CN111307911B - PH sensor and preparation method thereof - Google Patents
PH sensor and preparation method thereof Download PDFInfo
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- CN111307911B CN111307911B CN201811514391.3A CN201811514391A CN111307911B CN 111307911 B CN111307911 B CN 111307911B CN 201811514391 A CN201811514391 A CN 201811514391A CN 111307911 B CN111307911 B CN 111307911B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000010408 film Substances 0.000 claims abstract description 24
- 239000000758 substrate Substances 0.000 claims abstract description 16
- 229920002120 photoresistant polymer Polymers 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000003989 dielectric material Substances 0.000 claims abstract description 9
- 238000000151 deposition Methods 0.000 claims abstract description 6
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 5
- 230000008021 deposition Effects 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 239000011248 coating agent Substances 0.000 claims abstract description 4
- 238000000576 coating method Methods 0.000 claims abstract description 4
- 239000010409 thin film Substances 0.000 claims abstract description 4
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 3
- 238000000427 thin-film deposition Methods 0.000 claims abstract description 3
- 238000000206 photolithography Methods 0.000 claims description 3
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 abstract description 7
- 239000010410 layer Substances 0.000 description 9
- 238000001514 detection method Methods 0.000 description 7
- 230000005669 field effect Effects 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 5
- 238000000089 atomic force micrograph Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000012544 monitoring process Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 230000010354 integration Effects 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- 239000002356 single layer Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical group [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 230000006399 behavior Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 125000004434 sulfur atom Chemical group 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000010256 biochemical assay Methods 0.000 description 1
- 238000005842 biochemical reaction Methods 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000000835 electrochemical detection Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- -1 hydrogen ions Chemical class 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000036403 neuro physiology Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 239000007793 ph indicator Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/24—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only semiconductor materials not provided for in groups H01L29/16, H01L29/18, H01L29/20, H01L29/22
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
- H01L29/66007—Multistep manufacturing processes
- H01L29/66969—Multistep manufacturing processes of devices having semiconductor bodies not comprising group 14 or group 13/15 materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
- H01L29/68—Types of semiconductor device ; Multistep manufacturing processes therefor controllable by only the electric current supplied, or only the electric potential applied, to an electrode which does not carry the current to be rectified, amplified or switched
- H01L29/76—Unipolar devices, e.g. field effect transistors
- H01L29/772—Field effect transistors
- H01L29/78—Field effect transistors with field effect produced by an insulated gate
- H01L29/786—Thin film transistors, i.e. transistors with a channel being at least partly a thin film
Abstract
The invention discloses a pH sensor and a preparation method thereof. The pH sensor comprises an insulating substrate material, moS deposited on the insulating substrate material 2 A thin film, a source electrode, a drain electrode, and a dielectric material; wherein the source electrode, the drain electrode and the dielectric material are formed on MoS 2 The periphery of the film forms a closed sensor groove. The preparation method comprises the following steps: (1) cleaning a substrate, and coating a photoresist layer on the substrate; (2) Formation of MoS by exposure to photoresist 2 A thin film deposition region; (3) Deposition of MoS in this region using chemical vapor deposition techniques 2 Form MoS 2 A film; (4) Removing photoresist to preserve MoS 2 Film pattern, then in MoS 2 Forming a source electrode and a drain electrode on the outer side of the film pattern; (5) A dielectric material is deposited to form a sensor trench, resulting in a device cell of the pH sensor. The pH sensor constructed by the invention has the advantages of excellent electrical signal, high sensitivity and good stability.
Description
Technical Field
The invention relates to a pH sensor and a preparation method thereof, and belongs to the technical field of sensors.
Background
An Ion sensitive field effect transistor (Ion-Sensitive Field Effect Transistor, ISFET for short) is used as a sensitive device for detecting biochemical signals, is firstly proposed by a Netherlands scientist P.Bergveld in 1970 and is used for measuring neurophysiology, a new research prologue of a biochemical sensor is uncovered from the beginning, and new vitality is injected into the research of an electrochemical biochemical sensor, so that the Ion sensitive field effect transistor has epoch-making significance.
The most basic application of ISFETs is in pH detection, where many biochemical assays are based on monitoring pH changes in biochemical reactions, but want to make a breakthrough in the related art as if it were a long-lasting war in open field. For example, many species of bacteria need to grow in specific dishes and are isolated until their numbers are sufficiently large under oxidizing or fermenting conditions. Currently, if it is desired to detect changes in the pH of the surrounding environment produced by bacteria, it is generally necessary to use a colored pH indicator to obtain relevant experimental data in a lengthy wait of about 24-36 hours. Therefore, development of micro-detection techniques such as micro-fluidic devices and micro-sensors is imperative to improve the related detection techniques.
In recent years, with the unique structure of a Metal-Oxide-semiconductor field effect transistor (MOSFET), an ISFET has been designed to realize a novel biochemical sensor with excellent characteristics such as higher sensitivity, high resolution, and short response time. The sensor has the advantages of small volume, low manufacturing cost, easy integration, no damage, durable measurement and the like, can meet the requirements of various specific detection through changing corresponding sensitive materials, and can be widely applied to a plurality of fields of food safety, biomedicine, environmental monitoring, military aerospace, agricultural machinery, industrial control and judicial identification.
ISFETs differ from traditional biochemical sensors using ion selective electrodes in that they have smaller volumes, faster detection speeds, fewer detection samples are required for detection, and are more suitable for real-time and continuous systematic monitoring. The basic device structure of an ISFET is very similar to a MOSFET, and can be considered as a MOSFET with a metal gate removed, where a sensitive thin film is deposited on the gate dielectric layer and in direct contact with an electrolytic solution, and where certain ion concentration changes or certain specific behaviors in the solution can result in corresponding interface potentials and potential distributions that result in corresponding changes in the threshold voltage of the ISFET device. These changes can be obtained by measuring the change of the reference electrode potential under the same source-drain current or directly measuring the change of the source-drain current to obtain the change of the ion concentration in the solution and the generation of related specific behaviors.
For ISFETs, the choice of sensitive layer material directly determines the detection sensitivity of the ISFET device.
Disclosure of Invention
The invention aims to provide a pH sensor which selects a sensitive material with certain specificity and sensitivity to hydrogen ions and has extremely high sensitivity characteristics.
Another object of the invention is to provide a method for manufacturing said sensor.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a pH sensor includes an insulating substrate material, moS deposited on the insulating substrate material 2 A thin film, a source electrode, a drain electrode, and a dielectric material; wherein the source electrode, the drain electrode and the dielectric material are formed on MoS 2 The periphery of the film forms a closed sensor groove.
The invention uses MoS 2 The film is used as a sensitive layer material to prepare a pH sensor, and the pH sensor is a sensor based on a similar field effect transistor structure. MoS (MoS) 2 The material is a layered crystal. Each of its layer planes contains one unit cell and the planes are held together by van der waals forces. Each MoS 2 The unit cell is composed of sulfur atoms and molybdenum atoms sandwiched between the sulfur atoms. When peeled off into a single layer or few layers, two-dimensional MoS 2 The materials exhibit unique electrical, optical, mechanical and chemical properties. Like graphene and other two-dimensional nanomaterials, moS 2 The biosensing performance can be significantly improved due to its large surface area and good biocompatibility. And due to the existence of direct band gap, is based on MoS 2 The overall sensitivity of the FET biosensor is much greater than devices based on graphene and graphene oxide that do not have or have small bandgaps.
A method for preparing the pH sensor, comprising the steps of:
(1) Cleaning a substrate, and coating a layer of photoresist on the substrate;
(2) Formation of MoS by exposure to photoresist 2 A thin film deposition region;
(3) Deposition of MoS in this region using chemical vapor deposition techniques 2 Form MoS 2 A film;
(4) Removing photoresist to preserve MoS 2 Film pattern, then in MoS 2 Forming a source electrode and a drain electrode on the outer side of the film pattern;
(5) A dielectric material is deposited to form a sensor trench, resulting in a device cell of the pH sensor.
The invention has the advantages that:
(1) The operation is simple, and the time is saved. The invention constructs high-performance MoS 2 The pH sensor of (c) enables rapid monitoring.
(2) Economical. The construction of a sensor device using the present invention requires little cost.
(3) High yield and easy integration. Chip-type sensing devices can be fabricated using standard metal oxide semiconductor processes, and the smaller chip size facilitates future integration of other modules.
(4) The performance is excellent. The pH sensor constructed by the invention has excellent electrical signals and good stability.
Drawings
Fig. 1 is a schematic diagram showing a process for manufacturing a pH sensor according to the present invention.
Fig. 2 is a schematic cross-sectional structure of the pH sensor of the present invention.
Fig. 3 is a schematic diagram of the operation of the pH sensor of the present invention.
FIGS. 4 ((a) - (c)) are single-layer MoS in the pH sensor of the present invention 2 AFM image of film.
FIGS. 5 ((a) - (c)) are bilayer MoS in the pH sensor of the present invention 2 AFM image of film.
FIG. 6 is a graph showing the gate voltage versus leakage current for different pH values in the pH sensor according to example 1.
FIG. 7 is a graph showing the relationship between pH and threshold voltage and current when tested using the pH sensor of example 1.
Detailed Description
The invention is described in further detail below with reference to the drawings and examples, but is not meant to limit the scope of the invention.
As shown in fig. 1, the pH sensor of the present invention is a sensor based on a similar field effect transistor structure, and the preparation process is as follows; firstly, cleaning a silicon oxide substrate 1, coating a photoresist 2 on the silicon oxide substrate 1, and then exposing to MoS to be deposited 2 Pattern 3 of film, deposition of MoS by CVD method 2 Film 4, photoresist removed and MoS retained 2 Film pattern, then in MoS 2 And forming a source electrode 5 and a drain electrode 6 on the outer side of the film pattern, and finally depositing a dielectric material 7 to form a sensor groove, so that the device of the whole sensor is in a groove shape for the electrolyte to be detected and is isolated from the surrounding.
Example 1
FIG. 2 is a schematic cross-sectional view of the pH sensor according to the present invention. Specifically, the manufacturing method of the pH sensor comprises the following processes:
in SiO 2 Spin-coating SU-8 GM10xx series photoresist on (300 nm)/Si substrate, exposing to obtain MoS to be deposited with thickness of 3 μm 2 Patterning of the film, followed by deposition of MoS using CVD methods 2 The film comprises the following specific technical processes: the temperature of the growth zone is 650 ℃, the temperature of the sulfur zone is 180 ℃, the loading amounts of the sulfur source and the molybdenum source are 1000mg and 100mg respectively, the growth time is 20min, and the carrier gas flow rate is 10sccm. Then removing the photoresist to obtain MoS 2 And (5) film patterns. The source and drain electrodes are fabricated using photolithography and electron beam evaporation. The size of the individual chip is 10 μm. The thickness of the source electrode and the drain electrode is 500nm, and the interval between the two electrodes is 10 μm. Meanwhile, in order to enhance the adhesion between the Au electrode and the silicon oxide substrate, a Ti layer having a thickness of 20nm was additionally added therebetween. Then using photolithography and magnetron sputtering method to grow HfO 2 And the thickness of the dielectric layer is 500nm.
Fig. 3 is a schematic diagram of the operation of the sensor of the present invention, in which, before electrochemical detection, the electrolyte 9 to be measured is first dripped into the prepared sensor through a microflow control device, the Ag/AgCl reference electrode 8 is fixed beside the sensor, and a two-electrode system is adopted, so that the reference electrode clamp and the counter electrode clamp are connected together on the reference electrode to form a current loop with the working electrode, thereby evaluating the pH.
FIGS. 4 (a) - (c) are single-layer MoS in the pH sensor of the present invention 2 AFM image of film, measured MoS 2 The thickness is about 0.8 nm. FIGS. 5 (a) - (c) are double-layer MoS in the pH sensor of the present invention 2 AFM image of film, measured MoS 2 The thickness is about 1.5nm.
FIG. 6 shows the gate voltage versus leakage current curves corresponding to different pH values in the sensor test according to the present invention, and it can be seen that the different pH values are well distinguished.
FIG. 7 is a graph of pH versus threshold voltage and current for a sensor of the present invention. It can be seen that the sensor of the present invention has excellent sensitivity characteristics to pH.
Claims (1)
1. A pH sensor is characterized by comprising an insulating substrate material and MoS deposited on the insulating substrate material 2 A thin film, a source electrode, a drain electrode, and a dielectric material; wherein the source electrode, the drain electrode and the dielectric material are formed on MoS 2 A closed sensor groove is formed around the film; the preparation method of the pH sensor comprises the following steps:
(1) Cleaning a substrate, and coating a layer of photoresist on the substrate;
(2) Formation of MoS by exposure to photoresist 2 A thin film deposition region;
(3) Deposition of MoS in this region using chemical vapor deposition techniques 2 Form MoS 2 A film;
(4) Removing photoresist to preserve MoS 2 Film pattern, then in MoS 2 Forming a source electrode and a drain electrode on the outer side of the film pattern; the thicknesses of the source electrode and the drain electrode are 500nm, and the interval between the two electrodes is 10 mu m;
(5) Growing HfO using photolithography and magnetron sputtering methods 2 And forming a sensor groove by using the dielectric layer with the thickness of 500nm to obtain a device unit of the pH sensor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811514391.3A CN111307911B (en) | 2018-12-11 | 2018-12-11 | PH sensor and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811514391.3A CN111307911B (en) | 2018-12-11 | 2018-12-11 | PH sensor and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
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| CN111307911A CN111307911A (en) | 2020-06-19 |
| CN111307911B true CN111307911B (en) | 2024-01-09 |
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| CN201811514391.3A Active CN111307911B (en) | 2018-12-11 | 2018-12-11 | PH sensor and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008216038A (en) * | 2007-03-05 | 2008-09-18 | Matsushita Electric Ind Co Ltd | Chemical substance detection sensor |
| JP2012047763A (en) * | 2011-12-09 | 2012-03-08 | Dainippon Printing Co Ltd | Field effect transistor type biosensor |
| WO2012064179A1 (en) * | 2010-11-12 | 2012-05-18 | Mimos Berhad | Ph sensor |
| CN104198532A (en) * | 2014-09-05 | 2014-12-10 | 中国石油大学(华东) | Molybdenum disulfide thin film device with ammonia sensitive effect as well as preparation method and application thereof |
| CN105742191A (en) * | 2014-12-10 | 2016-07-06 | 北京有色金属研究总院 | Preparation method for molybdenum disulfide nanometer film with preset patterns |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI247113B (en) * | 2002-08-21 | 2006-01-11 | Univ Chung Yuan Christian | A method and fabrication of the potentiometric chemical sensor and biosensor on an uninsulated solid material |
-
2018
- 2018-12-11 CN CN201811514391.3A patent/CN111307911B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008216038A (en) * | 2007-03-05 | 2008-09-18 | Matsushita Electric Ind Co Ltd | Chemical substance detection sensor |
| WO2012064179A1 (en) * | 2010-11-12 | 2012-05-18 | Mimos Berhad | Ph sensor |
| JP2012047763A (en) * | 2011-12-09 | 2012-03-08 | Dainippon Printing Co Ltd | Field effect transistor type biosensor |
| CN104198532A (en) * | 2014-09-05 | 2014-12-10 | 中国石油大学(华东) | Molybdenum disulfide thin film device with ammonia sensitive effect as well as preparation method and application thereof |
| CN105742191A (en) * | 2014-12-10 | 2016-07-06 | 北京有色金属研究总院 | Preparation method for molybdenum disulfide nanometer film with preset patterns |
Non-Patent Citations (3)
| Title |
|---|
| Deblina Sarkar et al..MoS2 Field-Effect Transistor for Next-Generation Label-Free Biosensors.《ACS NANO》.2014,第8卷(第4期), * |
| MoS2 Field-Effect Transistor for Next-Generation Label-Free Biosensors;Deblina Sarkar et al.;《ACS NANO》;20140303;第8卷(第4期);第3992-4002页 * |
| 新型pH-ISFET芯片***研究;汪祖民 等;《电子与信息学报》;20071031;第29卷(第10期);第2525-2528页 * |
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