CN113418552B - Two-dimensional transition metal sulfide material flexible sensor and preparation method thereof - Google Patents
Two-dimensional transition metal sulfide material flexible sensor and preparation method thereof Download PDFInfo
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- CN113418552B CN113418552B CN202110641991.1A CN202110641991A CN113418552B CN 113418552 B CN113418552 B CN 113418552B CN 202110641991 A CN202110641991 A CN 202110641991A CN 113418552 B CN113418552 B CN 113418552B
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Abstract
A two-dimensional transition metal sulfide material flexible sensor comprises an electrode, a lead and a semiconductor material; wherein the electrode and the semiconductor material are connected through the wire, and the semiconductor material comprises a substrate, a two-dimensional transition metal sulfide, and a conductive strip connected with the substrate and the two-dimensional transition metal sulfide. The device has a simple structure, the two-dimensional material and the paper-based flexible substrate are easy to combine, the conductive electrode is convenient to build, and the overall preparation cost is low; meanwhile, the preparation process of the integral device has no special requirements on two-dimensional materials, other substances which are difficult to remove are not introduced, and the preparation method of the flexible sensor device has universality and stable performance and is suitable for large-scale production.
Description
Technical Field
The invention belongs to the technical field of semiconductor flexible device preparation, and particularly relates to a preparation method and application of a two-dimensional transition metal sulfide material flexible sensor.
Background
Transition Metal Sulfides (TMDs) are transition metal group elements M (e.g., mo, W, ti) and chalcogens X (e.g., S, se, te) formed with a chemical formula of MX 2 The layers of the layered structure material (2) are bonded by weak van der waals force, and are easily peeled. When the transition metal sulfide peels at least one layer or even a single layer, the indirect band gap semiconductor is converted into a direct band gap semiconductor, and the layered structure is converted from three dimensions into two dimensions, so that the two-dimensional transition metal sulfide has excellent electrical, optical and bending properties, and has great potential in application and preparation of novel flexible electronic devices.
At present, due to the limitations of the preparation methods (mechanical stripping method, liquid phase shearing method, vapor deposition method and the like) of the two-dimensional TMDs materials and the traditional flexible substrate materials (PET, PDMS, PI and the like), complex material transfer technology and high-cost evaporation electrodes are often needed to prepare flexible devices, so that flexible sensor elements with simple device structures, low cost and reliable performance cannot be obtained, and a reasonable device structure needs to be designed, and a preparation method which is suitable for the preparation of the two-dimensional TMDs materials and the suitable flexible device substrate can be found to obtain a stable and reliable two-dimensional TMDs material-based flexible sensor device.
Therefore, the technical personnel in the field need to solve the problem that a flexible sensor with simple structure and low cost and a preparation method thereof can be provided.
Disclosure of Invention
In view of the above, the invention provides a two-dimensional transition metal sulfide material flexible sensor and a preparation method thereof, and successfully solves the problem that a two-dimensional transition metal sulfide is difficult to prepare a flexible sensor device with a simple structure and low cost through reasonable and feasible device structure design.
In order to achieve the purpose, the invention adopts the following technical scheme:
a two-dimensional transition metal sulfide material flexible sensor comprises an electrode, a lead and a semiconductor material; wherein the electrode and the semiconductor material are connected through the wire, and the semiconductor material comprises a substrate, a two-dimensional transition metal sulfide, and a conductive strip connected with the substrate and the two-dimensional transition metal sulfide.
The device has the advantages of simple structure, easy combination of the two-dimensional material and the paper-based flexible substrate, convenient construction of the conductive electrode and low overall preparation cost.
Preferably, the substrate is a filter membrane having a pore size of less than 0.22 um.
Preferably, the substrate is any one of polyvinylidene fluoride, hydrophilic polycarbonate membrane and mixed cellulose.
The filter membrane substrate can tightly adsorb two-dimensional materials to form a membrane by a simple suction filtration method, which cannot be achieved by other flexible substrates; and has better mechanical bending strength, and the preparation and combination method is simple.
Preferably, the preparation method of the semiconductor material comprises the following steps:
(1) Mixing transition metal sulfide powder with n-butyllithium solution, heating and stirring at 40-60 ℃ for 24-48h, filtering, adding deionized water into the precipitate, and ultrasonically stripping for 1-1.5h to obtain suspension;
(2) Centrifuging the suspension, and removing precipitates to obtain a two-dimensional transition metal sulfide suspension;
(3) Pumping and filtering the two-dimensional transition metal sulfide suspension to a substrate, and then washing with water, washing with alcohol and drying to obtain a two-dimensional transition metal sulfide composite film;
(4) And connecting the conductive band with the surface of the two-dimensional transition metal sulfide and the surface of the filter membrane to obtain the semiconductor material.
Compared with the methods for preparing the two-dimensional transition metal sulfide by a mechanical stripping method, a vapor deposition method and the like, the method has the advantages of simple preparation, high yield, no impurity removal difficulty and easiness in subsequent suction filtration and adsorption treatment; and the conductive path is easy to build, and the conductive adhesive tape is bonded with the substrate.
Preferably, in the step (1), the transition metal sulfide powder is any one of molybdenum sulfide or tungsten sulfide, and the concentration of the n-butyllithium solution is 1.8-2.2mol/L.
The invention adopts raw materials which are easy to prepare, wide in purchase source and relatively low in cost.
Preferably, the mass-to-volume ratio of the transition metal sulfide powder to the n-butyllithium solution in step (1) is 0.3 to 0.8g.
In the proportion of the invention, the addition amount of the transition metal sulfide powder is large, and the yield of the prepared two-dimensional material is high.
Preferably, the mass volume ratio of the transition metal sulfide powder to the deionized water in the step (1) is 0.3-0.8g.
Preferably, the conditions of the centrifugation in step (2) are: centrifuging at 1500-3000r/min for 10-15min.
Preferably, the drying conditions in step (3) are: vacuum drying at 45-55 deg.C for 1.52h.
The preparation method of the two-dimensional transition metal sulfide material flexible sensor comprises the following specific steps: and connecting one end of a lead with the electrode, and attaching the other end of the lead to the tail end of the conductive belt to form a conductive path from the electrode to the semiconductor material, thus obtaining the two-dimensional transition metal sulfide material flexible sensor.
The invention has the advantages of simple and feasible electrode construction, no packaging difficulty and high success rate of device preparation.
Compared with the prior art, the invention has the following beneficial effects:
1) The device has a simple structure, the two-dimensional material is tightly combined with the paper-based flexible substrate through suction filtration, so that the adhesion degree is high, the conductive electrode is convenient to build, and the overall preparation cost is low;
2) The preparation process of the integral device has no special requirements on two-dimensional materials, other substances which are difficult to remove are not introduced, and the preparation method of the flexible sensor device has universality and stable performance and is suitable for large-scale production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a flow chart of a method for manufacturing a two-dimensional transition metal sulfide material flexible sensor according to an embodiment of the present invention;
figure 2 is a structural diagram of a two-dimensional tungsten disulfide-based flexible device in accordance with embodiment 1 of the present invention;
FIG. 3 is a graph of a response curve obtained by an example of the present invention;
FIG. 4 is a flow chart illustrating the preparation of a flexible sensor according to a comparative example of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
As shown in fig. 1, a method for preparing a two-dimensional transition metal sulfide material flexible sensor includes the following steps:
(1) Taking 0.6g of lamellar tungsten disulfide powder, placing the powder in a 30mL conical flask, and moving the conical flask into a glove box protected by inert gas; adding 15mL of n-butyllithium solution (the concentration: 2M, solvent: n-hexane) into a conical flask, sealing, heating at 60 ℃ and stirring for 24 hours; filtering the tungsten disulfide powder treated by the n-butyllithium by using n-hexane, removing n-butyllithium on the surface, placing the tungsten disulfide powder into a three-neck flask, adding 100mL of deionized water, ultrasonically stripping for 1h, and collecting the ultrasonically-treated suspension;
(2) Centrifuging the suspension at 1500r/min for 15min, and removing the un-peeled thick sheet to obtain a two-dimensional tungsten disulfide suspension;
(3) And (3) carrying out suction filtration on 30mL of suspension to a polyvinylidene fluoride filter membrane (Merke Millipore company, with the pore diameter of 0.22um, GVHHP04700), washing for three times with water and alcohol, removing impurities, placing at 45 ℃, and carrying out vacuum drying for 2 hours to obtain the two-dimensional tungsten disulfide composite film which is tightly attached to the filter membrane and is uniformly dispersed.
(4) According to the shape requirement of the device, trimming the two-dimensional tungsten disulfide composite film, attaching a proper double-sided conductive belt (single-sided adhesive) to the surface of the two-dimensional transition metal sulfide and the surface of the filter membrane, attaching a DuPont wire to the tail end of the conductive adhesive tape to form a conductive path from an electrode to a semiconductor material, and finally preparing the two-dimensional tungsten disulfide-based flexible sensor device (shown in figure 2) which is simple in structure and is tightly combined.
Example 2
As shown in fig. 1, a method for preparing a two-dimensional transition metal sulfide material flexible sensor includes the following steps:
(1) Taking 0.3g of lamellar tungsten disulfide powder, placing the powder in a 30mL conical flask, and moving the conical flask into a glove box protected by inert gas; adding 10mL of n-butyllithium solution (concentration: 1.8M, solvent: n-hexane) into a conical flask, sealing, heating at 60 ℃ and stirring for 24h; filtering the tungsten disulfide powder treated by the n-butyl lithium by using n-hexane, removing the n-butyl lithium on the surface, placing the tungsten disulfide powder into a three-neck flask, adding 80mL of deionized water, carrying out ultrasonic stripping for 1h, and collecting suspension after ultrasonic stripping;
(2) Centrifuging the suspension at 1500r/min for 10min, and removing the un-peeled thick sheet to obtain a two-dimensional tungsten disulfide suspension;
(3) And (3) carrying out suction filtration on 30mL of suspension to a polyvinylidene fluoride filter membrane (Merke Millipore company, with the pore diameter of 0.22um, GVHHP04700), washing for three times with water and alcohol, removing impurities, placing at 45 ℃, and carrying out vacuum drying for 1.5 hours to obtain the two-dimensional tungsten disulfide composite film which is tightly attached to the filter membrane and is uniformly dispersed.
(4) According to the shape requirements of the device, trimming the two-dimensional tungsten disulfide composite film, attaching a suitable double-sided conductive belt (single-sided adhesive) to the surfaces of the two-dimensional transition metal sulfide and the filter membrane, attaching a DuPont wire to the tail end of the conductive adhesive tape to form a conductive path from an electrode to a semiconductor material, and finally preparing the two-dimensional tungsten disulfide-based flexible sensor device (shown in figure 2) which is simple in structure and compact in combination.
Example 3
As shown in fig. 1, a method for preparing a two-dimensional transition metal sulfide material flexible sensor includes the following steps:
(1) Taking 0.8g of lamellar tungsten disulfide powder, placing the powder in a 30mL conical flask, and moving the conical flask into a glove box protected by inert gas; 20mL of an n-butyllithium solution (concentration: 2.2M, solvent: n-hexane) was put into a conical flask, and after sealing, the mixture was heated at 40 ℃ and stirred for 48 hours; filtering the tungsten disulfide powder treated by the n-butyllithium by using n-hexane, removing n-butyllithium on the surface, placing the tungsten disulfide powder into a three-neck flask, adding 100mL of deionized water, ultrasonically stripping for 1.5h, and collecting the ultrasonically-treated suspension;
(2) Centrifuging the suspension at 3000r/min for 15min, and removing the un-peeled thick sheet to obtain a two-dimensional tungsten disulfide suspension;
(3) And (3) carrying out suction filtration on 30mL of the suspension liquid to a polyvinylidene fluoride filter membrane (Merck Millipore, pore diameter of 0.22um, GVHHP04700), washing with water and alcohol for three times, removing impurities, placing at 55 ℃, and carrying out vacuum drying for 2 hours to obtain the two-dimensional tungsten disulfide composite membrane which is tightly attached to the filter membrane and uniformly dispersed.
(4) According to the shape requirements of the device, trimming the two-dimensional tungsten disulfide composite film, attaching a suitable double-sided conductive belt (single-sided adhesive) to the surfaces of the two-dimensional transition metal sulfide and the filter membrane, attaching a DuPont wire to the tail end of the conductive adhesive tape to form a conductive path from an electrode to a semiconductor material, and finally preparing the two-dimensional tungsten disulfide-based flexible sensor device (shown in figure 2) which is simple in structure and compact in combination.
Application example
(1) When the device prepared in example 1 was placed between the upper lip and the nose, a graph of the response of the two-dimensional tungsten disulfide flexible sensor device to relatively weak and deep respiratory signals was obtained, i.e., (a) in fig. 3; by detecting the change of the current signal intensity of the sensor, the product can detect and distinguish the conditions of weak respiration and deep respiration, and the main principle is that the difference of airflow intensity and water oxygen flow exists due to different expiration intensities, so that the change of the concentration of tungsten disulfide carriers of a sensitive material of the sensor can be caused, and the change of the current signal intensity is finally reflected.
(2) The device prepared in example 1 was tested in a real environment for a 500ppm concentration of continuously pulsed NH 3 Gas, resulting in a response curve, i.e., (b) in fig. 3; NH (NH) 3 Molecules and WS 2 Will adsorb to generate electronic interaction to induce WS 2 Change in baseline Current, WS at room temperature can be seen 2 For 500ppm of pulse NH 3 The response intensity of the gas is about 6%.
(3) The device prepared in example 1 was subjected to simultaneous bending response and 200ppm NH under a closed cavity 3 Response of gas, get the response curve chart, namely (c) in fig. 3, the inset shows the enlarged view of the curve of response of bending (the bending radius is 10 mm); by introducing NH 3 Bending experiments were performed on the sensor while gas was present, and it can be seen that the sensor showed NH response under the integral response 3 The gas has 6% response intensity, and the amplified signal diagram shows that the device also shows the phenomenon of regular current change for bending. This shows that the flexible sensor can simultaneously realize the acquisition and presentation of multiple signals of gas response and bending response.
(4) Detection of device prepared in example 1 was bent 8000 times and passed back and forthSensor pair 500ppm NH 3 The response curve of (a) in fig. 3 is obtained. Repeated bending experiments show that the flexible sensor can still keep good current response, and the two-dimensional transition metal sulfide flexible sensor prepared by the method is proved to have the advantages that materials are tightly combined with a flexible substrate, and the shedding phenomenon does not occur, so that the electrical performance of the device is stable.
Comparative example
A more advanced way of preparing two-dimensional transition metal sulfide-based flexible sensors in the current literature report is shown in FIG. 4, and the report by Zhao et al (reference: zhao Y, song J G, ryu G H, et al, low-temperature synthesis of 2D MoS) 2 on a plastic substrate for a flexible gas sensor[J]Nanoscale,2018,10 (19): 9338-9345) a vapor deposition method (CVD) of growing a two-dimensional molybdenum sulfide material on a conventional flexible substrate PI at a relatively low temperature (200 ℃), and then evaporating a titanium (Ti, 2 nm)/gold (Au, 40 nm) electrode onto the PI substrate on which the two-dimensional molybdenum sulfide material is grown by a mask by a thermal evaporation method, thereby preparing a two-dimensional molybdenum sulfide-based flexible gas sensor; the method has high experimental condition requirements on material preparation means, the experiment needs to be carried out under a high-temperature tube furnace, the substrate PI material needs to be subjected to strict cleaning steps and then can be used for material growth, the randomness of a material growth experiment is high, and the yield cannot be guaranteed; in addition, the electrodes can be adhered to the material only by a method of thermally evaporating metal electrodes through a complex and expensive mask plate, the preparation is complex and the cost is high, and a two-dimensional metal sulfide-based flexible sensor device cannot be prepared in a large scale.
The various embodiments are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the various embodiments can be referred to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A two-dimensional transition metal sulfide material flexible sensor is characterized by comprising an electrode, a lead and a semiconductor material; the electrode is connected with the semiconductor material through the lead, and the semiconductor material comprises a filter membrane substrate, a two-dimensional transition metal sulfide and a conductive band connected with the filter membrane substrate and the two-dimensional transition metal sulfide;
the preparation method of the semiconductor material comprises the following steps:
(1) Mixing transition metal sulfide powder with n-butyllithium solution, heating and stirring at 40-60 ℃ for 24-48h, filtering, adding deionized water into the precipitate, and ultrasonically stripping for 1-1.5h to obtain suspension;
(2) Centrifuging the suspension, and removing precipitates to obtain a two-dimensional transition metal sulfide suspension;
(3) Carrying out suction filtration on the two-dimensional transition metal sulfide suspension to a filter membrane substrate, and then carrying out water washing, alcohol washing and drying to obtain a two-dimensional transition metal sulfide composite film;
(4) And connecting the conductive band with the surface of the two-dimensional transition metal sulfide and the surface of the filter membrane substrate to obtain the semiconductor material.
2. The flexible sensor as claimed in claim 1, wherein the filter substrate is a filter with a pore size of less than 0.22 um.
3. The flexible sensor as claimed in claim 1, wherein the filter substrate is any one of a polyvinylidene fluoride filter, a hydrophilic polycarbonate microporous filter and a mixed cellulose filter.
4. The flexible sensor of claim 1, wherein in the step (1), the transition metal sulfide powder is molybdenum sulfide or tungsten sulfide, and the concentration of the n-butyllithium solution is 1.8-2.2mol/L.
5. The flexible sensor for the two-dimensional transition metal sulfide material according to claim 1, wherein the mass-to-volume ratio of the transition metal sulfide powder to the n-butyllithium solution in step (1) is 0.3-0.8g.
6. The flexible sensor for the two-dimensional transition metal sulfide material according to claim 1, wherein the mass volume ratio of the transition metal sulfide powder to the deionized water in step (1) is 0.3-0.8g.
7. A two-dimensional transition metal sulfide material flexible sensor according to claim 1, wherein the centrifugation in step (2) is performed under the following conditions: centrifuging at 1500-3000r/min for 10-15min.
8. A two-dimensional transition metal sulfide material flexible sensor according to claim 1, wherein the drying condition in step (3) is: vacuum drying at 45-55 deg.C for 1.5-2 hr.
9. The method for preparing the flexible sensor of the two-dimensional transition metal sulfide material according to any one of claims 1 to 8, characterized by comprising the following specific steps: and connecting one end of a lead with the electrode, and attaching the other end of the lead to the tail end of the conductive belt to form a conductive path from the electrode to the semiconductor material, thus obtaining the two-dimensional transition metal sulfide material flexible sensor.
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