized on the outer surfaces of the vertical SnSex nanosheets corresponding to the first area and the second area, so that the vertical SnSex nanosheets are only exposed at the tops; the spin speed of the spin coating is 1000 rpm-4000 rpm, and the thickness of the spin coating is 1-2 um;
(5) evaporating a back electrode: evaporating back electrodes at exposed positions of the tops of the vertical SnSex nanosheets in the first area and the second area by using an electron beam evaporation method, wherein the back electrodes are in contact with the SnSex and have the thickness of 8000-10000 nm; the back electrode of the first area is a Ni-Al-Ni fork electrode, and the back electrode of the second area is a Ni-Al-Ni full electrode;
(6) preparation of the microstructured film: forming a microstructure on a glass substrate by photoetching, filling polydimethylsiloxane by spin coating to form a PDMS microstructure film, separating the microstructure film from the glass substrate, and depositing Cr/Au on the microstructure film by thermal evaporation to form the PDMS/Au microstructure film; the thickness of the Cr/Au is 1nm/100 nm;
(7) assembling the microstructure film: depositing Cr/Au by thermal evaporation, assembling the PDMS/Au microstructure film to a third region, and contacting with SnSex; the thickness of the Cr/Au is 1nm/100 nm;
(8) packaging: and (3) connecting a lead, and packaging the first area, the second area, the third area, the lead and the substrate to prepare the multifunctional intelligent sensor, wherein the first area is used for measuring photoelectricity, the second area is used for measuring methane gas, and the third area is used for measuring pressure.
The invention has the beneficial effects that:
(1) the present invention utilizes a two-dimensional group IV-VI semiconductor material (SnSe)x) The method has the characteristics of multiple functions, the charge separation process of the two-dimensional layered material is more efficient, the photon-generated carriers with high density and longer service life can be easily obtained, the external quantum efficiency and the photoresponse rate of the detector can be improved, the detector has strong adsorption response to gas molecules, and the SnSe has strong adsorption responsexThe nano sheet can provide a large number of contact parts and enough roughness for pressure detection and the like, and is creatively integrated and designed on the same sensor, so that the three-in-one SnSe formed by growing the photoelectric detector, the pressure sensor and the gas sensor under the same substrate is obtainedxA semiconductor multifunctional sensor. The multifunctional sensor has the advantages of small size, strong function, centralized acquired information, convenience in processing and profound significance and influence on future semiconductor integration technology.
(2) The growth temperature of the invention is lower<250 ℃) and molecular migration energy is not enough to cross a potential barrier, so that the mode evolves to an in-situ longitudinal growth mode2The self-organization growth mechanism of the equal two-dimensional nanosheets is realized by regulating and controlling the substrate temperature and the vapor pressure to regulate and control SnSe2The migration energy and the nucleation density of the nano-sheets of (A) are controlled by optimizing the stoichiometric ratio of Se/Sn in the vacuum atmosphere2And (3) waiting for the components and defect density of the two-dimensional material to obtain the large-area high-quality high-density vertical nanosheet array.
Drawings
FIG. 1 is SnSe2A simplified view of a photosensor;
FIG. 2 is SnSe2A simplified diagram of a flexible high performance piezoresistive pressure sensor;
FIG. 3 is SnSe2A simplified view of a methane gas sensor;
FIG. 4 is a simplified diagram of a multi-functional smart sensor;
FIG. 5 is a flow chart of a process for making a multifunctional smart sensor;
FIG. 6 is a graph showing the results of a methane gas concentration test;
FIG. 7 is a graph of pressure test results;
fig. 8 is a graph of photoelectric test results.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention are described in detail below with reference to the accompanying drawings. Examples of these preferred embodiments are illustrated in the accompanying drawings. The embodiments of the invention shown in the drawings and described in accordance with the drawings are exemplary only, and the invention is not limited to these embodiments.
The invention provides a method based on SnSe2A semiconductor multifunctional smart sensor structure, as shown in fig. 4, comprising a substrate, a first area sensor, a second area sensor and a third area sensor; the substrate is of a semi-Mo metal-semi-glass structure, and the first area sensor and the second area sensor are positioned on the Mo metal layer on the substrate and are communicated with the Mo metal film; a third area sensor is located at a glass position on the substrate;
as shown in fig. 1, the left side of the arrow is a top view, the right side is a side view, the first area sensor is a photoelectric sensor, and the first area sensor sequentially comprises a Mo metal layer and a vertical SnSe after glue spreading from bottom to topxA nanosheet layer, a Ni-Al-Ni forked electrode layer;
as shown in fig. 3, the left side of the arrow is a top view, the right side is a side view, the second area sensor is a methane gas sensor, and the second area sensor sequentially comprises a Mo metal layer and vertically-arranged SnSe after glue homogenizing from bottom to topxA nanosheet layer, a Ni-Al-Ni full electrode layer;
as shown in fig. 2, the left side of the arrow is a top view, the right side is a side view, the third area sensor is a pressure sensor, and the third area sensor sequentially comprises a glass substrate layer and vertically-arranged SnSe after glue homogenizing from bottom to topxNanosheet layer, Au metal layerAnd a PDMS/Au microstructure layer.
In this embodiment, the vertical SnSexIn the nanosheet layer, the atomic ratio of Sn to Se is 1: (1.6-2.2), preferably 1: 2.
Vertical SnSe in sensor structurexThe nano-sheet layer grows under the same substrate to form three-in-one SnSexThe semiconductor multifunctional sensor is designed based on different areas, so that one sensor can measure photoelectricity, gas and pressure simultaneously.
The invention also discloses a preparation method of the multifunctional intelligent sensor, which is shown by combining the figures 4 and 5 and mainly comprises the following steps:
(1) substrate pretreatment: dividing the Mo-plated glass substrate into two parts, and utilizing H to make use of Mo metal film on half of the glass substrate2O2The solution was wiped off so that half of the substrate was a glass substrate and half was a Mo-plated glass substrate.
(2) Two-dimensional material growth: dividing a substrate into three areas by using a mask plate, wherein the first area and the second area are positioned on the Mo-plated glass substrate, and the third area is positioned on the non-Mo-plated glass substrate; and growing vertical SnSex nanosheets on the substrates of the three regions by using molecular beam epitaxy equipment, wherein x is 1.6-2.2.
(3) Thermal annealing: keeping the temperature for 30-60 min at 200-280 ℃ under the atmosphere of 2% H2S and 98% N2.
(4) Glue homogenizing: glue is homogenized on the outer surfaces of the vertical SnSex nanosheets corresponding to the first area and the second area, so that the vertical SnSex nanosheets are only exposed at the tops; the spin speed of the spin coating is 1000 rpm-4000 rpm, and the thickness of the spin coating is 1-2 um;
(5) evaporating a back electrode: evaporating back electrodes at exposed positions of the tops of the vertical SnSex nanosheets in the first area and the second area by using an electron beam evaporation method, wherein the back electrodes are in contact with the SnSex and have the thickness of 8000-10000 nm; the back electrode of the first region is a Ni-Al-Ni fork electrode, and the back electrode of the second region is a Ni-Al-Ni full electrode.
(6) Preparation of the microstructured film: forming a microstructure on a glass substrate by photoetching, filling polydimethylsiloxane by spin coating to form a PDMS microstructure film, separating the microstructure film from the glass substrate, and depositing Cr/Au on the microstructure film by thermal evaporation to form the PDMS/Au microstructure film; the thickness of the Cr/Au is 1nm/100 nm.
(7) Assembling the microstructure film: depositing Cr/Au by thermal evaporation, assembling the PDMS/Au microstructure film to a third region, and contacting with SnSex; the thickness of the Cr/Au is 1nm/100 nm.
(8) Packaging: and (3) connecting a lead, and packaging the first area, the second area, the third area, the lead and the substrate to prepare the multifunctional intelligent sensor, wherein the first area is used for measuring photoelectricity, the second area is used for measuring methane gas, and the third area is used for measuring pressure.
In the present example, in the two-dimensional material growth step in step (2), SnSexThe nano-sheet layer grows under the same substrate, and a high-purity selenium material source and a high-purity tin material source are respectively added into molecular beam epitaxy equipment (MBE), wherein the preferred purity of the selenium source and the tin source is 99.99%. Respectively heating the selenium material source and the tin material source through the molecular beam epitaxy device, and respectively spraying the selenium material source and the tin material source onto the substrate in the form of molecular beams or atomic beams.
The growth temperature of the invention is lower<250 ℃) and molecular migration energy is not enough to cross a potential barrier, thus the longitudinal growth mode of in situ is evolved2The self-organization growth mechanism of the equal two-dimensional nanosheets is realized by regulating and controlling the substrate temperature and the vapor pressure to regulate and control SnSe2The migration energy and the nucleation density of the nano-sheets of (A) are controlled by optimizing the stoichiometric ratio of Se/Sn in the vacuum atmosphere2And (3) waiting for the components and defect density of the two-dimensional material to obtain the large-area high-quality high-density vertical nanosheet array.
For prepared SnSexThe nano-sheet is tested, and the nano-sheet array has extremely high light trapping effect and 500-plus 600nm waveband lightThe absorption is more than 96%, the external quantum efficiency and the light responsivity of the detector can be greatly improved, the external quantum efficiency of the photoelectric detector is as high as 6.43 multiplied by 105%, and the response time is less than 20 ms.
The temperature of the selenium material source is 150 ℃ to 250 ℃, preferably 245 ℃; the temperature of the tin material source is 1000 ℃ to 1200 ℃, and 1100 ℃ is preferred; the substrate temperature at the three zones is 150 ℃ to 250 ℃, preferably 245 ℃; vacuum degree of 2X 105Pa, and the growth time is 1-40 min. The two-dimensional material obtained by final growth is SnSe2The height is 1-2 μm, and the thickness is 20-30 nm.
Regulating and controlling SnSe in the thermal annealing step of the step (3) by regulating the temperature of the substrate2The crystal quality of the nanosheets and the later thermal annealing treatment regulate and control the surface defect state, including the adsorption (electron trap) of the internal defects (Vsn, Vse and SnSe) of the material and the surface defects (SnSe 2) of the material to O in the air. The temperature of the substrate is controlled to be (150 ℃ -250 ℃), and the thermal annealing treatment mainly comprises the utilization of 2% H2S and 98% of N2The internal defects are regulated and controlled by controlling the temperature rise and the heat preservation temperature and time under the atmosphere, so that the temperature rise and the heat preservation time are controlled to be 30-60 min at 200-280 ℃. Wherein 2% of H2S and 98% of N2The atmosphere is a result of parameters obtained by a large number of experimental investigations.
In the spin coating process of step (4), PMMA glue, electron beam resist positive glue (RZJ-304), or epoxy negative glue (SN-100) can be used. The thickness of the spin coating is regulated and controlled by controlling the rotating speed, and then the thickness of the spin coating is tested by a film thickness meter. Wherein, the rotating speed range is controlled to be 1000-4000 rpm, the thickness is controlled to be 1-2 um, the light transmission requirement and the insulation requirement are required to be met after glue homogenizing, and the SnSe at the position2The nanosheets are not completely covered, and the conductivity of the top is retained.
After the glue is homogenized, a back electrode is evaporated by an electron beam evaporation method, wherein a Ni-Al-Ni electrode evaporated by the photoelectric sensor is a fork-shaped electrode, and a Ni-Al-Ni electrode evaporated by the gas sensor is a full electrode, so that the shape of the electrode is not required to be prepared by a mask. The electrode has high stability, can be uniformly prepared in a large area, is simple and easy to operate in the preparation method, and has the thickness controlled to be about 8000-10000 nm.
In the first step of the microstructured film fabrication process, a microstructured template is lithographically formed on a glass (PI) substrate. In the second step, the microstructure template is filled with polydimethylsiloxane by spin coating, and then the microstructure is reproduced on the PDMS film. In the third step, to separate the microstructured PDMS from the substrate, the photoresist was dissolved in an acetone solution. Finally, Cr/Au (1nm/100nm) is evaporated on the PDMS microstructure by thermal deposition, and finally the PDMS/Au microstructure film is formed. Micro-pattern PDMS/Au and SnSe2The nano-sheet two-dimensional thin film material is assembled by depositing Cr/Au (1nm/100nm) through thermal evaporation.
Finally, in the packaging process of the sensor, conducting wires are connected, as shown in fig. 4, wherein one conducting wire is connected with the substrate on which the Mo metal film is plated, and the other two conducting wires are respectively connected with the electrodes on the tops of the two sensors; on the substrate which is not plated with the Mo metal film, two wires are required to be respectively connected with the pressure sensor, and the top and the bottom of the pressure sensor are conducted.
The prepared multifunctional sensor was tested to obtain the following test results of fig. 6, 7 and 8, respectively. Fig. 6 shows the results of the methane gas concentration test, fig. 7 shows the results of the pressure test, and fig. 8 shows the results of the photoelectric test. Therefore, the detection line is extremely low, the response is sensitive, and the application can be further realized by fitting a corresponding curve.
The foregoing is directed to embodiments of the present application and it is noted that numerous modifications and adaptations may be made by those skilled in the art without departing from the principles of the present application and are intended to be within the scope of the present application.
Claims (7)
1. Based on SnSe2The semiconductor multifunctional intelligent sensor is characterized by comprising a substrate, a first area sensor, a second area sensor and a third area sensor; the substrate is of a semi-Mo metal-semi-glass structure, and the first area sensor and the second area sensor are positioned on the Mo metal layer on the substrate and are communicated with the Mo metal film; third zone sensor positionA glass location on the substrate;
the first area sensor is a photoelectric sensor and sequentially comprises a Mo metal layer and vertical SnSe after glue homogenizing from bottom to topxA nanosheet layer, a Ni-Al-Ni forked electrode layer;
the second area sensor is a methane gas sensor and sequentially comprises a Mo metal layer and vertical SnSe after glue homogenizing from bottom to topxA nanosheet layer, a Ni-Al-Ni full electrode layer;
the third area sensor is a pressure sensor and sequentially comprises a glass substrate layer and vertical SnSe after glue homogenizing from bottom to topxA nanosheet layer, an Au metal layer, and a PDMS/Au microstructure layer.
2. The SnSe-based of claim 12The semiconductor multifunctional intelligent sensor is characterized in that the vertical SnSe sensorxIn the nanosheet layer, the atomic ratio of Sn to Se is 1: (1.6-2.2).
3. The SnSe-based chip of claim 12The preparation method of the semiconductor multifunctional intelligent sensor is characterized by comprising the following steps of:
(1) substrate pretreatment: dividing the Mo-plated glass substrate into two parts, and utilizing H to make use of Mo metal film on half of the glass substrate2O2Wiping off the solution to ensure that one half of the substrate is a glass substrate and the other half of the substrate is a Mo-plated glass substrate;
(2) two-dimensional material growth: dividing a substrate into three areas by using a mask plate, wherein the first area and the second area are positioned on the Mo-plated glass substrate, and the third area is positioned on the non-Mo-plated glass substrate; utilizing molecular beam epitaxy equipment to grow vertical SnSe on the substrate of the three areasxNanosheets, x being 1.6-2.2;
(3) thermal annealing: at 2% H2S and 98% of N2Keeping the temperature for 30-60 min at 200-280 ℃ under the atmosphere;
(4) glue homogenizing: vertical SnSe corresponding to the first region and the second regionxThe outer surface of the nano sheet is subjected toGlue is homogenized so that the vertical SnSexThe nanosheets are only exposed at the top; the spin speed of the spin coating is 1000 rpm-4000 rpm, and the thickness of the spin coating is 1-2 um;
(5) evaporating a back electrode: vertical SnSe in first area and second area by electron beam evaporation methodxThe back electrode is evaporated at the exposed position of the top of the nanosheet, and the back electrode and SnSe are coatedxContacting, wherein the thickness is 8000-10000 nm; the back electrode of the first area is a Ni-Al-Ni fork electrode, and the back electrode of the second area is a Ni-Al-Ni full electrode;
(6) preparation of the microstructured film: forming a microstructure on a glass substrate by photoetching, filling polydimethylsiloxane by spin coating to form a PDMS microstructure film, separating the microstructure film from the glass substrate, and depositing Cr/Au on the microstructure film by thermal evaporation to form the PDMS/Au microstructure film; the thickness of the Cr/Au is 1nm/100 nm;
(7) assembling the microstructure film: assembling PDMS/Au microstructure film to the third region by thermal evaporation deposition of Cr/Au, with SnSexContacting; the thickness of the Cr/Au is 1nm/100 nm;
(8) packaging: and (3) connecting a lead, and packaging the first area, the second area, the third area, the lead and the substrate to prepare the multifunctional intelligent sensor, wherein the first area is used for measuring photoelectricity, the second area is used for measuring methane gas, and the third area is used for measuring pressure.
4. The SnSe-based of claim 32The preparation method of the multifunctional intelligent sensor of the semiconductor is characterized in that the method for growing the two-dimensional material in the three areas in the step (2) comprises the following steps: respectively adding a high-purity selenium material source and a high-purity tin material source into molecular beam epitaxy equipment, wherein the temperature of the selenium material source is 150-250 ℃, the temperature of the tin material source is 1000-1200 ℃, and the vacuum degree is 2 multiplied by 105Pa, and the growth time is 1-40 min.
5. The SnSe-based of claim 42The method for preparing multifunctional intelligent semiconductor sensor is characterized in that in the step (2), three are adoptedThe substrate temperature at the zone is 150 ℃ to 250 ℃.
6. The SnSe-based of claim 52The preparation method of the multifunctional intelligent sensor of the semiconductor is characterized in that the two-dimensional material obtained by growth is SnSe2The height is 1-2 μm, and the thickness is 20-30 nm.
7. The SnSe-based of claim 32The preparation method of the multifunctional intelligent sensor of the semiconductor is characterized in that PMMA glue, electron beam photoresist positive glue or epoxy negative glue is adopted in the glue homogenizing process in the step (4).
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