CN102621210A - Field effect gas sensor taking air gap as insulation layer and preparation method thereof - Google Patents
Field effect gas sensor taking air gap as insulation layer and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a field effect transistor gas sensor taking an air gap as an insulation layer and a preparation method. The preparation method mainly comprises the following steps of: spin-coating an organic insulation layer on an electric conducting substrate to serve as a device supporting layer, and etching a part of the device supporting layer to prepare an air gap groove; placing a micro-nano crystal above the air gap; and preparing source and drain electrodes of the device by utilizing a gold plate pasting electrode method or a photoetching technology, wherein the air gap between the micro-nano crystal and a grid electrode at the bottom of the groove is taken as a grid electrode insulation layer of the device. According to the field effect transistor gas sensor taking the air gap as the insulation layer and the preparation method, disclosed by the invention, the pollution and the damage to the surface of the nano-crystal due to the contact of the insulation layer in a preparation process is avoided; the point discharge effect is avoided favorably, and the stability of the sensor is increased; the success rate for preparing the device is greatly increased, and the device performance is improved; and an electric conducting channel is directly exposed in gas to be tested, and thus the field effect transistor gas sensor has a better air-sensitive performance. The field effect transistor gas sensor disclosed by the invention has the advantages of good stability, high sensitivity, detection limit reaching ppb (parts per billion) order and high response speed and recovery speed.
Description
Technical field
The invention belongs to field of sensing technologies, being specifically related to a kind of is the field effect gas sensor and preparation method thereof of insulation course with the clearance.
Background technology
Wait (Seiyama, T. from green hill wise man youth in 1962; Kato, A.; Fujiishi, K.; Nagatani, M. Anal. Chem. 1962,34,1502 – 1503) find that airborne active gases can change the electric conductivity of ZnO film under 400 ℃ of temperature after, the gas sensor of based semiconductor material begins by broad research.Because semiconductor-type gas sensor is with its high sensitivity, low cost, long-life and characteristics such as easy to use, through the exploitation of decades, the various semiconductor transducers that can be used for detection of gas at present are innumerable.
In recent years, gas sensor requires increasingly highly aspects such as microminiaturization, selectivity, stability, sensitivity, response time and serviceable life, so the research and development of new gas sensor also more and more come into one's own.Monodimension nanometer material is because itself bigger specific surface area with better repeatability and extremely people's concern (Comini, E.; Faglia, G.; Sberveglieri, G.; Pan, Z.; Wang, Z. L.
Applied Physics Letters 2002, 81(10), 1869), simultaneously, handling micro-nano structure and constructing aspect the device with it, scientists has also obtained gratifying progress (Huang, Y.; Duan, X.; Wei, Q.; Lieber, C. M..
Science 2001, 291(5504), 630-633), this is for to provide possibility based on one-dimensional micro-nanometer material gas application of sensor.
At present, be used to prepare the gas sensor monodimension nanometer material, comprise the organic-inorganic nano band, nano wire and nanometer rods etc.Compare with the conventional films material; These one dimension micro-nano monocrystal materials; Have very bigger serface and the less breadth wise dimension suitable with Debye length, this makes material behavior receive the surface state effect to strengthen greatly, thereby also particularly responsive to the change of surrounding environment.According to the device configuration, one dimension micro-nano monocrystalline gas sensor can be divided into two terminal device and three end field effect devices.Wherein two terminal device is able to broad research because configuration simply is easy to preparation.Three end field effect one dimension micro-nano monocrystalline gas sensors are in configuration based on field effect transistor, and its characteristics are that electric current through the micro-nano monocrystalline, can also be by independently the 3rd end grid control except the source-drain electrode regulation and control.Under the effect of grid voltage; Charge carrier in the material bodies all attracted to the interface between micro-nano monocrystalline and insulation course; Form the conducting channel that several atom/molecule layer thicknesses are only arranged; Charge carrier in the device mainly is implemented in the migration between source-drain electrode through this conducting channel, thereby the surface of facing mutually with conducting channel has bigger influence with respect to other surfaces of micro-nano crystal to device performance.Secondly, utilize the regulation and control of grid voltage can confirm optimum sensitivity more easily, this heats to confirm that best operating point is simple than traditional two terminal device utilization.In addition; The field effect transistor sensing device has more characterisitic parameter than two terminal device; Like field-effect mobility, threshold voltage and sub-threshold slope etc., these parameters are that the detection of gas provides more multiparameter, and also surveying for the selectivity of gas provides certain possibility.Therefore, current employing one dimension micro-nano single-crystal field effect transistor structure gas sensor has become focus (Patolsky, the F. of international research; Lieber, C. M.,
Materials Today 2005, 8(4), 20-28.) (Ramgir, N. S.; Yang, Y.; Zacharias, M.,
Small 2010, 6(16), 1705-1722.).
Yet the one dimension micro-nano single-crystal field effect gas sensor of report all is based on solid insulating layer in the world at present, and as previously mentioned, the releasing interface between semiconductor and insulation course has fundamental influence to the performance of sensor component.Charge carrier constraint on the contact interface, charge-doping, molecule (or atom) reconstruct, the formation of dipole and the chemical interaction that some are possible can both occur on semiconductor/interfacial dielectric layer, thereby reduce the performance and the stability of sensor.Main is that solid insulating layer has covered most of conducting channel interface the most responsive to absorbing molecules, has influenced the further raising of field effect gas sensitivity.These issues limit the development of field effect one dimension micro-nano monocrystalline gas sensor, slowed down the step that device miniatureization, nanometer direction develop.
Summary of the invention
The purpose of this invention is to provide a kind of is the field effect gas sensor and preparation method thereof of insulation course with the clearance.
Clearance provided by the present invention is that the field effect one dimension micro-nano monocrystalline gas sensor preparation method of insulation course mainly comprises the steps:
1) the substrate upper strata is a conductive material, and itself conducts electricity (like heavy doping Si or Si/SiO
2) or the top layer has the dielectric substrate (such as glass with metal film or ito thin film etc.) of conductive film, at first substrate is cleaned.
2) organic insulation (photoresists such as PMMA or AZ1505, MOR3B) is dissolved in the solvent (acetone, anisole, tetrahydrofuran, dimethyl formamide etc.), requires solvent not corrode substrate and lead and get final product.Drips of solution is added on the substrate then to set carries out spin coating, the spin coating time is 10s-60s, and rotating speed is 3000-5000 r/min.Be placed on the hot plate subsequently and dry.
3) prepare groove through electron beam exposure or photoetching technique, groove width is at 2-20 μ m.
4) select wide micro-nano single crystal semiconductor at 40-2000nm, the method that adopts mechanical probes to move, with its transfer to groove directly over, micro-nano single crystal semiconductor cross channel well width direction is put.
5) in order to protect supporting layer, adopt gold plaque pad pasting electrode method or mask plate legal system to be equipped with source-drain electrode, guarantee device architecture stable with the working alone of clearance, the source-drain electrode parallel subsides in groove edge of trying one's best are put.
6) clearance between micro-nano single crystal semiconductor and channel bottom grid promptly constitutes the gate insulator of device, and the thickness of supporting layer is the height of clearance insulation course, and two distance between electrodes are groove width.The channel width of micro-nano single-crystal field effect device is the width of micro-nano single crystal semiconductor, is 40-2000nm, and channel length is 2-20 μ m.The overall configuration of this gas sensor is as depicted in figs. 1 and 2.
7) can use the single or many root timbers material fabricate devices of micro-nano single crystal semiconductor, also can use different micro-nano single crystal semiconductors to make the field effect type device of bipolarity and other structures.
The advantage that this gas sensor is specific as follows:
1) do not have contacting of rigidity between semiconductor and insulation course, avoided that the micro-nano single crystal semiconductor contacts the damage to conducting channel in the preparation process with insulation course;
The gate surface of the channel bottom that 2) obtains with electron beam lithography is very smooth, and this helps being avoided the tip to put point effect, simultaneously the stability of the also smoother assurance sensor in groove edge and repeated;
3) can guarantee that under any circumstance insulation course and micro-nano single crystal semiconductor all have the excellent contact quality, thus can greatly improve the device preparation success ratio, improve device performance.
4) compare with solid-state insulation course, conducting channel is directly exposed in the tested gas, does not have blocking of solid insulating layer.Since the interface between air insulating layer and the micro-nano single crystal semiconductor is topmost charge carrier passage; When carrying out the gas molecule detection, the gas molecule adsorption effect of this charge carrier Entry Interface will be far longer than the influence of the gas molecule absorption on other interface/surfaces of micro-nano single crystal semiconductor to device performance to the influence of device performance.
5) find to obtain the gas sensor that good stability, highly sensitive, response speed and resume speed are exceedingly fast through experiment with this structure.
Description of drawings
Fig. 1 is the schematic side view of the field effect transistor gas sensor of insulation course for the clearance;
Fig. 2 is the schematic top plan view of the field effect transistor gas sensor of insulation course for the clearance;
Fig. 3 is the optical microscope photograph of the field effect gas sensor of Ti/Au for the grid of the single nano belt preparation of CuPc;
Fig. 4 is the stereoscan photograph of the field effect gas sensor of Ti/Au for the grid of the single nano belt preparation of CuPc;
Fig. 5 is the optical microscope photograph of the field effect gas sensor of heavy doping Si for the grid of the single nano belt preparation of CuPc;
Fig. 6 is the stereoscan photograph of the field effect gas sensor of heavy doping Si for the grid of the single nano belt preparation of CuPc;
Fig. 7 is the SO of the field effect gas sensor of the single nano belt preparation of CuPc to variable concentrations
2Response;
Fig. 8 is the SO of the field effect gas sensor of the single nano belt preparation of CuPc to variable concentrations
2Sensitivity.
Wherein: 1. 2. 7. two distance between electrodes of thickness or channel length 8. nanowire width of field effect transistor or the channel width of field effect transistor of supporting layer 3. source-drain electrodes 4. micro-nano single crystal semiconductors 5. clearance insulation courses 6. clearance insulation courses of substrate (grid); 9.Ti/Au grid 10. heavy doping Si grids
Embodiment
Embodiment 1,The clearance is the preparation method 1 of the field effect transistor gas sensor of insulation course:
Device fabrication processes clearance groove adopts the PMMA that is spin-coated on substrate surface to combine the electron beam lithography preparation.The source-drain electrode preparation adopts gold plaque pad pasting electrode method or photoetching process to obtain.The micro-nano monocrystalline adopts machinery to move method and is placed on the top, clearance.
Making provided by the present invention clearance is the field effect gas sensor of insulation course, comprises the steps:
(1) with standard silicon chip cleaning glass cleaning substrate, use the method for photoetching subsequently, preparation Ti/Au (10nm/20nm) electrode is as the grid of device;
(2) being equipped with mass volume ratio in the anisole solvent is 6% PMMA; And be added in the PMMA drips of solution that has prepared on the glass sheet; With sol evenning machine spin coating once (the spin coating time is 40s, and rotating speed is 4000r/min), baking 90 seconds on 185 ℃ the hot plate subsequently; Solvent among the PMMA is volatilized rapidly, finally can obtain the PMMA supporting layer of 200nm;
(3) on grid, preparing width through electron beam lithography is the smooth grooves in 3 microns bottoms (conductive material, i.e. grid), and channel bottom is Ti/Au, i.e. grid.The groove both sides are used to support the CuPc nano belt.
(4) the mobile mode of micro-nano crystal by adopting machinery is placed on the top, clearance to single CuPc nano belt, and micro-nano monocrystalline width is 500nm.
(5) adopt gold plaque pad pasting electrode method (Tang et al. Appl. Phys. Lett. 92,083309,2008) preparation source-drain electrode.
(6) semiconductor and channel bottom promptly constitute the gate insulator of device to the clearance between grid, and the thickness of PMMA supporting layer is the height of clearance insulation course, and two distance between electrodes are groove width.The channel width of the single field effect device of finally constructing of micro-nano monocrystalline is 500nm, and channel length is 3 μ m.The grid that Fig. 3 and Fig. 4 are respectively to the single nano belt preparation of CuPc is the optical microscope and the SEM photo of the field effect gas sensor of Ti/Au.
Step is following:
(1) cleans the grid of heavy doping Si with the standard silicon chip cleaning as device;
(2) adopt the two-layer PMMA of step (2) spin coating on Si among the embodiment 1, can obtain the PMMA of 510nm.
(3) on grid, preparing width through electron beam lithography is 10 microns grooves that the bottom is smooth, and heavy doping Si is a grid.The groove both sides are used to support the CuPc nano belt.
(4) mode that moves as step (4) micro-nano crystal by adopting machinery among the embodiment 1 is placed on the top, clearance to single CuPc nano belt, and micro-nano monocrystalline width is 350nm.
(5) adopt step (5) preparation source-drain electrode among the embodiment 1.
(6) semiconductor and channel bottom promptly constitute the gate insulator of device to the clearance between grid, and the thickness of PMMA supporting layer is the height of clearance insulation course, and two distance between electrodes are groove width.The channel width of the single field effect device of finally constructing of micro-nano monocrystalline is 350nm, and channel length is 9.41 μ m.The grid that Fig. 5 and Fig. 6 are respectively the single nano belt preparation of CuPc is the microscope and the SEM photo of the field effect gas sensor of heavy doping Si.
The monocrystalline micro-nano structure of other organic or inorganic semiconducting compounds is like ten hexafluoro copper phthalocyanines, lycid alkene, ZnO, SnO
2Method Deng also adopting 2 kinds of embodiment 1 and embodiment is prepared into the field effect transistor gas sensor.
Device is to SO
2Gas-sensitive property:
Ready-made device, utilize gold wire bonder to be connected on the homemade stainless steel air-sensitive test macro.Air pressure keeps an atmospheric pressure in the test process.Gas flow rate is 500sccm.In the test we to have selected grid voltage be V
G=-10 V, source-drain electrode voltage are V
SD=-15 V.Gas concentration is controlled with mass flowmeter, and balanced gas is N
2Tested gas SO
2Concentration be 0.5-20ppm, the tested gas feeding time is 15min, high-purity N subsequently
2The feeding time set is 30min.Test component is to SO
2Gas-sensitive property and sensitivity.
Fig. 7 and Fig. 8 are respectively the SO of the field effect gas sensor of the single nano belt preparation of CuPc to variable concentrations
2Response and sensitivity.The single field effect gas sensor of CuPc is to the SO of 0.5ppm
2Sensitivity can reach 220%.
?
Claims (2)
1. be the preparation method of the field effect gas sensor of insulation course with the clearance, it is characterized in that concrete steps are following:
1) the substrate upper strata is a conductive material, itself conducts electricity to be heavy doping Si or Si/SiO
2Or its top layer has the dielectric substrate of conductive film, at first substrate is cleaned;
2) organic insulation PMMA or AZ1505, MOR3B photoresist are dissolved in solvent acetone or anisole or tetrahydrofuran or the dimethyl formamide; Solvent can not corrode substrate; Drips of solution is added to then carries out spin coating on the substrate; The spin coating time is 10s-60s, and rotating speed is 3000-5000 r/min, is placed on the hot plate then and dries;
3) prepare groove through electron beam exposure or photoetching technique, groove width is at 2-20 μ m;
4) select wide micro-nano single crystal semiconductor at 40-2000nm, the method that adopts mechanical probes to move, with its transfer to groove directly over, micro-nano single crystal semiconductor cross channel well width direction is put;
5) adopt gold plaque pad pasting electrode method or mask plate legal system to be equipped with source-drain electrode, guarantee device architecture stable with the working alone of clearance, the source-drain electrode parallel subsides in groove edge of trying one's best are put;
6) clearance between micro-nano single crystal semiconductor and channel bottom grid promptly constitutes the gate insulator of device; The thickness of supporting layer is the height of clearance insulation course; Two distance between electrodes are groove width; The channel width of micro-nano single-crystal field effect device is the width of micro-nano single crystal semiconductor, is 40-2000nm, and channel length is 2-20 μ m;
7) single or many root timbers material fabricate devices with the micro-nano single crystal semiconductor also can use different micro-nano single crystal semiconductors to make the field effect type device of bipolarity and other structures.
2. with the clearance field effect gas sensor of insulation course by the preparation of the described method of claim 1.
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| CN102928473A (en) * | 2012-11-23 | 2013-02-13 | 电子科技大学 | Low-pressure flexible OTFT ammonia sensor and manufacturing method thereof |
| CN104713930A (en) * | 2015-03-17 | 2015-06-17 | 东北师范大学 | Gas type identifying method based on field effect gas sensor |
| CN105552123A (en) * | 2016-01-25 | 2016-05-04 | 南开大学 | Silk-screen printing type self-referencing-graphene field effect transistor biochemical sensor |
| CN106324046A (en) * | 2016-11-01 | 2017-01-11 | 苏州科技大学 | Sensitive film gas sensor and preparation method thereof |
| CN107144614A (en) * | 2017-06-08 | 2017-09-08 | 盐城师范学院 | A kind of preparation method of air nano-gap electrode |
| CN107340315A (en) * | 2017-05-18 | 2017-11-10 | 新疆工程学院 | A kind of FET formula gas sensors with composite insulation structure and preparation method thereof |
| CN107966165A (en) * | 2016-10-19 | 2018-04-27 | 华邦电子股份有限公司 | Resistance-type environmental sensor and resistance-type environmental sensor array |
| CN109580725A (en) * | 2018-12-10 | 2019-04-05 | 华中科技大学 | Two-dimentional transient metal sulfide gas sensor and preparation based on antenna structure |
| CN112505108A (en) * | 2020-12-18 | 2021-03-16 | 联合微电子中心有限责任公司 | Gas detection system and method |
| CN114646419A (en) * | 2022-03-23 | 2022-06-21 | 中山大学 | Gas pressure sensor, preparation method thereof and gas pressure detection method |
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| CN102928473A (en) * | 2012-11-23 | 2013-02-13 | 电子科技大学 | Low-pressure flexible OTFT ammonia sensor and manufacturing method thereof |
| CN104713930B (en) * | 2015-03-17 | 2017-07-21 | 东北师范大学 | A kind of method of the identification gaseous species based on field-effect gas sensor |
| CN104713930A (en) * | 2015-03-17 | 2015-06-17 | 东北师范大学 | Gas type identifying method based on field effect gas sensor |
| CN105552123B (en) * | 2016-01-25 | 2018-12-11 | 南开大学 | Screen printing type is from reference-graphene field effect transistor biochemical sensor |
| CN105552123A (en) * | 2016-01-25 | 2016-05-04 | 南开大学 | Silk-screen printing type self-referencing-graphene field effect transistor biochemical sensor |
| CN107966165A (en) * | 2016-10-19 | 2018-04-27 | 华邦电子股份有限公司 | Resistance-type environmental sensor and resistance-type environmental sensor array |
| CN106324046A (en) * | 2016-11-01 | 2017-01-11 | 苏州科技大学 | Sensitive film gas sensor and preparation method thereof |
| CN106324046B (en) * | 2016-11-01 | 2019-03-15 | 苏州科技大学 | A kind of sensitivity film gas transducer and preparation method thereof |
| CN107340315A (en) * | 2017-05-18 | 2017-11-10 | 新疆工程学院 | A kind of FET formula gas sensors with composite insulation structure and preparation method thereof |
| CN107144614A (en) * | 2017-06-08 | 2017-09-08 | 盐城师范学院 | A kind of preparation method of air nano-gap electrode |
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| CN114646419A (en) * | 2022-03-23 | 2022-06-21 | 中山大学 | Gas pressure sensor, preparation method thereof and gas pressure detection method |
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Application publication date: 20120801 |