CN108845017B - Flexible ion sensor based on tungsten diselenide - Google Patents
Flexible ion sensor based on tungsten diselenide Download PDFInfo
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- CN108845017B CN108845017B CN201810550806.6A CN201810550806A CN108845017B CN 108845017 B CN108845017 B CN 108845017B CN 201810550806 A CN201810550806 A CN 201810550806A CN 108845017 B CN108845017 B CN 108845017B
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- tungsten diselenide
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- boron nitride
- ionophore
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- ROUIDRHELGULJS-UHFFFAOYSA-N bis(selanylidene)tungsten Chemical compound [Se]=[W]=[Se] ROUIDRHELGULJS-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229910052582 BN Inorganic materials 0.000 claims abstract description 26
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000002555 ionophore Substances 0.000 claims abstract description 24
- 230000000236 ionophoric effect Effects 0.000 claims abstract description 22
- 229910052751 metal Inorganic materials 0.000 claims abstract description 19
- 239000002184 metal Substances 0.000 claims abstract description 19
- 239000000758 substrate Substances 0.000 claims abstract description 9
- 229910052737 gold Inorganic materials 0.000 claims abstract description 5
- 150000002500 ions Chemical class 0.000 claims description 34
- 239000010410 layer Substances 0.000 abstract description 46
- 239000000463 material Substances 0.000 abstract description 21
- 238000000034 method Methods 0.000 abstract description 12
- 230000035945 sensitivity Effects 0.000 abstract description 6
- 239000002356 single layer Substances 0.000 abstract description 6
- 238000005452 bending Methods 0.000 abstract description 5
- 239000011241 protective layer Substances 0.000 abstract description 2
- 239000007772 electrode material Substances 0.000 abstract 1
- XIMIGUBYDJDCKI-UHFFFAOYSA-N diselenium Chemical compound [Se]=[Se] XIMIGUBYDJDCKI-UHFFFAOYSA-N 0.000 description 8
- 230000007774 longterm Effects 0.000 description 6
- -1 tungsten diselenide ion Chemical class 0.000 description 6
- 238000000059 patterning Methods 0.000 description 4
- 229920002120 photoresistant polymer Polymers 0.000 description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 description 4
- 239000005020 polyethylene terephthalate Substances 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 description 3
- 229920005570 flexible polymer Polymers 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000223 sodium ionophore Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/403—Cells and electrode assemblies
- G01N27/414—Ion-sensitive or chemical field-effect transistors, i.e. ISFETS or CHEMFETS
- G01N27/4146—Ion-sensitive or chemical field-effect transistors, i.e. ISFETS or CHEMFETS involving nanosized elements, e.g. nanotubes, nanowires
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Electrochemistry (AREA)
- Biochemistry (AREA)
- Molecular Biology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
A flexible ion sensor based on tungsten diselenide belongs to the technical field of MEMS. The sensor array is characterized in that tungsten diselenide is adopted as a sensitive material; the sensor structure comprises an ionophore, a boron nitride layer, a tungsten diselenide layer and a flexible substrate from top to bottom. Two ends of the tungsten diselenide layer are connected with the metal electrode; the thickness of the ionophore is 20-200 micrometers; the boron nitride layer is a single layer or a plurality of layers; the metal electrode material is any one of Au, ag, cu, al, pt with the thickness of 20-200 nanometers; the tungsten diselenide layer is a single layer or a plurality of layers; the upper surface of the tungsten diselenide layer is completely covered by the ionophore and the boron nitride layer. According to the invention, tungsten diselenide is used as a sensitive material, boron nitride is used as a protective layer, and an ionophore is used as a selective layer, so that the sensitivity, stability and selectivity of the flexible ion sensor can be improved, and the sensor has excellent bending resistance and is easy to process.
Description
Technical Field
The invention relates to the technical field of MEMS (micro electro mechanical systems), in particular to a flexible ion sensor based on tungsten diselenide.
Background
The two-dimensional material tungsten diselenide has extremely large specific surface area, extremely low noise and energy gap of not 0, and the characteristics determine that the sensor based on the tungsten diselenide has extremely high sensitivity and extremely low detection lower limit; the tungsten diselenide can be prepared in a large area by a chemical vapor deposition method, is easy to process and has the potential of integration; tungsten diselenide has high fracture strain and excellent bending resistance, and the wearable flexible device often needs to generate large deformation, so that the tungsten diselenide is an ideal choice as a sensitive material of the flexible sensor. There is no report on a tungsten diselenide ion sensor.
The main problems of tungsten diselenide as a sensitive material are: 1. the upper surface of the tungsten diselenide is exposed in the air for a long time, and oxygen, water vapor and the like can gradually degrade the electrical characteristics of the tungsten diselenide, so that the performance of the device can be obviously drifted, and the long-term stability is influenced. 2. Tungsten diselenide has poor selectivity, can respond to any ion, and can not distinguish detected ions in actual liquid with complex components. Therefore, the problem of long-term stability and selectivity of the tungsten diselenide flexible ion sensor is important.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a flexible ion sensor based on tungsten diselenide, which adopts tungsten diselenide as a sensitive material, so that the sensor has extremely high sensitivity and extremely low detection lower limit and has excellent bending resistance; boron nitride is used as a protective layer, so that the long-term stability of the sensor can be improved; the ionophore is used as a selective layer to solve the problem of sensor selectivity.
In order to achieve the above object, the present invention is achieved by the following method:
the flexible ion sensor based on the tungsten diselenide is characterized by sequentially comprising an ionophore 1-1, a boron nitride layer 1-2, a metal electrode 1-3, a tungsten diselenide layer 1-4 and a flexible substrate 1-5 from top to bottom, wherein two ends of the tungsten diselenide layer 1-4 are connected with the metal electrode 1-3.
The thickness of the ionophore 1-1 is 20-200 micrometers.
The boron nitride layer 1-2 is a single layer or multiple layers, typically 1-10 layers.
The metal electrode 1-3 is made of any one of Au, ag, cu, al, pt with the thickness of 20-200 nanometers.
The tungsten diselenide layers 1-4 are single or multiple layers, generally 1-10 layers.
The upper surface of the tungsten diselenide layer 1-4 is completely covered by the boron nitride layer 1-2, and the surface areas of the ionophore 1-1 and the boron nitride layer 1-2 are larger than or equal to the tungsten diselenide layer 1-4; the surface area of the ionophore 1-1 is smaller than or equal to the surface area 1-2 of the boron nitride layer 1-2.
The beneficial effects of the invention are as follows:
(1) High sensitivity
The sensitivity of an ion sensor depends on the specific surface area and the energy band structure of the sensitive material. The tungsten diselenide has extremely large specific surface area and the forbidden bandwidth is not 0, so the tungsten diselenide-based ion sensor has extremely high sensitivity.
(2) High bending resistance
Wearable flexible sensors need to often undergo large deformations. The tungsten diselenide as the sensor sensitive material has excellent mechanical property and higher breaking strain (difficult breaking), so the sensor has strong bending resistance.
(3) Good selectivity
The tungsten diselenide sensor is covered with the ionophore, so that the interference of other ions in the solution can be eliminated, and the sensor has the capability of distinguishing the detected ions (excellent selectivity).
(4) Good long-term stability
The long term stability of an ion sensor depends on the stability of the sensitive material tungsten diselenide in air. The boron nitride layer is covered on the surface of the tungsten diselenide, so that the gradual degradation of the electrical characteristics of the tungsten diselenide caused by oxygen, water vapor and the like in the air can be avoided, and the long-term stability of the sensor is improved.
Drawings
FIG. 1 is a side view of a tungsten diselenide-based flexible ion sensor of the present invention, showing a 1-ionophore, a 1-2-boron nitride layer, a 1-3-metal electrode, a 1-4-tungsten diselenide layer, and a 1-5-flexible substrate.
FIG. 2 is a top view of a flexible tungsten diselenide-based ion sensor of the present invention showing a 1-ionophore, 1-3-metal electrode, 1-4-tungsten diselenide layer, 1-5-flexible substrate.
Fig. 3 is a flow chart of the process of the tungsten diselenide flexible ion sensor of the invention.
FIG. 4 is a graph of the response of a tungsten diselenide ion sensor to sodium ions of different concentrations.
Detailed Description
The technical scheme of the invention is further described below by referring to examples.
Referring to fig. 1 and 2, a flexible ion sensor based on tungsten diselenide is characterized in that the sensor sequentially comprises an ionophore 1-1, a boron nitride layer 1-2, a metal electrode 1-3, a tungsten diselenide layer 1-4 and a flexible substrate 1-5 from top to bottom, and two ends of the tungsten diselenide layer 1-4 are connected with the metal electrode 1-3.
The thickness of the ionophore 1-1 is 20-200 micrometers.
The boron nitride layer 1-2 is a single layer or a plurality of layers, generally 1-10 layers, and when the thickness of the boron nitride material is reduced to 10 layers or less, the boron nitride material becomes a two-dimensional material, and the material performance of the two-dimensional material is completely different from that of a bulk boron nitride material. The metal electrode 1-3 is made of any one of Au, ag, cu, al, pt with the thickness of 20-200 nanometers.
The tungsten diselenide layers 1-4 are single layers or multiple layers, generally 1-10 layers, and when the thickness of the diselenide material is reduced to 10 layers or less, the tungsten diselenide material becomes a two-dimensional material, and the material performance of the tungsten diselenide material is completely different from that of the bulk diselenide material.
The upper surface of the tungsten diselenide layer 1-4 is completely covered by the boron nitride layer 1-2, and the surface areas of the ionophore 1-1 and the boron nitride layer 1-2 are larger than or equal to the tungsten diselenide layer 1-4; the surface area of the ionophore 1-1 is smaller than or equal to the surface area 1-2 of the boron nitride layer 1-2.
The specific processing flow of the tungsten diselenide sensor array of the invention is as follows (figure 3):
preparation and patterning of tungsten diselenide
The tungsten diselenide 1-4 is prepared by adopting a chemical vapor deposition method. It was transferred to the surface of the flexible polymer PET (polyethylene terephthalate) substrate 1-5 by PDMS (polydimethylsiloxane). And adopting photoetching and plasma dry etching technology to realize tungsten diselenide patterning.
(II) sensor processing
A layer of negative photoresist is coated on the surface of the flexible polymer PET substrate in a spin mode (the rotating speed of a spin coater is 1000-4000RPM, the time is 30-90 seconds), and the photoresist is heated on a hot plate for 1-2 minutes at the temperature of 90-120 ℃. Patterning was performed by exposure (1-2 min), post-bake (90-120 ℃,2-3 min), and development (soaking in RD6 developer for 1-2 min). And growing gold with the thickness of 10 nanometers of titanium and 50-100 nanometers by adopting a sputtering process. The sample was immersed in acetone with the aid of ultrasonic vibration, with the aim of removing the photoresist and the metal adhering to the surface of the photoresist (stripping process). And patterning the metal layer through a stripping process to form the metal electrode 1-3. And transferring the boron nitride 1-2 prepared by the chemical vapor deposition method to the surface of the flexible polymer PET substrate by PDMS.
(III) modified ionophores
And (3) modifying a layer of ionophore solution on the surface of the tungsten diselenide by a spin coating method. After 5-10 minutes, the solid ion carrier layer 1-1 is formed after the solvent is volatilized. An ionophore is permeable to only one type of ion (e.g., sodium ionophore is permeable to only Na + )。
Calibration and test of tungsten diselenide sensor
Firstly, respectively immersing the tungsten diselenide sensor by using standard ion solutions with different concentrations, measuring the resistance value of the tungsten diselenide between two metal electrodes by using a universal meter or a semiconductor parameter tester after the sensor is stable for 1-5 minutes, and determining the change rule of the sensor along with the ion concentration through a calibration process. And then immersing the sensor part by using the measured solution, measuring the resistance value of the sensor after the sensor is stable, and comparing the resistance value with a calibration result, thereby obtaining the concentration value of the ions to be measured in the measured solution. Fig. 4 is a graph of the results of the tungsten diselenide ion sensor response to sodium ions of different concentrations, showing the feasibility of the tungsten diselenide ion sensor.
The working principle of the invention is as follows:
the diselenide sensor has a structure similar to a MOS tube. The metal electrodes (1-3) at the two ends of the diselenide (1-4) correspond to the source electrode and the drain electrode of the MOS tube, and the ionophore (1-1) is equivalent to the grid electrode of the MOS tube. After the ion to be detected enters the ionophore (1-1), the potential of the ionophore (1-1) is changed, which is equivalent to the change of the grid voltage, so that the conductivity (resistivity) of the diselenide is changed. The amount of change in gate voltage is related to the concentration of the measured ions in the solution. Information on the concentration of the ions to be measured can thus be obtained by measuring the amount of change in the electrical properties (resistivity) of the diselenide.
Claims (4)
1. The flexible ion sensor based on the tungsten diselenide is characterized in that the sensor sequentially comprises an ion carrier (1-1), a boron nitride layer (1-2), a metal electrode (1-3), a tungsten diselenide layer (1-4) and a flexible substrate (1-5) from top to bottom, wherein two ends of the tungsten diselenide layer (1-4) are connected with the metal electrode (1-3), the metal electrode (1-3) is positioned at two ends of the tungsten diselenide layer (1-4) and corresponds to a source electrode and a drain electrode of a MOS tube, the ion carrier (1-1) is equivalent to a grid electrode of the MOS tube, and after detected ions enter the ion carrier (1-1), the potential of the ion carrier (1-1) is changed and is equivalent to the change of the grid voltage, so that the conductive characteristic of the tungsten diselenide is changed;
the boron nitride layer (1-2) is 1-10 layers;
the tungsten diselenide layer (1-4) is 1-10 layers.
2. A flexible ion sensor based on tungsten diselenide according to claim 1, characterized in that the thickness of the ionophore (1-1) is 20-200 micrometers.
3. The flexible ion sensor of claim 1, wherein the metal electrode (1-3) is made of any one of Au, ag, cu, al, pt and has a thickness of 20-200 nm.
4. The flexible ion sensor based on tungsten diselenide according to claim 1, wherein the upper surface of the tungsten diselenide layer (1-4) is completely covered by the boron nitride layer (1-2), and the surface areas of the ionophore (1-1) and the boron nitride layer (1-2) are equal to or larger than that of the tungsten diselenide layer (1-4); the surface area of the ion carrier (1-1) is smaller than or equal to that of the boron nitride layer (1-2).
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| CN109297622B (en) * | 2018-11-08 | 2024-02-02 | 清华大学 | Miniature piezoresistive stress sensor based on tungsten diselenide |
| CN116926672A (en) * | 2022-04-07 | 2023-10-24 | 北京大学 | Method for vertical heteroepitaxy high-orientation metal platinum based on monocrystal tungsten diselenide |
| CN116839768B (en) * | 2023-06-30 | 2024-02-20 | 济南大学 | Miniature piezoresistive stress sensor based on tungsten diselenide |
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| CN106198676A (en) * | 2015-05-08 | 2016-12-07 | 中国科学院烟台海岸带研究所 | A kind of solid contact potassium ion-selective electrode and preparation thereof and application |
| CN107238648A (en) * | 2017-06-13 | 2017-10-10 | 复旦大学 | The method of low temperature preparation two-dimension flexible ion sensing fet |
| CN107449816A (en) * | 2016-05-30 | 2017-12-08 | 中国科学院化学研究所 | All solid state ISE, preparation method and biology sensor |
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| CN208366907U (en) * | 2018-05-31 | 2019-01-11 | 清华大学 | Flexible ion transducer based on two tungsten selenides |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US9548394B2 (en) * | 2014-04-22 | 2017-01-17 | Uchicago Argonne, Llc | All 2D, high mobility, flexible, transparent thin film transistor |
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Patent Citations (5)
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|---|---|---|---|---|
| CN106198676A (en) * | 2015-05-08 | 2016-12-07 | 中国科学院烟台海岸带研究所 | A kind of solid contact potassium ion-selective electrode and preparation thereof and application |
| CN107449816A (en) * | 2016-05-30 | 2017-12-08 | 中国科学院化学研究所 | All solid state ISE, preparation method and biology sensor |
| CN107238648A (en) * | 2017-06-13 | 2017-10-10 | 复旦大学 | The method of low temperature preparation two-dimension flexible ion sensing fet |
| CN107706260A (en) * | 2017-07-28 | 2018-02-16 | 中国空间技术研究院 | A kind of two tungsten selenide thin slices/indium oxide nano thread composite construction near infrared photodetector and preparation method thereof |
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