CN116754617A - GaN-Metal/PANI ammonia sensor and preparation method and application thereof - Google Patents
GaN-Metal/PANI ammonia sensor and preparation method and application thereof Download PDFInfo
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 112
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 80
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 34
- 239000002184 metal Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910021529 ammonia Inorganic materials 0.000 title claims description 52
- 238000000034 method Methods 0.000 claims abstract description 26
- 238000001514 detection method Methods 0.000 claims abstract description 16
- 238000000151 deposition Methods 0.000 claims abstract description 14
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 14
- 238000005530 etching Methods 0.000 claims abstract description 12
- 239000002082 metal nanoparticle Substances 0.000 claims abstract description 11
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 10
- 238000011065 in-situ storage Methods 0.000 claims abstract description 7
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 7
- 230000008569 process Effects 0.000 claims abstract description 7
- 238000001039 wet etching Methods 0.000 claims abstract description 7
- 230000003647 oxidation Effects 0.000 claims abstract description 4
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 42
- 239000000463 material Substances 0.000 claims description 27
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 21
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 18
- 239000002131 composite material Substances 0.000 claims description 16
- 238000002844 melting Methods 0.000 claims description 14
- 230000008018 melting Effects 0.000 claims description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 12
- 229910052710 silicon Inorganic materials 0.000 claims description 12
- 239000010703 silicon Substances 0.000 claims description 12
- 238000005229 chemical vapour deposition Methods 0.000 claims description 10
- 238000005516 engineering process Methods 0.000 claims description 9
- 230000008020 evaporation Effects 0.000 claims description 9
- 238000001704 evaporation Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 7
- 229910052749 magnesium Inorganic materials 0.000 claims description 7
- 239000011777 magnesium Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052738 indium Inorganic materials 0.000 claims description 6
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000013329 compounding Methods 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 229910052594 sapphire Inorganic materials 0.000 claims description 2
- 239000010980 sapphire Substances 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 abstract description 9
- 230000007774 longterm Effects 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 230000004888 barrier function Effects 0.000 abstract description 2
- 230000008021 deposition Effects 0.000 abstract 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 62
- 229910002601 GaN Inorganic materials 0.000 description 61
- 239000000243 solution Substances 0.000 description 47
- 239000007789 gas Substances 0.000 description 43
- 230000004044 response Effects 0.000 description 27
- 238000011084 recovery Methods 0.000 description 18
- 239000008367 deionised water Substances 0.000 description 16
- 229910021641 deionized water Inorganic materials 0.000 description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 7
- 241000282414 Homo sapiens Species 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 230000036541 health Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000012544 monitoring process Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 241001465754 Metazoa Species 0.000 description 2
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 210000004185 liver Anatomy 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 208000020832 chronic kidney disease Diseases 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001010 compromised effect Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000013399 early diagnosis Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 201000000523 end stage renal failure Diseases 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 208000017169 kidney disease Diseases 0.000 description 1
- 208000019423 liver disease Diseases 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 230000002503 metabolic effect Effects 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000618 nitrogen fertilizer Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 210000001533 respiratory mucosa Anatomy 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 238000001291 vacuum drying 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
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention belongs to the technical field of gas sensors, and relates to a GaN-Metal/PANI ammonia gas sensor, a preparation method and application thereof, wherein the GaN-Metal/PANI ammonia gas sensor is prepared by a wet etching process, magnetron sputtering deposition of noble Metal nano particles and an in-situ oxidation polymerization method. The ammonia gas sensor etches hexagonal pits on the GaN surface based on the etching process, thereby improving the specific surface of the materialThe area is increased, and gas adsorption sites are increased; heterojunction structure is built based on GaN and PANI surfaces, schottky barrier is generated between GaN and noble metal, electron mobility is promoted, and NH of a sensor is greatly improved 3 Can realize the sensitivity to NH at room temperature 3 Has good long-term stability in the lower limit detection of ppb level.
Description
Technical Field
The invention belongs to the technical field of gas sensors, and particularly relates to a GaN-Metal/PANI ammonia gas sensor, and a preparation method and application thereof.
Background
Ammonia (NH) 3 ) Is a colorless and toxic gas with strong pungent smell, mainly derived from the discharge of industrial waste gas, the use of nitrogenous fertilizer in agriculture and the metabolic products of animals in animal husbandry, and is widely applied to the fields of fertilizer, industrial refrigerant and the like. When NH 3 When the concentration is too high, the skin, eyes and respiratory systems (such as lung and respiratory mucosa) of a person can be stimulated, and injuries with different degrees are brought. The U.S. occupational safety and health administration prescribes that human body is 25ppm NH 3 The exposure time at the concentration is not more than 8 hours, at 35ppm NH 3 The longest exposure time at concentration is 15 minutes, otherwise health is compromised.
In addition, NH 3 Is also one of natural metabolites of human body, and has important significance for early diagnosis of diseases by detecting the ammonia content in human expiration. Excess NH in expiration 3 Possibly due to liver and kidney related diseases, average NH in expiration of patients with end-stage renal disease (ESRD) 3 The content may generally exceed 4.88ppm.
The gas sensor is a device for detecting the concentration of gas in the environment and converting the concentration of the gas into corresponding electric signals to be output, and has great significance in developing a high-performance ammonia gas sensor for the health and safety of human beings.
Conventional ammonia gas sensors are of a wide variety. The semiconductor metal oxide based gas sensor is widely studied due to the characteristics of high sensitivity, small equipment volume, low manufacturing cost and low cost, but the practical feasibility is limited due to the defects of high working temperature, high energy consumption, poor selectivity and the like.
Gallium nitride (GaN) semiconductor material is a third generation strategic advanced electronic material, has excellent characteristics of high electron mobility, carrier concentration, thermal stability, chemical stability and the like, and can detect gas transmission of various gases in trace quantityThe sensor field has great application prospect. In recent years, a plurality of researchers aim to develop a GaN gas sensor with a novel structure based on the advantages of good stability and high process compatibility of GaN materials for NO 2 、H 2 And detecting the gas. However, gaN exists for NH 3 The sensitivity is low.
In contrast, a semiconducting organic polymer ammonia sensor pair NH 3 Has better selectivity and can realize detection at low temperature and room temperature. The semiconductor organic polymer material Polyaniline (PANI) has the characteristics of good chemical and environmental stability, low raw material price, simple and convenient synthesis and doping process, controllable conductivity, unique doping mode and the like, and becomes NH with great market potential 3 Sensitive materials, widely used in NH 3 Is detected. However, the use of a single PANI material as a gas sensitive material has the problems of poor long-term stability, poor recovery performance, low sensitivity, and the like, and limits the further application thereof.
In summary, aiming at the current ammonia sensor field, a room temperature ammonia sensor with high stability, high sensitivity and low cost needs to be prepared so as to ensure the safety of industrial and agricultural production and the human health monitoring.
Disclosure of Invention
The invention aims to purposefully design a GaN-Metal/PANI ammonia sensor, and the GaN material is etched and is compounded with PANI and noble Metal nano particles, so that the synergistic effect among different materials is fully utilized to improve NH pair 3 For achieving a ppb level NH at room temperature 3 Is provided.
In order to achieve the above purpose, the invention firstly provides a GaN-Metal/PANI ammonia sensor, which is based on a GaN epitaxial wafer prepared by a chemical vapor deposition method, the etched GaN epitaxial wafer is obtained by wet etching in an alkali etchant environment with high temperature melting, ti/Au electrodes are deposited on two sides of the surface of the etched GaN epitaxial wafer by using a magnetron sputtering or evaporation technology, noble Metal nano particles with the thickness of 1-3 nm are deposited on the middle part, then the GaN epitaxial wafer with the noble Metal nano particles deposited on the surface is subjected to in-situ oxidative polymerization with ammonium persulfate solution in dilute HCl solution of aniline, and the PANI film is compounded on the surface of the epitaxial wafer, thus obtaining the GaN-Metal/PANI ammonia sensor.
In the GaN-Metal/PANI ammonia sensor of the present invention, the noble Metal deposited on the surface of the etched GaN epitaxial wafer may include, but is not limited to, any one of Au, pt, pd, rh, ru and the like.
The GaN epitaxial wafer used in the invention is obtained by adopting a conventional chemical vapor deposition (MOCVD) method and taking any one of sapphire, silicon or silicon carbide as a substrate to epitaxially grow a GaN layer.
More preferably, during the growth of the GaN epitaxial wafer according to the present invention, any one of elemental silicon, magnesium, aluminum or indium may be doped in the GaN layer thereof.
Specifically, the concentration of silicon element doped in the GaN layer in the GaN epitaxial wafer is (1-10). Times.10 18 cm -3 The concentration of the doped magnesium element is (1-5) multiplied by 10 18 cm -3 The doped aluminum or indium accounts for 1 to 30 weight percent of the mass of Ga element.
Secondly, the invention also provides a preparation method of the GaN-Metal/PANI ammonia sensor, which comprises the following steps:
1) Preparing a GaN epitaxial wafer doped with any one of elemental silicon, magnesium, aluminum or indium on a substrate by adopting a chemical vapor deposition method;
2) Cutting the GaN epitaxial wafer into a certain size, placing the GaN epitaxial wafer in an alkali etching agent environment with high-temperature melting, and etching by adopting a wet etching process to obtain an etched GaN epitaxial wafer;
3) Depositing Ti/Au electrodes at two ends of the etched GaN epitaxial wafer by using a magnetron sputtering or evaporation technology, and depositing noble metal nano particles with the thickness of 1-3 nm in the middle part;
4) Immersing a GaN epitaxial wafer deposited with noble Metal nano particles into dilute HCl solution of aniline, dropwise adding ammonium persulfate solution, and compounding a PANI film on the surface of the epitaxial wafer by adopting an in-situ oxidation polymerization method to prepare a GaN-Metal/PANI composite gas-sensitive material;
5) And washing and drying the GaN-Metal/PANI composite gas-sensitive material to obtain the GaN-Metal/PANI ammonia sensor.
In the preparation method, the wet etching is carried out by placing GaN epitaxial wafer into 240-330 deg. C melted alkali etchant environment, and continuously etching for 10-60 min.
Preferably, the alkali etchant is any one of KOH, naOH, liOH and the like.
More preferably, the thickness of Ti/Au electrode deposited at two ends of the etched GaN epitaxial wafer is 50-100 nm.
In the preparation method, the concentration of the ammonium persulfate solution for in-situ oxidative polymerization to form the PANI film is preferably 0.01-0.05 mol/L.
More specifically, after the ammonium persulfate solution is added dropwise, the reaction solution is preferably allowed to stand for 20-40 min to compound the PANI film on the surface of the GaN epitaxial wafer.
The GaN-Metal/PANI ammonia sensor is preferably obtained by cleaning the prepared GaN-Metal/PANI composite gas-sensitive material with 1-4 mol/L dilute HCl solution and drying at 60 ℃.
The GaN-Metal/PANI ammonia sensor prepared by the invention can be used as NH 3 Gas concentration detection sensor applied to NH in various occasions 3 In concentration detection.
And then detecting the gas-sensitive characteristic of the GaN-Metal/PANI sensor prepared by the invention by adopting a CGS-MT intelligent gas-sensitive analysis system.
Compared with the traditional NH, the GaN-Metal/PANI ammonia sensor prepared by the invention 3 The detection mode has the advantages of high detection sensitivity, high response and recovery speed, capability of realizing room temperature detection and the like, and the sensor is simple to prepare and low in cost.
According to the invention, the GaN-Metal/PANI ammonia sensor is prepared by depositing noble Metal nano particles with rich active sites and good catalytic effect on an etched GaN epitaxial wafer and polymerizing a PANI sensitive film by an in-situ oxidation polymerization method, the etched GaN and PANI form a surface n-p heterostructure, and a Schottky barrier is generated between GaN and noble MetalPromoting electron mobility and greatly improving NH pair 3 Has rapid response and recovery speed, and can realize NH detection 3 Has good long-term stability in the lower limit detection of ppb level.
The GaN-Metal/PANI ammonia sensor of the invention not only can realize NH in a plurality of chemical sites 3 The method has the advantages of rapid and stable monitoring, and has important significance for monitoring and preventing early liver and kidney diseases of human bodies.
Drawings
FIG. 1 is an SEM image of a GaN-Au/PANI composite gas sensitive material prepared in example 1.
FIG. 2 is a graph of the preparation of a GaN-Au/PANI ammonia sensor vs. NH from example 1 3 Is a response recovery graph of (2).
FIG. 3 is a graph of the preparation of a GaN-Au/PANI-2 ammonia sensor vs. NH in example 2 3 Is a response recovery graph of (2).
FIG. 4 is a graph of NH based on GaN-Pt/PANI ammonia sensor pair prepared in example 3 3 Is a response recovery graph of (2).
FIG. 5 is a graph of the preparation of GaN ammonia gas sensor vs NH for comparative example 1 3 Is a response recovery graph of (2).
FIG. 6 is a graph of NH versus pure PANI ammonia sensor prepared in comparative example 2 3 Is a response recovery graph of (2).
FIG. 7 is a graph of a GaN/PANI ammonia sensor vs. NH for comparative example 3 3 Is a response recovery graph of (2).
Detailed Description
The following describes in further detail the embodiments of the present invention with reference to the drawings and examples. The following examples are presented only to more clearly illustrate the technical aspects of the present invention so that those skilled in the art can better understand and utilize the present invention without limiting the scope of the present invention.
The production process, the experimental method or the detection method related to the embodiment of the invention are all conventional methods in the prior art unless otherwise specified, and the names and/or the abbreviations thereof are all conventional names in the field, so that the related application fields are very clear and definite, and a person skilled in the art can understand the conventional process steps according to the names and apply corresponding equipment to implement according to conventional conditions or conditions suggested by manufacturers.
The various instruments, equipment, materials or reagents used in the examples of the present invention are not particularly limited in source, and may be conventional products commercially available through regular commercial routes or may be prepared according to conventional methods well known to those skilled in the art.
Example 1
S1: the concentration of doped silicon element prepared by adopting a chemical vapor deposition (MOCVD) method is 5 multiplied by 10 18 cm -3 Is cut into 3 x 5mm size.
S2: and (3) placing a certain amount of KOH in a quartz boat, melting at the temperature of 330 ℃, placing a GaN epitaxial wafer, and performing KOH melting etching on the GaN epitaxial wafer for 50 minutes.
S3: and (3) using a magnetron sputtering or evaporation technology, depositing Ti/Au electrodes with the thickness of 100nm on the two ends of the etched GaN epitaxial wafer through a mask plate to prepare a sensor film, and then depositing Au nano particles with the thickness of 2nm on the middle part of the etched GaN epitaxial wafer.
S4: 0.1141g of ammonium persulfate powder is added into 50mL of deionized water, and stirred to obtain ammonium persulfate solution with the concentration of 0.01 mol/L; 8.3mL of concentrated HCl is taken, and diluted to 50mL by deionized water to obtain a dilute HCl solution with the concentration of 2 mol/L; 15mL of the solution is taken and added dropwise to 15mL of deionized water, and diluted to obtain a dilute HCl solution with the concentration of 1 mol/L.
S5: and (3) placing the GaN epitaxial wafer deposited with the Au nano particles into a centrifuge tube added with 0.05mL of aniline solution, dripping 10mL of dilute HCl solution with the concentration of 2mol/L to form a protonic acid environment, rapidly dripping 5mL of ammonium persulfate solution with the concentration of 0.01mol/L, and standing for 30min to prepare the GaN-Au/PANI composite gas-sensitive material.
FIG. 1 is an SEM image of the above GaN-Au/PANI composite gas-sensitive material, and it can be seen from the image that GaN etched with hexagonal pits has a larger specific surface area than original planar GaN, and the surface defects are more conducive to the recombination of PANI films, and the GaN-Au/PANI composite gas-sensitive material has a large number of gas adsorption sites, which is advantageousIn NH 3 Rapid adsorption and desorption of molecules.
S6: taking out the GaN-Au/PANI composite gas-sensitive material, washing with 1mol/L dilute HCl solution, and drying at 60 ℃ on a heating table to obtain the GaN-Au/PANI ammonia sensor.
The CGS-MT intelligent gas-sensitive analysis system is adopted, and under the conditions of (27+/-2) DEG C and relative humidity RH of 30 percent, the GaN-Au/PANI ammonia sensor pair prepared by the embodiment is tested 3 Is a gas-sensitive property of (2).
Representing its NH pair in terms of sensor Response (Response) size 3 The detection capability is strong or weak.
The response formula: response (%) = (Rg-Ra)/ra×100%. Wherein Ra represents NH injection 3 Baseline resistance of the front sensor in air, rg represents NH injection 3 Real-time resistance of the rear sensor.
GaN-Au/PANI ammonia sensor for NH with different concentrations 3 The change in responsiveness of (2) is shown in FIG. 2, and it can be seen that the sensor pairs NH 3 Has rapid response recovery speed, response time range of 20-80 s and recovery time of about 100s, and can reach NH 3 The lowest detection limit is 10ppb for ppb level detection. Wherein the illustration is a GaN-Au/PANI ammonia sensor pair NH 3 Responses at concentrations of 50ppb, 20ppb and 10ppb.
Example 2
S1: the concentration of doped silicon element prepared by adopting a chemical vapor deposition (MOCVD) method is 5 multiplied by 10 18 cm -3 Is cut into 3 x 5mm size.
S2: and (3) placing a certain amount of KOH in a quartz boat, melting at the temperature of 330 ℃, placing a GaN epitaxial wafer, and performing KOH melting etching on the GaN epitaxial wafer for 50 minutes.
S3: and (3) using a magnetron sputtering or evaporation technology, depositing Ti/Au electrodes with the thickness of 100nm on the two ends of the etched GaN epitaxial wafer through a mask plate to prepare a sensor film, and then depositing Au nano particles with the thickness of 3nm on the middle part of the etched GaN epitaxial wafer.
S4: 0.1141g of ammonium persulfate powder is added into 50mL of deionized water, and stirred to obtain ammonium persulfate solution with the concentration of 0.01 mol/L; 8.3mL of concentrated HCl is taken, and diluted to 50mL by deionized water to obtain a dilute HCl solution with the concentration of 2 mol/L; 15mL of the solution is taken and added dropwise to 15mL of deionized water, and diluted to obtain a dilute HCl solution with the concentration of 1 mol/L.
S5: and (3) placing the GaN epitaxial wafer deposited with the Au nano particles into a centrifuge tube added with 0.05mL of aniline solution, dripping 10mL of dilute HCl solution with the concentration of 2mol/L to form a protonic acid environment, rapidly dripping 5mL of ammonium persulfate solution with the concentration of 0.01mol/L, and standing for 30min to prepare the GaN-Au/PANI-2 composite gas-sensitive material.
S6: taking out the GaN-Au/PANI-2 composite gas-sensitive material, washing with 1mol/L dilute HCl solution, and drying at 60 ℃ on a heating table to obtain the GaN-Au/PANI-2 ammonia sensor.
The preparation of GaN-Au/PANI-2 ammonia sensor pair NH by the embodiment is tested by adopting a CGS-MT intelligent gas-sensitive analysis system under the conditions of (27+/-2) DEG C and relative humidity RH of 30 percent 3 Is a gas-sensitive property of (2).
GaN-Au/PANI-2 ammonia sensor pair NH 3 The results of the performance test of (2) are shown in FIG. 3, with a sensor pair of 200ppm NH 3 The response of the catalyst can reach 203 percent, the response/recovery time is 87s/56s, and NH can be realized 3 The detection of ppb level of (3) is 50ppb, wherein the illustration is GaN-Au/PANI-2 ammonia sensor vs. NH 3 Response at a concentration of 200ppb, 50 ppb.
Example 3
S1: the concentration of doped magnesium element prepared by adopting a chemical vapor deposition (MOCVD) method is 3 multiplied by 10 18 cm -3 Is cut into 3 x 5mm size.
S2: and (3) placing a certain amount of KOH in a quartz boat, melting at the temperature of 330 ℃, placing a GaN epitaxial wafer, and performing KOH melting etching on the GaN epitaxial wafer for 50 minutes.
S3: and (3) using a magnetron sputtering or evaporation technology, depositing Ti/Au electrodes with the thickness of 100nm on the two ends of the etched GaN epitaxial wafer through a mask plate to prepare a sensor film, and then depositing Pt nano particles with the thickness of 2nm on the middle part of the etched GaN epitaxial wafer.
S4: 0.1141g of ammonium persulfate powder is added into 50mL of deionized water, and stirred to obtain ammonium persulfate solution with the concentration of 0.01 mol/L; 8.3mL of concentrated HCl is taken, and diluted to 50mL by deionized water to obtain a dilute HCl solution with the concentration of 2 mol/L; 15mL of the solution is taken and added dropwise to 15mL of deionized water, and diluted to obtain a dilute HCl solution with the concentration of 1 mol/L.
S5: and (3) placing the GaN epitaxial wafer deposited with the Pt nano particles into a centrifuge tube added with 0.05mL of aniline solution, dripping 10mL of dilute HCl solution with the concentration of 2mol/L to form a protonic acid environment, rapidly dripping 5mL of ammonium persulfate solution with the concentration of 0.01mol/L, and standing for 30min to prepare the GaN-Pt/PANI composite gas-sensitive material.
S6: taking out the GaN-Pt/PANI composite gas-sensitive material, washing with 1mol/L dilute HCl solution, and drying at 60 ℃ on a heating table to obtain the GaN-Pt/PANI ammonia sensor.
The CGS-MT intelligent gas-sensitive analysis system is adopted, and under the conditions of (27+/-2) DEG C and relative humidity RH of 30 percent, the preparation of the GaN-Pt/PANI ammonia sensor pair NH by the embodiment is tested 3 Is a gas-sensitive property of (2).
GaN-Pt/PANI ammonia sensor pair NH 3 As shown in FIG. 4, it can be seen that the sensor of the present embodiment has a conductivity less than that of Au, for 200ppm NH 3 The response of (c) was 116.3% and the response/recovery time was 104s/298s, which was a decrease in performance compared to example 1.
Comparative example 1
S1: the concentration of doped silicon element prepared by adopting a chemical vapor deposition (MOCVD) method is 5 multiplied by 10 18 cm -3 Is cut into 3 x 5mm size.
S2: and (3) placing a certain amount of KOH in a quartz boat, melting at the temperature of 330 ℃, placing a GaN epitaxial wafer, and performing KOH melting etching on the GaN epitaxial wafer for 50 minutes.
S3: and depositing Ti/Au electrodes with the thickness of 100nm on the two ends of the etched GaN epitaxial wafer through a mask plate by using a magnetron sputtering or evaporation technology to prepare the GaN gas sensor.
The sample is tested by adopting a CGS-MT intelligent gas-sensitive analysis system under the conditions of (27+/-2) DEG C and 30% relative humidity RHComparative example preparation of GaN gas sensor vs NH 3 Is a gas-sensitive property of (2).
FIG. 5 shows the concentration of NH of GaN gas sensor 3 As can be seen from the response graph of (2) for GaN gas sensor to NH 3 Almost no response.
Comparative example 2
S1: 0.1141g of ammonium persulfate powder is added into 50mL of deionized water, and stirred to obtain ammonium persulfate solution with the concentration of 0.01 mol/L; 8.3mL of concentrated HCl was diluted to 50mL with deionized water to give a dilute HCl solution at a concentration of 2 mol/L.
S2: adding 0.05mL of aniline solution into a centrifuge tube, dropwise adding 10mL of dilute HCl solution with the concentration of 2mol/L to form a protonic acid environment, quickly dropwise adding 5mL of ammonium persulfate solution with the concentration of 0.01mol/L, and standing for 30min to prepare the PANI sensitive material.
S3: and (3) repeatedly washing and centrifuging the PANI sensitive material solution with absolute ethyl alcohol and deionized water respectively for 3 times, and drying the PANI sensitive material solution in a vacuum drying oven at 60 ℃ for 12 hours to prepare PANI powder.
S4: dispersing PANI powder in deionized water at a concentration of 5mg/mL, grinding and coating the powder on the Ag mutual-pointing electrode slice to prepare the pure PANI ammonia sensor.
The comparative example was tested to prepare pure PANI ammonia sensor pair NH by using CGS-MT intelligent gas-sensitive analysis system under the conditions of (27+ -2) deg.C and relative humidity RH of 30% 3 Is a gas-sensitive property of (2).
Pure PANI ammonia gas sensor according to fig. 6 for NH at different concentrations 3 It can be seen that the sensor is responsive to 600ppm NH 3 The response of (C) is only 112%, the response/recovery time is 400s/1000s, and the response/recovery time is visible to NH 3 Has low sensitivity and poor recovery performance, and can only realize NH 3 Ppm level of (a) in the above-mentioned test.
Comparative example 3
S1: the concentration of doped silicon element prepared by adopting a chemical vapor deposition (MOCVD) method is 5 multiplied by 10 18 cm -3 Is cut into 3 x 5mm size.
S2: and (3) placing a certain amount of KOH in a quartz boat, melting at the temperature of 330 ℃, placing a GaN epitaxial wafer, and performing KOH melting etching on the GaN epitaxial wafer for 50 minutes.
S3: and (3) using a magnetron sputtering or evaporation technology, and depositing Ti/Au electrodes with the thickness of 100nm on the two ends of the etched GaN epitaxial wafer through a mask plate to prepare the sensor film.
S4: 0.1141g of ammonium persulfate powder is added into 50mL of deionized water, and stirred to obtain ammonium persulfate solution with the concentration of 0.01 mol/L; 8.3mL of concentrated HCl is taken, and diluted to 50mL by deionized water to obtain a dilute HCl solution with the concentration of 2 mol/L; 15mL of the solution is taken and added dropwise to 15mL of deionized water, and diluted to obtain a dilute HCl solution with the concentration of 1 mol/L.
S5: putting the GaN epitaxial wafer into a centrifuge tube added with 0.05mL of aniline solution, dripping 10mL of dilute HCl solution with the concentration of 2mol/L to form a protonic acid environment, rapidly dripping 5mL of ammonium persulfate solution with the concentration of 0.01mol/L, and standing for 30min to prepare the GaN/PANI composite sensitive material.
S6: taking out the GaN/PANI composite sensitive material, washing with 1mol/L dilute HCl solution, and drying at 60 ℃ on a heating table to obtain the GaN/PANI ammonia sensor.
The comparative example was tested to prepare GaN/PANI ammonia sensor pair NH by using CGS-MT intelligent gas-sensitive analysis system under the conditions of (27+ -2) deg.C and relative humidity RH of 30% 3 Is a gas-sensitive property of (2).
GaN/PANI ammonia sensor pair NH 3 As shown in FIG. 7, it can be seen that the sensor pair has a NH concentration of 100ppm 3 The responsivity of the sensor is improved to 89.7%, the response/recovery time is 396s/500s, compared with a pure PANI ammonia sensor, the sensor has the advantages of high sensitivity, and the like 3 Although the sensitivity of the system is improved to a certain extent, the system still has slower response recovery speed and high detection lower limit, and can only realize NH 3 Ppm level of (a) in the above-mentioned test.
The above embodiments of the invention are not intended to be exhaustive or to limit the invention to the precise forms disclosed. Various changes, modifications, substitutions and alterations may be made by those skilled in the art without departing from the principles and spirit of the invention, and it is intended that the invention encompass all such changes, modifications and alterations as fall within the scope of the invention.
Claims (10)
1. A GaN-Metal/PANI ammonia sensor is characterized in that an etched GaN epitaxial wafer is obtained by wet etching in an alkali etching agent environment with high temperature melting based on a GaN epitaxial wafer prepared by a chemical vapor deposition method, ti/Au electrodes are deposited on two sides of the surface of the etched GaN epitaxial wafer by using a magnetron sputtering or evaporation technology, noble Metal nano particles with the thickness of 1-3 nm are deposited on the middle part, and then the GaN epitaxial wafer with the noble Metal nano particles deposited on the surface is subjected to in-situ oxidative polymerization with ammonium persulfate solution in dilute HCl solution of aniline, so that the GaN-Metal/PANI ammonia sensor is obtained by compounding PANI films on the surface of the epitaxial wafer.
2. The GaN-Metal/PANI ammonia sensor of claim 1, wherein the noble Metal deposited on the GaN epitaxial wafer surface is any one of Au, pt, pd, rh, ru.
3. The GaN-Metal/PANI ammonia sensor of claim 1, wherein the GaN epitaxial wafer is grown with any one of sapphire, silicon or silicon carbide as a substrate.
4. The GaN-Metal/PANI ammonia sensor of claim 1 or 3, wherein any one of elemental silicon, magnesium, aluminum or indium is doped during the growth of the GaN epitaxial wafer.
5. The GaN-Metal/PANI ammonia sensor according to claim 4, wherein the concentration of silicon doped in the GaN layer in the GaN epitaxial wafer is (1-10). Times.10 18 cm -3 The concentration of the doped magnesium element is (1-5) multiplied by 10 18 cm -3 The doped aluminum or indium accounts for 1 to 30 weight percent of the mass of Ga element.
6. The preparation method of the GaN-Metal/PANI ammonia sensor is characterized by comprising the following steps of:
1) Preparing a GaN epitaxial wafer doped with any one of elemental silicon, magnesium, aluminum or indium by growing on a substrate by adopting a chemical vapor deposition method;
2) Placing the GaN epitaxial wafer in an alkali etching agent environment melted at a high temperature, and etching by adopting a wet etching process to obtain an etched GaN epitaxial wafer;
3) Depositing Ti/Au electrodes at two ends of the etched GaN epitaxial wafer by using a magnetron sputtering or evaporation technology, and depositing noble metal nano particles with the thickness of 1-3 nm in the middle part;
4) Immersing a GaN epitaxial wafer deposited with noble Metal nano particles into dilute HCl solution of aniline, dropwise adding ammonium persulfate solution, and compounding a PANI film on the surface of the epitaxial wafer by adopting an in-situ oxidation polymerization method to prepare a GaN-Metal/PANI composite gas-sensitive material;
5) And washing and drying the GaN-Metal/PANI composite gas-sensitive material to obtain the GaN-Metal/PANI ammonia sensor.
7. The method for fabricating a GaN-Metal/PANI ammonia sensor according to claim 6, wherein the GaN epitaxial wafer is placed in an alkali etchant environment with a melting temperature of 240-330 ℃ and is continuously etched for 10-60 min by a wet etching process.
8. The method for fabricating a GaN-Metal/PANI ammonia sensor according to claim 6 or 7, wherein the alkaline etchant is one of KOH, naOH, liOH.
9. The method for fabricating a GaN-Metal/PANI ammonia sensor according to claim 6, wherein the thickness of the Ti/Au electrode is 50-100 nm.
10. GaN-Metal/PANI Ammonia sensor according to claim 1 as NH 3 Use of a gas concentration detection sensor.
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